3rd NED INTERNATIONAL

TEXTILE CONFERENCE 2018

Research, Innovation and Advancement

January 10-11, 2018

Textile Engineering Department
NED University of Engineering &
Technology, Karachi
FOREWORD

It gives me great pleasure to write this Foreword to the Proceedings of

the Third International Textile Conference held in Karachi, Pakistan,
January 10-11, 2018. The Third NED International Textile Conference
(NEDITC 2018) has been organized by Textile Engineering Department
at NED University of Engineering & Technology in collaboration with
Donghua University, Tianjin Polytecnic University, Minjiang University,
Zhejiang Sci Tech University, China. Higher Education Commission,
American Association of Textile Colorist & Chemist (AATCC) and
Society of Dyers & Colourist (SDC).

The papers presented in this conference contributed the most recent

scientific knowledge known in the field of textile product development
and their value addition technologies, nonwoven and composite
manufacturing, technical textiles, Nano technology and textile
sustainability. I believe that this conference will be an impulse to
motivate the researchers and the local textile industry to collaborate
closely for the research and developments in all those areas addressed in
the conference. I am grateful to the speakers and reviewers from
Pakistan and from different parts of the world for their contribution to
the conference. I want to pay my deepest gratitude to all the members of
the organizing committee for their untiring efforts to make this event
successful and memorable. My heartful thanks to the local textile
industry for their moral and financial support, it would be very difficult
to arrange this event without their contribution. This effort will
strengthen the bridge between academia and industry.

Dr. Sheraz Hussain Siddique

Conference Secretary
PROCEEDINGS
THIRD NED INTERNATIONALTEXTILE CONFERENCE 2018
Research, Innovation and Advancement

Published by:

NEDITC Secretariat-2018
Textile Engineering Department, NED University
Ph. No. +92 21 99261261-68, Ext : 2267-2365
Email: itc@neduet.edu.pk, siddique@neduet.edu.pk
URL: http://www.neditc.org, http://textile.neduet.edu.pk

All rights reserved. No part of this proceeding may be reproduced in any

form or by any other means, electronic, mechanical, photocopying,
microfilming, recording or otherwise without permissions in writing
from the publisher
 DISCLAIMER

The views/opinions/data expressed in the Papers are

entirely those of the authors. The editing and publishing
committee has reviewed and edited the papers but do not
assume any liability for any loss resulting from the
recommendations/ suggestions contained therein.

Dr. Sheraz Hussain Siddique

Conference Secretary
 CONTENTS

1. Synthesis and Filtration Properties of Polyimide Nanofiber Membrane/Carbon Woven

Fabric Sandwiched Hot Gas Filters for Removal of PM 2.5 Particles................................ 2
2. Preparation, In-vitro Release and Lipase Inhibitory Effects of Composite Fabric Loaded
with Microencapsulated Plant Extracts ............................................................................. 21
3. Electrospun composite nanofibers for photonic displays and environmental sensing ...... 30
4. The Pore Structure Characterization and Sound Absorption Performance of the
Intercalated Meltblowns .................................................................................................... 40
5. Preparation of Photochromic Polyester Fiber ................................................................... 52
6. Garment Production networks in South-Eastern Europe: Sociocultural Affinity and
Sustainable Practices ......................................................................................................... 58
7. Development of Textile Based Strain Sensor from Polypyrrole ....................................... 75
8. Mesoscale Finite Element Analysis Framework of 3D Woven Fabric Tensile ................. 82
9. Study on Luminance research of light-emitting fabrics made by POF ............................. 90
10. An Alternate Approach to Engineer Light Weight Composite Bullet Proof Vest .......... 101
11. A Novel Electrospun Polyacrylonitrile-Based Form-Stable Phase Change Composite
Fibrous Membranes for Storage and Retrieval of Thermal Energy ................................ 110
12. Manufacture and Thermo-regulated Performance of an Novel Composite Fabrics
Containing Phase Change Microcapsules ....................................................................... 123
13. Dyeing attributes of Dalbergia Sisso towards Cotton Fabric .......................................... 135
14. A Spinning Method of Staple Fiber/Staple Fiber Core-Spun Yarn ................................ 143
Synthesis and Filtration Properties of Polyimide Nanofiber
Membrane/Carbon Woven Fabric Sandwiched Hot Gas Filters for
Removal of PM 2.5 Particles
Qiannan Wang c, Yuying Bai c, Jianfei Xie d, Qiuran Jiang a,b,c,*, Yiping Qiu a,b,c,*
a
Key Laboratory of Textile Science &Technology, Ministry of Education, College of Textiles,
Donghua University, Shanghai, China.
b
Shanghai Key Laboratory of Advanced Micro & Nano Textile Materials, Shanghai, China.
c
Department of Textile Materials Science and Product Design, College of Textiles,
Donghua University, Shanghai 201620, China.
d
Guangzhou Fibre Product Testing and Research Institute, Guangzhou 510220, China.
* Co-Corresponding Authors:
Yiping Qiu, Email: ypqiu@dhu.edu.cn; Qiuran Jiang, Email: jj@dhu.edu.cn

ABSTRACT
In this work, hot gas filters composed of polyimide nanofiber membrane sandwiched between carbon
woven fabrics are fabricated to capture fine particles of PM 2.5 level. Polyimide (PI) nanofibers with
an average diameter of 190 nm are electrospun on supporting carbon fabrics as filtration layers. The
filtration performance tests show that the maximum filtration efficiency reaches 99.99% for PM 2.5,
while the maximum pressure drop is only 251.86 Pa after continuously testing for 25 min under a
constant flow rate of 20 L/min. As the areal density of the PI nanofiber membrane increases, the
filtration efficiency increases first and then levels off when the areal density reaches 11.64 g/m 2. In
regeneration performance test with back air flush at a pressure of 500 KPa, the composite filter
maintains a filtration efficiency of 99.99% and a pressure drop of about 410 Pa. After heat treatment
at 260 and 300ºC, the composite filter shows a relatively high filtration efficiency while the tensile
strength of the carbon fabric does not change significantly.

Key words: Hot gas filter; Polyimide nanofiber; Carbon woven fabric; Reusability; Filtration
performance

1. INTRODUCTION
Haze is defined as the phenomenon which leads to atmospheric visibility less than 10 km due
to suspended particles, smoke, and vapor in the atmosphere [1]. Due to the presence of gas
emission industries, such as electric power plants, metal refining/recycling and biomass/coal
gasification, and lack of efficient filtration for these industrial gases, atmospheric fine
particles (aerodynamic diameter less than 2.5 μm, PM 2.5) have played an important role in
occurrence of haze which could severely influence people’s health [2] as well as cause serious
economic losses [3].
Temperatures of most hot gas emissions are above 260ºC [4]. Most of the filters for hot gas
filtration are made of nonwoven fabrics of polytetrafluoroethylene (PTFE) [5], polyphenylene
sulphide (PPS) [6], glass [7], ceramic [8] and metal fibers [9]. However, nonwoven structures
composed of regular fibers with diameters around tens to hundreds of micrometers are too
loose to capture the small particles such as PM 2.5 [10, 11]. In order to overcome this problem,
electrospun nanofiber membranes of various polymers have been adopted and laminated on
the nonwoven fabrics to capture fine particles [12, 13]. These nanofiber filter media have

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large specific surface, low base weight, reasonably high permeability and small pore sizes,
enabling new levels of filtration performance [14]. Various polymers have been used to make
electrospun membranes for gas filtration such as nylon 6 [15], polyurethane (PU) [16],
polyacrylonitrile (PAN) [17], polymethylmethacrylate (PMMA) [18] and polyvinyl
chloride/polyurethane (PVC/PU) [19]. Nevertheless, those membranes may not be able to
withstand temperatures above 260ºC for a long-term service. Therefore, most of the current
gas filtration systems can only remove fine particles by condensing or quenching the raw gas,
resulting in high costs and low efficiency [3].
Polyimide is a polymer with superior heat and chemical resistance together with reasonable
mechanical properties [20, 21]. Therefore, it has been used for applications with temperatures
ranging from 200 to 400ºC [22, 23]. This makes PI an ideal candidate material for electrospun
membranes in hot gas filter media. So far little has been reported about application of PI
nanofiber membranes for hot gas filtration.
Another problem in the current nanofiber membrane based hot gas filtration media is that
base materials used in these filtration media are mostly nonwoven fabrics due to their low
cost and good processability [24, 25]. However, nonwovens have poor dimensional stability
and durability compared with woven fabrics.
In order to develop an efficient and durable hot gas filtration media, in this study, PI nanofiber
membranes were produced via electrospinning and served as filtration layers of the composite
filters, while carbon woven fabrics were selected as the supporting layers. These filtraation
and supporting layers were stitched together using PI yarns. The structural characteristics and
thermal stability of the PI nanofiber membrane and the carbon woven fabric were analyzed
using scanning electron microscopy (SEM), KES bending tester, universal tensile tester and
thermogravimetric analyzer (TGA), and the gas filtration performance of the filter media was
tested using an automated filter tester.

2. MATERIALS AND METHODS

2.1 Materials
Pyromellitic dianhydride (PMDA, CAS: 89-32-7, molecular weight: 218.12) and 4, 4’-
oxydianiline (ODA, CAS: 101-80-4, molecular weight: 200.23) were provided by the
Shanghai Synthetic Resin Institute. N, N-dimethylacetamide (DMAc, CAS: 127-19-5,
molecular weight: 87.12) was supplied by Shanghai Lingfeng Chemical Reagent Co., Ltd.
Carbon twill woven fabrics (T-300, carbon multifilament: 200 tex, fabric: 2/2, 220 g/m2) were
purchased from CHN Carbon Fiber Technology Co., Ltd. Carbon fabrics have high strength
and modulus, superior thermal stability and higher electroconductivity for fiber collection
during electrospinning. Thus, carbon fabrics were selected as the supporting layers in the
composite filters. The commercial needle punch nonwoven filters (Jiangsu FMS R&D
Materials Co., Ltd) were served as the control. The top and bottom layers of these filters were
made of PI fibers (P84) and the middle layer was glass fibers.

2.2 Electrospinning and imidization of nanofiber membranes

Polyamic acid (PAA), the precursor of PI, was produced by condensation polymerization of
PMDA and ODA at a molar ratio of 1:1 in DMAc at ‒3°C. To prepare spinning solutions,

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stock solutions of PAA were diluted from 20 to 17 wt.% with DMAc, aged with stirring for
24 h at room temperature, and sonicated for 1 h. The concentration of spinning solutions was
decided according to the results of preliminary studies. Before electrospinning, a carbon
woven fabric (26 cm × 26 cm) was mounted on the fiber collecting drum (8 cm in diameter).
Syringes filled with spinning solutions were mounted on a syringe pump (JZB-1800, Jianyuan
Medical Technology Co., Ltd, China). The needle tips of syringes were kept 21 cm away from
the drum. The electrospinning was carried out at an extrusion rate of 0.2 mL/h with an applied
voltage around 11 to 14 kV and a drum rotation rate of 5 rpm. The thickness of the PAA
nanofiber membrane was controlled by varying the spinning duration. The residual solvent
was removed by heating the membranes at 60°C overnight. During the thermal imidization
process, PAA nanofiber membranes were heated in oven at a temperature rising rate of 3
°C/min with a temperature sequence of 100, 200, 300, 350 and 370°C. Samples were kept at
each temperature for 30 min.

2.3 Chemical composition analysis

To confirm the imidization of PAA to PI, Fourier transform infrared (FTIR) spectra of
nanofibers before and after imidization were obtained by an attenuated total reflectance
spectrometer (Nicolet 6700, ATR) at a resolution of 4 cm-1 in the range of 400 - 4000 cm-1
for 10 times. The spectra were then analyzed by OMNIC 8.2 software.

2.4 Measurement of pore size and pore size distributions

Pore sizes and pore size distributions of PI nanofibers membrane and carbon fabrics were
measured using the bubble-point method on a PMI Capillary Flow Porometer (CFP-1100A,
Porous Materials Inc., USA). The specimens (9 cm2) were first wetted by a porometer wetting
fluid (PorofilTM, Quantachrome Instruments, Boynton Beach, FL, USA), and then placed and
sealed in the test cell (9 cm2). When gas pressure exceeded the capillary trapping force
between the wetting agent and the fiber surfaces, compressed air passed through samples in
the test cell gradually. Pore sizes could be calculated using the following equation:
2
r cos  (1)
P

Where r is the radius of the pore, P is the pressure difference,  is the surface tension of the
wetting agent and  is the wetting angle.

2.5 Evaluation of thermal stability

The thermal stabilities of PI nanofibers and carbon fabrics were evaluated. TGA curves of the
PI nanofibers were obtained on a thermogravimetric analyzer (TG209F1, NETZSCH,
Germany) from 30 to 900°C with a heating rate of 10°C/min in air. PI nanofibers and carbon
fabrics were heated at 260 and 300°C (set according to ISO 11057) for 24 h to mimic the
environment of hot gas filtration. The morphologies of the heated and unheated PI nanofibers
and carbon fibers were observed under a scanning electron microscope (SEM, JSM-5600LV,
JEOL, Japan) at a voltage of 15 kV and magnifications of 9000 and 3000×, respectively. The
diameters of PI fibers were then measured from SEM images using Nano Measurer 1.2 (6
images/ sample, 60 data/ image). The bending rigidities of the heated and unheated supporting

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layers were measured by a KES bending tester (KES-FB2-S, KATO TEKKO Co., Ltd., Japan).
The tenacities of the yarns in the carbon fabric samples were tested (10 specimen/ sample)
with a crosshead speed of 5 mm/min on a universal tensile tester (WDW-20, Shanghai
Hualong Test Instrument Co., Ltd., China).

2.6 Evaluation of filtration properties

Three-layer filters (Fig. 1A) were prepared with two twill carbon woven supporting layers
and one filtration layer with different amounts of PI nanofibers (6.16, 10.63, 11.64, 13.74,
15.97 g/m2). To reveal the influence of filter structure on filtration efficiency, a five-layer
filter was also prepared with three supporting layers and two filtration layers (Fig. 1B). The
supporting and filtration layers were bonded tightly by PI yarns in the thickness direction (Fig.
1C, D).
Filtration properties (penetration and pressure drop) of the samples were evaluated by an
automated filter tester (TSI 8130, TSI Inc., MN, USA) according to ISO 11057 (Air quality -
Test method for filtration characterization of cleanable filter media). According to TSI 8130
manual for the automated filter tester, polydisperse NaCl particles (mass mean diameter of
0.26 μm and count median diameter of 0.075 μm with geometric standard deviation not
exceeding 1.83) were used. This means that the particle size distribution of the generated
aerosol satisfied lognormal distribution and met the particle size distribution criteria in 42
CFR 84 Subpart K, Section 84.18118 for NIOSH certification [26]. These particles were
generated by the tester and fed into a filter holder with an effective area around 100 cm2. The
samples were tested at three flow rates of 20, 40 and 60 L/min, representing three different
face velocities of 2, 4 and 6 m/min, respectively, to reveal the performance of the filters with
increasing flow rates or face velocities. To mimic the pulse jet cleaning process, an
experimental device with air pump was built to provide back air flush (500 kPa) to filters
intended for repeated uses. To accelerate the test, instead of achieving 1000 Pa, the filters
were cleaned once the penetration was leveled off. The filtration efficiency, E, was calculated
using the following equation:
E =1−𝑃 (2)
where P is the particle penetration. Each sample was tested at least 3 times and the mean
values of the filtration efficiency were plotted.
To evaluate the effect of particle size on filtration efficiency, a Sub-Micron Aerosol
Spectrometer (Grimm 1.108, Grimm Aerosol Technik GmbH & Co., Germany) was used to
measure particle number concentrations in the diameter range of 0.3 − 2.5 μm. The ambient
air was aspirated into the experimental device via a pump at a velocity of 2 m/min. The
penetration of the particles was determined as the ratio of the number concentrations of
particles in the airflow before and after filtration. The filtration efficiency was calculated using
the following equation:
𝐶𝑑𝑜𝑤𝑛
E=1− (3)
𝐶𝑢𝑝
where Cup and Cdown are the number concentrations of particles in the airflow before and after
filtration. In order to reduce the statistical fluctuations, the counting of particles was
performed every 6 s during a 3 min measurement for both Cup and Cdown. The experiment was
repeated 3 times, i.e. the number concentrations of particles are the means of about 90

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measurement points.
To observe the distribution of particles, the supporting and filtration layers were observed
under SEM before and after filtration at a voltage of 15 kV.

2.7 Statistical analysis

Data were analyzed using one-way analysis of variance (ANOVA) with Tukey’s pairwise
multiple comparison. The confidence interval was set at 95%. Differences among data with a
p-value < 0.05 were considered to be statistically significant.

3. RESULTS AND DISCUSSION

3.1 Imidization confirmation
Imidization of PAA to PI was confirmed by FTIR scanning and TGA test. The FTIR spectrum
of the unheated nanofiber membrane displayed a typical pattern of PAA with several
absorption bands in the region around 3000 – 4000 cm-1 (Fig. 2A) [27]. These bands indicated
the stretching vibrations of O-H (in carboxyl group) and N-H (in amide group) in PAA [28]
and could hardly be identified in the spectrum of the heated nanofibers (Fig. 2B). New bands
were observed at 1776 cm-1 and 1722 cm-1 attributed to asymmetric and symmetric stretching
of C=O in imide ring, as well as 1378 cm-1 generated by stretching of C-N in imide ring [29].
This spectrum possessed a typical pattern of PI, indicating the imidization of PAA fibers to
PI fibers [30]. The TGA curve of the heated nanofibers was shown in Fig. 2C. The initial
thermal decomposition temperature T5%, at which the total mass loss of 5% occurred, was
around 544.8°C, similar to the results for pure PI nanofibers reported in literature [31, 32]. In
addition, the weight loss of the heat treated samples at 260°C was merely 0.26%, implying a
relatively high thermal stability of PI fibers required for hot gas filtration.

3.2 Observation of filters before and after filtration

In the filters, filtration layers were composed of yellow and uniform PI nanofibers around 190
±19 nm in diameter. The mean pore size was 2.01 μm (Fig. 3A), and most of the pores size
were less than 3.3 μm. There were two regions (around 0.1 − 0.5 μm and 1.7 − 2.9 μm) where
the percentage of each pore size was relatively high. While from 0.6 to 1.6 μm and 3.0 to 3.2
μm, each pore size almost occupied the same percentage. Supporting layers had a mean pore
size around 66.60 μm with two major distribution regions, below 240 μm and 460-640 μm
(Fig. 3B). Nearly 30% of pores in the carbon fabrics were below 60 μm in diameter, which
might be the sizes of intra-yarn gaps, while the large pores should be the inter-yarn gaps.
Fig. 4A shows the diagram of the particle distribution on a three-layer filter, and Fig. 4B
shows the cross-section of a layer of the PI nanofiber membrane attached on carbon woven
fabric. After filtration, agglomerated NaCl aerosols were found on the outer surfaces of the
top supporting carbon fabric. These granular aggregates were about tens of micrometers, and
thus large enough to be mostly blocked by the top supporting layer (Fig. 4C). Separated
aerosols were also seen to attach on the outer and inner surfaces of the carbon fibers in this
layer (Fig. 4C, D). A cake-layer of aerosols was formed on the top surface of PI nanofiber
membrane (Fig. 4E), rather than the carbon fabric supporting layer. In addition, aerosols were
densely entrapped in the inner section and even at the bottom of the PI nanofiber membrane
(Fig. 4F, G), revealing that the nanofiber layer played a dominant role in small particle

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filtration. This conclusion could be further confirmed by comparing the images of the top and
the bottom supporting layers (Fig. 4H) in which only a few aerosols could be seen.
In the carbon fabric supporting layer, 90.5% pores were larger than 20 μm. With these large
pores, the carbon woven fabrics could hardly be effective in small particle filtration. On the
contrary, in the PI nanofiber membrane, most of the large pores were about 2 − 3 μm. In
addition, the dense particle cake-layer formed on the top of the PI nanofiber membrane and
the large number of particles accumulated in the inner section could reduce the real pore sizes
in the membrane and thus enhance the filtration efficiency.

3.3 Effect of filter structure on filtration performance

To reveal the filtration function of the supporting layers, the filtration performance of carbon
woven fabrics was measured and the penetration was 94.80 to 95.60%. It could be deduced
that the filtration function of the filters was mainly provided by the PI nanofiber membrane,
rather than the carbon woven fabric supporting layers. Fig. 5A shows the filtration
performance of the filters in terms of the particle penetration. The commercial P84/glass fiber
nonwoven filters displayed poor filtration performance with a penetration of 71.00%. This
result indicated that ordinary hot gas filters might not be efficient in eliminating small particles
at PM 2.5 level. It is obvious that the nonwoven filter had a lower penetration than the carbon
woven fabric alone, which might be owing to the large inter-yarn pores in the woven fabric.
In contrast, the penetration of all the PI nanofiber membrane/carbon woven fabric composite
filters was lower than 26.10% or had an efficiency of 2.55 to 3.43 times as much as that of
the commercial filters.
To evaluate the effect of areal densities of the PI nanofiber membrane on filtration efficiency
of the composite filters, three-layer filters were prepared with the areal densities of the PI
nanofiber membranes varied between 6.16 and 15.97 g/m2 (Fig. 5A). It can be seen that the
nanoparticle penetration through composite filters (6.16 g/m2 to 15.97 g/m2) decreased as the
nanofiber areal densities increased. Meanwhile, it seemed that, below a critical value (about
11.64 % in this study), the nanofiber areal density of the filtration layer was of vital
importance to control the initial penetration of the filters. Once the areal density of the
filtration layer reached this value, further increase of the areal density did not substantially
affect the initial penetration of the filters [33]. Meanwhile, with prolonged operation duration,
the penetration of the filters with nanofiber densities below the critical value were decreased
first and then leveled off after around 10 min. It might be due to the fact that dust cake
formation played a crucial role in penetration of filters with a nanofiber density below the
critical value.
To assess how the number of filter layers could influence the filtration performance of the
filter, a five-layer filter was constructed with two PI nanofiber membranes sandwiched in
between three carbon fabric supporting layers. The nanofiber areal densities of the first and
the second PI nanofiber membranes were 5.46 and 3.78 g/m2, respectively. The total nanofiber
areal density was about 9.24 g/m2. The initial penetration of the five-layer sample was higher
than the penetration of all the three-layer samples. After filtration for 5 min, the penetration
of the five-layer filter became lower than that of the three-layer sample with 6.16 g/m2
nanofiber areal density while still higher than the three-layer sample with 10.63 g/m2
nanofiber areal density. Thereby, the total nanofiber density seemed to affect the final steady

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filtration performance, while the number of layers in the filter, especially the number of
supporting layers, might be a minor factor in the particle penetration performance for the filter
assembly.
As shown in Fig. 5B, the filter with a higher nanofiber areal density has a higher initial
pressure drop. While the pressure drop of the filters with nanofiber areal density below the
critical value were increased relatively quickly with filtration time. All the pressure drop
values tested within the operation duration were much lower than the required pulse-jet
cleaning pressure (1000 Pa, black line) defined in the ISO standard (ISO 11057). If the trend
of the pressure drop could be maintained over time, it could be predicted that the operation
duration would be around 5 h before the required first pulse jet cleaning. As we know, pushing
air through filters in cleaning requires significant pressure provided by powerful energy-
consuming equipment. Moreover, as the filtration media accumulates dust in its structures,
the required cleaning pressure could increase several folds. Thus, reasonably frequent
maintenance is needed to minimize the energy consumption [34, 35]. Based on the laboratory
scale experimental results shown in Fig. 5, it could be seen that the filter with nanofiber areal
density of 11.64 g/m2 showed a good filtration performance with high filtration efficiency
(99.99%) and acceptable pressure drop values. Therefore, this filter was selected for the
subsequent investigations.

3.4 Effect of flow rate on filtration performance

Fig. 6 illustrates the influence of the flow rate on penetration and pressure drop of the
composite filter with a nanofiber areal density of 11.64 g/m2. When the flow rate was set at
20 L/min (face velocity of 2 m/min) according to ISO Standard 11057, the penetration was
0.44% initially and could reduce to 0.01% after 26 min (Fig. 6A). Once the flow rate increased
to 40 and 60 L/min, meaning the face velocity increased to 4 and 6 m/min, the initial
penetration increased to 4.74% and 12.60%, respectively. As the flow rate (face velocity) was
raised, the initial pressure drop displayed a nearly linear increasing trend (181.30, 462.56 and
657.58 Pa) as shown in Fig. 6B. When the filtration duration was prolonged, all the pressure
drops tested at different flow rates rose linearly. The pressure drop at 20 L/min increased to
251.86 Pa after 26 min. Based on this trend, it might take about 5 h to reach 1000 Pa, the
required critical pressure drop for pulse jet cleaning. In the contrast, to reach the critical
pressure drop using flow rates of 40 and 60 L/min, it could need only 23 and 4 min,
respectively. Thus, according to the results of laboratory scale experiments, the flow rate of
60 L/min (face velocity of 6 m/min) was too high for efficient filtration, but 40 L/min (face
velocity of 4 m/min) could be used if a higher flow rate was preferred. The flow rate at 20
L/min provided stable and high quality filtration with a reasonable gas pressure and a cleaning
frequency allowed for a longer service life of filters.
It is widely accepted that the capture of dust particles by the fibers in a filter can be resulted
from several mechanisms, including inertial impaction, interception, diffusion (Brownian
motion) and electrostatic forces [36]. According to the single fiber collection efficiency theory
of a filter based on a fan model (Kirsh et al., 1975) [37], the Peclet number (Pe) represents
the relative strength between interception and diffusion mechanisms, and the diffusion effect
is relatively small for large Pe. Fig. 6C shows the change of penetration and pressure drop
with respect to Pe calculated as follows:

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Pe  u0 d f / D (4)
R  dp / d f (5)
kBTCc
D (6)
3 d p
2   d p 
Cc  1  1.257  0.4exp  0.55  (7)
dp    
where u0, df, dp, kB, T, μ and  are the filter face velocity (2 m/min, 4 m/min and 6 m/min),
fiber diameter (190 nm), particle diameter (0.26 μm), Boltzmann’s constant (1.38 × 10-23 J/K),
temperature (297.13 K), gas viscosity (1.8×10-5 Pa∙s) and the mean free path of carrier gas
(0.0653 μm), respectively. Interestingly, a lot of the particles had diameters larger than those
of the PI nanofibers, leading to high filtration efficiency by interception. However, the
diameters of a certain number of particles were smaller than those of the PI nanofibers. For
these smaller nanoparticles, particle collection is typically diffusion dominated [38]. As
shown in Fig. 6C, when the flow rate was raised from 20 to 40 L/min (face velocity increased
from 2 to 4 m/min), Pe doubled and the penetration increased. It could be because a higher
flow rate reduced the retention time of the particles moving through and increased the shear
force to remove deposited particles in the nanofiber membrane, and thus decreased the chance
for the particles to deposit on the fibers by diffusion. Meanwhile some particles could be
captured by impaction and interception acquired momentum and passed through the filters.
However, the filtration efficiency at 40 L/min was still maintained at a relatively high level,
about 95%. When flow rate increased to 60 L/min, Pe increased to about 120, some relatively
large particles acquired more momentum at this high flow rate and therefore could pass
through the filters more easily [39]. So the initial penetration increased again, while filtration
efficiency was able to reach 98.57% after the filtration duration prolonged to 4 min.

3.5 Effect of particle size on filtration performance

Fig. 7 shows the penetration as a function of interception parameter (R). R is the diameter
ratio of particle to fiber, or dimensionless particle radius. Particles in the size range of 0.3 −
2.5 μm were tested, so R value changed from about 1.8 – 13.2. Particle collection was typically
interception-dominated when the diameters of particles were much larger than that of the
nanofibers [36]. When the particle diameters were about twice as large as those of the
nanofibers, the penetration of the filter was about 2.0 % under a flow rate of 20 L/min. When
the R value increased to about 13, almost no particle was able to pass the filters. In addition,
it can be seen that penetration decreased with the increasing of R value. It indicated that the
most penetrating particle size (MPPS) should be less than 0.3 μm. When all the other filtration
performance in this work were tested by using the automated filter tester -TSI 8130, the
aerosol particles with a mass mean diameter of 0.26 μm was used which close to the MPPS.
This is why high efficiency particulate air (HEPA) filters testing is often recommended by
using challenge particles with a diameter of 0.3 μm [40]. Meanwhile, the generated aerosol
met the particle size distribution criteria in 42 CFR 84 Subpart K, Section 84.18118 for
NIOSH certification. The test results showed that the initial filtration efficiency of the

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composite filter with the nanofiber areal density of 11.64 g/m2 was 99.56%, which was higher
than the filter efficiency criterion (95%) of National Institute for Occupational Safety and
Health (NIOSH).

3.6 Regeneration performance of filters

In industry, the cake layer and part of the dusts in filters are removed periodically via pulse
jet cleaning to reduce the flow resistance of the filters. Therefore, the regeneration
performance of the filters is important to determine their filtration properties and service lives.
When the cake layer formed on the filter surfaces and the dusts entrapped in the filters can be
removed efficiently, it means that this filter possesses a better cleaning efficiency (or
regeneration efficiency) [41]. Fig. 8 shows the penetration and the pressure drop trends of
seven-cycle regeneration performance of the filter with nanofiber areal density of 11.64 g/m2.
For the laboratory scale cleaning experiments, in the first five cycles, the pressure drop
increased almost linearly with time in each cycle, and was reduced 55 to 62% by back air
flushes although it could not return to its original value [42]. In addition, the pressure drop
change rate was increased with number of regeneration cycles. It implied that, in each cycle,
a portion of the dust was entrapped, which could resulting in finer pore structures in the filter
to facilitate the entrapment of finer dust, leaving even smaller pores, which could increase the
pressure drop after each back air flush [43]. While after the first five cycles or the so-called
conditioning period, the pressure drop curve reached an equilibrium state, at which the amount
of dust collected was roughly the same as that was cleaned out, which could last for a long
time [36].
The influence of back air flush on filtration efficiency was much milder than that on
pressure drop. During the seven cycles, filtration efficiency was maintained above 99.50%.
The initial filtration efficiency was reduced slightly by the back air flush probably due to the
removal of dust cake layer, but could be raised and kept to above 99.99% after several minutes.

3.7 Thermal stability of filters and its effect on filtration performance

Since the composite filters were aimed to be used for hot gas filtration, high thermal stability
and stable filtration performance at elevated temperatures for the filters were required. In Fig.
9, the PI nanofibers did not show substantial morphological change after being heated at 260
and 300°C for 24 h. Before and after the heat treatments, diameters of the nanofibers were
similar and distributed mainly in two regions around 167 and 222 nm with diameter
percentiles of about 63% and 37%, respectively. Fig. 10 presents the influence of the heat
treatment on supporting layers. Comparing the SEM images of the untreated and the treated
carbon fabrics shown in Fig. 10 A-C, it could be noticed that the sizing (most likely an epoxy)
on carbon fibers were vitrificated or charred after being heated at 260°C, but the surface of
the fibers treated at 300°C was clean indicating the removal of sizing probably caused by
thermal degradation. The mean tensile strength of the carbon tows was maintained at 1.92
GPa after heat treated at 260°C, but reduced to 1.52 GPa (about 21%) as the temperature
increased to 300°C (Fig. 10D). Although carbon fibers could withstand the environment
below 400°C without oxidation, the degradation of epoxy sizing at 300°C decreased binding
among carbon filaments, leading to a loose yarn and fabric structure with certain degree of
decreased orientation of fibers. Thus, the tensile strength of the carbon tows was substantially

Page 10 of 150
reduced due to uneven loading of the filaments in tensile tests, although could still be
sufficient to support the structure of the filters. In addition, the carbon fabric supporting layer
became stiff after heat treatment (Fig. 10E). The bending rigidity (B values) of carbon woven
fabrics were elevated from 0.024 cN cm to 7.68 and 0.093 cN cm after heat treatment at 260
and 300°C, respectively. It was obvious that epoxy sizing was cured at 260°C that contributed
to the increase of rigidity of the fabrics, which could facilitate maintaining the integrity of the
filter.
In Fig. 11, it can be seen that the initial penetration of the heat treated filters were increased
from 0.44% to 5.85% at 260°C and 6.29% at 300°C, but the subsequent filtration efficiency
decreased to lower than 1% after continuously testing for 8 min at 260°C and 14 min at 300°C.
Therefore, the composite filters could possess sufficient structural integrity and filtration
performance stability as well as mechanical properties for potential hot gas filtration
applications according to the laboratory scale experiments.

4. CONCLUSION
Polyimide nanofiber membrane/carbon woven fabric sandwiched composite filters were
successfully designed and fabricated. The PI membranes played a dominant role in the
filtration process, while the carbon woven fabric with large pore size reduced the pressure
drop in favor of dust cleaning. As the areal density of the PI nanofiber membrane increased,
the initial filtration efficiency increased first and then leveled off at a critical areal density,
while the pressure drop increased steadily with the areal density. The selected filter
maintained reasonable filtration efficiencies and pressure drops during a seven-cycle filtration
test with repeated back air flush. In addition, the same filter could maintain high filtration
efficiency and good mechanical properties after thermal treatment at 260°C. This type of
composite filters exhibited excellent filtration performance and good reusability for hot gas
filtration not only because of the excellent thermal and chemical stability of the PI nanofibers
and the carbon fibers, but also owing to the unique structure of the filter.

ACKNOWLEDGMENTS
This work was supported by the State Key Program of National Natural Science of China
(Grant No. 51035003), the Natural Science Foundation for the Youth (Grant Nos. 50803010
and 60904056), the Fundamental Research Funds for the Central Universities (Grant No.
CUSF-DH-D-2013030 KLTST201404, 2232015D3-02, ERCTT project 15D10133) and the
Young Faculty initiation fund (14D210106). The authors want to thank the Shanghai
Synthetic Resin Institute for supplying some of the chemicals.

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Figures

Figure 1. The structure of the composite filter. (A) Three layer; (B) Five layer filter; (C, D) Diagram
and digital image of bound composite filters.

Page 14 of 150
Figure 2. Imidization confirmation by FTIR and TGA. (A) FTIR spectrum of unheated nanofibers
(PAA); (B) FTIR spectrum of heated nanofibers (PI); (C) TGA curve of heated nanofibers (PI).

Figure 3. Pore size distributions of (A) PI nanofiber membrane and (B) carbon woven fabrics.

Page 15 of 150
Figure 4. Particle distribution in a three-layer filter after filtration. (A) Particle distribution illustration;
(B) Cross-section of the filter; (C, D) the outer and inner surfaces of the top supporting layer; (E) the
cake layer of NaCl aerosols on the surface of PI nanofiber membrane; (F, G) the top and bottom of the
PI filtration layer; (H) the outer surface of the bottom supporting layer.

Page 16 of 150
Figure 5. Effect of filter structure on filtration performance. (A) Penetration and (B) pressure drop of
composite filters with different structures measured with continuous flow rate fixed at 20 L/min.

Figure 6. Effect of flow rate on filtration performance. (A) Penetration and (B) pressure drop of the
composite filter with nanofiber areal density of 11.64 g/m2 tested at different flow rates; (C)
Penetration and pressure drop as a function of Peclet number.

Page 17 of 150
Figure 7. Effect of particle size (dimensionless particle radius) on filtration performance.

Figure 8. Regeneration performance. Penetration and pressure drop of the composite filter with
nanofiber areal density of 11.64 g/m2 tested at 20 L/min.

Page 18 of 150
Figure 9. SEM images and fiber diameter distributions of untreated and treated PI nanofiber
membrane. (A, A-1) untreated, (B, B-1) heat-treated at 260°C and (C, C-1) heat-treated at 300°C.

Page 19 of 150
Figure 10. SEM images and mechanical properties of untreated and treated carbon woven fabrics. (A,
B and C) SEM images of carbon tows untreated and heat treated at 260 and 300°C, respectively; (D)
the tensile strength of carbon tows before and after heat treatments at different temperatures; (E) KES-
FB2S tests of carbon fabrics before and after heat treatment at different temperatures.

Figure 11. Penetration of the composite filter before and after heat treatment at different temperatures.

Page 20 of 150
Preparation, In-vitro Release and Lipase Inhibitory Effects of Composite
Fabric Loaded with Microencapsulated Plant Extracts
Rui Wang, Mengxuan Li, Xing Liu, Yanli Sun
School of Textiles, Tianjin Polytechnic University, Tianjin 300387, China.

ABSTRACT
The plant extracts (PLE), a mixture of camellia japonica extracts, clover extracts and coco extracts,
were microencapsulated into polyvinyl alcohol-glutaraldehyde hydrogel. The fabricated
microcapsules were then composited with polyester spunlace non-woven fabric by coating finishing.
The microcapsules were characterized by Fourier transform infrared spectroscopy (FTIR), scanning
electron microscope (SEM), and thermogravimetric analysis (TGA). The in-vitro release property of
the microcapsules and the composited fabric were studied by ultraviolet-visible spectroscopy (UV-
VIS). It is observed that the release processes of the microcapsule and the composite fabric, which
occur according to non-fickian diffusion mechanical, may last for over 24h in phosphate buffer
solution (PBS). And the inhibitory effects of the microcapsules and the composited fabric were
characterized by titration. The results indicate that the surface of PEL microcapsules are smooth, and
the average particle size is 14.5 μm. The microcapsules with a drug loading ratio of 38.5% show good
thermal stability. The lixivium of the microcapsules and the composite fabric have Lipases inhibitory
rates of 26.6%, 21.3%, respectively. Accordingly, the composite fabric is promise to be used as a kind
of baking fabric, which is good for improving the effect of losing weight, in shapewear and tights.

1. INTRODUCTION
With the improvement of living standard, obesity is becoming a serious problem which affect
the health of body. There is a strong scientific agreement that obesity significantly increase
the risk of hypertension, cardiovascular diseases, obstructive sleep apnea syndrome and fatty
liver.[1] The main reason causes obesity is excess food intake and low physical activity.[2] A
variety of methods are used to lose weight including diet, exercise, drugs and surgical
operation. Thinking about the surgical risk and the side effects caused by the drugs, most
people trend to achieve and maintain a healthy weight by diet and exercise. Besides, people
also use some herbals and supplements such as the plant extracts to improve weight losing
effect. Compared with other weight losing drugs, PLEs are safety and adverse effects resulting
hospitalizations have been reported.[2] In addition to some plant-derived oral supplements,
many kinds of PLE are made into cataplasm, essential oil and cream. Through this way, the
active constituents could not be prematurely metabolized by the liver which improves the
bioavailability of the active constituents.[3] Although the cataplasm, essential oil and cream
improve the bioavailability of PLE and lengthen their action time, there are still some
problems to be solved. For example, the cataplasms will make people feel uncomfortable and
they are easily fall off from skin when people sweating because they’re pasted onto the skin
by adhesives. The essential oil and cream may smear clothes when they are painted on body.
And they can’t provide the PLE a relatively long release period. As a result, it is necessary to
develop new methods to reduce the discomfort feeling of the body and lengthen the release
time of the PLE. For most of the PLEs are easily affected by the environment conditions, a
suitable carrier which can give them slow-release property and improve their chemical and
thermal stability is necessary. Microencapsulation has been investigated to be an effective

Page 21 of 150
way to give drugs with slow-release property. Using this technology, soluble or insoluble
drugs can be coated by polymer shells and protected from being affected by the environment
conditions.[4] It is very suitable for drug delivering system. Many kinds of natural and
synthetic polymers could be used to form microcapsule shells including, chitosan,[5] polyvinyl
alcohol (PVA),[4] and poly-L-lysine.[6] Depending on the physical and chemical properties of
both the encapsulated substance and the capsule materials, microcapsules could be prepared
by many methods such as internal phase separation,[7] in-suit polymerization[8] and interfacial
polymerization[9]
This study aims at the microencapsulation of the PLE through interfacial polymerization
method and composited with polyester nonwoven fabric, preparing a kind of drug release
lining fabric. The PLE used in this study is a mixture of lactococcus ferment extracts from
camellia sinensis leaf, colver flower and cocoa flower. The main active constituents are
isoflavone, theobromine, thephyline, and caffeine. Its main functions are promoting fat
decompose, inhibiting the proliferation of fat cells and inhibiting the activity of pancreatic
lipase. The microcapsules are prepared through interfacial polymerization method. The wall
materials are prepared by a condensation reaction of PVA and glutaraldehyde (GA) in acid
medium. The morphology, particle sizes, release properties and lipase inhibitory effects are
characterized by SEM, FTIR, TG, and UV-VIS spectrometer. Then the microcapsules are
composited with the polyester nonwoven fabric by calcium alginate hydrogel through coating
finishing. The addition of microcapsules, drying method and the lipase inhibitory effects are
studied.

2. MATERIALS AND METHODS

2.1 Regants
PLE was purchased from Guangzhou Eco-Nature Biotechnology Co. Ltd (China). Polyvinyl
alcohol (PVA, (Mw) = 1788±50) was obtained from Chengdu Kelong Chemical Co. Ltd
(China). Span-80 (HLB = 4.3) and OP-10 (HLB = 14.5) were purchased from Shanghai
Shenyu Pharmaceutical & Chemical Co. Ltd (China). Hydrochloric acid (36 wt% water
solution) and sodium hydroxide were supplied by Tianjin Fengchuan Chemical Reagent
Technologies Co Ltd (China). Glutaraldehyde (25 wt% water solution), n-hexane and
phosphate buffer saline (PBS, pH = 6.68) were obtained from Tianjin Damao Chemical
Reagent Factory (China). Sodium alginate (SA) and calcium chloride anhydrous was
purchased from Tianjin Yongda Chemical Regaent Co Ltd (China). Lipase (porcine pancreas)
was obtained by Nanjing Oddo Foni Biology Technology Ltd (China). Polyester nonwoven
fabrics (50 g/m2) were supplied by Jiangyin Yongxing adhesive-bonded fabric factory
(China).

2.2 Preparation of PVA/PLE microcapsules

PVA was used as the wall materials and PLE was used as the core materials. During the
preparation processes PVA (4 wt% water solution) and PLE were mixed in a weight ratio of
1:1 at the speed of 3000 rpm by a homogenizer (XHF-D, Scientz, China).Then, 6 g mixture
was added to 40 mL n-hexane containing 5% mass fraction of surfactant span-80 and heated
to 40oC in water bath and agitated using a mechanical stirrer (DW-3-50, Yuhua Instruments,
China) at 500 rpm for 20 min. After that, the cross-linking agent and catalyst, a mixture of

Page 22 of 150
2.0 mL GA and 0.1 mL hydrochloric acid was added dropwise to the system at the speed of
0.4 mL/min. Then kept on stirring for another 60 min at 500 rpm. Afterwards, the pH of the
reaction system was adjusted to 6~7 using 5 wt% sodium hydroxide solution. The
microcapsules were obtained by extraction filtration and were washed with isopropyl alcohol
and distilled water to air dry.

2.3 Preparation of PLE-loaded Fabric

The finishing solutions were prepared by dispersing varying weight ratios (2 wt%, 4 wt%, 6
wt%, and 8 wt%) of microcapsules in 2 wt% SA solution for 20 min at 40 oC. OP-10 (5 wt%)
was added as dispersing agent. Afterwards, the finishing solutions were finished on the
polyester nonwoven fabrics (30 × 30 cm) using a coating machine (KTF, Wemer Mathis,
Switzerand). The coating thickness was 0.5 mm. Then 10 mL 10 wt% calcium chloride
solution was sprayed onto each piece of the composite fabrics. After 10 minutes’ standing,
the composite fabrics were dried in the following ways：1）dried at 40 oC for 5 min and
cured at 80 oC for 3 min; 2) freeze dried at -40 oC for 6 h using a freezdryer (FD-1CL,
JIANGDONG China) and 3) natural dried at 25 oC.

2.4 Imaging and particle size analysis of the PVA/PLE microcapsules

The structure of the PVA/PLE microcapsules was observed using a scanning electronic
telescope (SEM, S4800, Hitachi, Japan). The particle size of microcapsules was measured
with NanoMeasurer® software program on the SEM photos and more than 300 microcapsules
were counted.

2.5 Fourier transform infrared spectroscopy (FTIR)

FTIR spectral data of the GWM extractive, microcapsules and the wall materials were
obtained using FTIR spectrophotometer (TENSOR37 FTIR, Bruker Corporation, German).
The samples were prepared by processing compressed KBr disks and scanned from 4000 cm-
1
to 600 cm-1 at a resolution of 4 cm-1.

2.6 Thermogravimetric analysis (TG)

The thermal stability was measured by a thermogravimetric analyzer (TG, STA 449F3,
Netzsch, German), at a scanning rate of 10 oC/min between the temperature of 40 oC and 630
o
C in a static nitrogen atmosphere.
2.3.4 Slow-release property and drug-loading ratio of the PVA/GWM microcapsules
In order to obtain the slow-release data of PLE from microcapsules, 10 mg of PVA/PLE
microcapsules were dispersed into 30ml phosphate buffer solution (PBS, pH = 6.68) and
incubated at 30oC in a water bath, stirring at 80 rpm. Aliquots (3 mL) were withdraw at
interval of 2 h and the dissolution media was replenished with fresh PBS to maintain the total
volume after each withdraw. Samples were collected by a UV-VIS spectrophotometer at 205
nm.
To determine the release profile of the PLE, a curve was elaborated to show the relationship
between the drug concentration and time. The release curve was calculated by the ratio
between the concentration of drug release at specific time and at equilibrium according to
Korsmeyer-Peppas model (showed in eq.1).

Page 23 of 150
 F=k KP t n (1)
Where F presents the release degree (%), t presents the release time (h), kKP is a kinetic
constant and n is the diffusional exponent that can be related to the drug release mechanism.
When n ≤0.45, the drug release mechanism is Fickian diffusion. When 0.45 < n ≤ 0.89, the
drug release mechanism is non-fickian diffusion. And when n ≥ 0.89, the release mechanism
is bull erosive release.[10]
In order to collect the data of drug loading effect, 5 mg of PVA/PLE microcapsules were
grinded and dispersed into 30 ml PBS and incubated at 80 oC in a water bath, stirring at 500
rpm. The drug loading ratio was calculated by eq. 2.

P= m PLE 100% (2)

m mc
Where P is the drug loading ratio (%) of the microcapsules, mPLE is the mass of PLE
encapsulated in the microcapsules, mmc is the mass of the microcapsules.

2.7 Lipase Inhibitory Effects teat

The lipase inhibitory effects test was acted according to GB/T 23535 – 2009 standard. The
lipase was diluted 500 times. The enzyme activity was calculated eq.3.
（V -V ） c  n  50 1
X= B S  (3)
0.05 t
Where X is enzyme activity (μ/g), VB represents the volume of NaOH solution used in
titrating the blank solution (ml), VS represents the volume of NaOH solution used in titrating
the sample solution (ml), c is the concentration of NaOH solution (mol/L) , n is the dilution
rate of the lipase and t is the reaction time (min).
The activity inhibition ratios of each sample solutions were calculated by eq. 4.
XB  X S
F= 100% (4)
XB
Where F is the activity inhibition ratio (%), XB is the enzyme activity of the blank solution,
XS represents the enzyme activity of the sample.

3. RESULT AND DISCUSSION

3.1 Structure and particle size distribution

(a) (b)

Page 24 of 150
 (c) (d)

Figure 1. SEM images of (a) microcapsules; (b) outer surface of a single microcapsule; (c) the core-
shell structure of the microcapsule, and (d) the graph of particle size distribution of PVA/PLE
microcapsules

Figure 1a shows the outer surfaces of the PVA/PLE microcapsules. All the microcapsules
show relatively smooth outer surfaces. Figure 1b indicates that the outer surfaces of the
microcapsules are very compact. Figure 1c shows the core-shell structures of the PVA/PLE
microcapsules. The size distribution (Figure 1 d) indicates that the particle sizes of the
PVA/PLE microcapsules are almost identical and have a mean diameter of 14.5μm.

3.2 FTIR spectra of PVA/GWM microcapsules

Figure 2. FTIR spectras of the blank microcapsules (a) and PVA/PLE microcapsules (b)

Page 25 of 150
In Figure 2 a, the peak at 2924.16 cm-1 refers to the C-H stretching vibration from alkyl
groups. The peak at 1376.02 cm-1 due to the –CH2 stretching vibration. The C-O stretching
vibration at 1128.68 cm-1 relates to the formation of C-O-C group and shows the PVA has
been crosslinked with GA. As it is showed in Figure 2 b, the peak at 3118.94 cm-1 showed in
Figure 2 b refers to N-H stretching vibration. The N-H deformation vibration and C-N bending
vibration peak at 1702.91, the C=C stretching vibration peak at 1650.84 cm-1 and the C-NH
bending vibration peak at 1559.23 cm-1 indicate the existence of caffeine. The appearance of
characteristic peaks of the shell at 2919.82 cm-1, 1373.61 cm-1 and 1133.50 cm-1 indicate that
PLE has been coated successfully.

3.3 Thermal stability of PVA/PLE microcapsules

To evaluate the thermal stability of the core materials and the PVA/PLE microcapsules, TG
was used. The results of TG experiments (Figure 3) reveal that the PLE start to lose weight at
about 59 oC, and substantial weight loss occurs when it was heated to 79 oC. The residual
mass may be attributed to impurities. The PVA/PLE microcapsules show an excellent thermal
stability when they were heated up to about 220 oC, and substantial weight loss appeared at
261 oC.

Figure 4. TG curves of Figure 5. Real and fitting

PVA/PLE microcapsules and release curves of PVA/PLE
PLE microcapsules

3.4 Release property of PVA/PLE microcapsules

The drug loading ratio calculated by eq. 2 is 38.5%. And the release curve (Figure 5) shows
that the PVA/GWM microcapsules had excellent release properties. The outcome of the
model fittings is shown in Figure 5, and the fitting equation is shown in eq. 5. The release
mechanism is associated with Fickian diffusion (n < 0.45). The results also show the
microcapsule can consist releasing for more than 24 h.
F=21.337t 0.366 (5)
When the PVA/PLE microcapsules are used in tights and shapewears, the microcapsules
would not be entirely wetted in a short time. Therefore, they would be hardly able to swell
completely and diffuse out in a short time.

3.5 Effects of microcapsules adding on composite fabric

In order to evaluate the dispersing and bonding effects of the PVA/PLE microcapsules

Page 26 of 150
different mass of microcapsules were added. As Figure 6 shows, the fabrics are coated by the
calcium alginate hydrogel，and the PVA/PLE microcapsules are adhered to the surface of
the nonwoven fabrics intensively. When a small amount of microcapsules (Figure 6 a, b) is
added into the finishing liquor and coating on the fabric, the microcapsules were relatively
adhered on the fabric uniformly. With the increasing of the microcapsule addition, the
aggregates of microcapsules increased. As it is shown in Figure 6 c, d, more aggregates could
be found on the surface of the fabrics. That may be caused by the bodiness effect of the
microcapsules during the mixing process. When a large amount of aggregates existing in the
finishing liquor, as figure 6 d shows, the bondiness fastness decreased. And the microcapsules
will drop off when the composite fabric is rubbed. Considering the microcapsule capacity and
the dondiness fastness, 4 wt% microcapsule addition is applicable.
(a (b
) )

(c) (d
)

Figure 6. Composite fabric with different microcapsule adding ratio: (a) 2 wt%, (b) 4 wt %, (c) 6 wt%,
and (d) 8 wt%

3.6 Effects of drying method on composite fabric

In order to find an appropriate drying method of the composite, three kinds of drying method
have been used including freeze drying, air drying and stoving. Figure 6 shows the surface
morphology of fabric dried by freeze drying (Figure 6 a), air drying (Figure 6 b) and stove
drying (Figure 6 c). The fabrics dried by the three ways all have relatively smooth surface and
there are no significant different among them. Considering time and cost, the stove drying is
more suitable for prepare the composite fabric.

Page 27 of 150
 (a) (b)

(c)

Figure 6. Composite fabrics dried by different methods: (a)Freeze drying, (b) air drying and (c)
stove drying

3.7 Lipase inhibitory effects of PVA/PLE microcapsules and the composite fabric

Figure 7. Enzyme activity inhibition ratio

The results of enzyme activity test are shown in Figure 7. PLE added sample has the lowest
enzyme inhibitory effect. The results show that PLE has the highest inhibitory effect ratio of
44%. The inhibitory effect ratios of microcapsule and composite fabric are 26.6% and 21.3%.
That difference may be caused by the different concertation of PLE which linked with the
inhibitory effects. The microcapsules and its composite fabric have a certain Lipase inhibitory
effects prove that microencapsulation and coating finishing will not destroy the biological
activity of PLE.

Page 28 of 150
4. CONCLUSIONS
PVA/PLE microcapsules with a 14.5 µm mean diameter were successfully prepared through
interfacial polymerization. FTIR experiments showed that PLE had been confined in the
microcapsules. TG tests indicated that the thermal stability of the PLE was significantly
improved through microencapsulation. The in-vitro release studies showed that the drug can
consist on releasing for more than 24 h. Its release mechanism can be classified as Fickian
diffusion. 4 wt% is the prefer microcapsule addition when prepare composite fabrics. And
stove drying can be used to improving the production efficiency. The enzyme activity test
results prove the availability of the microcapsule and the composite fabric. In conclusion,
these controlled-release PVA/PLE microcapsules composite fabric can be applied as lining of
some shapewear and tights and Play a subsidiary role in weight control.

REFERENCES
[1] Asl B H, Vaez H, Imankhah T, et al.. Advanced Pharmaceutical Bulletin. 2014, 4(1): 83.
[2] Xing S, Sharp L K, Touchette D R.. Patient Education and Counseling. 2017, 100(3): 592-
597.
[3] Zorec B, Préat V, Miklavčič D, et al. Zdravniški Vestnik. 2013, 82(5): 339-356.
[4] Li M, Wang R, Liu X. Polymer Korea. 2017, 41(3): 404-412.
[5] Hui P C, Wang W, Kan C, et al. International Journal of Biological Macromolecules. 2013,
55: 32-38.
[6] Haque T, Chen H, Ouyang W, et al. Molecular Pharmaceutics. 2005, 2(1): 29-36.
[7] Abulateefeh S R, Alkilany A M. AAPS PharmSciTech. 2015: 1-7.
[8] Ghayempour S, Montazer M. Cellulose. 2016, 23(4): 2561-2572.
[9] He Z, Jiang S, Li Q, et al. Composites Science and Technology. 2017, 138: 15-23.
[10] Dash S, Murthy P N, Nath L, et al. Acta poloniae pharmaceutica. 2010, 67(3): 217-223.

Page 29 of 150
Electrospun composite nanofibers for photonic displays and environmental
sensing
Shah Mohammed Reduwan Billah
Department of Chemistry, Durham University, Durham DH1 3LE, UK
E-mail: reduwan.shah@gmail.com

ABSTRACT
A series of electrospun composite nanofibers incorporated with photonic materials have been
produced and some of these microfibers have shown high-quality functional properties suitable for
advanced applications. Composite electrospun microfibers doped with photonic materials can be
further functionalised using a range of functional materials (such as, stimuli-responsive materials,
conductive materials) for specifically designed targeted applications. This current paper briefly
presents different features of electrospun composite nanofibers functionalised with selected photonic
materials along with other advanced materials and their potentials in photonic displays and
environmental sensing applications.

Key words: electrospun composites, molecular switches, photonic displays, environmental sensing.

1. INTRODUCTION
Electrospinning, a very popular technique, provides the required flexibility for significant
variations in processing and tailoring nanostructures. For example, electrospun fibres can be
produced using suitable additives (such as, electrolytes) to the electrospun solution which
sometime may not significantly degrade the optical properties of electrospun nanofibres
produced from different polymers. [1] Polymer based electrospun nanofibers can be designed
to have excellent chemical and functional properties suitable to be used as active elements in
different devices that include – (a) light-emitting sources, (b) lasers, (c) energy harvesters,
and (d) sensors. [1] This type of electrospun nanofibres have potential applications in
electronic devices for realising hybrid functionalities, some of which include – interplaying
with optical and lasing properties. [1] In addition, as an emerging field, the development of
light-emitting electrospun nanofibres for optoelectronics and photonics can be employed by
using either optically inert polymers doped with fluorescent molecules (typically organic
dyes), inorganic quantum dots, organic semiconducting polymers or similar other materials.
[2-3] Polymeric nanomaterials have potential applications as sub-micron light sources,
waveguides, as active components of lasers and transistor devices with electro-optical
interplay, and as nanoscale sensing elements. [4 –7] Thus, electrospun nanostructures have
very high potential to be used as functional building blocks for their potential applications in
organic photonic and electronic devices. [1-4] A comparative high throughput for the
fabrication technique is suitable for industrial scale exploitation of many of these easily
available nanomaterials. [5-6] During this investigation functional electrospun nanofibers and
microfibers have been produced from a range of polymers that include – (a) polystyrene, (b)
polyisobutylene, (c) PVDF, (d) gelatine, (e) polyamide, (f) polybutadiene, (g) polyisoprene,
(h) polyacrylonitrile; where both pristine and composite nanofibres were functionalised using
a series of functional materials (such as, quantum dot, stimuli-responsive materials,
cyclodextrins, carbon nanotubes) to perform specific purposes which include environmental

Page 30 of 150
sensing, controlled 3D cell culture, photonic display applications. This current paper briefly
presents different selected features of functional materials (such as, quantum dot and
environmentally responsive molecules) doped into pristine and composite electrospun
nanofibres and their particular application potentials for photonic displays and environmental
sensing applications.

2. EXPERIMENTAL
Environmental stimuli-responsive functional microfibres and nanofibres were synthesised by
doping a series of stimuli-responsive materials (such as, photo-responsive photonic materials)
and quantum dots into the structure of pure and composite polymers using electrospinning
technique. [1-5] The fibre morphology was probed using different microscopic techniques
(SEM, TEM, Fluorescence Microscopy, Confocal Laser Scanning Microscopy), crystallinity
levels, environmentally stimuli-responsive characters and photophysical properties were also
investigated using appropriate techniques. [1-5, 7, 8]

3. RESULTS AND DISCUSSION

Figure 1 illustrates the structural morphology of quantum dot (CdSe/ZnS) doped polystyrene
based electrospun microfibres probed by SEM (Figs. 1a and 1b), Fluorescence Microscopy
(Fig. 1c) and TEM technique (Fig. 1d). Both SEM and TEM images revealed that there is no
phase separation on the doped electrospun fibres and they also show a uniform distribution of
quantum dot throughout the surface of the electrospun fibres. The fibre diameters of QD-
doped electrospun microfibers are in the range of 4.31 µm to 6.72 µm while the porosity levels
of electrospun fibres based mats are in the range of 11.4 µm to 22.4 µm.

Figure 1. The structural morphology of quantum dot (CdSe/ZnS) doped polystyrene based electrospun
microfibres probed by SEM (1a and 1b), Fluorescence Microscopy (1c) and TEM (1d).

Fluorescent microscopic study on quantum dot doped composite fibres show visibility under
both visible light and UV light excitation and they are fluorescent with excitation from the
UV light (Fig. 1c). In addition, quantum dot doped composite electrospun microfibres show
interesting optical properties (such as, photoluminescence) suitable for a range of high-tech
applications. [7, 8] Scheme 1 illustrates the space filling diagrammatic structures of the
molecular switches 1-3 used in this investigation.

Page 31 of 150
Scheme 1. The space filling diagrammatic structures of the molecular switches 1-3 used in this
investigation.

Figure 2. Electrospun micro-fibres produced by doping molecular switch 1 (SEM images 2a and 2b);
and by doping molecular switch 2 (SEM images 2c and 2d).

Figure 2 demonstrates fibre morphology, structure, diameter of electrospun fibres and level
of porosity of the electrospun mat where the fibres are doped with fluorescent heterocyclic
molecular switches based systems (diagrammatic structures of the molecular switches are
shown in Scheme 1). It shows that the electrospun fibres produced from a fluorescent
heterocyclic molecular switch doped synthetic polymer (polystyrene) are mostly uniform with
fibre diameters in the range from 4.78 μm to 6.22 μm. However, the pore sizes of electrospun
mats are from 2.33 μm to 19.72 μm and this wide range is mainly due to the inhomogeneous
distribution of fibres in different areas of the electrospun mats. All of these doped electrospun
fibres show photo-responsive colour change due to a change in the nature of conjugation (pi-
electrons) of the photo-responsive materials when exposed to UV light which transform from
a colourless state to a coloured state where the colourless state is less polar compared to the
respective coloured state(s). [2-5]

Page 32 of 150
Figure 3. Fibre morphology of electrospun microfibers doped with carbon nanotube probed by SEM
(3a) and TEM (3b), they are further functionalised by additionally doped with molecular switch 1
probed by SEM (3c) and TEM (3d); while Raman spectra of pristine carbon nanotube (SWNT) and
polystyrene doped electrospun microfibers are shown in (3e).

Figures 3(a) and 3(b) illustrate the fibre morphology of electrospun microfibers doped with
carbon nanotube which are probed by SEM and TEM respectively, while figures 3(c) and 3(d)
demonstrate images probed by SEM and TEM which are further functionalised by additional
doping using molecular switch 1. Figure 3(e) shows the Raman spectra of pristine carbon
nanotube (SWNT) and carbon nanotube doped polystyrene based electrospun microfibers.
SEM images (3a and 3c) show an apparent uniformity of nanofibers doped with carbon
nanotubes while TEM images illustrate the nature of dispersion and distribution of carbon
nanotubes inside electrospun microfibers. In addition, both TEM figures (3b and 3d) and
Raman spectra (3e) clearly indicate the presence of carbon nanotubes in electrospun
nanofibers and they show some conductive properties. In general, the typical conductivity
levels are in the range from 1.5 x 10-10 S/m to 1.01 x 102 S/m and this conductivity levels
dependent on a number of factors including the nature of loading of carbon nanotubes into the
electrospun nanofibres produced from a range of polymers. This conductive electrospun
microfibers have many application potentials including their uses in the fabrication of devices
for sensing applications. [7]

Page 33 of 150
Figure 4. Fibre morphology of electrospun microfibers/beads polybutadiene (4a), polybutadiene and
polystyrene based composite (4b, 4c and 4d) probed by SEM and FTIR spectra of polystyrene,
polystyrene-polybutadiene- molecular switch 1 based composite, polystyrene-polybutadiene-
cyclodextrin – molecular switch 1 based composite and polystyrene-cyclodextrin based composite
electrospun microfibers (4e).

Figure 4(a) indicates that apparently no microfibers form during electrospinning by using
elastomer polybutadiene and only some beads are formed. However, when this polybutadiene
was crosslinked with polystyrene in presence of a photoinitiator and then electrospinning was
carried out, it produced electrospun microfibers. [7] SEM images 4b, 4c and 4d show the
nature of crosslinked polybutadiene and polystyrene based composite electrospun fibres,
while 4b show the fibre morphology before UV irradiation and 4c shows the nature of UV
cured crosslinked polybutadiene and polystyrene based composite electrospun fibres. Figure
4e shows the nature of chemical interactions electrospun microfibers produced from pristine
polystyrene and composite microfibers produced from the composite mixture of polystyrene,
polybutadiene, ß-cyclodextrin after functionalised with molecular switch 1 studied by using
FTIR. Fig. 4(e) clearly indicate the presence of different polymers and materials used in the
electrospun composite microfibres production (for detail explanation, please see reference 7).
In addition, Fig. 4(d) shows the nanoscale controlled porosity of composite electrospun
nanofibres. During electrospinning polystyrene and polybutadiene based systems showed
phase separations, so rigorous studies were carried out to produce electrospun composite
nanofibers from this set of composite polymer mixtures (along with photoinitiator, based on
thiol-ene chemistry) to facilitate crosslinking after UV curing to impart required level of
mechanical and certain chemical resistances. [7] On an average the composite fibre diameter
is 8 µm and porosity level of composite fibres based electrospun mat is 31 µm (Fig. 4).

Page 34 of 150
 0.5 Photophysical properties of
electrospun composite fibres
PS-PB-BCD
0.4 PS-PB-BCD-6FDA
PS-PB-BCD-6FDA - UV 1 min
PS-PB-BCD-SPCH2OH
0.3 PS-PB-BCD-SPCH2OH - UV 1 min
K/S

0.2

0.1

0
400 450 500 550 600 650 700
Wavelength (nm)
Figure 5. Photo-responsive properties of electrospun composite microfibers before and after exposure
to the source of UV irradiation for specific period (such as, UV irradiation for 1 minute or UV 1 min).

Figure 5 shows the photophysical properties of different electrospun composite microfibers

where polystyrene, polybutadiene and ß-cyclodextrin based composite electrospun
microfibers (PS-PB-BCD) were functionalised by doping molecular switch 3 (or 6FDA, in
the graph) and 1 (or SP-CH2OH, in the graph) based photo-responsive fluorescent systems to
produce photo-responsive fluorescent electrospun composite microfibers (PS-PB-BCD-
6FDA and PS-PB-BCD-SP2CH2OH). Electrospun PS-PB-BCD-6FDA microfibers do not
retain any background colour while electrospun PS-PB-BCD-SPCH2OH based microfibers
retain a pale reddish-purple background colour but both of these electrospun microfibers
demonstrate a high level of reddish purple (with maximum absorption around 580 nm) colour
build up when exposed to UV light for a specific period (Fig. 5). Electrospun PS-PB-BCD-
6FDA microfibers do not show thermal relaxation but go back to their original colourless state
at about 2 to 10 minutes when removed from the source of UV irradiation. This nature of
reversion to the original colourless state from the colour build up state depends on a number
of factors including the strength of UV light used for excitation, nature of both host and guest
system also the nature of surrounding environment. [2-5] On the other hand, electrospun PS-
PB-BCD-SPCH2OH microfibers illustrate a high level of photo-responsive colour build up
and show thermal relaxation and go back to the nearly colourless state within 3 to 5 minutes
when removed from the source of UV irradiation. In addition, all these electrospun composite
fibres (doped with molecular switches 1 and 3) are responsive to sunlight and show relatively
higher technical properties (such as, quick photo-response and the retention of switchable
character for a long time) that make them suitable for a number of applications including in
controlled cell culture on electrospun 3D scaffolds, sensing surrounding environments. [7]

Page 35 of 150
 12

Colour difference (ΔE)

10
8
6
4
2
0
SP doped Acid vapour Ammonia Ammonia -dry - Ammonia - dry-
polyamide Acid vapour Acid vapour -
dry-Ammonia
Exposure of SP doped electrospun substrates to different environmental conditions for
sensing applications
Figure 6. The nature of colour change on molecular switch 1 doped electrospun polyamide microfibers
(or SP doped polyamide) after exposure to different controlled environmental conditions.

Figure 6 illustrates the nature of colour change on molecular switch 1 doped electrospun
polyamide microfibers (termed as SP doped polyamide in the graph) after their exposure to
different controlled environmental conditions in order to observe their response to controlled
acidic condition (shown as, response to acid vapour) and alkaline condition (demonstrated as,
response to ammonia). In comprehensive rigorous studies, it has been revealed that the
stability of photomerocyanine or PMC (also called the open form or the excited state) of
molecular switch 1 depends on a number of factors. Certain environment (such as, a particular
type of solvent medium) and the addition of bases (e.g. ammonia) contribute to slow down or
accelerate the thermal reversion reaction. On the contrary, the addition of acids (such as, acid
vapour, in this current study) always slowed down thermal back reaction and also cause a
decay of PMC isomers. This slowdown of thermal back reaction or prolonged thermal
relaxation process contributes for the retention of the coloured photomerocyanines for a
prolonged period that eventually control the mode of colour change (Fig. 6). So, this Fig.6
clearly shows different types of stabilisations of photomerocyanines of the of molecular
switch 1 doped electrospun polyamide microfibers by the addition of both acid and base which
provide an interesting opportunity for the fabrication of optical switches with improved
bistability. [7]
Additionally, one of the main objectives of this study is to investigate photochromic switching
as a means to gain photonic control of molecular level phenomena. The observed results
reveal the versatile scopes to use photochromic switches (1-3) in the photonic modulation of
fluorescence emission which can be exploited for the fabrications of molecular switch based
devices with many application potentials including in photonic displays and environmental
sensing applications. [8] As an organic optical fibre with a diameter comparable to or less
than the wavelength of light, polymer based electrospun nanofibers can be used as a platform
to manipulate light at the nanoscale. This article has briefly presented different features of
electrospun polymer fibres produced by doping CdSe/ZnS quantum dot and photo-responsive
compounds doped electrospun fibres that have the capabilities of generating, propagating,
converting and modulating light at the nanoscale suitable for photonic device fabrications. [8]
For example, Fig. 7 illustrates basic schematic diagrams for the constructions of electronic
devices for different applications including photonic display applications (7a and 7b) and

Page 36 of 150
modelled structures of photo-responsive compounds and their working mechanism in
response to UV light (7c). Detail construction and working principles of quantum dots and
photo-responsive molecular switches based devices (such as, Organic Light Emitting Diode,
Organic Field Effect Transistor, Field Effect Transistor) are available elsewhere. [8]

Figure 7. Basic schematic diagrams for the constructions of electronic devices for different applications including photonic
display applications (7a and 7b) and modelled structures of photo-responsive compounds and their working mechanism in
response to UV light (7c).

Photochromic switching as shown in Fig. 7c can be exploited to modulate the luminescence

of ordered upconversion nanopatterns to provide a rewritable two-dimensional optical storage
medium. A suitable functionalization of electrospun microfibres (such as, Figs. 2 and 4 using
molecular switches 1-3) allows selective host-guest interactions to be induced that can cause
modifications in the optical features of the photochromic molecules and very often such
interactions can be conveniently modulated by using photo-irradiation (as shown in Fig. 7c).
Usually, this type of molecular switches can be inkjet printed or coated using specialised
techniques to produce Organic Field Effect Transistors (or OFET) for different applications
(as an example, Fig. 7a illustrates a basic construction of this type of device). Typically,
OFETs (of this kind) are very important components for different technologies including
future displays and nano-electronics due to their low-cost solution processes for mass
production of flexible and large-area devices. [8, 9] In OFETs, charge carrier mobilities and
on/off ratio are some of the most important factors that control the electrical properties. As a

Page 37 of 150
result, specially functionalised organic semiconductor based electrospun nanofibres have
significant potentials to provide a solution for active channels in OFETs to improve their
electrical characteristics (a typical diagrammatic construction is shown in Fig. 7b).

4. CONCLUSIONS
Different selected features of electrospun composite microfibers doped with quantum dot and
molecular switches have been presented in this paper. It also shows selective methods of
additional functionalisation of electrospun fibres using different functional materials in order
to tune the properties of electrospun pristine and composite microfibres. It clearly shows the
scope of various potential applications of these functionalised composite electrospun fibres
where some of these advanced applications of functionalised composite electrospun fibres
include photonic displays and environmental sensing. In addition, this paper only provides
very selective and specific outlines from a range of detailed comprehensive studies where the
main pieces of work using these types of functional materials will constitute our future
publications elsewhere that will provide in-depth information on the applications and
fabrications of devices using functional electrospun nanofibres.

REFERENCES
1. Shah M. Reduwan Billah, Synthesis of quantum dot doped electrospun cellulose and other
polymer based-nanocomposites and their applications, Book on ‘Nanocellulose, cellulose
nanofibers and cellulose nanocomposites: Synthesis and applications’ – M I H Mondal
(editor); Nova Science Publishers, New York, USA, 2015, ISBN: 978-1-63483-885-6,
pages 387-424.
2. Shah M. Reduwan Billah, Synthesis of Photochromic Dye doped Cellulose Composite
based Electrospun Nanofibres for High-Tech Applications, Book on ‘Nanocellulose,
cellulose nanofibers and cellulose nanocomposites: Synthesis and applications’ – M I H
Mondal (editor); Nova Science Publishers, New York, USA, 2015, ISBN: 978-1-63483-
885-6; pages 425-442.
3. Shah M. Reduwan Billah, Chapter 8. Environmentally Responsive Smart Cellulose
Composites, in the Book on ‘Cellulose and Cellulose Derivatives: Synthesis, Modification
and Applications’ – M I H Mondal (editor); Nova Science Publishers, New York, USA,
published on 1st September 2015, ISBN: 9781634831277 (hardback), 978-1-63483-150-5
(e-book), pages 211-242 .
4. Shah M. Reduwan Billah, Molecular switches and their applications in intelligent paper,
textile and leather substrates, Letters in Applied NanoBioScience, Volume 4(2), June 2015,
Pages 281-287.
5. (a) S. M. R. Billah, et al.; Photochromic dye-doped electrospun nanofibre-based scaffolds
for cell culture, security and optical data storage applications; IUPAC 10th International
Conference on Advanced Polymers via Macromolecular Engineering, August 18th-22nd
2013 Durham, UK; (b) Shah M Reduwan Billah, Robert M. Christie, Roger H Wardman,
Inkjet printed textile based molecular switches, Conference proceeding of Textile Institute
World Conference, November 3-4, 2010, Manchester, UK, page 1-10, ISBN: 978-0-
9566419-1-5.

Page 38 of 150
6. Shah M. Reduwan Billah, Chapter 7. Smart textiles and the effective uses of photochromic,
thermochromic, ionochromic and electrochromic molecular switches; in the book on
‘Textiles: History, Properties & Performance and Applications’, edited by M.I.H. Mondal,
published in 2014, ISBN: 978-1-63117-274-8; Nova Publishers, New York, USA; pages
187-238.
7. (a) Shah M. Reduwan Billah, ‘Chapter No. 46 Micro- and Nano-Composites’ (total 65
pages), Springer Handbook of Functional Polymers, M. J. Mazumder, H. Sheardown, A.
A. Ahmed (editors), Springer, Germany, Book in press; (b) Shah M. Reduwan Billah, Neil
R. Cameron, A comprehensive study on electrospun composite nanofibers doped with
carbon nanotubes and environmentally responsive functional materials for advanced
applications, Macromolecules, article under review.
8. Shah M. Reduwan Billah, Neil R. Cameron, Photonic displays and environmental sensing
using electrospun nanofibers, Molecular Crystal and Liquid Crystals, article under review.
9. Himchan Cho, Sung-Yong Min, Tae-Woo Lee, Electrospun Organic Nanofiber Electronics
and Photonics, Macromolecular Materials and Engineering, 2013, pages, 1-12.

Page 39 of 150
The Pore Structure Characterization and Sound Absorption Performance
of the Intercalated Meltblowns
Liu Ya a, Wu Hui a, Wu Hanze a，Zhen Lei b, Cheng Bowen a
a
School of Textile, Tianjin Polytechnic University, Tianjin, 300387, China.
b
Tiandingfeng Nonwoven Co. Ltd., Shandong, 266071, China.

ABSTRACT
Noise is a kind of annoyance that causes people to be irritable or excessive sound, which is harmful to
human health. Adding 35% PET staple fiber by weight into polypropylene meltblown filament, the
intercalated sound absorbing meltblown materials of different areal densities were prepared. The
complex pore structures were characterized by the fractal theory and image analysis technique of
MATLAB. The results indicated that the pore distribution had obvious fractal characteristics, and there
was better compression resilience and strength compared with traditional PP meltblown materials with
same areal density. Furthermore, the pore structure played a significant role in the sound absorption
performance. Therefore, the relationship between the pore fractal dimension and the sound absorption
coefficient of the intercalated meltblowns was studied through the tests on the pore fractal dimension
and the sound absorption. The results showed that the pore fractal dimension increased from 1.6749
to 1.8370 with the increase of areal density from 101 g/m2 to 403 g/m2, and the sound absorption
performance of the intercalated meltblowns was better. It made a contribution to improve the sound
absorption performance of meltblowns, control the noise pollution, improve the quality of life and
helpful to develop the harmonious relationship between human and nature.
Keywords: noise; intercalated meltblowns; pore structure; sound absorption; fractal dimension

1. INTRODUCTION
With the development of modern industry and transportation industry, automobile noise has
become the main source of city noise. These noises not only seriously destroy the hearing
system of people, make people feel tired and even cause deafness, but also affect the accuracy
and service life of vehicle meters, which could cause great risks to the safety driving [1-4].
Sound absorption materials were one of the most effective materials for absorbing the
automobile noise, manufacturing and machining noise [5].
Polypropylene (PP) meltblowns is prepared by melt-spinning process with hot air blowing,
which form a three-dimensional structure of extremely fine fiber. The method has the
advantages of simple production process, low cost, and meet the requirements with light
weight, etc. In addition, the three-dimensional reticular structure with micro-fibers has good
sound absorption and sound insulation performance because of the small average pore
diameter and high porosity [6-9]. In addition, it can be cut freely without cutting off edges,
which is suitable for automobile sound absorbing materials [10]. PET staple fiber was added
to the PP meltblowns to form the bi-component intercalated sound-absorbing material. It
possessed high performance such as low density, high anti compression and elastic recovery
performance, with less material to meet the requirements of sound absorption.
It was difficult to describe and calculate the traditional geometrical structure of the
Nonwovens [11], especially intercalated meltblowns because of the random distribution of
PET fibers in the web, various and complex pore shapes and sizes. Furthermore, the
measurements of the pore shape and size took a lot of trouble, and could do unrecoverable

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damage to the samples. Fractal theory was proposed by B. B. Mandelbrot [12] to study the
irregular geometry. It could effectively describe various complicated problems encountered
in nature and scientific research [13,14].
Adding 35% PET staple fiber by weight into polypropylene meltblown filament, the
intercalated meltblown materials of different areal densities were prepared. Combining with
fractal theory and MATLAB image processing method, the shortcomings of traditional testing
methods successfully solved. The relationship between the pore fractal dimension and sound
absorption performance was obtained without damaging the pore structure. It made a
contribution to improve the sound absorption performance of meltblowns, control the noise
pollution, improve the quality of life and helpful to develop the harmonious relationship
between human and nature.

2. PREPARATION OF INTERCALATED MELTBLOWNS

2.1 Materials
Meltblown PP chips, provide by Shanghai Expert in the Developing of New Material Co.,
Ltd. Its melting temperature is 168 ℃ and the melt flow rate (MFR) is 1100g/10min. Hollow
PET staple, provide by Sinopec Yizheng Chemical Fibre Limited Liability Company. The
specification was 4D×51mm, and the addition amount was 35% by weight.

2.2 The Principle and Preparation for Intercalated Meltblowns

Before the high crimp hollow fibers blown into the meltblown superfine PP fibers, they were
fed into a carding machine to be separated into almost single fiber, then increasing the blowing
wind to make the separated short fiber evenly distributed in the PP meltblown fibers.
Therefore, the uniformity of intercalated meltblowns was improved. Meanwhile, the pore
structure of the material effectively improved by the compensation of the rigid high crimp
coarse short fiber, and the poor performance of the pressure resistance and elastic recovery
solved. The sound absorption property of the intercalated meltblowns greatly improved
accordingly [15]. Figure 1 showed the schematic diagram of intercalated bi-component
meltblowns.

Figure 1. Schematic diagram of intercalated bi-component meltblowns

After repeated tests, the main process parameters of the intercalated meltblowns and carding
roller were shown in Table 1 and Table 2.

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 Table 1. The process parameters of the intercalated meltblowns
Temperature of extruder (℃) Hot air Speed of
Die temperature Die-to-collect
zone zone zone zone temperature convey curtain
(℃） distance (cm)
1 2 3 4 (℃) (m/min)
150 180 230 230 235 300 25 12

Table 2. The process parameters of of carding roller

Cylinder working roll Stripper roll High speed random roll Doffer
(m/min) (m/min) (m/min) (m/min) (m/min)
1009 58 156 590 43

Under these process conditions, five series intercalated meltblowns of different areal
densities were obtained through changing the amount of screw extrusion and the feeding
amount of short fiber. The series number of the materials and their areal densities were
shown in Table 3.

Table 3. The number of the materials and areal densities

Sample number 1# 2# 3# 4# 5#
Areal densities (g/cm2) 101 152 247 347 403

3. STRUCTURAL CHARACTERIZATION-PORE FRACTAL DIMENSION

There are four main methods to measure the fractal dimension of pore structure: adsorption
method, discrete method, scattering method and mercury intrusion method [16]. Nonwovens
were often treated by traditional methods, but the accuracy is usually affected by
simplification or subjective factors [17].
The binaryzation image processing method based on the MATLAB software was used in this
paper. It could be used to study the microstructure and mechanism of the materials, which
helped to improve the accuracy of fractal dimension, contributed to increase the sound-
absorbing performance of the intercalated meltblowns, made the designing process more
reasonable.
Sierpinski carpet method [18] was used in this paper to solve the area fractal dimension Df of
the material. The carpet was divided into 9 squares, it formed a first level carpet with a pore
area of A1 and a carpet area of S1 by removing the middle square. Then the remained 8 squares
were divided into another 9 squares for each and removed the middle of each square to form
a second level carpet with a pore area of A2 and a residual area of S2. A series of An and Sn
could be obtained if the process went on indefinitely. The principle was shown in Figure 2.
The relationship between pore area and pore radius could be gained by this principle, which
appeared the linear relation on the dual logarithmic coordinate diagram. If the slope of the
straight line was k, then Df equaled to 2-k.

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 Figure 2. Schematic diagram of Sierpinski carpet method

3.1 Image Acquisition

TM-1000 electron microscope was used to obtain the image at 100 multiples (pixel size is
256 × 256), and the electron microscope image of each sample was shown in Figure 3.

1# 2# 3#

4# 5#

Figure 3. Electron microscope image of each sample

3.2 Image Processing

3.2.1 Image Enhancement
It was difficult to distinguish the pore area and fiber zone because of the low contrast of the
materials image, the gray stretching technology was used to increase the contrast sensitivity.
The original narrow distributed gray range was extended to 0-255, the image contrast was
enhanced greatly and it was easy to separate the pore area and fiber zone. The images after
gray stretching was shown in Figure 4.

1# 2# 3#

4# 5#

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 Figure 4. Sample images after gray stretching

3.2.2 Image Binaryzation

By choosing the proper threshold and taking it as the boundary, the gray stretching image with
256 gray levels could be changed into two gray level images, which indicated that all the
pixels were turned into black (pixel value 0) and white (pixel value is 1). This was the binary
image process [19]. There were obvious differences between the gray pore area and the fiber
zone. By selecting the appropriate threshold, the pore area could be turned into the white point
(the largest gray) if it was greater than or equal the threshold boundary, and the fiber zone
could be turned into black point (gray minimum) because it was less than the threshold
boundary. This image binaryzation process could depart the pore area and fiber zone quickly.
The binary image was shown in Figure 5.
1# 2# 3#

4# 5#

Figure 5. Sample images after binary image process

3.2.3 Binary Morphological Operations of the Image

After image binaryzation, there would be some small white spots interspersed in the image,
which may bring errors to the quantitative analysis of pore size, percentage etc. These small
white spots could be removed through corrosion and expansion on the web image.
Mathematical morphology processing and signed images was shown in Figure 6.
1# 2# 3#

4# 5#

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 Figure 6. Mathematical morphology processing and signed images

3.3 Calculation of morphological structure parameters of the Intercalated Meltblowns

The morphological structure of the intercalated meltblowns image was obtained by using
MATLAB programming. The porosity, the number of pores and the average single pore area
were gained. The structure parameters were shown in Table 4.

Table 4. The structure parameters of the intercalated meltblowns

Sample Average single pore
Porosity (%) Number of pores
number area ( Pixel number）
1# 32.5 166 394.8
2# 35.9 184 356.2
3# 35.7 207 316.6
4# 36.1 222 295.2
5# 40.4 231 283.7

It showed in Table 4 that the porosity and number of pores of the meltblowns increased with
the increase of the areal density. While the average single pore area decreased.

3.4 Calculation of Pore Fractal Dimension

The pore parameters for the binary segmentation of the web image were calculated first.
According the pore area measure in the images, the radius of the circle which corresponding
to the area could be calculated, then arranged the radius from big to small. The area fractal
dimension Df of the material could be calculated according to the following steps.
(1) Select the radius R (pixel number).
(2) Count the pore area A (pixel number) which larger than or equal to R.
(3) Count the remaining area S, which was subtracted from the whole area of radius greater
than or equal to R.
(4) Change the size of R, repeat steps (1) - (3).
(5) Draw the double logarithmic plots of log (R) -log (S).
(6) Judge the data region with good linear relationship, the linear slope k was obtained by
linear fitting with least square method.
(7) Calculate the fractal dimension of pore size distribution, Df = 2 – k.
Figure 7 showed the log (R) -log (S) double logarithmic linear fitting map of each sample.

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 Figure 7. log (R) -log (S) double logarithmic linear fitting map

The pore fractal dimension could be obtained from Figure 7, and the values were shown in
Table 5.

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 Table 5. Fractal dimension value of intercalated meltblowns
Sample number 1# 2# 3# 4# 5#
fractal dimension
1.6749 1.7231 1.7359 1.7423 1.8370
D(f)
correlation
0.9557 0.9749 0.9337 0.9794 0.8998
coefficient

It was showed in Table 5 that the fractal dimension of the meltblowns increased with the
increase of the areal density.

4. THE PERFORMANCE OF THE INTERCALATED MELTBLOWNS

4.1 Physical and mechanical performance
According to Chinese GB /T 24218, the areal density of the material was measured by
FA2004A electronic balance, the thickness by YG141L digital fabric thickness tester and the
breaking strength by YG028 universal material testing machine. The diameters of 50 fibers
were measured by VH-1000 optical microscope, and the mean value was calculated. The
compressive resiliency was measured by YG141L digital fabric thickness tester according the
GB/T 18840 . The results were shown in Table 6.

Table 6. The basic performance of the intercalated meltblowns

Sample Thickness Meltblown fiber Tensile strength Compression
number (mm) diameter（μm） （N/5cm） resilience（%）
1# 2.88 4.45 43.4 34.23
2# 3.62 4.56 45.6 48.46
3# 5.47 3.98 49.7 59.25
4# 8.18 4.23 52.2 61.35
5# 13.92 4.19 54.1 72.29

It showed in Table 6 that the average diameter of the meltblown fibers were changed little
because of the same melt blowing process. With the increase of the areal densities and the
addition of hollow PET fiber, the thickness of the materials increased, and the strength and
compression elasticity of the material gradually increased.
In order to study the compressive resilience performance of the intercalated meltblowns, the
same amount of traditional meltblowns was used as the contrast sample. It was found that the
thickness of the traditional PP meltblowns was 5.04 mm and the compression resilience was
28.32% for sample with the areal densities of 400 g/m2. It showed that after adding PET staple,
the thickness increased by 176% and the compression resilience increased by 155%.
Meanwhile, another sample of 100 g/m2 showed the same results, the thickness increased by
78% and the compression resilience increased by 47%. Therefore, the bulkiness and
compression resilience of meltblowns were greatly improved due to the insertion of high
crimp hollow PET short fibers.

4.2 Sound Absorption Performance

According to GB/T18696.1, the sound absorption coefficient of the material was measured
by SZZB- double channel standing wave tube. The result was shown in figure 8.

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 Figure 8. The curve between sound absorption coefficient α and frequency Hz

It showed in figure 8 that in the full frequency band, the sound absorption coefficient of the 5
samples tends to increase with the increase of the areal density, which was consistent with the
reporter [20]. But in some frequency range, there were some fluctuations in the absorption
coefficient curve. In the low frequency range, the sound absorption coefficient of the sample
were relatively low and the absorption capacity was relatively poor. This was because the
vibration times of air in the pore reduced per unit time at the low frequency, which had little
effect on the frequency of acoustic attenuation, so the absorption coefficient was very low
[21].
In order to evaluate the sound-absorbing performance, four octave average noise reduction
coefficient (NRC) of 250Hz, 500Hz, 1000Hz and 2000Hz were used to characterize the
acoustic performance according to the test standard of the intercalated meltblowns [22]. The
results showed in Table 7.

Table 7. The noise reduction factor of the intercalated meltblowns

Sample number 1# 2# 3# 4# 5#
Noise reduction factor
0.35 0.40 0.45 0.50 0.65
(NRC）

It showed in Table 4 that with the increase of the areal density, the noise reduction coefficient
also increases in turn.

5. RELATIONSHIP BETWEEN FRACTAL DIMENSION AND SOUND

ABSORPTION PERFORMANCE OF THE INTERCALATED MELTBLOWNS
The meltblown sound absorption material belonged to the opening porous sound-absorbing
material. There were a lot of tiny gaps and continuous air in the material, so it had a certain
ventilation. When the sonic wave entered into the porous sound-absorbing meltblown
material, the air in the pore and fiber in the web vibrated together. Because of the friction and
viscous resistance and heat conduction of the fiber, part of the sound energy tuned into heat
and lost, another part of energy transfer for material mechanical energy. The air vibration,
viscous action and friction resistance in the web were greatly affected by the sound frequency
and porosity. High frequency sound waves could accelerate the vibration of air particles in

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the web, and the heat exchange between the air and the pore wall accelerated accordingly.
This made porous materials possess the performance of good high frequency sound absorption
[23].

Figure 9. The curve between the fractal dimension and the noise reduction factor

The relationship between the fractal dimension and the noise reduction factor of the
intercalated meltblowns were shown in Figure 9. It showed in Figure 9 that the sound
absorption coefficient of the intercalated meltblowns increased with the increase of pore
fractal dimension. Because the larger the pore fractal dimension was, the more the number of
pores it had, and the closer the area of each pore was in the web. When the sound wave entered
into the intercalated meltblowns, the more contact with the inner wall of the hole, the greater
the friction and viscous resistance were, and the more sound energy converted into heat
dissipation, the better the sound absorption performance was.
Compared with the relation curves between pore fractal dimension and noise reduction
coefficient and the areal densities in Table 3, it showed that the fractal dimension of pore
increased with the increase of areal densities. This was due to the number of fibers per
densities in the intercalated meltblowns increased with the increases of web areal densities
quantitatively. The probability that the fiber divided the web into small pore increased
accordingly. Meanwhile, the smaller pores in the web were usually easy to be split into smaller
ones when the fiber was continuously added to the web during the random web-forming
period. The disappearing velocity of the hole slowed down when the aperture decreased. As
a result, the slope k of the fitting straight line in the log (R) -log (s) curve decreased. Therefore,
the fractal dimension Df increased, and the sound absorption property of the sample increased
accordingly.

6. CONCLUSIONS
In this paper, series of intercalated meltblowns were successfully fabricated, the structural
characterization and the sound absorption performance were analyzed and researched. The
results showed that the bulkiness and compression resilience of meltblowns were greatly
improved due to the insertion of high crimp hollow PET short fibers. The binaryzation image
processing method based on the MATLAB software was used successfully to treat the
complex structure of intercalated meltblowns. From the relationship between pore fractal

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dimension and sound absorption performance, it showed that the fractal dimension of pores
played an important role in studying the relationship between structure and performance of
the materials. It could improve the sound absorption performance of intercalated meltblowns
by increasing the pore fractal dimension Df.

ACKNOWLEDGEMENTS
This research is supported by the National Natural Science Foundation of China (No.
51403155), Tianjin Science Technology Research Funds of China (No. 15JCYBJC47200).

REFERENCES
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transportation noise in Hong Kong. Applied Acoustics 70 (2009) 1-10.
[4] Van Kempen E, Fischer P, Janssen N, et al. Neurobehavioral effects of exposure to
traffic-related air pollution and transportation noise in primary schoolchildren.
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[6] Y.Chen, N.Jiang. Carbonized and Activated Non-wovens as High-performance
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[7] Jinjing Chen, Zheng Guo. The Acoustic Insulation Property of a New Non-Woven
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[8] J.Sobieszczanski-Sobieski, S.Kodiyalam, R.Y.Yang. Optimization of car body under
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[9] Newman NC, Ryan P, Lemasters G et al. Traffic-related air pollution exposure in the
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[10] Xianfeng Ding, Hong Wang. Study on PET /PP scattered composite melt-blown sound-
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[12] Alexander A. Potapov. Chaos Theory, Fractals and Scaling in the Radar: A Look from
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Understanding Complex Systems. Springer, Cham (2016) 195-218.
[13] Jianli Liu, Wei Bao, Lei Shi, et al. General regression neural network for prediction of
sound absorption coefficients of sandwich structure nonwoven absorbers. Applied
Acoustics 76 (2014) 128-137.
[14] T.Yamamoto, S.Maruyama, S.Nishiwaki et al. Topology design of multi-material
soundproof structures including poroelastic media to minimize sound pressure levels.
Computer Methods in Applied Mechanics Engineering 198 (2009) 1439-1455.

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[15] Yihong He, Nanping Deng, Lanlan Fan et al. Progress in the Research and Application
of Melt-blown Nonwoven Technology. China Textile Leader S1 (2016) 71-80.
[16] Yanlin Yin. Research progress in the measurement and application of fractal dimension
of pore structure. Inner Mongolia Petrochemical Industry 9 (2008) 109-111.
[17] Shu Yang, Weidong Yu , Ning Pan. Effect of nonwovens pore fractal dimensions on
their acoustic absorption behaviors. Journal of Textile Research 31 (2010) 28-32.
[18] A. Ebrahimi Khabbazi, J. Hinebaugh, A. Bazylak. Analytical tortuosity-porosity
correlations for Sierpinski carpet fractal geometries. Chaos, Solitons & Fractals 78
(2015) 124-133.
[19] Lianying Ji, Fawen Guo, Lifang Liu. New method of determining the pore fractal
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[20] Bang One Lee, Jung An Ko, Sang Won Han. Characteristics of PP/PET Bicomponent
Melt Blown Nonwovens as Sound Absorbing Material. Advanced Materials Research
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nonwovens in automobiles. Technical Textiles 34 (2016) 1-7.
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Development Trend of Porous Absorption Materials. Materials Review 26 (2012) 303-
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Preparation of Photochromic Polyester Fiber
Yonggui Li a, Mohan Zhan b，Huizhen Ke b
a
Fujian Key Laboratory of Novel Functional Fibers and Materials, Minjiang University,
Fuzhou, China.
b
College of Clothing & Design, Minjiang University, Fuzhou, Fujian, China.

ABSTRACT
Conventional photochromic fibers are produced by dyeing with photochromic dyes or solution
spinning adding photochromic pigment. Conventional photochromatic pigments are not suitable for
melt spinning because of their poor thermo-stability. In order to develop the spinning technique for
photochromic fiber, a photochromic polyester fiber is prepared by melt spinning, mixing
photochromic pigment and PET. The colour change properties of the photochromic fiber is observed
by measuring the chromatograph and spectrum, and its surface morphology is characterized by SEM.
The functional groups of the fiber are investigated by IR. The technical performance (wash fastness
and photostability) are evaluated using specifically adapted colour measurement methods. SEM
photographs indicated that photochromic pigments are distributed evenly in the fiber. The excitation
spectrum shows narrow bands in the ultraviolet and visible light regions. The colour change property
increases with the content of the photochromic pigment in the fiber and the content of 0.5% is enough
for practical application. The spinning temperature T ≤ 200 ℃ are suitable for preparing the
photochromic fiber. The photochromic fiber shows good wash fastness. The colour change property
decreases with exposure to ultraviolet.
Keywords：photochromic fiber, PET fiber, melt spinning, process optimization

1. INTRODUCTION
Under the irradiation of sunlight or ultraviolet light, photochromic textiles change color and
they will change back to the original color irreversibly when the light source is removed.
Photochromic fabric can be produced by coating or pigment printing method [1,2]. However,
the products show poor resistance to washing. John et al. proposed a process to make the
photochormic fiber by electrospinning [3]. However, only super-fine fiber can be produced.
At present, it does not apply batch production. Most research activity has focused on the
manufacture of photochromic fiber by dying with photochromic dyes [4-6]. However, the
commercial available photohromic dyes are disperse dyes, unsuitable for natural fibers.
On theory, the photochromic fiber can be produced by spinning technique. However,
conventional photochromatic pigments are not suitable for spinning fiber because of their
poor thermo-stability.
In order to develop the melt spinning technique for photochromic fiber, in the present study,
a photochromic pigment is incorporated into a polyester fiber by melt spinning. The
morphology and spectral properties of the product are investigated.

2. EXPERIMENTAL
2.1Sample preparation
The partially oriented yarn (POY) of the photochromic fiber is prepared from PET with
melting point of 170 ℃ by melt spinning technique, incorporating the photochromic pigment
at 0.2-1.0 wt%. We change the content of the photochromic pigment in the fiber c and

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spinning temperature T, and compare the fiber's coloristic and mechanical properties, and then
obtain the reasonable c and T.

2.2 Characterization
The photochromic material and fiber are examined under a scanning electron microscope
(SEM; SU1510, Hitachi Inc.). Groups of the products are investigated by Fourier transform
infrared spectroscopy (FT-IR, Thermo Fisher Scientific Co., Ltd.). Excitation spectra are
recorded using a F4600-type fluorescence spectrophotometer (Hitachi Inc.).
Tensile properties of the fiber are determined using a YG020 series electronic single yarn
strength tester, according to the standard ISO2062: I993. The standard ISO 105-C10 is used
for determining the washing fastness of the photochromic fiber. The weathering effects are
investigated according to ASTM G154, using a QUV accelerated weathering tester (Q-Lab
Corporation).

3. RESULTS AND DISCUSSION

3.1 Effect of the photochromic pigment content on the property of photochromic fiber
Photochromic fibers are prepared at T = 190℃ firstly, by following change in c shown in Table
1. The linear density of the yarn is 16.1 tex. After 30s irradiation in full, bright sunlight, their
colouristic and mechanical properties are measured. It turns purple on irradiation with
ultraviolet or exposure to sunlight.
As shown in Tab.1, the colour change property of the photochromic fiber increases with c,
and it is enough for practical application at c = 0.5%. The degree of photocoloration increases
slowly with c when c is above 0.5%. The chrominance appears to be stationary when c is
increased to 1%. Therefore the rational value of c is considered to be in the range of c from
0.5 % to 1%. There is no need to increase c above 1%. The effect of c on the mechanical
property of the photochromic fiber can be neglected in the range c ≤ 1%.

Table 1. Properties of photochromic fiber at different content of photochromic pigment in fiber c.

Color after Pantone color Strength
C, %
irradiation code (cN·dtex-1)

1 265U 2.27

0.8 265U 2.25

0.6 2655U 2.37

0.5 2655U 2.31

0.4 2645U 2.28

0.2 2635U 2.32

0 2.10

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3.2 Effect of spinning temperature on the properties of photochromic fiber
As shown in Tab. 2, with an increase in T, the photocoloration effect of the photochromic
fiber becomes worse and the strength of the fiber decreases obviously when T ≥200℃. The
spinning temperature must be below 200 ℃ for preparing the photochromic fiber.

Table 2. Colouristic and mechanical properties of photochromic fiber at different spinning

temperature T.
Color of the fiber Pantone color Strenth
T, ℃
after irradiation code (cN·dtex-1)

190 2655U 2.31

195 265U 2.50

200 2655U 2.78

205 2635U 2.77

210 270U 2.76

215 2.65

3.3 Morphology of photochromic pigments and photochromic fibers

As shown in Fig. 1, well-defined boundaries could be observed for each particle. The
majority of the particles are spherical, and the particle size is less than 8 um. The
photochromic pigment can be applied to the preparation of coarse fiber.

Figure 1. SEM images of the photochromic pigment.

Figure 2 shows SEM images of the photochromic fiber. The photochromic polyester yarn has
obvious bumps on its surface. These pointy bumps distributing relatively even. The yarn’s
surface is coarser than normal polyester fibers which may cause the reduction of mechanical
propert

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 Figure 2. SEM image of the photochromic fiber.

3.4 Infra-red spectrum (IR) analysis

The characteristic peak of the photochromic pigment in Fig. 3(a) can be observed in the
wavelength range of 500 - 4500 nm in Fig. 3(b). The reason is considered as the following.
photochromic pigment was not destroyed in the spinning process. Therefore, the addition of
photochromic pigment in the PET fiber at a low content has a negligible effect on the
mechanical property of the fiber.

(a) Photochromic pigment

(b) Photochromic fiber (c = 0.5%)

Figure 3. IR spectrums of photochromic pigment and fiber(c = 0.5%).

3.5 Excitation spectra of the fiber

The samples were illuminated by the light of wavelength 254 nm. As shown in Fig. 5, the
excitation spectrum shows narrow bands in both ultraviolet (250 nm – 270 nm) and visible
regions (505 nm – 525 nm). The photochromic pigment absorbs ultraviolet radiation strongly

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at wavelengths around 260 nm. This indicates that ultraviolet light or sunlight can activate the
photochromic pigment and causes the color change of the photochromic fiber.
The excitation wavelength of the photochromic fiber lies within the narrow region 252-275
nm, with excitation peak at 257 nm, and the narrow region 504 nm - 544 nm, with excitation
peak at 520 nm. The photochromic fiber absorbs both ultraviolet and visible light.

Both of the excitation wavelength of photochromic pigment and fiber lie within the narrow
regions. This is the reason why their coloration and fading rates are fast.

(a) Photochromic pigment

(b) Photochromic fiber

Fig. 5. Excitation spectrum of the photochromic pigment and the photochromic fiber.

3.6 Washing fastness

The colour change property of the photochromic fiber is nearly unchangeable after a standard
washing for 4 hours as described in Sec. 2.2, and then is reduced after further washing. It
disappears after washing for 6h.
A continuous washing in 4 hours did not change the photochromic effect. With an increase in
washing time, the photostability of photochromic polyester fiber gradually weakens. After 5
hours, the color is obviously lighter, 6 hours later it tends to be colorless because the structure
of photochromic pigment has been damaged.

3.7 Resistance to weathering.

UV absorbers are not recommended for photochromic fiber products because they dissipate
the absorbed light energy from UV rays. This reduces the absorption of UV rays and hence
reduces the photochromic effect if they are applied to the photochromic fiber products.

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Exposing photochromic polyester fiber to the simulated environment under ultraviolet light’s
irradiation (10 min / 50 ℃), it can be observed that the photochromic effect receded with time
and faded away after 2 hours tests. This indicates that the internal structure of the
photochromic pigment has changed. The results showed that the photochromic polyester
fibers may be instructed to refrain from excessive sun or heat exposure.
The colour change property of the photochromic fiber decreases with the exposure time to
ultraviolet, and disappears after 2h exposure. This indicates that the photostability of
photochromic fiber need to be improved and made lifetime longer.

4. CONCLUSIONS
The photographic powder content of 0.5% and the spinning temperature T ≤ 200 ℃ are suitable
for preparing the photochromic fiber. The photochromic particles are well distributed in the
fiber. The structure of the polymer is not significantly altered by the presence of the
phochromic pigment. The excitaion spectra of the photochromic pigment and photochromic
fiber are similar and show narrow bands in both the ultraviolet and visible regions, with peaks
at 257 nm and 520 nm, respectively. The obtained photochromic fiber has good optical and
mechanical properties. Its wash fastness and resistance to weathering are needed to improve.

ACKNOWLEDGMENT
This work was supported by The Fujian Province Department of Science & Technology [No.
2015H0030] and Minjiang University Research Project [MJY14004].

REFERENCES
[1] T Cheng, T Lin, J Fang et al. Textile Research Journal, 77(12): 923-928 (2007).
[2] A F Little, R M Christie. Color. Technol., 127, 275-281(2011).
[3] F R John, B Andrea. WO Patent 2005090654A1, 2005.
[4] W H Foster, J Kazan. Textile Research Journal, 37(5): 376-380 (1967).
[5] Y A Son, Y M Park, S Y Park, et al. Dyes and Pigments, 2007, 73: 76- 80.
[6] M Aldib, R M Christie. Color. Technol., 127, 282-287(2011).

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Garment Production networks in South-Eastern Europe: Sociocultural
Affinity and Sustainable Practices
Konstant Agrofiotis
Hsuan Chuang University, Taiwan

ABSTRACT
Regional manufacturing networks operating in the South-eastern fringes of Europe after a
devastating decade of diminishing orders, due mainly to the “China price” factor, have recently
started to produce specialized clothing for European upper-middle fashion companies. These
South-eastern European manufacturers currently possess the relevant experience in higher quality
production. They also engage with sustainable production practices and employ workers who are
paid if not living, at least fair wages. An important aspect of this reshoring activity can be
attributed to a certain sense of socio-cultural affinity. In it, all members involved in production
and retail operations perceive a loose interpretation of European solidarity which can be
translated into stable orders and as a result into job retention within European borders. The
concepts of global production networks form the theoretical background of the study. The theory
lends support to retail-led production, and also to the assumption that commercial transactions
among network members together with non-economic actors, such as the EU and civic
associations, can play an influential role in regional production arrangements. Qualitative
methods are employed in this study following the philosophical view of the interpretivist
methodology. In a single case study of a small production network of a specialized retail brand
operating in the Balkans and the Black Sea regions, the authors explore all major parameters of
clothing production. The findings broadly confirm that near-shoring more than reshoring
currently occurs in Europe as well as that all supply chain participants engage with sustainable
practices which can form a viable and simultaneously competitive manufacturing strategy.
Keywords: Garment production, South-eastern European networks, Socio-cultural affinity,
Sustainable practices, Near-shoring.

1. INTRODUCTION
Reshoring, a new term denoting that clothing production has the potential of returning to
European shores has gathered momentum in the recent past (Groom and Powley, 2014).
The rationale for reshoring, apart from concerns and mounting pressure regarding
sustainable practices can also be attributed to the so-called Total Landed Costs which
have arisen in other clothing manufacturing countries, such as China. This gives rise to
the concept of some production returning to within European borders after decades of
neglect (EPRS, 2014). Realistic benefits include improvements in quality, certainty,
production efficiencies and the made in Europe “label” with the heritage, quality, labor
and environmental sensitivities associated with it (Za, 2014).
The theory of Global Production Networks (GPNs) helps to explain the reshoring flow
of production in its European dimension, as it is based on transnational relational
networks which engage with production arrangements. Furthermore, the theory
incorporates the so-called non-economic actors in the networks’ configuration, as for
example, the role of the EU and its regional policies can induce and subsequently enhance
the networks’ performance and competitiveness. Other non-economic actors include
civic associations which voice concerns on environmental sustainability and also the

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issue of workers’ wages (Coe, Dicken and Hess, 2008).
Peripheral Southeastern European networks after a devastating period due to the
migration of production especially to China seem to be recovering some production
capacity as specialization, quality and proximity factors prevail in the reshoring logic
(Pickles and Smith, 2011). This can also be attributed to a loose interpretation of
European solidarity, as Western European higher level brand owners have acknowledged
the cachet of “made in Europe” production. Mounting pressure induced by civic
associations can also be included, as customers want to know where their clothes are
made and under what conditions (Friedman 2010).
In a single case study of a company operating in a European cross-border production
network, the authors attempt to empirically explore the feasibility of reshoring of better
quality production within European borders. The EU’s regional policies are also
addressed as they shape the manufacturing landscape and influence its competitive
outcome. All actors involved in the case study namely, the owners of the retail brand, the
manufacturing companies and the EU’s policies point to the direction that sustainable
development can be a viable production strategy in European production networks. The
case also demonstrates that nearshoring more than reshoring to the original country of
origin currently occurs in this part of Europe. Thus, nearshoring can be a viable strategy
among manufacturers producing for upper-middle fashion brands, as all parties involved
are interested in keeping some production within European borders, demonstrating
sensitivities for the environment and also presenting convincing evidence of sustainable
actions to their end customers. The thorny issue of living wages as opposed to fair wages
is still debatable although the companies in the study have taken some corrective
measures.

2. THE SUSTAINABILITY ISSUE IN THE FASHION INDUSTRY

Sustainability in the fashion industry forms a fraction of the bigger picture of sustainable
development. However, it is widely recognized that the clothing industries, (including
textile production) are possibly the second most polluting industries after petrochemical
companies worldwide (De Brito et al, 2008).
The fast fashion business model is certainly partly responsible for this global
environmental deterioration (Cline, 2013; Fletcher, 2008). This model is based on
shortening each season’s time slots between production and retail by inducing customers
to buy more, as stores’ shelves are replenished approximately every 30 days with fresh
merchandise. Customers’ attachment to fast fashion is to demand new ranges every
month because the traditional pattern of two fashion seasons is now replaced by 6 fashion
cycles of new merchandise per season. This is combined with the race to the bottom for
the cheapest possible production location where fashion’s flavor of the month has an
irresistible price tag attached to it (Remy et al, 2016). This aggressive retailing model,
praised by business analysts and economists alike, compels contract manufacturers to cut
costs in every possible way (Remy et al, 2016; Siegle, 2011). This is translated to the
lowest common denominator in labor costs (especially for women who are principally
employed in garment factories), quality, and environmental considerations since speed is
the imperative concern to the detriment of all other variables in the retail equation

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(Barrientos, 2013; Cline, 2013).

2.1 The Fashion Industry and Ethical Practices

Ethical consumption can be described as consumers not taking buying decisions based
solely on their personal interests but also incorporating societal and environmental
parameters. However, it can be argued that in some cases, fashion companies which claim
to be ethical, may engage in practices which may not be entirely ethical with regard to
the environment and/or workers’ rights (Goworek, 2011; Friedman, 2010; Siegle, 2016).
These activities, termed greenwashing, are usually devised by unscrupulous marketing
and public relations managers who lead customers to believe that fashion companies
demonstrate deference to ethical labor practices and the environment, whereas in fact the
opposite happens (Siegle, 2016).
Despite greenwashing, in Europe, a number of clothing companies together with trade
bodies, Universities, the European Parliament and European Commission have
responded to sustainability demands by instigating public awareness, promoting ethical
practices and forming associations (Goworek, 2011). Civic society and non-
governmental organizations pursue similar agendas by taking initiatives on the reduction
of poverty of garment workers, cleaning up the supply chains, supporting sustainable
practices and raising environmental standards in the T&C sectors.

2.2 Transparency in Clothing Supply Chains

The traceability of materials and assembly operations in upstream production networks
can form part of the sustainability architecture in the T&C sectors (Martin, 2013). The
transformation of supply chains from the current state to a greener future can be a
daunting task and perhaps more suitable for the brave among manufacturers. However,
the subject of the UN report on the traceability of supply chains may serve as a useful
guide for the sustainability architecture in the T&C sectors. Traceability in the report is
defined as “the ability to identify and trace the history, distribution, location and
application of products, parts and materials.” In other words, it is a system that monitors
inputs as they enter the supply chain and are processed into end products. Incorporating
the sustainability parameter into the system, traceability addresses also the sustainable
origin of inputs, together with safeguarding good practices, respect for workers and
obviously the environmental impact of these actions. It should be noted that traceability
or life cycle analysis as it is known in the trade is slowly becoming an accepted practice.
The EU has set a number of directives on certification programs for companies operating
within sustainable requirements. Coordination difficulties among stakeholders represent
a considerable challenge as well as investments in technology remote manufacturing
locations, language barriers and local managerial skills to access technology (United
Nations Global Compact Office, 2014). The traceability report recommends a best
practice model based on what it calls the “Global Collaborative Scheme,” which is shown
in Figure 1.

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Fiber/Yarn Textile Garment factories Brands/Retailers
producers mills/Supporting
industries  Certified to the  Participation in a
 Participation in scheme global sustainability
global sustainability  Certified to the  Trust/Dependence/ initiative
initiative scheme Fairness  Trust/Dependence/
 Trust  Trust/  Labor Fairness
 Sharing information Dependence conditions/wages  Instigating network
 Reputation  Sharing network  Sharing network certification
resources resources  Resource productivity
 Sharing  Resource initiatives
information productivity  Sharing network
 Reputation/pride implementation resources
 Sharing  Reputation
information  Sharing
 Reputation/ pride information

Figure 1. A global Collaborative Scheme in the Textile and Clothing Sectors- Buyer Driven
Global Value Chain ((Adapted from: United Nations Global Compact Office 2014)

2.3 Resource Productivity and Sustainable Materials Management

In manufacturing terminology, resource productivity refers to the sensible utilization of
material resources in a production process by also measuring the environmental impact.
The goal is to use less and produce more with given resources. This entails cost
efficiencies that contribute towards production optimization processes as economizing
on resources saves money for clothing companies in a production network (Martin, 2013).
Resource productivity in manufacturing can also be achieved by upgrading machinery
especially in garment factories where in many cases it is outdated. This does not represent
an investment on a big scale, although smaller manufacturers may experience difficulties
in borrowing capital (Martin, 2013). However, in the event that machinery upgrading
occurs, manufacturers calculate the business they can capture in accordance with the
factory’s capacity. This happens because the factory becomes more specialized so
manufacturers may attract buyers of better brands thus participating in more upgraded
networks. Advanced machinery can also raise productivity in garment assembly, enhance
quality of manufacturing (Shih and Agrafiotis, 2015), and this in turn can have a positive
impact on workers’ wages without necessarily triggering the next wave of relocation
(Martin, 2013).

2.4 The Labor Conditions Issue

It is a well-known fact that the T&C sectors are the first industries of any developing
country which is moving along the path to industrialization (Dicken, 2015). The clothing
industry in particular is the most widely spread manufacturing sector and it has long been
the epicenter of the globalization process and a testing ground for workers’ conditions
(Cline, 2013; Martin, 2013; Dicken 2015). Unfortunately, the World Trade Organization
(WTO) which is the official mediator of trade agreements has failed to include the social
dimension in its provisions. This has led to a multiplicity of private initiatives addressing

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the issue of labor conditions (Bair et al., 2014).
Since the middle of 1990s these initiatives have evolved into corporate social
responsibility programs (CSR) which led to auditing systems set up for the purpose of
monitoring contractors’ compliance. These programs are in essence risk management
tools which can safeguard against reputational damage for brand owners/retailers in the
event of sweatshop scandals, which unfortunately occur often in garment factories (Bair
et al., 2014; Cline, 2012; Martin, 2013).
Notwithstanding CSR policies exercised by the buying companies, the labor issue is far
more complicated than a CSR program. It is not unusual for the inspections delegated by
retailers/brand owners to independent auditors to be fraught with audit frauds. In this,
auditors either turn a blind eye to breaches of labor and/or environmental regulations or
recommend minor remedial actions (Siegle, 2011). In other cases, fake certification
documents are produced or buyers are shown demonstration factories but the majority of
work is subcontracted to uncertified garment factories (Cline, 2013; Martin, 2013).
The problem is also compounded by the fact that the least developed countries rely
heavily on clothing exports and simultaneously on the employment of large numbers of
semi or unskilled workers, and in these countries, in many cases working conditions are
often squalid and wages in garment factories are pitiful (Barrientos, 2013; Cline, 2012;
Martin, 2013). One of the major labor issues is workers’ wages and especially living
wages as factory owners may pay legal minimum wages but these are far from what the
World Bank calculates as wages above the poverty line (Barrientos, 2013; Cline, 2013).
The cost pressure to cut prices is constant and in some cases drastic cuts are demanded
by buyers. In Eastern European countries labor conditions are not a lot better, as
according to a recent report by an NGO it calls the “Made in Europe” label, the cheap
labor garment factory for Western Europe an fashion brands (Rankin, 2014; Luginbuhl
and Musiolek, 2014). Despite the EU’s pledge of reducing poverty and social exclusion
by 2020, in fact it seems that garment workers in countries like Bulgaria and Romania
are still far from achieving the living wages ideal. What is even more surprising in the
report is that in 2013 legal minimum wages in these two countries were lower than China
(Luginbuhl and Musiolek, 2014; Rankin, 2014). Therefore, it is naïve to believe that
proximity to the Western EU markets and industrial upgrading can necessarily benefit
garment workers, and women in particular, although some benefits can be achieved for
workers in more skilled positions such as pattern cutters and garment technicians
(Barrientos, 2013).

3. THE RATIONALE FOR RESHORING PRODUCTION

In its generic context, reshoring describes a currently occurring situation where some
production, after decades of neglect, may be returning to advanced economy countries.
Reshoring as the name suggests is the opposite of off-shoring, a term associated with the
hollowing out of production in advanced economies, usually associated with high worker
salaries (Fernandes, 2012; Za, 2014; Groom and Powley, 2014). According to the
European Parliament Research Service, reshoring is described as: “the partial or total
return of production previously offshored to low-wage countries to the original country,
to serve local, regional or global demand. It is also referred to as: in-shoring, reverse

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offshoring, on-shoring, back-shoring and insourcing” (EPRS, 2014). However, this
reshoring movement needs to be more closely examined, as companies may return some
production to the homeland while simultaneously offshoring other parts of their
production to cheaper locations. Moreover, reshoring production and job creation, despite
the media reports, represent a tiny fraction of what they used to be in the years of mass
manufacturing employment (The Economist 2013; Sirkin et al, 2011).
An important factor is the strategic and operational risks associated with reshoring as
companies need to examine closely their supply chains and see the network effect with
regard to their component suppliers and cost escalation in seven crucial variables. These
include labor namely, staff shortages and training, as well as higher wage structures, since
in Europe labor cost is approximately 15 times higher than in China,
logistics/transportation, utilities, real estate, duties/taxes and incentives provided by
national governments and other regional government authorities. This amounts to the so-
called total landed cost which is a key measure for companies considering reshoring
production as it calculates the end-to-end supply chain costs (Wingard and Connerty,
2014; ERPS, 2014; Ellram et al, 2013).
Notwithstanding the risks, reshoring presents benefits in the following areas, those of
improvements in the quality of finished products, protecting intellectual property,
certainty and production efficiencies in the form of smaller batches, switching production
schedules and introducing faster new products, decreasing transportation costs, and
reducing disruptions in long supply chains. Moreover, reshoring is a desirable condition
for national governments instigating social policies for the simple reason that reshoring
creates jobs (Groom and Powley, 2014; Wingard and Connerty, 2014). Lastly, domestic
manufacturing holds the potential for exports increase and imports decrease (Groom and
Powley, 2014; EPRS, 2014). Despite the perceived benefits of reshoring, a balanced
sourcing strategy is recommended as companies need to trade off product categories with
regards to region(s) of manufacture, thus reaping comparative advantages (EPRS, 2014;
Groom and Powley, 2014; Wingard and Connerty, 2014).

3.1 Reshoring Production in the European Textiles & Clothing Sectors

In European terms, reshoring can be a realistic scenario since western European
companies, especially under the Single Market agreement, have sought to manufacture
within EU borders benefiting from the low labor wages of Eastern European countries
without trade barriers (Ellram et al, 2013). Furthermore, under the EU’s Outward
Processing Trade arrangement with countries outside EU borders, partial duties are only
paid on the added value of the assembled garments since fabrics and trim come from
European mills (Cernat and Pajot, 2012). The reshoring trend has been observed mainly
among the Southern European countries of Italy, Spain, Portugal and Greece as well as
Eastern European countries such as Bulgaria, FYR Macedonia and Romania (Za, 2014).
Turkey as it was revealed during the interviews, remains one of the most favorable
locations not only for its proximity to the EU but for the fact that the country’s textile
mills, trim manufacturers and garment factories can provide complete end-to-end supply
chain solutions which are very appealing to retail brands. Despite Turkey’s prominence,
the “made in Europe” label is alluring in fashion and since the Eurozone crisis has hit the

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economies of Southern European states harder, trade unions were willing to renegotiate
wage terms with employers (Za, 2014).
Frequent changes in design, smaller batches, and quality improvements in materials,
craftsmanship and timely deliveries to retail outlets constitute common reasons for
reshoring to those stated in the generic rationale of returning production to the homeland.
Moreover, a balanced sourcing strategy also prevails in managerial decisions as there are
always trade-offs between lower costs and quality, lower costs and supply chain
uncertainty, and/or lower costs and speed to market, among other considerations.

4. THEORETICAL FRAMEWORK: GLOBAL PRODUCTION NETWORKS

Globalization ushered the world into a new era of competition as production was
massively outsourced to developing countries thus reconfiguring trade patterns and
production on a global scale. This global shift has also led to the restructuring of
companies as they needed to configure new formations in order to organize their activities
(Gereffi and Lee, 2012; Dicken, 2015).
Global production networks (GPNs) can explain in a more cohesive manner how the
global economy functions as the transnational network is critical in its geographical
complexity, for it reflects the relational and also the structural nature of how production,
distribution and consumption is organized. In this GPNs exist, actors engage and shape
the geographies of political, cultural and social conditions as well as the transformation
process of production. This means that GPNs are not confined only to the “free market”
relationship of buyers and suppliers but extend their scope by integrating other
influencing actors into the equation. This occurs because any market economy is
constructed socially as well as commercially; therefore, in this market configuration
social forces and the state can play an influential role (Barrientos, 2013; Coe, Dicken and
Hess, 2008). In this dense circuit configuration GPNs integrate all sets of mediators and
links involved in a profound relationality mode within the production, distribution,
consumption network (Coe, Dicken and Hess, 2008, p. 273). The net-chain is according
to Coe, Dicken and Hess (2008) the prevailing framework which is comprised of a set of
networks in horizontal and vertical configurations. Horizontal connections refer to
relations among actors on the same layer of transactions, while vertical connections refer
to commercial relations among firms on different layers. These horizontal and vertical
net-chains can be either short or long as this will depend on the number of companies
involved in the vertical configuration (production/distribution sequences) and also the
horizontal actors involvement (states, trade agreements, civic society associations,
environmental factors, labor issues). The interdependent nature of networks is of
fundamental importance as it impacts governance and power factors within the network.
Power asymmetries in GPNs as in all bargaining situations do exist but it is not always
the bigger player who wields power with respect to the weaker one. Of course, companies
struggle for resources and positioning in the network against weaker commodity
competitors; however, companies evolve over time depending on contingent
circumstances prevailing in the network. This mobility may facilitate upgrading to a more
elevated status in a network.

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 Vertical Commercial Actors

Horizontal Actors
Textile Mills

Trade Agreements Garment Factories

Labor Policies Textile & Apparel

Agents
The State Local Authorities
Fashion Firms

Civic Society Commercial Agents/

Associations
Distributors
Activist Retailers
Organizations

Customers

Figure 2. The Net-Chain Configuration of Global Production Networks

It should be noted that, GPNs do not solely engage with commercial parameters
embedded in firms, as they are also driven horizontally by non-economic agents where
at times either all or parts of them participate (Barrientos, 2013). The role of states,
regional powers such as the EU, civic associations, the World Trade Organization and
various trade agreements, international standards such as the ISO, labor issues and the
environment can exert varying degrees of influence in GPNs. These relationships can be
cordial and cooperative and simultaneously can be conflictual and competitive as
frictions often arise among actors in their struggle for new power arrangements (Dicken,
2015; Barrientos, 2013; Coe, Dicken and Hess, 2008).

5. PERIPHERAL PRODUCTION NETWORKS IN THE EUROPEAN

CONTINENT
Europe’s T&C manufacturing landscape has changed dramatically as Eastern European
countries (following deindustrialization after the collapse of the Soviet bloc in 1989)
were re-inserted rapidly into European production networks as garment assembly
manufacturers for western European brand owners and branded manufacturers. The EU
in its Outward Processing Trade had a profound leverage in manufacturing and trade in
this region. However, after the abolition of the Multi-Fiber Arrangement (MFA) in 2005
and the subsequent wholesale relocation of production to mainly China, Turkey and India,
orders in Eastern European countries (EEC) dropped dramatically, thousands of jobs
were lost, and factories closed, a fact that brought about renewed desperation and poverty

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in the region (Pickles et al, 2006; Pickles and Smith, 2011).
Reform and restructuring was urgently needed and manufacturing firms responded in a
variety of ways to this new reality. Some manufacturers have managed to upgrade their
production capabilities by manufacturing garments of higher complexity such as men’s’
tailoring. Some manufacturers on the more upgraded side of the business have started
sub-contracting assembly operations in other EEC countries such as Albania. Others have
directed their manufacturing capacity into producing low end garments for local markets;
others have opted for full upgrading to brand owner status selling mainly to domestic
markets following the emergence of local middle classes. In some cases, manufacturers
who had connections with buyers in Western Europe have managed to sell full package
services to Western European brand owners.
It must also be noted, that backward linkages, namely fabric and trim suppliers after years
of experience with Western European buying firms, had already reached a level of export
quality. This was triggered by mainly Italian and Greek textile mills which had relocated
part if not all of their production capacity to EEC countries and as a result they had trained
local textile engineers in the production of superior materials (Pickles and Smith, 2011;
Pickles et al, 2006).
Following manufacturing reforms, the EEC countries’ response to the so-called China
price seems to have sustained some production as manufacturers have managed
specialization of their production by serving niche brand owners. According to Pickles
and Smith (2011), there are principally three reasons for this manufacturing resilience. It
can be attributed to the fact that Chinese price competition usually focuses on lower-end
garment production where EEC manufacturers are unable to compete; thus, they have
relinquished production in this clothing section and opted to upgrade to higher
complexity garments. Proximity to the markets especially in the fast fashion sector is
another important factor as retail replenishment needs to be rapidly manufactured and
distributed to Western European retailers. Lastly, the quality and specialization factors
come to the fore especially in tailored garments where fabrics, trims and assembly
operations need to reach certain quality standards (Pickles and Smith, 2011).

6. RESEARCH METHODOLOGY AND METHODS

The authors adopt the philosophical view of Interpretivism inherent in the logic of
interpretation and observation in order to understand the context of the world. This
approach is integral to the qualitative research tradition. Moreover, the researchers’ own
setting can configure their interpretation because they position themselves in the
situational investigation. Both authors’ working experience in the clothing industry as
well as the second author’s experience as a consultant in the clothing sector for
companies seeking alliance partners in the Black Sea region as well as the Balkans was
very helpful as it enabled them to comprehend and analyze the subject in depth. Therefore,
the researchers’ intent is to interpret a pattern of meanings which is configured by the
actors who shape the research content (Creswell, 2009).
Qualitative research methods are employed in this research, because the study aims to
explain the subjective processes and meanings of how individuals or groups take action
or cope in a particular social situation as this is based on the social construction of reality

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(Creswell, 2009). Qualitative methods are deemed more appropriate for this study
because the inherent meanings of reshoring production and sociability of ethical
manufacturing can be difficult subjects to quantify. Therefore, the case study approach is
employed in this study as it explicitly explores managerial thinking, perceptions,
activities and expanding horizons with regards to current strategic moves in the Balkan
region (Yin, 2009). This may provide an in-depth understanding of how
owners/managers perceive the transnational network of companies and how they operate
in this part of the world in terms of all the above mentioned variables ranging from
sustainable practices to garment factory workers’ livelihoods.
Interviews are used as the primary data collection method as they represent rich, in-depth
and relevant information for the study. Interviews allow researchers to explore and
capture important insights of the research through the interviewees’ explanations (Yin,
2009). Unscripted questions with a flexible approach are also used in follow-up interview
sessions, allowing interviewers to capture relevant details within a situation comfortable
for the interviewees (Oppenheim, 1992).
Selection criteria for the case study can be summarized to the fact that the retail brand
owners, after decades of manufacturing in China, decided recently to re-shore some
production in Europe as they were initially convinced by two major parameters. These
included the brand’s retail customers questioning the origin of clothing in relation to the
retail price and other ethical concerns, as well as speed to regional markets.
The interviews were conducted during the summer (July-August) of 2016 in Thessaloniki,
Greece, Sadanski in Bulgaria and Korce in Albania. Interviewees included the retail
brand owners, and the garment factory owners in Bulgaria and Albania as researchers
sought to have a holistic overview on the subject. All interviews were transcribed and
then sent back to the interviewees for clarification and verification as this can enhance
the reliability of this study.
Data analysis according to Yin (2009) includes data examination, categorization and
tabulation. Qualitative data analysis relies heavily on the researchers’ knowledge and
understanding to interpret, analyze and categorize the data in order to make logical
assumptions about the corresponding linkages between the collected data and its
interpretation into the study’s topic. Nevertheless, in order to avoid bias, the researchers
have triangulated data not only from interviews, but also have made use of their personal
observations and secondary sources such as trade documents and current affairs articles
in local and international newspapers.
In the next section the authors discuss the case study and its production arrangements in
two Eastern European countries.

7. CASE STUDY
The case study involves the fashion brand Julia B established in Thessaloniki, Greece in
the early 1970s as ready to wear took center stage in the European fashion industry at the
time. Julia B started as a wholesaler selling its seasonal collections to small independent
retailers and manufacturing small batches of clothing using local contract garment
factories. By 1982, the company’s wholesale operations were multiplied in quantities as
the brand introduced new fashion categories every season. As a result, the three owners

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decided to relocate all production to Hong Kong through a textile agent who was also
starting to produce across the border in China. This wholesale/manufacture formula
lasted until the mid-1990s when the company’s owners decided to convert Julia B into a
retail brand by opening stores.
At present, the brand covers Greece completely with 52 stores nationwide and it has also
extended its retail operations through master franchisors in the Balkan and Black Sea
regions. As of 2016, stores were opened in Bulgaria, Albania, Fyr-Macedonia, Serbia,
Armenia and Georgia bringing the total to approximately 60 stores. The recent
proliferation of stores combined with pressures to drop fresh merchandise on a monthly
basis prompted the owners to rethink their manufacturing strategy. The other reason was
that ordering 6-8 months in advance carries a lot of risk as it is impossible to predict
accurately fashion changes which are instigated continuously throughout the season. This
resulted in unsold merchandise and deep discounts which eroded retail margins.
Following advice from consultancy the company’s owners directed their interests into
producing in EEC countries in close proximity to the Greek headquarters. It was agreed
that the part of the collections which is subject to unpredicted seasonal changes must be
manufactured closer to the markets and in smaller batches, while the remainder which
was of more stable demand as well as being in clothing categories where Eastern
European manufacturers could not easily function, would remain in China. Southern
Bulgaria and Southern Albania were chosen, as in the region a number of manufacturers
could produce smaller batches in a flexible manner for various European retail brands.
It should be noted that these manufacturers had already achieved manufacturing
standards of export quality, paid fair wages to their workers and observed safety
conditions in the garment factories stipulated by the EU as well as the local Labor
Inspectorates. 80% of fabric and trim was sourced mainly from Greece and Italy and the
remaining 20% from Turkey. The company’s owners also wished to respond to customers’
demands in terms of the origin of the clothing ranges as well as adverse market comment
of profiteering from the so-called China price.
Interestingly, the garment manufacturer in Bulgaria was very happy to receive orders as
the factory was running at a 60% capacity. The brand owners supported the Bulgarian
manufacturing plant by purchasing some updated sewing machinery to improve quality
and speed. They also got involved in a joint ownership with the Albanian factory and
instigated a program of training staff partly subsidized by the EU’s Regional
Development Funds. The Albanian factory which was on the verge of closing within a
two year period was renovated, some workers were re-hired, trained, paid fair wages.
Workers were also allowed to make clothing for their family members from cloth
remnants after working hours. The above close knit relationship with the two factories
would have been unthinkable a couple of years earlier and it brought about positive
results. These included the European origin of a larger part of the collections which
helped to reduce adverse comment from customers, as they realized that jobs were being
retained within European borders. Better quality monitoring due to proximity, vast
improvements in market response due to smaller batches of production resulted, thus
responding to actual rather than forecast demand. Lastly, a certain socio-cultural
understanding with neighboring regions was achieved as Julia B’s owners realized that a

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combination of contract manufacturing and vertical integration needs to take into account
an improvement overall in the workers’ lives. The latter had also a reputational advantage
as the company had opened stores in major cities in both countries.
In the following section four constructs identified in the literature and the case study are
discussed.

8. ANALYSIS & DISCUSSION

The four constructs are as follows, transnational production networks, traceability of the
supply chain, productivity of manufacturing resources and labor conditions. It should be
noted that the constructs do not operate independently but they are closely intertwined.

8.1 Transnational Production Networks

The literature on transnational production networks broadly concurs with the case study
(Coe, Dicken and Hess, 2008; Pickles and Smith, 2011). Relational operations prevail
because according to GPNs theory the market economy is socially constructed as well as
commercially, meaning that in this production configuration social forces can play an
influential role (Coe, Dicken and Hess, 2008). This was made clear to the researchers
during the interviews with the Julia B owners who stated that a spirit of cooperation
prevails in their business transactions with manufacturers. Both parties realize that this
is the only way forward, thus, they refrain from power struggles as both understand where
they stand in the supply chain. This partially contradicts the literature which advocates
that competition for resources and positioning in the supply chain features high in power
struggles among brand owners and manufacturers: this socio-cultural affinity is not well
documented in the literature (Gereffi and Lee, 2012, Coe, Dicken and Hess, 2008; Cline,
2013). Moreover, as was revealed in the interviews with both the brand owners and
manufacturers, the EU does play an influential role as Outward Processing Trade
especially in Albania’s case was beneficial for production. Additionally, the EU’s
Regional Development Funds and Coherence Funds supported training programs for all
garment workers in both countries. Support came in the form of financial benefits to
workers for a year as well as for Julia B in the form of subsidies, as the company had to
hire local instructors to train all workers involved in the program. The above confirms
the literature which supports the net-chain argument as commercial actors and the state
are intertwined in transnational production configurations (Coe, Dicken and Hess, 2008).

8.2 Traceability of the Supply Chain

Traceability features high on the agenda of brand owners as they are currently under
pressure from activist organizations and the public to demonstrate ethical production
practices in terms of labor concerns. Civic association’s voice concerns in favor of ethical
fashion, meaning that the provenance of production needs to be closely monitored
(Greenpeace, 2012). This has repercussions for Julia B’s brand owners as their reputation
is put at risk by not conforming to transparent practices. Thus, nearshoring production
features as a high priority in their sourcing decisions and Europe represents one of the
best production locations. Sourcing continues to occur in China for clothing categories
of more stable and hard to find materials. This concurs with the literature on a balanced

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sourcing strategy (Groom and Powley, 2014; Wingard and Connetry, 2014). On the
consumption side, customers are willing to pay a little more for their clothing which can
provide superior quality and durability along with the ethical guarantee. The above were
revealed during the interviews as the company’s owners stated that for them it was not in
reality a matter of compliance with EU regulations or pressure from the public, but it was
rather imperative to instigate these necessary changes as the viability of the business
depended upon them demonstrating transparency of operations. Moreover, Julia B’s
owners stated that operating within Europe meant that companies along the supply chain
of production/distribution needed to cooperate closely because markets, brands, products
and manufacture are common in all European markets so there was no point in being
unethical as this could easily produce a bad reaction with detrimental effects for all
businesses involved (manufacturers-brand owners). The above partially contradicts the
literature which postulates that only unethical practices prevail in the industry (Cline,
2013; Siegle, 2016). The brand owners acknowledged that they could face reputational
damages for unethical practices and they have elected to steer clear from them.

8.3 Productivity of Manufacturing Resources

Sewing machinery which was bought for the garment factories does not necessarily
produce goods faster as productivity did not rise considerably to a noticeable degree.
Sewing machinery rather performed a different role, this of better quality of manufacture.
For example, a new fully automatic buttonholing machine can obviously produce faster
but it can also make better buttonholes which in turn make the garment look more
appealing. The other notion of resource productivity in terms of better production
pertains to the fact that upper middle brands rely heavily on better sewing techniques and
craftsmanship in order to justify higher retail prices. The above partially concurs with the
literature where investments in machinery can enhance the production outcome.
Simultaneously, productivity rises are not necessarily connected to upgraded machinery
especially in slower production techniques as the literature suggests (Martin, 2013)
because sewing craftsmanship requires more time in assembling more complex garments.
Moreover, smaller orders means that frequent retooling is required as higher brands by
nature produce smaller quantities which slows down the speed of production.
As regards economization in materials, manufacturers’ procurement of European fabrics
in agreement with Julia B’s owners, meant that fabrics are more expensive in comparison
with the yarn/fabric and trim supply of the company’s previous engagement with the
Chinese textile agent. In this regard, smaller quantities in high material prices mean that
in the cutting rooms of both garment factories fabric economization is paramount.
Additionally, nearly all fabric remnants, after order deliveries, are given to garment
workers to make their own clothing. Some of them at the time of the authors’ visits were
making children’s wear not as a pastime but to clothe their children.

8.4 Labor Conditions

In terms of labor, factory workers in both manufacturers’ facilities are treated with dignity.
This means that in all factory floors there is enough space for each sewing operator to
conduct his/her work. There is enough ventilation and natural light, and health and safety

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regulations seem to apply in all departments as exits are clearly marked, fire stations are
in place, there are no wires hanging from the ceilings, big posters hang from the walls
reminding all workers of the company’s code of conduct and there is a resident nurse
with a full infirmary room on site. All workers take half hour break for lunch as well as
two 10 minute breaks for coffee/tea in the morning and late afternoon at the company’s
cafeteria. Also the factory floor supervisors turn a blind eye for a couple of cigarette
breaks within working hours. Work starts at 7 in the morning and ends at 4 in the
afternoon unless there is overtime of mainly one hour. This rarely exceeds two hours on
a day and this usually occurs on some Friday evenings as trucks collect all garments for
the Thessaloniki distribution center. Most Saturdays and Sundays all factories are shut,
complying with the forty hour week stipulated by the EU and local Labor Inspectorates,
unless there are last minute orders for delivery to the stores. The above do not represent
demonstration factories as the literature suggests (Cline, 2013) because all production is
carried out on the specific factory locations without contracting out production. Contract
manufacturing to uncertified garment workshops which admittedly forms part of clothing
production in the Balkans does not occur at Julia B as higher quality production cannot
be easily outsourced because it requires specialized machinery and elevated worker skills.
All garment operations are subject to quality controls on a daily basis by quality
controllers from both manufacturers. Despite the fact that Julia B and the allied
manufacturers treat their workers with dignity, the thorny issue of wages rising to living
standards did not feature highly in the discussions during the interviews, with the
exception of highly skilled pattern cutters, garment technicians and other skilled positions.
The owners stated that they fully comply with labor laws in both countries regarding
wages, overtime and holidays. However, wages were not upgraded to living wages
despite higher prices paid for production by the brand owners. This, as it was explained
in the interviews, was due to the fact that profit margins were thin after machinery
amortization as well as due to the higher prices of fabric/trim coming mostly from Europe.
Monetarily speaking, workers were not better off but they enjoyed some non-monetary
perks, such as Christmas and Easter food packages, Sunday excursions every two months
with all expenses paid for by Julia B and the manufacturers, access to free fabric remnants
to make their own clothing after working hours, one free refreshment in the factories’
cafeterias daily and first instance private medical cover. The above concurs with the
literature as wages in Eastern Europe are not a lot higher in comparison to wages paid in
developing countries and this applies especially for women who in the case study form
approximately 80% of all employees (Rankin, 2014; Cline, 2013).

9. CONCLUDING COMMENTS AND PERSPECTIVES

Production networks operating at Europe’s fringes demonstrate a renewed dynamism by
collaborating closer with brand owners. In this relational scheme, a form of socio-cultural
solidarity prevails as all parties acknowledge that interdependences are paramount factors
for success. Thus, despite power asymmetries all members of the supply chain understand
their position as a spirit of cooperation permeates all operations. Civic society’s pressure
also seems to work as nobody can risk reputational damages. The EU’s Regional and
Coherence funds are commendable as they play a pivotal role by facilitating sustainable

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development practices and simultaneously retaining jobs in an admittedly sensitive
industrial sector. Therefore, the net-chain production-distribution-consumption
configuration together with the state’s influence can be confirmed as all players in the
network can influence its outcome.
In terms of transparency, pressure coming from customers as well as acknowledgement
on the brand owners’ part that it is important to prove the provenance of clothing in
assembly as well as fabric procurement. The fabrics coming from European mills carry
all necessary certification but this was less clear in relation to fabric sourcing from China.
Another important parameter confirmed by the literature and the case study is that brands
need to exercise a balanced sourcing strategy as not every clothing category can be
sourced from a single region, so it is advisable to seek other manufacturing locations and
be able to monitor sustainable practices whenever possible. Overall, it seems that
sustainable practices form the new imperative in fashion at present and will continue to
do so in the future.
Perhaps the most significant contribution of the study is that speed to market is
acknowledged as one of the major variables of reshoring production in the literature;
however, the owners of the garment factories stated that higher quality clothing requires
a degree of craftsmanship and specialized knowledge which slows down production as
well as with frequent machinery retooling due to smaller production batches. In reality,
speed to market refers to proximity but simultaneously higher complexity in assembly
refers to slower production methods advocated by the slow fashion movement. So the
duality of speed and slowness merit further investigation in future research.
Last but not least, the thorny issue of workers’ living wages as opposed to wages
stipulated by Labor Inspectorates seems to remain unsolved as in the case study the
owners preferred to offer other perks instead of raising salaries to decent living standards.
On balance, the authors recommend that upgrading to the elevated status of
manufacturing specialized clothing for niche fashion brands can be a viable strategy at
least within its European context. Reshoring and sustainable development are compatible
tactics for manufacturing/distribution and this is also instigated by the EU’s regional
policies. For manufacturing companies and brand owners who wish to survive in this
new reality it is perhaps one of the major routes to competitiveness.

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Barrientos, S. (2013). Corporate purchasing practices in global production networks: a
socially contested terrain. Geoforum 44: 44-51.
Bair, J., Dickson, M., & Miller, D. (2014). Workers' rights and labor compliance in global
supply chains, is a social label the answer? Routledge, Taylor & Francis Group, Oxen.
Cernat, L., & Pajot, M. (2012). Assembled in Europe- the role of processing trade in EU
export performance. The European Commission, Brussels.
Cline, E. (2013). Overdressed: the Shockingly High Cost of Cheap Fashion. Portfolio,
Penguin Books, New York.
Coe, N. M., Dicken, P., & Hess, M. (2008). Global production networks: realizing the
potential. Journal of Economic Geography 8: 271-295.
Creswell, J. W. (2009). Research design: qualitative, quantitative and mixed methods

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approaches (3rd ed.). Sage Publications Inc., California.
De Brito, M., Carbone, V., & Blanquart, M. (2008). Towards a sustainable fashion retail
supply chain in Europe: organization and performance. International Journal of
Production Economics 114: 534-553.
Dicken, P. (2003). Global Shift (4th ed.). Guilford Press, New York.
Ellram, L., Tate, W., & Peterson, K. (2013). Offshoring and reshoring: An update on the
manufacturing location decision. Journal of Supply Chain Management 49(2): 14-22.
European Parliamentary Research Service (2014). Reshoring of EU manufacturing.
Strasbourg European Parliamentary Research Service.
http://www.europarl.europa.eu/EPRS/140791REV1-Reshoring-of-EU-manufacturing-
FINAL.pdf
Fletcher, K. (2008). Sustainable fashion & textiles: design journeys. Earthscan, London.
Friedman, V. (2010, February 5th). Sustainable fashion: what does green mean? Financial
Times.
Gereffi, G., & Lee, J. (2012). Why the world suddenly cares about global supply chains.
Journal of Supply Chain Management 48(3): 24-32.
Greenpeace International (2012). Toxic threads: the big fashion stitch up. Greenpeace
International, Amsterdam.
Groom, B., & Powley, T. (2014, March 3). Reshoring driven by quality, not costs, say
UK manufacturers. Financial Times.
Luginbühl, C., & Musiolek, B. (2014). Stitched up: poverty wages for garment workers
in Eastern Europe and Turkey. Clean Clothes Campaign.
http://digitalcommons.ilr.cornell.edu/cgi/viewcontent.cgi?article=2842&context=global
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Martin, M. (2013). Creating sustainable apparel value chains: a primer on industry
transformation. Impact Economy, Geneva.
Oppenheim, A. (1992). Questionnaire design, interviewing and attitude measurement (1st
ed.). Cassell Wellington House, New York.
Pickles, J., & Smith, A. (2011). Delocalization and persistence in the European clothing
industry: the reconfiguration of trade and production networks. Regional Studies, 45(2):
167-185.
Pickles, J., Smith, A., Buck, M., Roukova, P., & Begg, R. (2006). Upgrading, changing
competitive pressures, and diverse practices in the East and Central European apparel
industry. Environment and Planning A, 38(12): 2305-2324.
Rankin, J. (2014). Fashion brands violate labour laws in Eastern Europe, NGO report
finds. The Guardian https://www.theguardian.com/business/2014/jun/10/fashion-brands-
violate-labour-laws-eastern-europe.
Remy, N., Speelman, E., & Swartz, S. (2016). Style that's sustainable: a new fast-fashion
formula. McKinsey & Company, Sustainability & Resource Productivity.
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Siegle, L. (2011, 8th May). Why Fast Fashion is Slow Death for the Planet. The Observer,
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Development of Textile Based Strain Sensor from Polypyrrole
Abdul Malik Rehan Abbasi
Department of Textile Engineering, BUITEMS, Quetta, Pakistan
Email: rehan_abbaci@hotmail.com
ABSTRACT
The conducting polymers are polyconjugated, which possess electronic properties of metals,
while retaining the mechanical properties and processability of conventional polymers.
Conductive polymers can only withstand limited strain before breaking and cannot perform
well in evaluating large strains. The aim of this study was to develop a low cost, small to large
strain sensor using Polypyrrole and Latex/Polyamide 6 yarn. The stretchable yarn was chosen
as the substrate due to its excellent resilience and elasticity. Polypyrrole was coated as thin
film onto the substrate by means of vapour deposition technique. The response of resistance
of the samples on 2% deformation and relaxation during 40 cycles was analysed. The
sensitivity or the change in resistance per unit deformation was used as a tool to figure out the
suitability of strain sensor. The high resistive sample gave better sensitivity as well as
uniformity as compared to low resistive sample which made it suitable to use as a strain
sensor.
Keywords: Latex/Polyamide 6 yarn, Polypyrrole, Vapour Deposition Technique

1. INTRODUCTION
Electrically conducting polymer films can only withstand limited strain before breaking and
cannot perform well in evaluating large strains (Murray, 1998). To overcome this problem,
substrates were employed to provide the necessary support and the surface for conducting
polymer film deposition. Generally, fabricating a strain sensor using this approach means that
the mechanical properties are highly attributed to the substrate while the conducting polymer
introduces the electrical conductivity. This practice is commonly found in the research field
of smart textiles which are conductive fabrics produced by coating conducting polymers onto
commercial fabrics such as nylon, polyester and Lycra (Li et al. 2005)(Xue et al. 2007)(Wu
et al. 2005)(Molina 2008). Although excellent results have been demonstrated with smart
textiles using conducting polymers, the intended applications are mainly aimed at enhancing
the usability of fabric beyond its current use as a protective layer. As a general purpose strain
sensor, the substrate requires having some degree of rigidity and fabrics are not an ideal
material due to its soft structure. Furthermore, repetitive strain can cause permanent
elongation on individual fibres where the strain may not be distributed equally. This can lead
to individual fibres having different mechanical properties that will affect the strain sensing
performance. The proposed solution is to replace fabric with Latex/PA6 stretchable yarn,
which has good combination of rigidity and elasticity. One of the studies has succeeded in
fabricating a strain sensor using PPy and natural rubber substrate where PPy powder is
embedded into the structure of the rubber directly (Bunsomsit et al. 2002). Compared to the
coating methods, that approach requires knowledge of rubber manufacture as well as an access
to the equipment to produce rubber with consistent mechanical properties.
This work is aimed at developing a low cost, small to large strain sensor using PPy and
Latex/PA6. This stretchable yarn was chosen as the substrate due to its excellent resilience
and elasticity. Commercial Latex/PA6 strip was purchased and used to produce the strain

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sensor. PPy as thin film was coated onto this substrate by means of vapour phase
polymerisation technique that provides a good adhesion between the two components of the
strain sensing element.
2. MATERIALS
2.1.Latex/polyamide-6
For developing the strain sensor, PA6 wrapped Latex yarn produced by PEGA® Czech
Republic, has been selected as a substrate for the deposition of PPy. The microscopic image
is shown in Figure 1 and the specifications of this yarn are described in Table 1.
Table 1: The particulars of PA6 wrapped latex yarn

Properties Index
Diameter of Latex [mm] 0.6
(*) Effective diameter of whole thread [mm] 0.68
Linear density of Latex [tex] 36.8
Fineness of PA6 [tex] 22x3
No. of turns of PA6 around Latex [cm-1] 12
Composition PA6 42
[%] Elastodiene 58
• Yarn packing density was assumed as μ = 0.525 (Militky et al. 2004)

Figure 1. The microscopic image of Latex wrapped with PA6

2.2.Chemicals
Pyrrole is available in the market with different synonyms such as 1H-Pyrrole,
Divinylenimine, Imidole, Azole, Monopyrrole, 1-Aza-2,4-cyclopentadiene. For this study
Pyrrole 98% was received from Alfa Aesar® and was used after distillation to remove
colouring impurities.
Anhydrous Iron(III) Chloride 97% was ordered from Sigma-Aldrich® and was used as
received. It has molar mass 162.2 g.mol-1 and 2.898 g.cm-3 density. Tetraethylammonium p-
toluenesulfonate also called tosylate (TsO-) was obtained from Aldrich and was used as
received.

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3. METHODOLOGY
3.1. Sample preparation
An aqueous liquor bath was prepared using 2:1 molar ratio of FeCl3 and TsO-. This molar
ratio between oxidant and dopant was optimized by the series of experiments in our previous
work (Abbasi et al. 2013). As FeCl3 follows exothermic reaction when comes in contact with
water, ice was used to reduce the temperature of the solution around 20°C. The yarn sample
was immersed in bath for 1 min followed by squeezing at 70% pickup (maximum pickup by
yarn) with the help of pneumatic squeezing rollers. Sample was then placed with the help of
holders in a glass desiccator filled with pyrrole vapours immediately after padding and
squeezing. The temperature of desiccator was kept at 20±2°C and sample was remained into
it for 6 h under ambient atmospheric pressure. Sample was then taken out and washed with
ethanol in order to stop polymerization and subsequently with plenty of distilled water for
several times to remove biproducts and unreacted chemicals. Finally, sample was dried in air
at 20±2°C for 24 h. Three different samples were prepared in exactly the same way by varying
the concentration of FeCl3 and TsO- as mentioned in the Table 2.
Table 2: Recipes for the preparation of PPy coated Latex/PA6 yarn samples.
Sample label Iron Chloride Tosylate
Latex/PA6 [mol/L] [mol/L]
SY1 2.0 1.0
SY2 0.6 0.3
SY3 0.1 0.05

3.2. Measurement of electrical resistivity of PPy coated Latex/PA6 yarn samples

With the intention of measuring electrical resistance R of PPy coated Latex/PA6 samples,
stainless steel clamps were used to hold the sample together with connecting wires and a
digital multimeter. The electrical resistivity ρ of the yarn sample was calculated from the
Equation 1, by knowing average cross-sectional area of the yarn sample “a” and the length of
the sample “L” between two measuring electrodes A and B.
𝑎
𝜌=𝑅
𝐿
With the objective of determining the dependence of electrical resistance on length of a
sample, the resistance was measured by varying the distance from 5cm to 90cm between
measuring electrodes.
3.3. Measurement of sensitivity of PPy coated Latex/PA6 yarn samples
With the objective of characterizing sensitivity of PPy coated Latex/PA6 yarn samples against
deformation, all the samples from Table 2 were subjected to cyclic loading by using tensile
testing machine Labtest from LaborTech® Ltd Czech Republic. The cycle was set for 2%
strain at the jaw moving speed of 100mm/min with a rest of 1 second at relaxed or initial
position to synchronize normal human breathing rhythm.
One set of measurement includes 40 cycles, therefore in this way 5 sets of readings were
recorded and sensitivity 𝑑𝑅⁄𝑑𝜀 of the yarn sample was monitored. Here dR is the average
change in resistance (R1-Ro) of the specimen calculated from 5 sets of 40 cycles during

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extension of 2% and dε is the change in length [mm]. R1 is the resistance of specimen at 2mm
extension whereas Ro is the resistance at relaxation or initial point.
4. RESULTS AND DISCUSSION
4.1. SEM micrographs
The SEM micrographs were taken from TESCAN® VEGA and corresponding to sample SY3
is depicted in Figure 2. It can be perceived from the figure that by vapour deposition
technique, each individual fibre is covered by PPy thoroughly, even though the structure of
Latex/PA6 stretchable yarn is very compact as shown in Figure 1.

Figure 2: SEM micrographs of PPy coated Latex/PA6 yarn sample SY3 (a) low magnification (b)
high magnification

4.2.Linear dependence of resistance on length

In order to determine the dependence of resistance on the length of PPy coated Latex/PA6
yarn, sample was clamped between two stainless steel clamp type electrode and resistance
was measured by varying the distance between them as described earlier. It was found that
resistance of PPy coated Latex/PA6 stretchable yarn is a linearly increasing function of the
distance between the electrodes holding the yarn as shown in Figure 3. By the least squares
regression for this model this relationship can be expressed as:
R=ZD+r
where, R is the resistance [kΩ] of PPy coated Latex/P!6 yarn sample, D the distance between
measuring electrodes and r the resistance of the electrodes found to be 0.0001kΩ approx. in
this work. However the slope Z is the directly proportional to the resistivity ρ in [kΩ.cm] of
the PPy coated Latex/PA6 yarn samples for this experiment and can be calculated as:
Z=275.63∙ρ-0.0769

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 Figure 3: Dependence of electrical resistance of PPy coated Latex/PA6 yarn samples on length

4.3. Sensitivity of strain sensor against cyclic loading

The Latex/PA6 stretchable yarn samples were coated by PPy through vapour deposition
technique and each PPy coated sample was subjected to cyclic loading for 40 cycles. The
response of resistance of the samples on 2% deformation and relaxation during 40 cycles are
plotted in Figure 4.

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 Figure 4: Response of PPy coated Latex/PA6 samples at 2% deformation for 40 cycles

From the Figure 4 it can be observed that SY1 gives almost equal response dR against
deformation in terms of magnitude but this response is not consistent with the number of
cycles. The SY2 gives neither an equal response against deformation (decreases with number
of cycles) nor the consistency of the response. Whereas SY3 is the best among all the samples
and it gives not only an equal response upon deformation but also the level of consistency of
the response after each cycle is outstanding. The average response in terms of change in
resistance against deformation has been calculated from 40 cycles and named as sensitivity
𝑑𝑅⁄ of each sample. The sensitivity levels of all PPy coated Latex/PA6 samples are shown
𝑑𝜀
in Figure 5. Although SY3 has the highest resistivity among all three samples under study,
however it outperformed SY1
and SY2 in terms of response against small extension. The sample SY2 has been found as the
worst in terms of sensitivity and its deviation in the results. The standard deviations of the
specimens were calculated as 0.182, 0.315 and 4.49 [kΩ.cm\ for SY1, SY2 and SY3
respectively.
Although SY3 has the highest resistivity among all three samples under study, however it
outperformed SY1 and SY2 in terms of response against small extension. The sample SY2
has been found as the worst in terms of sensitivity and its deviation in the results. The standard
deviations of the specimens were calculated as 0.182, 0.315 and 4.49 [kΩ.cm\ for SY1, SY2
and SY3 respectively.

Figure 5: Dependence of sensitivity of the strain sensor on longitudinal deformation

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5. CONCLUSION
PPy was coated on PA6 wrapped Latex yarn samples through vapour phase polymerization
by varying concentration of oxidant and dopant thus samples were varied in resistivity levels.
It was found that resistance of all the samples follow exactly a linear function of length and
hence follow Ohm’s law.
The sensitivity or the change in resistance per unit deformation is a useful tool to figure the
suitability of the strain sensor out. The high resistive sample gives best sensitivity as well as
uniformity or the consistency of the response against small cyclic deformation (2%) whereas
low resistive samples fail to give the equal and uniform response. Therefore, it is suggested
that this product can be used to monitor human body movements even for very small
deformations such as breathing.
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Mesoscale Finite Element Analysis Framework of 3D Woven Fabric Tensile
S. A. Ghani a, B. Zahid b, M.F. Yahya a,*
a
Textile Research Group, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450
Shah Alam, Selangor, Malaysia
b
Textile Engineering Department, NED University of Engineering & Technology, University
Road, Karachi,75270, Pakistan
*
Corresponding author: mfy@salam.uitm.edu.my

ABSTRACT
Mesoscale modelling approach has shown close simulation approximations of woven fabric tensile
performance. The main purpose of the work is to develop understanding of geometrical model
development, finite element analysis procedure and to compare the differences of 2D and 3D woven
fabric uniaxial tensile stress-strain. 3D woven fabric structures selected for the work is three-layer
orthogonal woven fabrics. The woven structure will have 2 through-thickness warps, 4 non-crimps
warp and 6 wefts. Through-thickness warp yarn will apply plain 1/1 weave structure for stitching all
weft layers and non-crimps weft yarn together. Woven geometric models were developed with pre-
processor program at detail yarn configurations. Simulation results showed that 3D orthogonal woven
fabric had a better tensile response than its 2D woven fabric structures.
Keywords: 3D, orthogonal woven, uniaxial tensile, weave unit cell, finite element analysis

1. INTRODUCTION
Complex woven textiles have many versatile characteristics that enabled them to infiltrate
technical textiles application, particularly automotive, medical textile, sports and leisure.
Engineers and scientists have realised that complex woven, particularly 3D fabrics, with
reinforcement built into the longitudinal, transverse and thickness axes, offer strong,
lightweight and mouldable material that can be manufactured with specific strength
requirement using high performance fibres. 2D woven structure will provide in-plane
stiffness, compression and strength in both warp and weft directions, but poor in interlaminar
performance [1]–[3]. In addition to that, 2D laminated is difficult to be mould for complex
shape. Higher manufacturing cost is also anticipated since 2D laminates need to be cut during
fabrication process [1]. 3D fabric such as angle interlock and orthogonal weaves will provide
stiffness not only in-plane direction, but also in through-thickness or in x-y-z directions [4].
The presence of through thickness reinforcement in z-direction also resulted in higher
delamination resistance for 3D woven fabric [1], [5]–[8]. 3D woven fabric becomes serious
candidates for impact resistance and energy absorbent composites [9]–[12].

2. RESEARCH BACKGROUND
3D woven fabric properties are highly correlated with crimp, non-crimp and through thickness
yarn. Crimp is often associated with weave structure. The higher number of interlacing, then
the higher number of crimps would be. Plain weave will have the highest number of crimps
compared to twill and satin weave. Crimps presence in the woven fabric will allow greater
non-linear rate on a tensile extensional curve. In view to this, Yang [2] reported that, crimp
density in the orthogonal weave is mainly governed by vertical segment density of binder
warp yarn and weft density, which determines the curve shape of load extension at low strain

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region. Similarly, Whitcomb conducted research to understand the waviness or crimp effect
to woven composites. The work developed a 3-dimensional model to evaluate the waviness
properties of plain, twill and satin weaves. The work highlighted that waviness properties are
also depended to weaves. It was reported that in-plane modulus E1 is strongly responded to
crimp change [13].
The non-crimp fabric is produced by minimizing interlacing sequence in the woven structure.
The orthogonal fabric is an example of non-crimp fabric. In the structure, the fabric is bonded
together when warp yarn performed stitching from top to bottom fabric layers. At the same
time, additional “straight” yarns known as warp fillers and weft fillers are also introduced in
the structure to increase fabric layers and thickness. Gu worked on tensile properties for
various 3D woven fabric, had found that, yarn bending behaviour is a major factor when
considering strength of the composites. Stronger composites are attributed to straight filament
arrangement or reduce bending effect as much as possible [14]. Additionally, Adanur
reported woven fabric modulus can be increased by reducing crimp in loading direction and
crimp interchange in transverse direction with consideration of exploiting higher yarn
modulus [15].
Many works reported that 3D woven fabric posse’s high delamination resistance, due to the
presence of through thickness yarn or sometimes referred to as z-binder [16], [17]. Different
fabric layers are bonded together, enhancing structural toughness and integrity during loading
deformation cycle.
The ability of 3D weaving to produce near net shape can greatly reduce the cost of the
component by reducing material wastage, the need for machining and joining and the amount
of material handled during lay-up. In terms of moudability, 3D woven fabric can be moulded
in several shapes to fit its new technical application. For the same reason, mouldability will
prevent inherent cut and sew process, which would reduce strength due to destruction in fibre
continuity. For example, lightweight aircraft seat can be made from moulded 3D textile
reinforcement to form specific shapes without wrinkles [18]. Another application is as
military helmets, where a single piece of fabric is used as a precursor for protective reason.
Chen highlights that, mouldability of angle-interlock fabrics is closely related to fabric
density, shear rigidity and number of weft layers [19]. Additionally, most 3D structures fabrics
can be produced using conventional dobby and jacquard looms. This allows immediate
production and product availability with competitive product cost.
3D woven fabrics are also reported to have several properties drawbacks. One of the main
drawbacks of 3D weaving is the inability of current looms to produce fabrics that contain in-
plane yarn other than 0 and 90°. The fabric is considered too anisotropic. This in turn leads to
poor shear and torsion performance. Mouritz highlights that, if 2D and 3D has similar
stiffness, 3D fabric will have lower compression strength at 15-20%. This is mainly due to
high in-plane alteration by binder yarn [20]. Also, due to limited databases, it is difficult to
evaluate the lifetime performance of 3D woven fabric in actual application. Failure
mechanism of 3D fabric not extensively characterized. Many works on compression, tension,
flexure and fatigue properties are made on carbon-epoxy composites [20]. The third drawback
is high weaving distortion could cause difficulty to achieve the idealized 3D woven structure.
In fact, there is a limited publication deal on loom control system for reducing in-plane yarn
distortion for 3D fabric[1]. In view of the situation, Clarks investigated the effect of 3D

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orthogonal weaving process to fibre damage [34]. The work was conducted due to concern
on extensive shedding operation might damage the fibre. The fabrics were woven into the
orthogonal structure by using 300 tex warp, 1200 tex weft and 68 tex z-binder yarn of E-glass
yarns. Warp and through thickness yarn were taken from the loom at different weaving stages
to examine fibre damage level and its respective residual tensile strength. It was concluded
that, extensive yarn movement during shedding had caused z-binder yarn to reduce its strength
about 50% [21].

3. RESEARCH METHODOLOGY
3.1 Geometry model development
Warp, weft and non-crimp yarns geometrical models will have a lenticular cross section.
Based on experimental stereomicroscope done during first year, yarn width and thickness are
measured as 2.41 mm and 0.35 mm, respectively. With the value, yarn aspect ratio is
calculated from yarn width and thickness to be 6.8. For computer aided design work in
ABAQUS pre-processor, equivalent yarn aspect ratio is adopted for yarn geometrical model
from 0.4 mm width and 0.0588 mm thickness.

3.2 Yarn Path

Yarn path geometry defined should able to accommodate yarn movement in the z-direction
for packing all weft yarn layers. To design efficient warp yarn path movement in a through-
thickness direction, twelve lenticular shape geometries are prepared to represent weft and non-
crimp warp. Geometrical notation to represent yarn path is defined in the following equations
1 to 4.

1 1
Structural length, l = p + w + p + w + p = 1.5 p + 2w Equation 1
2 2

Yarn spacing, p = t Equation 2

Through thickness yarn path, z = 5t
Equation 3
Bending zone, c = 0.5587 x2  0.0294  y
Equation 4
Yarn bending in zone c is calculated from a polynomial function ax 2  bx  c  y of lenticular
shape derived of three distinct coordinates, namely (0.0294,0), (-0.2294,0) and (0, 0.2294).
By plugging x=0 and y=0.0294 in the polynomial function, the value of c can be determined.
Later, a and b values can be found by simultaneously solving two polynomial equations of
two remaining sets of coordinates. However, for both non-crimp warp and weft yarn, the value
of c and z is zero, since no interlacing effect is considered. Since both of these yarns are
straight, yarn path equation is simplified according to the following equation 5 and 6. The
following Figure 1 and Figure 2 described non-crimp warp and weft yarn paths. The figures
also highlighted the Wnc, w, p and Wf notations in detail.

Non-crimp warp path, Wnc = 2w + p Equation 5

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 Weft path length, Wf = 4w Equation 6

Figure 1: Non-crimp warp path Figure 2: Weft yarn path

3.3 Yarn linear density consideration

Another important issue to be considered is to incorporate yarn linear density effect in the
model. Yarn linear density not only influenced fabric fineness or coarseness but also its
mechanical properties such as tensile. An approach has been made to convert yarn linear
density in Tex into fabric density in gm cm-3. An individual yarn mass (gm) can be determined
by measuring yarn model lengths and using tex definition, i.e grams in 1000 meters. Later,
yarn and fabric density are known by determining ratios between yarn mass (gm) and yarn
volume (cm-3). Fabric or yarn density should be the same at 1.44 g cm-3, regardless the
dimension size. The calculated fabric density is 1.423 g cm-3, which is closed to yarn density
adopted in the research.

3.4 Material definition

Equivalent material properties are applied to through-thickness warp, non-crimp warp and
weft yarns in a 3D orthogonal woven. Yarns in the 3D orthogonal woven fabric will be
assigned isotropic behaviour at 19,000 MPa, Poisson ratio 0.37 and density 1.44 g cm-3.
Additional plastic behaviour is given to the yarn to acknowledge yarn behaviour changes from
elastic to plastic region. Yarn plastic behaviour is determined from its yarn uniaxial tensile
test result and shown in Table 1.

Table 1: Yarn plastic property

Nominal Nominal True True Plastic

Stress (Pa) strain Stress (Pa) strain strain
390000 0.024 399360 399.36 0.0000000
420000 0.026 430920 430.92 0.0030413
460000 0.029 473340 473.34 0.0037337

3.5 Load, boundary condition and mesh

Through thickness and non-crimp warp are assigned with “encastre” type boundary condition
at boundary condition zone. Warp yarns are restrained to move in lengthwise or rotational
wise. At the same time, uniaxial force is the applied in loading zone at 844 MPa per yarn.
The force is based on 5000 N load imposed during tension test on 6 warp yarns. The approach
is necessary to establish uniaxial yarn tension effect for analysis. Figure 3 outlines boundary
condition and the load applied in 3D orthogonal woven fabric. Yarn interactions in 3D

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orthogonal woven fabric are defined to have an explicit general contact at 0.2 coefficients.
This method will acknowledge yarn mobility in the 3D structure and not completely fused as
in the case of 2D woven fabrics. Many literatures have indicated 3D woven fabrics to have
lower shear due to the presence of through thickness yarn [22], [23]. Tetrahedron element has
been selected for meshing yarns prior to finite element analysis to commence. Tetrahedron
element is adopted as it allows mesh formation for nonlinear geometrical set-up. Total
elements established from the procedure are 46,456. More elements are seeded in weft yarn
because of additional length it has compared to through-thickness warp and non-crimp warp.
The following Figure 4 illustrates 3D orthogonal woven fabric after meshing procedure and
Table 2 presented mesh for each component in the model.

Figure 3: Loading and boundary Figure 4: mesh

condition

Table 2: Mesh breakdown

Mesh per Number Total
yarn of yarns mesh
Through thickness warp 4165 2 8330
Non-crimp warp 2417 4 9668
Weft 4743 6 28458
Total mesh 46456

4. RESULTS
4.1 Stress-strain results
Simulation results of 3D orthogonal woven fabric model and 2D woven fabric is presented
together for comparison in Figure 5. It is very clear that 3D orthogonal woven fabric showed
superior stress-strain performance compared to plain (PW), twill (TW) and satin (SW) woven
fabric models. 3D orthogonal woven fabric reported highest 76 MPa stress, which is twice
than SW at 2.2% strain. Within equivalent strain, PW the reported lowest stress at 16 MPa,
followed by TW at 25 MPa and SW at 38 MPa. Additionally, 3D woven fabric has continued
to report stress increment beyond 3% strain, while all 2D woven fabrics have started to yield
constant or declining stress. Non-crimp yarn presence in 3D woven fabric has drastically
improved its uniaxial tensile behaviour. Less crimp in woven fabric structure would assist in
further load bearing capacity, leading to higher stress-strain results. This is consistent with

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finding made by other researchers [3], [24], [25]. The presence of non-crimp yarn in 3D
woven fabric would promote higher and linear stress-strain curve as compared to the non-
linear behaviour of 2D woven fabric models. This finding is in tandem with following Figure
6 that presented higher stress concentration to occur more in non-crimp yarn compared to
through-thickness warp yarn.

Figure 5: 3D vs 2D woven fabric stress Figure 0 : Stress distribution in the

strain comparison model

5. CONCLUSIONS
Experimental and finite element analysis of yarn and woven fabrics for uniaxial tensile of
3D orthogonal woven fabrics were reviewed and validated, by using isotropic elastic-plastic
material properties. Non-crimp yarn in 3D orthogonal woven fabric would assist higher
uniaxial tensile performance. The non-crimp yarn has fewer built-in stresses as compared to
its respective crimp yarns, and responded immediately to uniaxial tensile. The finding is
consistent with yarn and satin woven fabric uniaxial tensile test. The simulation allowed
stress distribution during uniaxial tensile and allow better selection of load bearing yarn for
use.

REFERENCES
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Applications for Advanced Three-Dimensional Fibre Textile Composites,” Compos. Part A
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[5] S. Z. Sheng and S. V Hoa, “Modeling of 3D angle interlock woven fabric
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no. 12, pp. 3967–3984, 1994.
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[14] H. Gu, “Tensile Behaviours of Woven Fabrics and Laminates,” School of textiles and
Clothing, Tianjin Polytechnic University, Tianjin, 2005.
[15] S. Adanur and T. Liao, “3D Modeling of Textile Composite Preforms,” Compos. Part
B, vol. 29B, pp. 787–793, 1998.
[16] W. Hufenbach, A. Hornig, M. Gude, R. Böhm, and F. Zahneisen, “Influence of
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tensile failure with mode I energy release rates in carbon fibre textile composites,” Mater.
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[17] F. M. Z. Nasrun, M. F. Yahya, S. A. Ghani, and M. R. Ahmad, “Effect of weft
density and yarn crimps towards tensile strength of 3D angle interlock woven fabric,” AIP
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[22] H. Talebi, S. V Wong, and A. M. S. Hamouda, “Finite element evaluation of
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Composites,” Knitted fabric composites. pp. 181–191, 1999.

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Study on Luminance research of light-emitting fabrics made by POF
Zhili Zhong, Ruoxing Shi, Jia Wan, Xiao Zhang, Chen Lv
College of Textile, Tianjin Polytechnic University, Tianjin, China
*
Corresponding author: shiruoxing11@163.com; zhongzhili@tjpu.edu.cn

ABSTRACT
By principles of the transport and divergent light of optical fiber, the PMMA / Fluorine polymer
resin optical fiber was interleaved with cotton or polyester monofilament. Then, they were treated
by the cluster with a diameter of 5mm high brightness white led lights as a light source, and
coupling connection with light was made to form POF light-emitting fabric. To discuss the influence
of various parameters of POF light-emitting fabric structure on the brightness, a multiple regression
model was applied to optimize the brightness of POF light-emitting fabric, and the color of light
emitting portion. The POF light-emitting fabrics were tested by LumiCam 1300 imaging photometer.
The results showed that the fabric structure design parameters, fabric structure parameters, weft
coverage and other parameters have a very important influence on the brightness of the light-
emitting polymer fiber fabric. The best polymer POF fabric structure parameters were found to be:
Warp density is 360m root/ 10cm, weft density is 200 / 10cm, the number of yarns of fabric weave
cycle is 8, when n is 3, the predicted brightness is 10.813 cd/m2; The POF fabric has the uneven
brightness problem; POF light-emitting fabric has the same luminous colors with light source and the
fabric overall color is even when the fabric is light-emitting.
Keywords: Polymer optical fiber; POF light-emitting fabric; fabric structure
parameters; weft coverage

1. INTRODUCTION
Polymer optical fiber (POF) refers to a kind of conducting optical power transmission line
which was used of polymer material or an organic material. It has some advantages, such as
good flexibility, good bending performance, good wearability performance, low price and
so on. At present, more and more domestic scholars pay attention to POF so as to the study
on POF has been greatly improved in our country. The polymer fiber can be woven to
polymer fiber fabric. This fabric has good flexibility, light weight, excellent wearability, the
long-lasting use security, easy link with light source. Currently, there are three methods to
make luminous fabric: Firstly, the use of photoluminescent material. Secondly, the use of a
light-emitting diodes. Thirdly, the use of POF.
Compared with photoluminescent material luminous fabric , POF luminous fabric can
make up the shortcomings of no color effects, the dark brightness, fast light intensity decay.
Compared with light-emitting diodes in fabric, POF luminous fabric has a lot advantages,
such as uncharged, no heat, good flexibility, good impact resistance, no electromagnetic
radiation, low power consumption and so on. The POF luminous fabric has been widely used
in many fields of clothing, home textiles, decorative lighting, security alerts, medical
phototherapy and a flexible display.
The purpose of this paper is to investigate the influence of the law of luminescence, the
change of chromaticity, weft yarn coverage in different weave fabrics and bending radius on
the brightness of POF. To discuss the influence of various parameters of POF light-emitting

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fabric structure on the brightness, a multiple regression model to optimise the brightness of
POF light-emitting fabric. It provides a reference f o r the further to the intelligent,
diversified development of POF light-emitting products.

2. EXPERIMENTAL
2.1 Materials
In this study, the 14.58tex/2 Cotton yarn and 300D Polyester monofilament were obtained
from Huafusefang Company. The diameter of PMMA / Fluorine polymer resin optical
fiber is 0.25mm fiber core refractive index is 1.49, the numerical aperture is 0.35.The
Diameter of the brightness white LED light is 5mm.

2.2 Samples preparation

This Fabric is made by DWL1150 manual semi-automatic loom. Reed No.120.And at both
ends of the fabric leaving a certain length of weft for cluster processing. The structural
parameters is shown in Table 1.

Table 1. Structure parameters of polymer optical fiber fabric

Weft Fabric Warp/Weft Weft Fabric Warp/Weft

NO. GSM NO. GSM
yarns weaves density yarns weaves density
1 Cotton 1/1 240/175 215 13 Polyester 8/3sateen 240/116 193
2 Cotton 1/2↗ 240/235 221 14 Polyester 1/1 240/64 206
3 Cotton 2/2↗ 240/225 223 15 Polyester 3/1↗ 240/102 212
4 Cotton 2/2basket 240/290 216 16 Polyester 2/2↗ 240/92 209
5 Cotton 3/1↗ 240/235 225 17 Polyester 2 3 /1 2 240/92 215
6 Cotton 3/2↗ 240/275 220 18 Polyester 8/3sateen 240/112 211
7 Cotton 1/4↗ 240/265 217 19 Polyester 1/1 240/56 230
8 Cotton 5/3 sateen 240/270 215 20 Polyester 3/1↗ 240/86 228
9 Polyester 1/1 240/68 198 21 Polyester 2/2↗ 240/84 234
10 Polyester 3/1↗ 240/106 195 22 Polyester 2 3 /1 2 240/90 231
11 Polyester 2/2↗ 240/104 187 23 Polyester 8/3sateen 240/104 229
12 Polyester 2 3 /1 2 240/106 192

The every twenty root weft of polymer fiber fabric is bundled. Then the light emitting
diode make coupling connection with POF.Then with appropriate voltage according to the
designed circuit so that to complete the link. As shown in figure1.

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 Figure 1. Light connection of polymer optical fiber fabric
2.3 Testing
The POF light-emitting fabrics are tested by LumiCam 1300 imaging photometer, we use
XY-axis motion platform to adjust POF light-emitting fabrics height and distance,so
that we make a complete presentation of the test fabric in the test area.Each sample were
tested by line brightness and different sizes and positions surface brightness. As shown in
figure 2.

Figure 2. Luminance test of polymer optical fiber fabric

With a helium-neon gas laser HN-600 as a light source, output light of 632.8nm wavelength.
The polymer fiber is wound on the cylinder of different diameter. Light through the wave
plate into the fiber by the coupling lens, then through the lens coupled into the test
system which is constituted by the power meter. As shown in figure 3.

1：He-Ne lasers, 2: Polarizer, 3: Coupling lens, 4: POF and Bending axis, 5:Power Measurement
System
Figure 3. POF bend loss test schematic diagram

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3. RESULT AND DISCUSSION
3.1 The effect of fabric structure Parameters
POF makes use of the principle of polymer side light emitting transfer light and surface
dispersed light so that the fabric surface appears light effects. Its basic principle is that POF
dissipated light in the process of transmission of light from the fiber surface so that light
dissipated from the fiber surface. The specific principle is shown in Figure 4.

Figure 4. POF side light-emitting principle

The Brightness of POF light-emitting is not only effected by absorption loss of the fiber
material fabric and scattering loss caused by the fiber structure but also it causes losses
because of the bending. The relation of bending loss and bending radius is shown in Figure
5, we can see that the POF have a diameter of 0.25mm, its critical bend radius is about
6mm.When bending radius is less than the critical bend radius 6mm, the bending losses
in sharp decline as exponentially. When bending radius is larger than the critical bend radius,
POF is bend loss remained unchanged, and tended to a small stable value, basically can be
ignored.

Figure 5. Relationship of bending loss and bending radius of POF

At the same light source and the same number of POF bundles light conditions. There are
two major factors to influent POF brightness. (1) weft coverage; (2) bending radius. Weft
coverage can be get by the formula.

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 Sa

Sb
So,
dw ndwdj
 -
b Rab

Among them: δ is the Weft coverage, Sa is the weft area of an organization loop, Sb is an
organization loop area, dw, dj are warp and weft diameter, R is the number of cycles weave
yarn, n are points of the weft in an organization loop.
The oretical values of different organizations bending radius can be calculated as the
following formula:
n  1Lwarp
dr   di

sin
2

Among them: dr is the bending radius, n is free number warp, Lwarp is the distance
between the two warps, γ is the Bending angle, dt is the diameter of the warp.
The coverage weft reflects the proportion of the POF in per unit area of fabric surface
polymer fiber, Bend radius reflects the POF bend condition in the fabric. The parameter of
eight different organizations of the fabric is shown in Fig 6, The brightness of different POF
light-emitting fabric is shown in table 2.

Figure 6. The main factor effect luminance of POF light-emitting fabric

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 Table 2. The average brightness of different organizations POF light-emitting fabric
Structure 1/1 1/2↗ 2/2↗ 2/2 basket 3/1↗ 3/2↗ 1/4↗ 5/3 sateen
Brightness
0.8264 1.182 0.8057 1.771 0.7612 1.206 2.29 0.991
(cd/m2)

It can be seen, in the eight kinds of fabric organizational structure, the highest brightness is
1/4↗, its weft coverage and bending radius are the largest, bend radius is larger than the
critical bend radius, its bending loss is negligible. Obviously weft large coverage plays an
important role, the area of the POF in the fabric surface is large, and so the highest brightness
is 1/4↗.
Secondly highest brightness is 2/2 basket, its weft coverage is large, and bend radius in the
middle of the eight organizations, So, its brightness is higher; next are 1/2↗ and 3/2↗, the
brightness are close, this is because the weft coverage and bending radius of these two
organizations are close, but because weft weave it’s of the coverage is less than 2/2basket,
so its brightness is lower. The most weak brightness are 1 / 1,2 / 2↗, 3 / 1↗ and 5/3 sateen.
That is because both of them weft coverage are small, so the brightness of these four
organizations is significantly lower than the other organizations.
This shows that fabric structure design parameters, such as fabric structure parameters, Warp
and weft density and weft yarn diameters latitude, all have a very important influence on the
brightness of the light-emitting polymer fiber fabric. Rational design the fabric structure
parameters will in a certain degree increase the brightness of the POF light-emitting fabric.

3.2 Multiple regression model

We utilization the method of HDD in RSM (response surface methodology) to establish
multiple regression model for polymer optical fiber luminous fabric of monofilament
polyester of 15 different parameters organizational structure. By Design expert software we
designed response value of HDD experimental samples and luminance, as shown in Table 3.

Multiple regression model of brightness of polymer optical fiber light-emitting fabric: By

Design-Expert 7.0. 0 software for data regression analysis, quadratic regression model has
been obtained as (1).
y=0.39-0.56A+0.31B-3.96C+1.80D-1.56E+0.38AB-0.28AC+0.012AE+2.57BD+3.08
CD-3.08C2+0.70E2 (1)

The obtained fit (R2) of regression model is 0.9786, the SNR (adeq precision) is 91.864,
the above values have shown that the model fit is better. Figure 7 is predicted and experimental
values of brightness of monofilament polyester polymer fiber light-emitting fabric of
different fabric structure parameters. It is seen that they can fit better. The biggest difference
is 0.03cd/m2. So it can be explained that the model of sample prediction model is effective
within a certain range.

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 Table 3. HDD test samples and response
Warp Weft The number Thickness Brightness
NO. Density Density of cycles NO.
（mm） （cd/m2）
(root/10cm） (root/10cm） weave yarn
1 240 68 2 1 0.68 0.4875
2 240 106 4 3 0.85 0.4755
3 240 104 4 2 0.95 0.1231
4 240 106 8 5 0.95 0.2125
5 240 116 8 1 0.43 0.5299
6 300 64 2 1 0.66 0.4930
7 300 102 4 3 0.85 0.2670
8 300 92 4 2 0.95 0.3872
9 300 92 8 5 0.94 0.4342
10 300 112 8 1 0.45 0.6414
11 360 56 2 1 0.65 0.7638
12 360 86 4 3 0.89 0.5940
13 360 84 4 2 0.84 0.6959
14 360 90 8 5 0.95 0.7261
15 360 104 8 1 0.41 0.6405

Figure 7. Comparison of experimental and predicted values

Analysis of variance and significance of the model are shown in Table 4,P value of factors
A, C, D, E, AB, AC, AD, BD, CD, C2 and E2 is Less than 0.05,it showed that Impact of
these factors on the fiber diameter is significant, influence of other factors on the fiber
diameter is not significant, among them, the factor B, as a single factor, has no significant
effect on the emission brightness of polymer fiber fabric, when it takes joint action with the
warp density and thickness of the fabric(AB, BD),it is significant for influence of light-
emitting polymer fiber fabric brightness.

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 Table 4. The variance of the regression model and its significance analysis

coefficient standard
F value P value
estimates deviation
model 0.39 0.084 747.48 0.0286
A -0.56 0.021 687.94 0.0243
B 0.31 0.043 50.79 0.0887
C -3.96 0.26 237.11 0.0413
D 1.80 0.13 196.30 0.0454
E -1.56 0.067 541.13 0.0274
AB 0.38 0.013 887.80 0.0214
AC -0.28 0.019 224.04 0.0425
AD 0.52 0.034 240.11 0.0410
AE 0.012 0.018 0.41 0.6359
BD 2.57 0.18 206.41 0.0442
CD 3.08 0.22 194.01 0.0456
C2 -3.08 0.17 322.50 0.0354
E2 0.70 0.043 273.12 0.0385

Optimization and prediction of brightness of polymer optical fiber luminous fabric: this
model is first choice for structure parameters of highest brightness. According to the
experimental, the warp density of polyester monofilament POF light-emitting fabrics shall
be within the range of 200-360 root / 10cm. Based on this result, the warp density 200-400
root / 10cm is set as the model of dependent variable to solve, a stable set of optimal fabric
structure parameters is derived by calculation of the model: Warp density is 360m root / 10cm,
weft density is 200 / 10cm,the number of yarns of fabric weave cycle is 8,when n is 3,the
predicted brightness is 10.813 cd/m2.

3.3 Even and orderly of brightness

The POF luminous fabric is used for further development for a variety of light-emitting
products, such as the light-emitting clothing, light-emitting household textiles and other light
therapy textile, they have higher requirements for brightness leveling of POF luminous fabric,
However, in practical application of the polymer optical fiber, it is still difficult for POF
luminous fabric to avoid the problem of uneven brightness. In this study, we found problem
of fabric uneven brightness from 23 kinds of test samples.
The figures are 1/1, 1/4↗ cotton POF light emitting as the example, we can see clearly
different from the overall color of the crest, this represents a significant increase in the
brightness of this point. This is probably because in the weaving process damage to the POF,
fabric defects and unstable optical circuit connection are caused the fabric unevenness in
brightness.

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 1/1 1/4↗

Figure 8. POF light emitting fabric color test

3.4 Colorimetric of POF light emitting fabric

We test the POF luminous fabric color light emitting portion, X, Y, Z are coordinates of the
chromaticity, each fabric color coordinates shown in Table 3.5.

Table 5. Color coordinate of POF light emitting fabric

NO. X Y Z NO. X Y Z

1 0.2762 0.2787 0.4452 13 0.2774 0.2731 0.4495

2 0.2744 0.2659 0.4597 14 0.2736 0.2728 0.4536
3 0.2724 0.2607 0.4669 15 0.2753 0.2685 0.4561
4 0.2774 0.2725 0.4502 16 0.2724 0.2730 0.4546
5 0.2714 0.2619 0.4667 17 0.2753 0.2679 0.4567
6 0.2391 0.2391 0.5218 18 0.2825 0.2797 0.4378
7 0.2249 0.3684 0.4068 19 0.2766 0.2701 0.4534
8 0.2739 0.2610 0.4651 20 0.2710 0.2704 0.4586
9 0.2443 0.3023 0.4535 21 0.2784 0.2711 0.4505
10 0.2353 0.3128 0.4519 22 0.2857 0.2826 0.4317
11 0.2789 0.2696 0.4516 23 0.2556 0.3305 0.4139
12 0.2753 0.2678 0.4568

As the International standard chromaticity diagram, we can get the color of X, Y, Z

coordinates, its shown in Figure 9

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 Figure 9. The color of POF light-emitting fabric X, Y, Z color coordinates corresponding point

Through the above test can be seen that POF lemitting fabric is the same luminous colors as
light source (High-brightness white LED),In the process of forming the POF light-emitting
fabric, the various processes to optical fiber caused Fiber bending and breakage and so on. It
Does not change the light in the propagation of the POF lemitting fabric. Secondly, in the
POF light-emitting fabric, the color coordinate in different parts of the basic are basically the
same, the colors are white, the fabric overall color is even when the fabric is light-emitting.

4. CONCLUSIONS
1. Fabric structure design parameters, such as fabric structure parameters, Warp and weft
density and weft yarn diameters latitude, both have a very important influence on the
brightness of the light-emitting polymer fiber fabric. Rational design the fabric structure
parameters will in a certain degree increase the brightness of the POF light-emitting fabric.

2．In the eight kinds of fabric organizational structure, due to the impact of different weft
coverage and bending radius, the brightness of the eight kinds of fabric are different, the weft
coverage of 1/4↗fabric is larger than the other fabrics, so the highest brightness is 1/4↗.

3. Through the study of the different organizational structure POF light-emitting fabric caused
different losses, And establish the relevant multiple regression model, a stable set of optimal
fabric structure parameters is derived by calculation of the model: Warp density is 360m root
/10cm, weft density is 200 /10 cm, the number of yarns of fabric weave cycle is 8, when n is
3,the predicted brightness is 10.813 cd/m2.

4. The POF fabric has the uneven brightness Problem, this has big connection with weaving
process damage to the POF, fabric defects and unstable optical circuit connection.

5. POF light-lemitting fabric has the same luminous colors with light source (High-brightness
white LED). In the POF light-emitting fabric, the color coordinate in different parts of the
basic are basically the same, the colors are white, the fabric overall color is even when the

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fabric is light-emitting.

REFERENCES

[1] Harlin A, Makinen M, Vuorivirta A. Development of polymeric optical fibre fabrics as

illumination elements and textile displays[J]. Autex Research Journal,2003.3(1);67-72.
[2] Hecht, J, and L. Long. Understanding fiber optics[C]. Vol.3. 2002: Prentice Hall
Columbus.
[3] Witt J, Schukar M, Krebber K. Medical textiles with integrated polymer optical fibers for
respiration monitoring[J]. Technishes Messen Technical Measurement,2008,75(12):670-677.
[4] Cochranea C, et al. Flexible displays for smart clothing: part I-overview[J]. Indian Journal
of Fiber &Textile Research,2011.36:422-428.
[5] Deflin, E, et al. Bright optical fiber fabric: A new flexible display[J].Textile
Asia,2002.33(5):25-28.
[6] Koncar V, Deflin E. Weill A. Communication apparel and optical fiber fabric display[J].
Wearable Electronics and Photonics,2005:155-176.
[7] Mordon S.et al. Innovative engineering design of a textile light diffuser for photodynamic
therapy[J].13th International Photodynamic Association World Congress(IPA),2011:147-
151.
[8] Graham-Rowe D, Photonic fabrics take shape[J]. Nature Photonics, 2007. I (1):6-7.
[9] Rothmaier M, Luong MP, Clemens F. Textile pressure sensor made of flexible plastic
optical fibers[J]. Sensors,2008.8(7):4318-4329.
[10] Suhuster J, et al. Influence of fabric ties on the performance of woven-in optical fiber[J].
Composites Part A: Applied Science and Manufacturing,2003,34(9):855-861.
[11] Spigulis J, et al. Glowing optical fiber designs and parameter[J].1997.2967:231-236.
[12] Krebber K, et al, Distributed fiber optic sensors embedded in technical textiles for
structural health monitoring[C]. Proceedings of SPIE-The International Society for Optical
Engineering, Portugal: American Society of Mechanical Engineers,2010:387-391.
[13] Bang Hj, Shin HK, Ju YC, Structural health monitoring of a composite wind turbine
blade using fiber Bragg grating sensors[C]. Proceedings of SPIE-The International Society
for Optical Engineering. San Diego: American Society of Mechanical Engineers,2020:456-
461.
[14] Measures RM, et al. Fiber optic sensors for smart structures[J]. Optics and Lasers in
Engineering,1992.16(2-3):127-152.
[15] Zubia J, Arrue J. Plastic optical fibers: An introduction to their technological processes
and applications, J. Optical Fiber Technology,2001.7(2):101-140.

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An Alternate Approach to Engineer Light Weight Composite Bullet Proof
Vest
Syed Zameer Ul Hassan *,a, Ali Raza Shafqat a, Salman Naeem b, Saqib Siddiqui a, Ali Asghar
a
, Muhammad Kashif a, Nadar Baz a, Ikramullah a
a
Department of Textile Engineering, Faculty of Engineering, Balochistan University of
Information Technology, Engineering and Management Sciences, Quetta, Pakistan.
(zameer_51214@hotmail.com)
b
Department of Garments Manufacturing, National Textile University, Faisalabad, Pakistan.

ABSTRACT
Impact resistance of Fiber-reinforced composites with high modulus and high strength fibers has been
under extensive investigation subject to their specific properties. The impact response of thermoplastic
composite armor made from unidirectional Kevlar reinforcement and thermoplastic matrix was
investigated on real time. Kevlar unidirectional sheets were produced and used as reinforcements to
fabricate composite armor panel under high pressure. Stiffness property of resin was improved by
integrating graphite powder using toluene as solvent which further improved the hardness of
composite. Reduced density was observed in Kevlar thermoplastic composite as compared to
conventional thermoset composite. Impact tests of composite armor were imparted via 9 mm bullets,
total four fires were shot at different distances of 5m, 10m, 15m, and 20m. All the bullets were captured
by armor plate, no bullet passed through.
Keywords: Bulletproof, Body armor, Thermoplastic, Kevlar, Unidirectional composite, Impact
resistance.

1. INTRODUCTION
Anti-Ballistic Textiles are extensively used in Defense, Civil Defense, Police, Fire Fighting,
Aerospace & Aviation etc. as protection textiles against heavy impact, bullets, stabbing etc.
A silicon-infiltrated ceramic based on a reaction-bonded silicon carbide body is a popular
anti-ballistic material. Apart from anti-ballistic properties, it also offers excellent protection
against knife and ice pick threats. One attribute of this fabric is its ability to reduce the trauma
conventionally caused by the impact of a ballistic projectile, even though the projectile is
stopped from penetrating the fabric. Fabrics in Para Aramid fibers and Polyethylene HT
fabrics are also often used in manufacture of anti-ballistic textiles.
Composite materials that contain unidirectional high performance fibers as reinforcement are
branded by a great specific strength due to which they are exclusively used in light weight
applications [1].
A bulletproof jacket, bulletproof vest, ballistic vest or bullet-resistant vest is an item of
personal armor that helps absorb the impact from firearm-fired projectiles and shrapnel from
explosions, and is worn on the torso. Soft vests are made from many layers of woven or
laminated fibers and can be capable of protecting the wearer from small-caliber handgun and
shotgun projectiles, and small fragments from explosives such as hand grenades. This textile
is commonly worn by police forces, private citizens who are at risk of being shot (e.g., national
leaders), security guards, and bodyguards, whereas hard-plate reinforced vests are mainly
worn by combat soldiers, police tactical units, and hostage rescue teams. It is also called safety
textile [2]. When a handgun bullet strikes body armour, it is caught in a “web” of very strong

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fibers. These fibers absorb and disperse the impact energy that is transmitted to the bullet
proof vest from the bullet, causing the bullet to deform or “mushroom.” Additional energy is
absorbed by each successive layer of material in bullet proof vests, until such time as the
bullet has been stopped. Soft body armor is manufactured from multiple plies of fabric without
any matrix that is sewn together with Z-pinning.
The NIJ standard other than general impact strength testing also offers standards for armor’s
testing under strained conditions like agitation, water immersion, humidity levels and
temperature [3]. To Manufacture a unidirectional Kevlar fabric for composite fabrication, to
develop a Unidirectional fiber reinforced composites using Elvax (resin) for bulletproof vest.
Bulletproof vests are currently manufactured by foreign companies; these companies earn
huge profit on their goods. Pakistan has huge demands for protective textiles and till date we
don’t have any local facility to manufacture protective goods according to international
standards.
The Indian researcher Aswani Kumar et al. [4] research about Ballistic impact performance
of hybrid thermoplastic composite armors reinforced using high performance fiber. In this
research, the material they used are Kevlar 29 of 1111 dTex and basalt yarns of 3000 dTex
were selected to produce 2D and 3D fabrics with polypropylene (pp). Two types of hybrid
armors were manufactured with polypropylene (PP) as a matrix: one with a non-symmetric
[H1] stacking sequence and the other with a symmetric [H2] stacking sequence. Three types
of 2D fabrics were produced: two monolithic fabrics with Kevlar and basalt yarns and one
hybrid fabric with basalt yarns in the warp direction and Kevlar yarns in the weft direction.
Similarly, three types of 3D fabrics namely, two monolithic fabrics with Kevlar and basalt
yarns and one hybrid fabric with basalt yarns as stuffer yarns and the remaining yarns with
Kevlar, were produced. Clegg et al. [2] highlighted use of composites for body armor could
provide light weight protection with increased strength. Kocer et al. [4], noticed presence of
meagre resin in fabrics can increase energy absorption than high resin contents subjected to
unequal load distribution. FRC’s are preferred since they have low density but high tensile
strength compared to ceramics. Further it was noticed that without matrix fibers can only
withstand tensile stresses where as in composite they fiber and reinforcement work in
correspondence, thus it increases stiffness leading to reduced deformation and effective
ballistic performance. IN 2016 joanna et al [5] . Concerns the ballistic resistance of hybrid
composite shields. The analysis covers three types of two-layer composites. The first shield
layer were plates of tungsten carbide (WC), ceramic balls Al2O3 (aluminum oxide 92) or steel
balls (100Cr6 steel) embedded in a polymer matrix. The second layer was aluminates
consisting of 10 layers of Aramid fabric in a matrix of styrene-butadiene-styrene (SBS)
copolymer. The study presents the analysis of damage caused by a ballistic impact, further
compared to the results of computer simulations conducted using the finite element method
(FEM). Samples were overshot along the ballistic track from the Beryl rifle. The 5.56 _ 45
mm ammunition with the bullet of SS109 MESCO type was used. Samples were overshot
along the ballistic track from the combat gun - 5.56 mm Beryl rifle produced in Poland. The
ammunition 5.56 _ 45 mm with the projectile of the SS109 type produced by MESCO in 2005
was used for the study. The velocity was measured using the Doppler Wable SL-525p radar.
The test parameters are Summarized in the conclude that the Despite punching the laminates
with the Projectile 5.56 mm Type SS109, the value of the absorbed kinetic Energy was

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determined for each shield. The shield absorbed a small amount of energy, however this quite
valuable information provides only the overview of the percentage of the energy that is
absorbed at this stage. When trying to estimate the energy required to deform a projectile one
can focus on the layers of the ballistic shield of the type add on armor. However, in further
works the parameters of molding composites should be modified in order to improve the
saturation of the weft and warp threads of the Aramid fabric with the polymer.

2. MATERIALS AND METHODS

2.1 Materials
For manufacturing of Composite sheet Kevlar was used as reinforcement which was
developed by Dupont. Elvax was used as resin which is thermoplastic resin offered by Dupont.
Toluene was used as solvent to reduce viscosity of resin. To harden the samples Graphite
powder was used as filler.

2.2 Sample Preparation

First of all, we have to find out the melting point of thermoplastic resin (Elvax 760A).
Therefore, we determine the melting point of DuPont Elvax™® 760 in Material testing lab
BUITEMS, which was 260 °C, which was very high and difficult to achieve for whole process
of making composite, so we decide that to search that solvents in which DuPont Elvax™®
760 is soluble. The solvents in which the Elvax soluble are:
a. Toluene
b. Cyclohexane
c. Tetrahydrofuran
But in Quetta’s market only toluene solvent was available therefore we choose the toluene
solvent for thermoplastic resin and again we determine the melting point of Elvax in solvent
which was 140°C and process temperature 150°C.

Figure 1: Composite of Woven cotton Figure 2: Sample of woven cotton with

without graphite powder (soft sample) graphite (Hard sample)

After determining the melting point of solution (Toluene + Elvax) we made a composite
(sample) of woven cotton fabric and noticed that composite is soft. We performed different
agents for hardening the composite sheet and found that graphite powder has significant effect
on hardness. The difference between the Zinc Powder and Graphite can be seen in the
following figures.

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2.3 Pre-preg Manufacturing
We had to made unidirectional sheet of Kevlar filament (1000 denier). We prepared a winding
board as shown in the Fig.3 in order to make unidirectional Kevlar sheets.

Figure 3: Winding Board

2.4 Winding process

We wound the Kevlar filament parallel and close to each other (so that no gap or space remain
between two adjust filaments) on winding board in order to make a unidirectional sheet of
Kevlar as shown in Fig 4.

Figure 4: Complete Unidirectional Kevlar sheet on winding Board

2.5 Preparation of resin

At the same time we prepared a thermoplastic resin as shown in Fig 5 (400ml toluene,100g
Elvex and 20g graphite powder) at temperature 140°C for each sheet of length 30” and width
14 ½”.

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 Figure 5: Preparation of thermoplastic resin

2.6 Applying the resin

The number of filaments per inch was 38 filaments and we prepared one complete
unidirectional sheet on winding board in three hours. After manufacturing one complete
unidirectional sheet we cover a whole sheet by resin uniformly and placed it for some time to
dry as shown in fig 6.

Figure 6: covered sheet by resin

2.7 Cutting the sample

After that we cut the sheet and placed on smooth and flat surface to cover the back side by
resin uniformly. Using the same technique, we prepared total 12 sheet and cut each sheet
further into two pieces of length 15” and width 14 ½” in order to get total 24 sheets shown in
fig 7.

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 Figure 7: Single sheet of size (15"by 14.5")

2.8 Stacking sequence or Manufacturing Structure

we had total number of 24 sheets and the stacking sequence of sheets is shown in below table
1 in which the first row shows number of sheets and the second row show orientation (angle)
of sheets.

Table 1: Stacking sequence of 24 sheets

Sheets No 1 2 3 4 5 6 7 8 9 10 11 12
Orientation 0° 45° 0° 90° 0° 45° 90° 0° 45° 0° 90° 0°
Sheets No 13 14 15 16 17 18 19 20 21 22 23 24
Orientation 0° 90° 0° 45° 0° 90° 45° 0° 90° 0° 45° 0°

2.9 Molding
We placed the 24 sheets at the above sequence to make a proper structure as shown in Fig
8.In molding we put the whole structure in two heavy molds the one mold is concave and
other is convex then we compress it in simple manual compression machine for 90 minutes at
BUITEMS mechanical Engineering work shop shown in Fig 9.

Figure 8: Total 24 sheets Figure 9: Concave and convex mould

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2.10 Curing
After molding we placed the whole structure(mold) in small metal gripper as shown in Fig
and put in oven for 4 hours at a temperature of 240 °C to stack the sheets with each other and
to evaporate the solvent if remain in structure, we took out the structure time by time and tight
the bolts to more compress the structure after that we remove the molds and got the raw
structure then we mark the proper shape on the raw plate and cut the extra edges according to
marker to get the proper shape.

Figure 10: Compressed mold

2.11 Final Product

After curing we finished the whole plate with resin to get our final product. As shown in Fig11.

Figure 11: Finished torso

3. RESULTS AND DISCUSSION

In order to measure the performance of the ballistic material, it has to be tested with firearms.
To stop the bullet, the ballistic material should able to dissipate the energy of the bullet at the
muzzle point. Thus the test had to measure the impact strength of the material indirectly.

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Tests were carried out in field conditions, with the following procedure using “NIJ 0101.06”
standard [6].

Weight of the bulletproof vest (front torso) = 1.2 kg

Sample size – 9”× 13”
Type of firearm – 9 MM FMJ Grand master made in USA Model - 2011
Barrel length – 5”
Weight of the bullet – 124g
Total 4 fires
Distance 1st fire from 20 m
2nd fire from 15 m
3rd fire from 10 m
4th fire from 5 m
The sample captured all the bullets is shown in below figure 12.

Figure 12: (a) Front side of sample after four shot (b) Back side of sample

In the right figure it can be seen that the back side of 4th fire which is fired from 5 meter
damaged the back side sheet and the other three shot have no effect on back side.

4. CONCLUSIONS
It was found that 24 unidirectional sheets layers of a Kevlar-29 with Elvax resin can stand
impact energy of 9 mm bullet type that fired at a distance of 20 meter, 15 meter, 10 meter and
5 meter respectively. Elvax was found suitable for composite fabrication but under high
pressure, temperature and high amount of solvent. Graphite filler is found to be suitable for
increasing hardness of composite. The composite bullet resistance body armor that is made
from 24 unidirectional sheets layers of Kevlar-29 fiber with Elvax Resin weights only about
1.2kg and if back and front side were used it only weights about 2.4 Kg which is the most
recommended and preferable for foot soldier due to its mobility advantage.

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FUTURE WORK
Different reinforcements and concentrations can be utilized to improve the performance.
Impact can be analysed in terms of different testing procedures.

REFERENCES
[1] INDIAN JORNAL OF FIBER & TEXTILE RESEARCH, VOL: - 22, 1997, PP- 274-
291.
[2] International Journal of Scientific & Engineering Research, Volume 4, Issue 5, May-
2013, ISSN 2229-5518 IJSER.
[3] J. K. Fink, Handbook of Engineering and Specialty Thermoplastics: Polyolefin’s and
Styrene’s, Scrivener Publishing, 2010, p. 35.
[4] Mechanics_of_Ballistic_Resistance_of_Textile_Assemblies_and_its_Measurement,
publication/279187784.
[5] Naveen Kumar: Bulletproof Vest and Its Improvement: January 2016 IJSDR | Volume 1,
Issue 1.
[6] Jared Henderson “BALLISTIC BODY ARMOR” CMGT 564 Strategic Standardization
August 2008.

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A Novel Electrospun Polyacrylonitrile-Based Form-Stable Phase Change
Composite Fibrous Membranes for Storage and Retrieval of Thermal
Energy
Huizhen Ke
Fujian Key Laboratory of Novel Functional Fibers and Materials, Faculty of Clothing and
Design, Minjiang University, Fuzhou, Fujian, 350108, China,
Email: kehuizhen2013@163.com

ABSTRACT
A series of the capric-palmitic-stearic acid ternary eutectic mixture/polyacrylonitrile/sliver
nanoparticles (CA-PA-SA/PAN/Ag-NPs) form-stable phase change composite fibrous membranes
(PCCFMs) with different Ag-NPs content were fabricated by electrospinning and physical adsorption
methods. The morphological and chemical structures, thermal energy storage properties and heat
transfer rates of the prepared CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs were characterized by
scanning electron microscopy (SEM), Fourier transformation infrared spectroscope (FT-IR),
differential scanning calorimeter (DSC) and measurement of melting and freezing times, respectively.
The SEM images showed that electrospun PAN/Ag-NPs composite nanofibrous membranes with
different Ag-NPs content can be used as novel supporting materials for the preparation of form-stable
PCCFMs due to the effect of capillary and surface tension force. The DSC results suggested that
the melting peak temperature and enthalpy of the CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs
were about 24 o C and 138 kJ/kg, respectively. The heat transfer rates of the CA-PA-SA/PAN/Ag-
NPs form-stable PCCFMs were significantly enhanced owing to the addition of Ag-NPs.
Keywords: Phase change composite fibrous membranes; Capric-palmitic-stearic acid ternary
eutectic mixture; Polyacrylonitrile; Silver nanoparticles; Thermal energy storage property;

1. INTRODUCTION
Thermal energy storage technologies for reducing energy consumption and improving energy
efficiency have become increasingly important with the growth of population and the
development of industry. Among the available strategies for energy storage, latent heat
storage technology using phase change materials (PCMs) is considered as one of the most
promising technologies. According to the reported literatures, PCMs have been widely
researched and successfully applied in numerous fields such as solar thermal collector [1],
heat recovery systems [2], residential and commercial buildings [3], refrigerated containers
[4], greenhouse systems [5], Li-ion battery thermal management [6] and thermal regulating
fibers [7], etc.
There are three types of PCMs including organic PCMs (e.g., paraffin waxes, fatty acids,
fatty acid eaters and sugar alcohols), inorganic PCMs (e.g., salt hydrates) and their eutectic
mixtures (e.g., fatty acid eutectics and inorganic salts eutectic mixtures) [8]. It is interesting
to note that fatty acid eutectics, as a derivative of fatty acids, have the same desirable
properties as those of fatty acids such as good thermal and chemical stabilities, high latent
heat storage capacities, reversible phase change behavior, no phase segregation and
supercooling, non-toxicity, non-corrosive and cost effectiveness, etc [9-10].

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However, low thermal conductivity and the ease of liquid leakage of solid-liquid PCMs and
their eutectic mixtures (e.g., fatty acids and fatty acid eutectics) during phase change
processes limit their engineering applications. Therefore, extensive research efforts have
been made to overcome these two shortages of solid-liquid PCMs. These efforts include the
use of various methods such as electrospinning [7], adsorption method [11], sol-gel method
[12], esterification reaction method [13], vacuum impregnation [14] and mixing method
[15] to prepare form-stable PCMs, which can effectively resolve the liquid leakage problem.
Moreover, in order to improve the heat transfer rates of PCMs, numerous technologies have
also been applied such as dispersing the fillers with high thermal conductivity in the
phase transition systems [14-16], selecting the metal foams as supporting skeletons [17-
18] and adding metal fins [18], etc.
Silver nanoparticles (Ag-NPs) possess excellent properties such as good thermal stability,
large specific surface area and the highest thermal conductivity of all metal materials (about
429 W/mK) [16], thus they can be chosen as effective thermal conductive enhancers for the
improvement of heat storage and release rates of PCMs. However, to the best of our
knowledges, the development of electrospun polyacrylonitrile-based (PAN-based)
composite nanofibrous membranes loading different amount of Ag-NPs as the novel
supporting materials have never been reported. Therefore, the present work studied that the
capric-palmitic-stearic acid ternary eutectic mixture (CA-PA-SA) was prepared and adsorbed
into the three-dimensional porous network structure of electrospun PAN/Ag-NPs composite
nanofibrous membranes with different mass ratios acting as supporting materials by physical
absorption method. The effects of the loaded Ag-NPs on the morphological and chemical
structures, phase change temperatures and enthalpies, heat transfer rates of form- stable
phase change composite fibrous membranes (PCCFMs) were characterized by scanning
electron microscope (SEM), Fourier transformation infrared spectroscope (FT-IR),
differential scanning calorimeter (DSC) and measurement of melting and freezing times,
respectively.

2. EXPERIMENTAL
2.1 Materials
The silver nanoparticles (Ag-NPs) with 99.9 wt.% purity, about 80-90 nm average diameter,
were supplied by Nanjing XFNANO Materials Tech Co., Ltd (Nanjing, China). The
chemicals of N, N- dimethyl formamide (DMF), capric acid (CA), palmitic acid (PA) and
stearic acid (SA) were all obtained from the Sinopharm Group Chemical Reagent Co., Ltd.
(Shanghai, China). The polyacrylonitrile (PAN, M w=150,000) powder was purchased from
Polysciences, Inc. All of the chemicals were used as received without further purifications.

2.2 Preparation of electrospun PAN/Ag-NPs supporting materials

The PAN powder was fully dissolved in DMF solvent at room temperature with a fixed
concentration of 10 wt.% for 24 h. Thereafter, the Ag-NPs were dispersed to the above PAN
solution with different mass fractions [ 𝑊𝐴𝑔 : (𝑊𝑃𝐴𝑁 + 𝑊𝐴𝑔 ) ] of 5 wt.% and 10 wt.%.
Subsequently, the PAN/Ag-NPs composite solutions were kept under constant stirring at
room temperature to achieve the homogeneous solutions for electrospinning.

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The solutions were electrospun through a metallic nozzle with the inside and outside
diameters of 0.6 mm and 0.9 mm using a syringe onto the aluminum foil placed on a roller
collector. The parameters such as applied voltage, collecting distance, solution feed rate,
rotating speed of the roller were set at 30 kV, 18 cm, 1 mL/h and 200 rpm, respectively. All
experiments were conducted at room temperature and at a relative humidity between 20 %
and 30 %. The codes of electrospun composite nanofibrous membranes were referred as PAN,
PAN/Ag-NPs5 and PAN/Ag-NPs10, respectively.

2.3 Preparation of CA-PA-SA/PAN/Ag-NPs phase change composite fibrous

membranes
The CA-PA-SA ternary eutectic mixture was prepared as solid-liquid PCMs through melt-
blending followed by ultrasonication, which has been reported by my previous literatures [9].
The eutectic mass ratios of CA-PA-SA was determined at 83.82/10.19/5.99. The form-stable
phase change composite fibrous membranes (PCCFMs) were prepared by physical adsorption
method. The prepared CA-PA-SA ternary eutectic mixture was completely melted in a culture
vessel at 60 oC. The electrospun PAN and PAN/Ag-NPs nanofibrous membranes with
different amount of Ag-NPs were respectively cut into the samples with sizes of 5 cm × 5 cm
and then immersed into molten CA-PA-SA ternary eutectic mixture until saturated absorption.
Thereafter, the prepared PCCFMs were hung in an oven at 60 oC for 10 h to remove residual
CA-PA-SA ternary eutectic mixture on the surface of membranes. Finally, the samples were
cooled down to the room temperature for characterization. The codes of samples were referred
to as CA-PA-SA/PAN, CA-PA-SA/PAN/Ag-NPs5, CA-PA-SA/PAN/Ag-NPs10,
respectively.

2.4 Characterizations
2.4.1. Scanning electron microscopy
The morphological structures of electrospun PAN, PAN/Ag-NPs5, PAN/Ag-NPs10
nanofibrous membranes and the CA-PA-SA/PAN, CA-PA-SA/PAN/Ag-NPs5, CA-PA-
SA/PAN/Ag-NPs10 PCCFMs were observed using a Hitachi S-3400N SEM.

2.4.2. Fourier transformation infrared spectroscope

The FT-IR spectra of the Ag-NPs, CA-PA-SA, electrospun PAN and PAN/Ag-NPs10
nanofibrous membranes, as well as the CA-PA-SA/PAN and CA-PA-SA/PAN/Ag-NPs10
phase change composite fibrous membranes were recorded by Fourier transformation infrared
spectroscope (FT-IR, Nicolet iS10) in the wavenumber range of 400-4000 cm-1.

2.4.3. Differential scanning calorimeter

The phase change temperatures and enthalpies of the CA-PA-SA eutectic mixture and the
CA-PA-SA/PAN, CA-PA-SA/PAN/Ag-NPs5, CA-PA-SA/PAN/Ag-NPs10 PCCFMs were
tested by differential scanning calorimeter (DSC-Q200) with the heating and cooling rates of
8 oC/min at temperatures of -20-70 oC under a constant stream of argon at a flow rate of 50
mL/min. The accuracies of measurements for temperature and enthalpy were approximately
±0.5 oC and ±2.0 kJ/kg, respectively.

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2.4.4. Thermal energy storage and release performances
Thermal energy storage and release rates of electrospun CA-PA-SA/PAN/Ag-NPs form-
stable PCCFMs with different Ag-NPs content during melting and freezing processes were
investigated using the experimental equipment as my previous reported literatures [19-20].
Firstly, about 10 g samples were cut and put into a test glass bottle. Subsequently, a
thermocouple was inserted into the center of the glass bottle and tightly surrounded with the
samples. Thereafter, this test glass bottle was placed into a water basin at a constant
temperature of 40 oC for being heated. When detected temperature of the thermocouple was
reached balance at 35 oC, the glass bottle was rapidly transferred into a refrigerator with a
constant temperature of -10 oC, where the samples performed the thermal energy release
process. After the cooling process was finished, the bottle was immediately transferred into
the above water basin, where the samples subjected thermal energy storage process again. The
temperature values of the samples versus time were automatically recorded by PC using a
data logger with the temperature measuring accuracy of ±2 oC.

3. RESULTS AND DISCUSSION

3.1 Morphological structure
Representative SEM images of electrospun PAN, PAN/Ag-NPs5 and PAN/Ag-NPs10
nanofibrous membranes are presented in Figure 1. It can be clearly seen from Figure 1 that
electrospun PAN, PAN/Ag-NPs5 and PAN/Ag-NPs10 nanofibers were collected and formed
the three-dimensional uniform porous network structure during electrospinning process. As
revealed in the Figure 1, the average fiber diameter of electrospun PAN, PAN/Ag-NPs5 and
PAN/Ag-NPs10 nanofibers were about 200-230 nm and the Ag-NPs additives have no
significantly influence on the morphological structures of electrospun composite nanofibrous
membranes. Figure 2 illustrated the morphological structures of the prepared CA-PA-
SA/PAN, CA-PA-SA/PAN/Ag-NPs5 and CA-PA-SA/PAN/Ag-NPs10 form-stable PCCFMs.
Figure 2 showed that the CA-PA-SA ternary eutectic mixture was uniformly and effectively
encapsulated into the three-dimensional porous network structure and surface of electrospun
PAN/Ag-NPs nanofibrous membranes with different Ag-NPs content due to the effect of
capillary and surface tension force. Moreover, it is interesting to note that there was no leakage
phenomenon during the process of SEM observation although the working temperature of
SEM characterization (about 25 oC) was similar with the melting peak temperature of the CA-
PA-SA ternary eutectic mixture (see Table 1). Based on the SEM observation, it can be
concluded that the effect of capillary and surface tension force between the multi- porous
network structure of electrospun PAN/Ag-NPs nanofibrous membranes and CA-PA-SA
ternary eutectic mixture can effectively prevent the leakage of molten CA-PA-SA ternary
eutectic mixture from membranes.

3.2 FT-IR analysis

The chemical compatibility between CA-PA-SA ternary eutectic mixture and electrospun
PAN/Ag-NPs nanofibrous membranes were investigated by FT-IR analysis. Figure 3 showed
the FT-IR spectra of Ag-NPs, electrospun PAN and PAN/Ag-NPs10 nanofibrous membranes,
CA-PA-SA ternary eutectic mixture, as well as the prepared CA-PA-SA/PAN and CA-PA-
SA/PAN/Ag-NPs10 form-stable PCCFMs. Obviously, there was no strong absorption peak

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in the FT-IR spectrum of pure Ag-NPs, as illustrated in Figure 3(a). It can be clearly observed
from Figure 3(b) that the sharp absorption peak at about 2242 cm-1 was attributed to the
stretching vibration of nitrile groups (-C≡N) in PAN molecules. The characteristic absorption
bands at approximately 2928 cm-1 and 1450 cm-1 were ascribed to the asymmetrical and
symmetrical bending vibrations of methylene groups (-CH2-), respectively. The same results
have also been reported by previous literatures [20]. As shown in Figure 3(c), the FT-IR
spectrum of electrospun PAN/Ag-NPs10 nanofibrous membrane have similar absorption
peaks with those of electrospun PAN nanofibrous membrane due to the same PAN molecular
chain. The FT-IR spectrum of CA-PA-SA ternary eutectic mixture can be seen in Figure 3(d),
typical absorption peaks at around 1704 cm-1, 1275 cm-1 and 929 cm-1 corresponding to the
stretching vibrations of C=O, C-O and -OH bonds of carboxyl (-COOH) groups of fatty acid,
the absorption peaks at the wave numbers of approximately 1461 cm-1 and 719 cm-1 were
represented to the deformation vibration of CH2 or CH3 groups and the rocking vibration in
(-CH2-)n (n≥4) groups, respectively. The absorption peaks assigned to the asymmetric and
symmetric stretching vibrations of C-H bond were also found at about 2920 cm-1 and 2851
cm-1 in the Figure 3(d), respectively [19]. Figure 3(e) indicated that the characteristic
absorption peaks belonging to the PAN molecular chain and CA-PA-SA eutectic molecular
chain were also clearly observed in the spectrum of the CA-PA-SA/PAN form-stable
PCCFMs. It is worthwhile to note that there was no significant peak shift in the spectrum of
the CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs compared with the CA-PA-SA/PAN
form-stable PCCFMs, as shown in Figure 3(f). The results of the FT-IR analysis suggested
that there are no chemical reaction between solid-liquid PCM (i.e., CA-PA-SA ternary
eutectic mixture) and supporting material (i.e., electrospun PAN/Ag-NPs nanofibrous
membranes with different amount of Ag-NPs), and the loaded Ag-NPs additive has no
dramatically effect to the chemical structure of form-stable PCCFMs.

3.3 Thermal energy storage properties

Thermal energy storage and release properties were characterized by DSC analysis. Figure 4
showed the DSC curves of electrospun PAN and PAN/Ag-NPs10 nanofibrous membranes,
the CA-PA-SA ternary eutectic mixture and the CA-PA-SA/PAN/Ag-NPs form-stable
PCCFMs with different Ag-NPs loadings from 0 wt.% to 10 wt.% during melting and freezing
processes. The obtained phase change temperatures (i.e., peak onset temperatures (To),
melting peak temperatures (Tm), freezing peak temperatures (Tf), peak end temperatures (Te))
and enthalpies (i.e., melting enthalpies (ΔHm) and freezing enthalpies (ΔHf)) were summarized
in Table 1. As illustrated in Figure 4 and Table 1, the CA-PA-SA ternary eutectic mixture has
phase change temperatures in the range of about 6-33 oC and its DSC plot reveal a melting
peak onset temperature of approximately 20 oC with the peak position at about 25 oC. As seen
in Table 1, the melting peak end temperatures of all the CA-PA-SA/PAN/Ag-NPs form-stable
PCCFMs shift to lower temperature and fall in the range of 26-29 oC, and their freezing peak
end temperatures also increase by 5-6 oC to above 11-12 oC in comparison to those of the CA-
PA-SA ternary eutectic mixture. The changes in phase change temperatures of the CA-PA-
SA/PAN/Ag-NPs form-stable PCCFMs loading different Ag-NPs content might be attributed
to the weakly attractive interaction between CA-PA-SA ternary eutectic mixture molecules
and inner surface wall of three-dimensional porous network structure of electrospun PAN/Ag-

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NPs nanofibrous membranes. The same findings were also reported by literatures [21-22].
Table 1 also presented that phase change enthalpies of the CA-PA-SA ternary eutectic mixture
were measured as about 145 kJ/kg. For the CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs
including different amount of Ag-NPs, phase change enthalpies slightly decreased due to the
certain mass fraction of supporting materials of electrospun PAN or PAN/Ag-NPs
nanofibrous membranes contained in the form-stable PCCFMs. The data listed in the Table 1
indicated that phase change temperatures and enthalpies of the CA-PA-SA/PAN/Ag-NPs
form-stable PCCFMs were not significantly affected by the Ag-NPs additives. Based on the
results of DSC analysis, the developed CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs with
various mass fractions of Ag-NPs have a suitable phase change temperatures of about 12-26
o
C and high phase change enthalpies of about 133-138 kJ/kg.

3.4 Thermal energy storage and release performance

The heat transfer efficiencies of the CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs were
evaluated by melting and freezing times. Figure 5 showed the temperature-time relational
curves of the CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs with different weight
percentage of Ag-NPs during thermal energy storage and release processes. The melting and
freezing peak temperatures of specimens were determined at around 25 oC and 17 oC,
respectively. As shown in Figure 5, the overall melting times were shortened by nearly 32 %
and 45 % as the mass fraction of the Ag-NPs increase (i.e., 5 wt.% and 10 wt.%) compared to
that of the CA-PA-SA/PAN form-stable PCCFMs, respectively. Furthermore, Figure 5 also
revealed that the required freezing times to reach 17 oC were decreased by 32 % and 51 % for
the CA-PA-SA/PAN/Ag-NPs5 and CA-PA-SA/PAN/Ag-NPs10 form-stable PCCFMs
respectively, which suggested an evident improvement in thermal energy release efficiency.
Based on the above results, it is concluded that the heat transfer rates of the CA-PA-
SA/PAN/Ag-NPs form-stable PCCFMs could be significantly improved by loading the Ag-
NPs additive with high thermal conductivity, which have important contributed for formation
of heat transfer path.

4. CONCLUSIONS
To sum up the conclusions of this work, electrospun PAN/Ag-NPs composite nanofibrous
membranes with different weight fractions of Ag-NPs (5 wt.% and 10 wt.%) were developed
as novel supporting materials for preparation of form-stable PCCFMs. The SEM images
showed that the CA-PA-SA ternary eutectic mixture was successfully loaded into the three-
dimensional multi-porous network structure of electrospun PAN/Ag-NPs composite
nanofibrous membranes due to the effect of capillary and surface tension force. The FT-IR
spectra suggested that there was no chemical reaction between electrospun PAN/Ag-NPs
composite nanofibrous membranes and the CA-PA-SA ternary eutectic mixture. The DSC
analysis revealed that the melting temperature and enthalpy of form-stable PCCFMs were
about in the range of 19-29 oC and 138 kJ/kg, respectively. Moreover, the results also
indicated that the melting/freezing times were significantly shorten by about 32 %/32 % and
45 %/51 % for the CA-PA-SA/PAN/Ag-NPs5 and CA-PA-SA/PAN/Ag-NPs10 form-stable
PCCFMs due to the addition of Ag-NPs with high thermal conductivity. It is concluded that
the developed CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs can be considered as a novel

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thermal energy storage materials for the applications related to storage and retrieval of thermal
energy.

ACKNOWLEDGEMENTS
This research was financially supported by the National Natural Science Foundation of China
(No. 51706092), Education Science Research Program for Young and Middle-aged Teacher
of Fujian Province (No. JAT170445), the Open Project Program of Key Laboratory of Eco-
textiles, Ministry of Education, Jiangnan University (No. KLET1610), the Science and
Technology Pre-research Program of Minjiang University (No. MJY16001).

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Table 1. The peak onset temperatures (To), melting peak temperatures (Tm), freezing peak
temperatures (Tf), peak end temperatures (Te), melting enthalpies (ΔHm) and freezing
enthalpies (ΔHf) of the CA-PA-SA ternary eutectic mixture and CA-PA-SA/PAN/Ag-NPs
form-stable PCCFMs with different Ag-NPs content

Melting process Freezing process

Samples To Tm Te ΔHm To Tf Te ΔHf
(oC) o
( C) o
( C) (kJ/kg) o
( C) ( C) (oC) (kJ/kg)
o

CA-PA-SA 19.72 25.12 33.08 145.7 17.64 15.60 6.29 144.5

CA-PA-SA/PAN 19.10 24.06 27.02 138.6 17.50 17.17 11.30 137.4
CA-PA-SA/PAN/Ag-NPs5 19.27 23.91 29.61 138.2 17.70 17.55 11.71 134.1
CA-PA-SA/PAN/Ag-NPs10 19.57 23.47 26.25 138.1 18.25 17.97 12.51 133.6

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Figure 1 Representative SEM images of electrospun nanofibrous membranes: (a) PAN, (b) PAN/Ag-
NPs5 and (c) PAN/Ag-NPs10

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Figure 2 Representative SEM images of form-stable PCCFMs: (a) CA-PA-SA/PAN, (b) CA-PA-
SA/PAN/Ag-NPs5 and (c) CA-PA-SA/PAN/Ag-NPs10

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Figure 3 FT-IR spectra of (a) Ag-NPs, electrospun (b) PAN and (c) PAN/Ag-NPs10 nanofibrous membranes,
(d) CA-PA-SA ternary eutectic mixture, (e) CA-PA-SA/PAN and (f) CA-PA-SA/PAN/Ag-NPs10 form-stable
PCCFMs

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Figure 4 DSC curves of electrospun PAN and PAN/Ag-NPs10 nanofibrous membranes, CA-
PA-SA ternary eutectic mixture and CA-PA-SA/PAN/Ag-NPs form-stable PCCFMs with
different Ag-NPs content

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Figure 5 Thermal energy storage and release curves of the CA-PA-SA/PAN/Ag-NPs form-stable
PCCFMs with different Ag-NPs content: (a) thermal energy release and (b) thermal energy storage

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Manufacture and Thermo-regulated Performance of an Novel Composite
Fabrics Containing Phase Change Microcapsules
Xing Liu a,b, Yanli Sun a , Rui Wang a,b, Mengxuan Li a, Hua Yang a and Bo Li a
a
School of Textiles, Tianjin Polytechnic University, Tianjin 300387, China
b
Key Laboratory of Advanced Textile Composites, Minstry of Education, Tianjin Polytechnic
University, Tianjin 300387, China

1. INTRODUCTION
For developing antifreezing protection material, a novel composite fabric containing phase
change microcapsules (PCMc) was designed and manufactured. The urea-modified melamine
PCMc was firstly prepared through in situ polymerization, and the surface morphology
and particle size distribution were studied by scanning electron microscopy (SEM). The
microcapsules were then sintered on cotton fabric by dry coating with waterborne
polyurethane and polyacrylate as binder. The results show that polyacrylate finishing fabric
surface was denser and smooth with better heat preservation effect. Waterborne polyurethane
was selected as adhesive for its proper hand feeling instead of polyacrylate. The ΔHm and
ΔHc of the 40% micro PCMc waterborne PU coated fabrics was tested and use to
evaluating the reduction of the temperature changing rate with the external
environment. It had excellent thermo-regulated property and could satisfy the requirements
for applications in thermo-regulated.
With the development of science and technology, textiles have to enhance its performance
according to consumers’ demand. Functional textiles have become the developmental trend
of the textile and attracted more and more attention. Thermo-regulated textile is a
functional textile that has the property of offering suitable response to changes in external
temperature[1, 2]. Phase-change materials (PCM) can store and release large amounts of latent
heat energy during the phase-transition p rocess[3, 4]. PCM have been used to manufacture
thermo-regulated textiles to improve thermal comfort of the human body.
Solid-liquid PCM, like paraffin waxes, are widely applied[5, 6]. When they are applied in
textiles, solid-liquid PCM should be put into microcapsules[7, 8]. Otherwise they will leak
during the melting process, and this affects its energy utilization ratio.
Microencapsulation technology can solve these problems and pack the PCM core with
organic/inorganic shells [9-11]. Incorporating microencapsulated PCM (PCMc) into the fiber
through dispersing it in spinning solution or coating or padding fibers and /or fabrics with
PCMc is an important method to obtain thermo-regulated textiles. F. Salaüna et al.[12]
manufactured a thermo-regulated fabric based on the incorporation of melamine-
formaldehyde microcapsules containing an n-alkane mixture. The results indicate that a
mass ratio binder to PCMc taken between 1:2 and 1:4 is suitable to manufacture thermo-
regulated textile. Luz Sa’nchez-Silva et al.[13] prepared a thermo-regulated textile
using Rubitherm-RT31 microcapsules. Microcapsules were fixed into seven fabric substrates
by a coating technique. The experimental results show that all the coated textiles with 35
wt% of PCMc showed high latent heat storage capacities and significant thermoregulatory
effects.

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Many factors affect the performance of thermo-regulated textiles, such as the binder, the
PCMc compositions, preparation technology and so on. To prepare fabrics with excellent
thermo-regulated property, in this study, we examined the synthesis of PCMc based on a n-
octadecane (C18) core and a melamine-urea-formaldehyde (MUF) shell through in situ
polymerization. Then the PCMc were sintered on cotton fabric by coating technique. The
surface morphology and particle size distribution of PCMc were studied by scanning
electron microscopy (SEM). The effect of the binder type and the PCMc concentration
on the microstructure, phase-change behavior, and thermo-regulated properties of thermo-
regulated fabric also were discussed.

2. EXPERIMENTAL
2. 1 Materials
N-octadecane (C18) was used as a kind of core material provided by Alfa Aesar, U SA.
Melamine (M) with a purity (Tianjin Guangfu Fine Chemical Institution, China), Urea (U)
with a purity (Tianjin Guangfu Fine Chemical Institution, China) and 37% Formaldehyde
solution (F) (Sigma-Aldrich, USA) were used as shell materials. Sodium dodecyl sulfate
(SDS) and polyvinyl alcohol (PVA) were used as emulsifying agents were purchased from
ianjin Kemiou Chemical Reagent Co., Ltd., China. Citric acid and triethanolamine were
used to control the pH were obtained from Tianjin Guangfu Fine Chemical Institution,
China. Waterborne polyurethane (PU) and polyacrylate (PA) were used as binders were
supplied by Tianjin East Printing and Dyeing Factory. Cotton weft knit fabric was
manufactured by us.
2.2 Synthesis of PCMc
PCMc was synthesized by in situ polymerization. The microencapsulation process includes
three key stages; (i) preparation of melamine-urea-formaldehyde (MUF) prepolymer; (ii)
generation of n-octadecane droplets through the SDS and PVA aqueous emulsifier
solution, and (iii) polymerization of the shell materials. The whole procedure is outlined in
Fig.1.

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Figure1. Procedure to synthesize the melamine-urea-formaldehyde (MUF) microcapsules containing
n-octadecane by in situ polymerization

First, the MUF prepolymer was prepared according to our previous studies. [14, 15] 3.81g
melamine and 6.89 g formaldehyde aqueous solution with 70 mL distilled water were
mixed. The pH value of the system was adjusted to 8.5 with triethanolamine. The system
was heated at 70℃ under mechanical stirring for 20 min until became transparent, then
the mixture was cooled down to room temperature (RT=25℃) and 0.915g urea was
added until complete dissolution to obtain the MUF prepolymer solution. Second, 15g
n-octadecane, 1.5g SDS, and 90mLdistilled water were mixed and dispersed under 40℃
at 1000 rpm for 30 min to a form stable oil in-water (O/W) emulsion. Third, after being
adjusted to pH 5 by citric acid, the stirring rate of emulsion was adjusted to 300 rpm，
the temperature was adjusted to 75℃ and the MUF prepolymer solution was
subsequently added dropwise to emulsion, and then followed by reacting for 3.5 h.
Finally, the obtained suspension solution was cooled, PCMc were filtrated and dried at
room temperature.

2.3 Preparation of fabric composited PCMc

PCMc were finished on cotton weft knit fabrics by means of a coating technique, using a
coating machine (supplied by Werner Mathis Co., Ltd., Switzerand). The finishing solution
was prepared by mixing 10.0 wt.% distilled water, binder (waterborne polyurethanes or
polyacrylate), and PCMc at various concentrations. Then the finishing solution was evenly
coated to the surface of the fabric by coating machine and the coating thickness was 0.5mm.
Finally, the finished fabric was pre-baked for 15 min at 80 ℃ environment and baked for 3 min
at 120 ℃ environment. Table I shows the specific process parameters.

Table 1. Finishing solution compositions

sample Micro PCMs/wt% Binder/wt% Distilled

PU PA water/wt%
S1 0 90 10
S2 20 70 10
S3 30 60 10
S4 40 50 10
S5 20 70 10

2.4 Characterization of the PCMc

Fourier transform infrared (FTIR) spectra of the C18, MUF shell, and PCMc were obtained by
FTIR spectroscopy (TENSOR37, Bruker, Germany) in the spectral range from 4000 to 500
cm-1 at a resolution of 4 cm-1.The surface morphologies of the PCMc were observed by using
a field emission scanning electron microscope (SEM) (S-4800, Hitachi, Japan). The particle
size distribution of the PCMc was measured with Image-Pro Plus analysis software, and over
300 PCMc were counted. The thermal properties of the C18 and PCMc were measured with a

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differential scanning calorimeter (Netzsch204F1, Germany) at a heating/cooling rate of 5
℃/min from -20 ℃ to 60 ℃ under a nitrogen atmosphere. Thermogravimetric analysis
(Netzsch STA 409 PC/PG TG–DTA, Germany) was applied to check the thermal stability of
the C18 and microPCMs at a heating rate of 10 ℃/min under a nitrogen atmosphere from room
temperature to 600 ℃.

2.5 Characterization of the fabric composited PCMc

A field emission scanning electron microscope (S-4800, Hitachi, Japan) or scanning electron
microscope (TM3030, Hitachi) was used to observe the surface and cross-section
morphologies of PCMc-treated fabrics. The heat storage capacity of PCMc-treated fabrics was
measured with differential scanning calorimeter. The heating/cooling rate is of 5℃/min from -
20℃ to 60℃ under a nitrogen atmosphere.
There is no standard method for measuring the thermo-regulated properties of thermo-
regulated fabric; we choose to use a heating/cooling test. Heating test: the PCMc-treated
fabrics were put in the constant temperature and humidity laboratory for 24h, and then they
were placed on the flat heat preserve tester at 40℃. The surface temperature of the fabrics was
measured with the infrared thermometer, and the data was recorded in every 20 seconds.
Finally, the heating curve was plotted according to the obtained data. Cooling test: the PCMc-
treated fabrics were placed in a 40 ℃ vacuum oven for 1 h, and then they were put on a on the
flat heat preserve tester at 20℃. The surface temperature of the fabrics was measured with the
infrared thermometer, and the data was recorded in every 20 seconds. Finally, the cooling curve
was plotted according to the obtained data.

3. RESULTS AND DISCUSSION

3.1 The Surface Morphologies and the Particle Size Distribution of the PCMc
The microstructures and surface morphologies of the PCMc were investigated with scanning
electron microscopy, and the results are shown in Figure 2. As shown clearly in Figure2 (a),
the majority of the PCMc was intact and well dispersed. Figure2 (b) shows that the surface of
PCMc was smooth and their shape was close to spherical. However, as shown distinctly in
Figure 2, all of the surfaces of the PCMc had some dimples. The reason was that C18 shrank
from the melting state to the crystal state during the phase-change process as a result of the
shrinkage of expansion space[16, 17].
The particle size distribution of the PCMc is presented in Figur3, and broadened particle size
distributions were obtained. The particle size distribution of the PCMc generally presented the
characteristics of Gaussian distribution. The average particle size of the PCMc was
approximately 45.15μm.

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 Figure 2. SEM images of PCMc: (a) ×100; (b) ×1000

Figure 3. Particle size distributions of PCMc

3.2 FTIR Spectra of the MicroPCMs

The FTIR spectra of the C18, MUF shell, and PCMc are presented in Figure4. In the spectrum
of C18 [Figure 4(a)], the peaks at 2923 and 2851 cm-1 were identified as the stretching
vibrations of C-H, the peak at 1466 cm-1 corresponded to -CH2 and -CH3 deformation
vibrations, and the peak at 719 cm-1 corresponded to -CH2 in-plane rocking vibrations. As
shown in Figure 4(b), a broad and strong absorption peak around 3431 cm-1 was caused by the
stretching vibrations of N-H and O-H, the peaks at 1588 and 1339 cm-1 belonged to C=N and
C-N stretching vibrations, the bending vibration characteristic of the triazine ring was found at
approximately 812 cm-1. As mentioned before, the characteristic peaks of the C18 and MUF
shell appeared in the spectrum of the PCMc [Figure 3(c)], and no new peak was observed. This
verified that the core and shell had just physical interactions, and C18 was encapsulated in the
PCMc.

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 Figure 4. FTIR spectra of C18 and micro PCMs: (a) C18, (b) MUF shell, (c) PCMc.
3.3 Phase-Change Properties and Thermal Storage Capability of the PCMc

Figure 5. DSC thermograms of C18 and PCMc.

Table 2. The phase change properties of C18 and PCMc

Samples Tm(℃) ΔHm(J/g) Tc(℃) ΔHc(J/g)

C18 27.2 307.1 25.5 298.8
microPCMs 26.6 239.8 24.8 242.8

The phase-change behaviors of the C18 and the PCMc were investigated by differential
scanning calorimetry (DSC). The thermograms are displayed in Figure5 and the specific data
of the phase-change characteristic are presented in Table II.. From Figure5, the melting
temperature (Tm) and crystallization temperature (Tc) of the PCMc were found to shift to
slightly lower temperatures in comparison with those of C18 because the PCMc had bigger
surface areas and the motion of C18 was confined inside a narrow space[18, 19].
In addition, the crystallization enthalpy (ΔHc) and melting enthalpy (ΔHm) of the PCMc were
found to decrease significantly in comparison with those of C18. The shell never underwent
any phase change, and only C18 as PCM could release and store latent heat in the DSC

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scanning temperature range. Therefore, the phase-change enthalpies of the microPCMs
decreased. The ΔHc and ΔHm of the PCMc was 239.8 and 242.8J/g, respectively.

3.4 Thermal Stability of the PCMc

Thermogravimetry diagrams of the C18 and PCMc are presented in Figure 6. It is clearly
showed that the weights of C18 and PCMc decreased with increasing temperature. C18
demonstrated a typical one step degradation process; it begins to lose weight around 150℃ and
degradation was completed at about 225℃. This revealed the poor thermal resistance of C18.
However, the PCMc present a roughly similar two-step degradation process. The first stage of
weight loss started at approximately 21℃; this resulted from C18 thermal degradation,
including evaporation from inside the PCMc and leakage from the ruptured shell. The second
stage of weight loss occurred at about 390℃; this was ascribed to the thermal degradation of
the MUF shell. This illustrated that the shell could have protected C18 from losing weight
quickly.

Figure 6. Thermogravimetry spectra of C18 and PCMc.

3.5 The Surface Morphologies and Phase-Change Properties of the Microcapsules

Coated Fabrics with Different Adhesives
The surface morphologies of the PCMc coated fabrics with different adhesives were
investigated with scanning electron microscopy (SEM), and the results are shown in Figure7.
As shown in Figure7, the PCMc coated fabrics have a distinct appearance before and after
coating. Polyacrylate finishing fabric surface is denser and smooth, waterborne polyurethane
finishing fabric surface is better but there are a few holes. The reason was that the interfacial
tension of the polyacrylate is better than that of the waterborne polyurethane, which made
polyacrylate and PCMc were adhered on the surface of fabric to form a layer of film, so the
surface of the polyacrylate finishing fabric was better.

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Figure 7. SEM images of the surface morphologies of the PCMc coated fabrics with different adhesive:
(a) Raw cotton knitted fabric;(b) Waterborne polyurethane finishing fabric;(c) Polyacrylate finishing
fabric.

The phase-change behaviors of the PCMc coated fabrics with different adhesives were
investigated by DSC, and the thermograms are showed in Figure8. According to the figure8,
theΔHm andΔHc of the waterborne polyurethane finishing fabric is 19.8 and 18.65J/g,
respectively; theΔHm andΔHc of the polyacrylate finishing fabric is 30.57 and 28.17J/g.
Therefore, under the condition of the same phase change microcapsule content, the heat
enthalpy of the polyacrylate finishing fabric was larger and the energy storage effect was better
due to the polyacrylate could better bond with fabric and PCMc. However, polyacrylate
finishing fabric had a harder hand feeling and was not suitable for textile applications. So we
use waterborne polyurethane as adhesive.

Figure 8. DSC thermograms of the microPCMs coated fabrics with different adhesive.

3.6 The Surface Morphologies, Phase-Change Properties and thermo-regulated

properties of the Microcapsules Coated Fabrics with Different Concentration
The cross-section morphologies of the PCMc coated fabrics with different concentration were
investigated with SEM, and the results are shown in Figure9. As the Figure9 shows, the PCMc
attached to the surface of the fabrics gradually increase with the increase of the mass fraction
of the PCMc. The waterborne polyurethane had good interfacial compatibility with the surface
of the cotton knitted fabric. The adhesive was not impregnated into the fabric and also could
ensure the soft hand feeling of the fabric after finishing.

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Figure 9. SEM images of the cross-section morphologies of the PCMc coated fabrics with different
concentration: (a) 0% ;(b) 20% ;(c) 30% ;(d) 40%.

The phase-change behaviors of the PCMc coated fabrics with different concentration were
investigated by DSC, and the thermograms are showed in Figure10. As shown, when the coated
fabric uses the finishing solution without PCMc, the fabric has no store and release heat energy.
While the coated fabric uses the finishing solution contain PCMc can store and release heat
energy during cooling/heating process, and the heat enthalpy gradually increases with the
increase of the mass fraction of PCMc. TheΔHm of the PCMc coated fabrics with different
concentration was 19.8(20%), 32.7(30%), and 39.5(40%)J/g, respectively; theΔHc was
18.65(20%), 29.24(30%), and 38.85(40%)J/g, respectively.

Figure 10. DSC thermograms of the PCMc coated fabrics with different concentration.

The thermo-regulated properties of the PCMc coated fabrics with different concentration were
investigated with heating/cooling test, Figure11 (a), (b) presents the heating curve and the
cooling curve, respectively. According to figure11 (a), the heating rate of different samples is
not obviously difference at the initial stage of heating. From the results of the previous DSC
test, the Tm of PCMc was 26.6 ℃, so when the temperature rise to about 27 ℃, the heating
rate of the PCMc coated fabrics have significantly slowed, and the trend is more obvious with
increase of the mass fraction of PCMc. During the process of heating, when the temperature
was higher than the transformation point of the PCMc, the core material C18 began to phase
transformation behavior and absorb heat, the heating rate of the PCMc coated fabrics slowed
down[20]. As the heating time continues to lengthen, C18 completely melted and cannot absorb
heat; the temperature of different samples is gradually consistent.
As shown distinctly in Figure 11(b), the cooling curve of the coated fabric without PCMc is
smooth and has no obvious inflection point with time lengthen. However, the cooling curves
of the PCMc coated fabrics generally appear inflection point around 25℃, and the cooling rate
slowed down. The trend is more obvious with increase of the mass fraction of PCMc. When

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the temperature continues to decrease, the cooling rate presents an accelerated trend, and the
temperature is basically the same as that of the coated fabric without PCMc. During the process
of cooling, C18 began to phase transformation behavior and release heat, the cooling rate of
the PCMc coated fabrics slowed down. As the cooling time continues to lengthen, C18
completely crystallized and cannot release heat; the temperature of different samples is
gradually consistent. Compared with the coated fabric without PCMc, the heating rise and
cooling rate of the PCMc coated fabrics significantly slowed down. It shows that the prepared
fabric has good thermo-regulated property.

Figure 11. The heating curve and the cooling curve of the microPCMs coated fabrics with different
concentration: (a) heating curve; (b) cooling curve.

Based on the above analysis, with the increase of the content of PCMc in the finishing solution,
the more PCMc attached to the surface of fabric and the larger heat enthalpy was obtained.
TheΔHm and ΔHc of the 40% PCMc coated fabrics was 39.5 and 38.85J/g, and has excellent
thermo-regulated property.

4. CONCLUSIONS
PCMc based on a C18 core and a MUF shell was successfully synthesized through in situ
polymerization. The resulting PCMc exhibited a spherical and smooth morphology, a well-
defined core-shell structure, and a broadened size distribution. Moreover, there was no
chemical reaction among the C18 and MUF. The heat enthalpy of the PCMc still reached more
than 230 J/g. Polyacrylate finishing fabric surface was denser and smooth, theΔHm andΔHc
of the polyacrylate finishing fabric is 30.57 and 28.17J/g. However, polyacrylate finishing
fabric had a harder hand feeling, so waterborne polyurethane as adhesive. With the increase of
the content of PCMc in the finishing solution, the more PCMc attached to the surface of fabric
and the larger heat enthalpy was obtained. TheΔHm and ΔHc of the 40% PCMc coated fabrics
was 39.5 and 38.85J/g, and has excellent thermo-regulated property. It could satisfy the
requirements for applications in thermo-regulated.

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[17] YOU M, ZHANG X X, WANG J P, et al. Polyurethane foam containing
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Dyeing attributes of Dalbergia Sisso towards Cotton Fabric
Muhammad Jawad Ul Rehman, Muhammad Tahir Hussain*, Munir Ashraf, Asfand Yar
Khan, Abdur Rehman
Functional Textile Research group, National Textile University, Faisalabad, Pakistan
*Corresponding author: mtahirhussain@gmail.com

ABSTRACT
Due to growing environmental concerns, the usage of natural dyes for coloration of textiles is gaining
special attention nowadays. The present study deals with dyeing of cotton fabric with natural dye
extracted from leaves of Dalbergia Sissoo. The as-extracted dye when applied on cotton fabric using
potash alum, ferrous sulfate and zinc sulfate as mordants showed reasonably good tinctorial strength
on fabric. The shade, hue and strength depended upon the type of mordant used. The color strength
of dyed fabric was determined by K/S values.

1. INTRODUCTION
Natural dyes may be a rich source of dye stuff in developing countries and it also may prove
to be source of income through sustainable harvest and sale of these plants because these
plants are main source of natural dyes. Some animals have also been used a source of coloring
molecules which can be used as a coloring source for different materials.
When the synthetic dyes were discovered in 1856, then dyeing of textiles by the use of natural
dyes fell down greatly because synthetic dyes possessed very much versatile properties, easy
preparation, low cost and reproducibility of performance properties. Presently it is estimated
that over 10,000 different dyes and pigments are used in industry amounting to almost
10,000,000 tons per annum [1]. Serious health and environmental hazards are posed during
their production process. Their application results into the release of huge amounts of unfixed
colorants resulting to a disturbed eco-balance. Presently awareness among the people about
these environmental and health hazards has increased resulting to an increased trend towards
natural dyes because of their have better biodegradability and higher compatibility with the
environment. Moreover, natural dyes are renewable, non-carcinogenic and non-toxic [2].
Majority of natural dyes have been derived from plant sources [3]. Dalbergia Sissoo is an
evergreen tree found allover Pakistan that reaches a height between 15-30 meters. It has
alternately arranged compound deep green elliptical to ovate leaves which are tapering to a
point, usually 2.5-3.6 cm in diameter. It is a source of commercial economic and durable
timber used for preparation of household furniture [4].
Dalbergia Sissoo is a very common tree and its leaves are available most of the time in a
year, so we tried to evaluate its leaves for ecofriendly natural dyeing of cotton. For this
purpose natural colorant was extracted from leaves for dyeing of cotton fabric and different
dyeing parameters were optimized to achieve adequate color and fastness results. Different
mordanting techniques were also used to improve shade depth and fastness properties on
cotton.

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 Figure 1: Dalbergia sissoo leaves

2 MATERIALS AND METHODS

2.1 Source
Leaves of Dalbergia sissoo (Figure 1) were collected from National Textile University,
Faisalabad, Pakistan. These were dried in shade and then ground to fine powder.

2.2 Substrate
Plain weave 100% cotton fabric, having gsm 121g/m2 with 87 epi and 70 ppi, was purchased
from local market and used for dyeing.

2.3 Chemicals used:

AR grade metallic salts zinc sulphate, ferrous sulphate, alum (K2SO4, Al2(SO4)3.24H2O)
were used as mordants. Laboratory grade NaOH, CH3COOH and NaCl were used. Soaping
off of the dyed cotton fabric was made by a commercially available detergent “teepol”.

2.4 Extraction
Natural dye from shade dried and powdered leaves (40 g/L) was extracted by 1% NaOH
solution at 95C. The filtrate was used as dye liquor without further dilution. The dyeing
liquor wherever mentioned was prepared with a material to liquor ratio of 1:25.

2.5 Application of Dye

Exhaust method was used for application of the extracted dye on bleached and scoured 100%
cotton fabric. After adding the fabric to the dye bath, NaCl was added as exhausting agent.

2.6 Optimization of Dyeing Parameters

For maximum dye uptake and color strength of cotton fabric, following parameters were
optimized.

2.6.1 pH
Dyeing with dyeing liquor was studied at six different pH values of 7, 8, 9, 10, 11 and 12
using goods to liquor ratio of 1:25 at temperature 95C for time interval of 45 min. Dyed
samples were soap washed using 2g/L detergent at 60C for 10 minutes.

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2.6.2 Temperature
Fabric was dyed at five different temperatures (C) of 60, 70, 80, 90 and 100.

2.6.3 Dyeing time

Cotton fabric was dyed for four different time intervals of 30, 45, 60 and 75 minutes at 95C,
using goods to liquor ratio of 1:25 at pH 7 followed by soap washing of the samples using
2g/L detergent at 60oC for 10 minutes.

2.6.4 Mordanting
Effect of mordants was studied by three different techniques: meta-mordanting, post-
mordanting and pre-mordanting. Potassium aluminum sulfate (potash alum), ferrous sulfate
and zinc sulfate mordants were used [5].
During pre-mordanting, before dyeing, cotton fabric was soaked in mordanting solution (40
g/L) with constant stirring with a goods to liquor ratio of 1:25 for 20 minutes at 60C. For
post-mordanting, similar treatment was given to the fabric after dyeing process while for
meta mordanting (simultaneous), the mordants were mixed in the dyebath during dyeing
process. The fabric sample was dyed at goods to liquor ratio of 1:25 with pH 7 at 95C
temperature for 45 minutes duration followed by soap washing.

2.6.5 Salt (NaCl)

Different amounts of salts (NaCl) were added to dyeing bath to study their effect on
exhaustion of dye from dye bath towards substrate during dyeing process.

2.7 Testing
Colour fastness to washing, light and rubbing were determined by standard test methods ISO
105-C06:2010, ISO 105-B02:2014 and AATCC 8-2007 respectively. The K/S values were
calculated by Kubelka-Munk equation K/S= (1 − R)2 / 2R. In this equation, “R” shows
reflectance at λmax, “K” indicates absorption coefficient and “S” is scattering coefficient.

3. RESULTS AND DISCUSSIONS

3.1 Effect of dyeing conditions and mordanting techniques on color strength and CIE
Lab values
3.1.1 pH
Effect of change in pH of dyeing bath on color strength (K/S value) is shown in Table 1. It
shows maximum color strength at pH-7. By increasing the pH values, the shade depth was
decreased. At neutral pH value, the exhaustion rate was satisfactory and hence shade depth
was maximum. But as the pH of dyebath was increased from neutral, the exhaustion rate of
dye was decreased resulting to a decreased color yield. This may be due to creation of similar
negative charges at alkaline pH on both the cellulose and dye molecules since the natural dye
molecules are mostly polyphenolic compounds which are converted to negatively charged
phenoxide ions at basic pH.

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 Table 1. Effect of dyeing pH on color strength
pH value CIE L* CIE a* CIE b* CIE C* CIE h K/S
7 75.68 -2.95 13.68 13.99 102.17 1.112
8 77.65 -3.33 10.31 10.84 107.88 0.704
9 78.67 -2.97 9.71 10.15 107.01 0.549
10 78.04 -4.09 10.82 11.57 110.68 0.668
11 78.79 -3.41 9.47 10.06 109.83 0.503
12 78.62 -2.18 7.86 8.16 105.49 0.44

3.1.2 Temperature
Effect of increasing temperature of dyeing bath on shade depth K/S values is given in Table
2 which indicates that K/S values are generally increased with increasing temperature. This
effect is usually due to swelling of fibers at higher temperatures thus making the penetration
of colorant molecules easier into the amorphous sections of fibers.

Table 2. Effect of dyeing temperature on color strength

Temperature
CIE L* CIE a* CIE b* CIE C* CIE h K/S
(C)

60 79.79 -1.70 7.50 7.69 102.78 0.506

70 78.92 -1.72 8.00 8.19 102.13 0.574

80 80.50 -1.56 7.17 7.34 102.29 0.444

90 77.40 -2.21 10.66 10.88 101.73 0.85

100 77.10 -2.34 10.98 11.22 102.03 0.86

3.1.3 Dyeing Time

Table 3 shows the effect of dyeing time on K/S values. It is evident that color strength is
increased with increase in dyeing time until dye exhaustion reaches equilibrium and there is
no significant increase in color strength after further increases in dyeing time

Table 3. Effect of dyeing Time on color strength

Time
CIE L* CIE a* CIE b* CIE C* CIE h K/S
(Min.)
30 76.81 -2.71 12.46 12.75 102.25 1.025

45 75.72 -2.54 12.01 12.28 101.95 1.031

60 76.86 -2.11 11.26 11.45 100.63 0.847

75 75.00 -1.96 12.17 12.32 99.13 1.062

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 3.1.4 Goods to liquor ratio
The effect of goods to liquor ratio on K/S values was evaluated using different liquor
ratios. The maximum dye uptake was obtained at goods to liquor ratio of 1:25. When dye
exhaustion reaches equilibrium, then there was no significant increase in dye uptake by
further increase in liquor ratio.

3.1.5 Effect of mordants

Table 4 given the effect of different mordants on K/S and CIE Lab values. The mordanting
activity sequence for the pre-mordanting method was FeSO4 > ZnSO4 > No mordant (NM)
> AlK2(SO4)2 and the meta-mordanting AlK2(SO4)2 > FeSO4 > No mordant (NM) > ZnSO4.
In the post-mordanting technique, the sequence FeSO4 > AlK(SO4) > ZnSO4 > NM was
observed. Ferrous sulfate mordant yielded best dyeing results in all cases except in meta
mordanting. It was observed that cotton fabrics dyed with aluminum potassium sulfate and
zinc sulfate produced a variety of greenish shades.

Table 4. Effect of mordants on color strength

Mordantin Type of
CIE L* CIE a* CIE b* CIE C* CIE h K/S
g mordanting
No
NM 76.24 -2.11 10.58 10.79 101.28 0.865
mordanting
AlK(SO4)2.12H2O 77.94 -1.8 8.48 8.67 101.99 0.592
Pre-
Mordanting FeSO4.7H2O 67.08 3.54 15.81 16.2 77.39 1.574
ZnSO4.7H2O 73.92 -3.16 10 10.49 107.56 0.889
AlK(SO4)2.12H2O 71.38 -1.91 20.52 20.61 95.31 1.859
Meta-
Mordanting FeSO4.7H2O 70.32 1.61 17.25 17.33 84.68 1.425
ZnSO4.7H2O 75.89 -1.27 11.5 11.57 96.3 0.694
AlK(SO4)2.12H2O 75.24 -1.68 14.47 14.56 96.61 1.118
Post-
FeSO4.7H2O 72.42 -0.59 19.09 19.1 91.78 1.652
Mordanting
ZnSO4.7H2O 74.26 -5.2 13.56 14.52 110.98 1.081

3.1.6 Effect of salt

The effect of salt (NaCl) was studied by adding its different amounts during dyeing process.
Table 5 shows that addition of salt increased the exhaustion of dye from dye bath towards
substrate. Shade depth and K/S values were increased as the amount of salt was increased
which can be attributed to neutralization of negative charge due to zeta potential of cotton by
sodium ions in the dye bath.
Table 5. Effect of salt on color strength
Salt CIE L* CIE a* CIE b* CIE C* CIE h K/S
No salt 77.74 -1.59 8.56 8.7 100.52 0.635
5 g/L 76.26 -1.72 10.76 10.9 99.07 0.854
15 g/L 76.5 -2.74 12.26 12.56 102.61 0.951

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3.2 Effect of dyeing conditions and mordanting techniques on colorfastness properties
3.2.1 Effect of pH
Table 6 shows the effect of pH on colorfastness properties like wash fastness, light fastness,
wet rubbing fastness and dry rubbing fastness which were found: fair, poor and good to
excellent respectively. It is very clear from Table 6 that the fixation of dyes to cotton fiber is
weak at high pH values which ultimately results in poor colorfastness properties. A pH range
of 7-8 was found optimum for achieving good colorfastness.

Table 6. Effect of dyeing pH on colorfastness

Condition Leaves Extract
Wet Dry
Dyeing Wash Light
Rubbing Rubbing
pH fastness fastness
fastness fastness
7 2-3 1-2 4-5 5
8 2 1 4-5 5

9 1-2 1 4-5 5
10 2 1 4-5 5

11 3 1 5 5

12 1-2 1 4-5 5

3.2.2 Effect of Temperature

The effect of dyeing temperature on colorfastness properties is shown in Table 7. Wash
fastness, light fastness, wet rubbing fastness, and dry rubbing fastness were found: fair to
good, poor and good to excellent respectively. The temperature range of 100C was found
optimum for achieving good colorfastness.

Table 7. Effect of dyeing temperature on colorfastness

Condition Leaves Extract
Dyeing
Wash Light Wet Rubbing Dry Rubbing
Temperature,
fastness fastness fastness fastness
C
60 2-3 1-2 4-5 5

70 2-3 1-2 5 5
80 2-3 1 4-5 5

90 2-3 1-2 4-5 5

100 2-3 1 4-5 5

3.2.3 Effect of dyeing time

Variation in colorfastness properties with respect to dyeing time is shown in Table 8. A
longer dyeing time has resulted higher color strength until dye exhaustion reaches

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equilibrium and there is no significant increase after further increases in dyeing time. At
equilibrium state, most of the fiber ionic sites are occupied by colorants and there are very
little chances for further attachment. The optimum time for dyeing of cotton fabrics was
obtained at 60-70 min.

Table 8. Effect of dyeing Time on colorfastness

Condition Stem bark Extract
Dyeing Wash Light Wet Rubbing Dry Rubbing
Time (min) fastness fastness fastness fastness
30 2 1-2 4-5 5

45 2 1-2 5 5

60 2 1-2 4-5 5

75 2 2 4-5 5

Table 9. Effect of mordanting techniques on colorfastness

Type of Wash Light Dry Rubbing Wet Rubbing

Mordanting K/S
mordanting Fastness Fastness Fastness Fastness

No
NM 2 1-2 5 5 0.865
mordanting
AlK(SO4)2.12H2O 1-2 1-2 5 5 0.592
Pre-
Mordanting FeSO4.7H2O 2-3 7-8 5 3-4 1.574
ZnSO4.7H2O 2-3 1-2 5 5 0.889
AlK(SO4)2.12H2O 1-2 3-4 5 4-5 1.859
Meta-
Mordanting FeSO4.7H2O 3 6-7 5 4-5 1.425
ZnSO4.7H2O 1-2 2-3 5 4-5 0.694
AlK(SO4)2.12H2O 2-3 2-3 4-5 4-5 1.118
Post-
FeSO4.7H2O 3-4 4-5 4-5 3 1.652
Mordanting
ZnSO4.7H2O 1-2 1-2 5 4-5 1.081

3.2.4 Effect of Mordanting

The effects of different mordants and mordanting techniques are shown in Table 9, the
sample dyed without mordant resulted in good washing and rubbing fastness but poor light
fastness. Ferrous sulfate delivered the overall good to excellent light and rubbing fastness
and good wash fastness properties while zinc and potassium aluminum sulfate delivered fair
light fastness, excellent rubbing fastness and fair to good wash fastness. In general, wash
fastness, light fastness and rubbing fastness properties have been observed to be increased
by mordanting.

4. CONCLUSIONS
The natural dye extracted from leaves of Dalbergia Sissoo plant was applied to 100% cotton
fabric (scoured and bleached) through exhaust dyeing process. Optimum dyeing effect and

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good color strength were achieved at temperature near to boiling (100C) for 60-70 minutes
dyeing time at pH 7 for leaves extract using goods to liquor ratio of 1:25. The shade depth
was improved at higher dyeing temperature and time. Mordanting was also helpful in
achieving a variety of color shades. Dyed cotton fabric exhibited good to excellent color
fastness to rubbing and poor to fair light fastness which was improved to good to excellent
by mordanting with ferrous sulfate. Overall wash fastness was rated fair to good. These
results show that Dalbergia Sissoo can prove to be a candidate for good quality natural dyeing
of cotton fabrics.

ACKNOWLEDGEMENT
This research was supported by National Textile University, Faisalabad, Pakistan.

REFERENCES
[1] H. Goodarzian and E. Ekrami, 2010, World Applied Sciences Journal, 9(4), 434-436.
[2] S.S. Kulkarni, A.V. Gokhale, U.M. Bodake and G.R. Pathade, 2011, Universal Journal
of Environmental Research and Technology, 1(2): 135-139.
[3] T. Bechtold and R. Mussak, Handbook of natural colorants. John Wiley and Sons Ltd,
2009.
[4] “Dalbergia sissooo Roxb . ex DC . Fabaceae - Papilionoideae” 2009.
http://www.worldagroforestry.org/treedb/AFTPDFS/Dalbergia_sissoo.PDF.
[5] L. Janani, L. Hillary and K. Phillips, International Journal of Scientific and Research
Publications, vol. 4, no. 10, pp. 1-6, 2014.

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A Spinning Method of Staple Fiber/Staple Fiber Core-Spun Yarn
Dong Weiguo
Tianjin Polytechnic University, China

ABSTRACT
This paper presents a spinning method of staple fiber/staple fiber core-spun yarn on a modified ring
spinning frame. The forth roller and a top rubber-covered roller with a circumferential groove are
used before the front roller in the traditional three-roller drafting mechanism. Thus, two fiber strands
are delivered in unequal length and staple fiber/staple fiber core-spun yarn is formed since the longer
fiber strand wraps the shorter one. The unequal delivery principle and the condition of being coated
completely are analyzed theoretically. The polyester staple fiber/cotton staple fiber 65/35 core-spun
yarn with polyester as core yarn was spun and the characteristics of yarn in 28tex were tested. The
results show that the core yarn is coated completely by the outer wrapping fiber and that the
performances of yarn are good. The strength of yarn is 16.84cN/tex and the CV is 5.9 %.
Keywords: staple fiber/staple fiber core-spun yarn; spinning method; principle; theoretical analysis

1. INTRODUCTION
It has been the most used and mature method of spinning core-spun yarn that a filament
feeding mechanism is added beside the original drafting mechanism on ring spinning frame.
The filament and staple fiber sliver are merged at the front nipper jaw then the core-spun
yarn with the filament as core yarn is formed after twisting and winding. Polyester, spandex,
nylon and other synthetic filaments can be used as the core filaments. Natural fibers, such as
cotton, wool, silk, linen, synthetic staple fibers and these blended fiber strands can be used
as the outer wrapping fibers.
A method of producing two rovings and filament core-spun yarn was presented based on
traditional spinning methods [1, 2]. Many researchers have investigated the property of core-
spun yarns. Some tensile properties of polyester filament/Wool Core-Spun Yarns were
studied [3]. The relationship between the wrinkle resistance and twists in the fabric of
nylon/cotton core-spun yarns was analyzed [4]. A comparison of cotton/polyester core and
staple blend yarns was made and the differences of the main mechanical factors were
discussed [5]. The properties of polyurethane filament/cotton core-spun yarn were measured
then the factors influencing the strength and the elastic performance of this yarn were
discussed and the breaking strength of this yarn was predicted on the basis of the mechanical
properties of polyurethane filament and cotton yarn [6].
The method of spinning staple fiber/staple fiber core-spun yarn on ring spinning frame by
use of staple fiber strands emerged in the 1990s. There is little description of this method in
current papers. Sawhney et al developed a method of producing cotton-covered polyester
staple-core yarn on their own slightly modified ring spinning frame on which three rovings
were combined and twisted in traditional ring spinning way to form the core-spun yarn [7].
This paper describes a method of spinning staple fiber/staple fiber core-spun yarn and study
the principle of its spinning. This method and the relevant device have gained a China
Invention Patent [8].

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2. THE SPINNING PRINCIPLE OF STAPLE FIBER/STAPLE FIBER CORE-SPUN
YARN
2.1 The spinning mechanism and process
As shown in figure 1, on a ring spinning frame, the forth roller 7 was set in front of the front
roller 1 in the original drafting mechanism. A rubber-covered roller 10 with a circumferential
grooved additional head top roller 10 with circumferential groove 9 was on the forth roller
7. The forth roller and the front top roller formed a head nipper jaw. The gauge of the forth
roller nip and drafting nip could be adjusted. Besides, a fiber strand positioned device 2 was
set between the forth roller 7 and the front roller 1 to fix the distance of the core fiber strand
and the wrapped fiber strand. Figure 1 shows the principle of spinning staple fiber/stapler
fiber core-spun yarn.
A core staple fiber strand 5 was drafted by the three-roller drafting mechanism, guided by
the groove 4 of positioned device 2, sent into the head nipper jaw formed by the forth roller
7 and the fourth top roller 10 to be held and delivered. The outer wrapping fiber strand 3 was
also drafted by the three-roller drafting mechanism, guided by the groove 8 of positioned
device 2 , delivered to the circumferential groove 9 without being held. Then the two fiber
strands were combined and twisted into the staple fiber-core/staple fiber-covered spun yarn
6 at the head nipper jaw. The practical process of spinning staple fiber/staple fiber core-spun
yarn is shown in Figure 2.

Figure 1: The principle of spinning staple fiber/stapler fiber core-spun yarn. 1—the front roller of
the three-roller drafting mechanism the three rollers 2—positioned device 3—the outer wrapping
fiber strand 4、8—left and right grooves 5—the core fiber strand 6—the core-spun yarn 7—the
fourth roller 9—circumferential groove 10—the fourth top roller

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 Figure 2: The practical process of spinning staple fiber/staple fiber core-spun yarn

2.2 The spinning principle of staple fiber/staple fiber core-spun yarn

According to the spinning mechanism and process, there are three twisting triangles that are
A, C, O in producing the staple fiber/staple fiber core-spun yarn, as shown in Figure 3, and
the three locations A is the nipping point of the outer wrapping fiber strand, C is the nipping
point of the core fiber strand, and O is the convergent point of the two strands .
In the spinning process, the path length gauges from the convergent point to the nipping
points of the two fiber strands are not equal: the path length gauge of the outer wrapping
fiber strand is OBA and that of core fiber strand is OC. The OBA gauge of the outer wrapping
fiber strand is far longer than the OC fiber length while the gauge of core fiber strand is
shorter than it. Therefore, the controlled states of two fiber strands are different. Then the
core fiber strand is controlled strictly by the head nipper jaw without extra elongation and
the outer wrapping fiber strand is drafted owing to the relative slippage of fibers in the strand
under the spinning tension. For this reason, in the triangle formed of the three points B, C,
O, the side OB is longer than the side OC. The outer wrapping fiber strand is overfed to the
core fiber strand and thus the outer fiber strand wraps the core fiber strand in the form of
spiral when twisted. Ideally, three points form a right triangle with the outer fiber strand as
the hypotenuse and the center of core-spun yarn coincides with the center of outer fiber
strand, as shown in Figure 3.
Based on the mechanical analysis of convergent point, the formation mechanism that the side
OB is longer than the side OC in the triangle BCO is drawn. The assumption is proposed that
the wrapping yarn and core yarn above the convergent point and the core-spun yarn under
the convergent point all have a circular cross section. According to the theoretical mechanics,
the force analysis of convergent point in normal state is presented. The mechanical relations
are shown in Figure 4.

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Figure 3: The schematic drawing of twisting triangles and path lengths of fiber strands mechanical
analysis on the convergent point

Figure 4: The mechanical analysis of the convergent point

 Fx =0  F1 sin 1  F2 sin 2  0 （1）

 Fy  0 F1 cos 1  F2 cos  2  F  0
（2）
My  0
（3）
Mc1 sin 1  Mc 2 sin 2  F1 sin 1R1  F2 sin 2 R2  M1 cos1  M 2 cos2  M  0
0<1  90 0   2  90
（4）

Where,
F—the spinning tension;
F1 、F2——the tension of the wrapping yarn and core yarn above the convergent point
respectively;
R1、R2——the radius of the cross section in wrapping yarn and core yarn respectively;
M——the torsional moment under the convergent point;
M1、M2——the torsional moment of wrapping yarn and core yarn above the convergent
point respectively;
Mc1、Mc2——the bending moment of wrapping yarn and core yarn respectively;

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θ1、θ2—— the angle between the wrapping yarn and core yarn and the Y axis respectively.
Formula (1) and Formula (2) are converted.
F sin  2 （5）
sin  = 2
1
F1

F  F2 cos  2 （6）
cos 1 
F1
Formula (5) and Formula (6) are squared and added up.

 F 2  F12  F22 
1  cos 1   （7）
 2 FF1 

 F 2  F22  F12 
 2 = cos 1   （8）
 2 FF2 

The tension of the wrapping fiber strand is the total frictional force, namely drafting force,
when the faster fibers draw out from the slower fibers in relative fiber slippage in strands in
OBA. The drafting force is related to frictional force in fibers, the length and fineness of
fibers and the draw ratio. When the draw ratio is bigger, the stretching force is smaller.
In initial stage of spinning, the tensions of the fiber strand OB and strand OA are equal, then
F1=F2. When the tension F1 is greater than the strand stretching force, there is mutual
OB
slippage in fiber strand and the draw ratio E  . The draft force decreases along with the
OC
increasing draw ratio, so F1 is smaller than F2. According to Formula (1), it can be concluded
that the angle θ1 is bigger than θ2 and that the angle θ2 is quite small. The twist becomes
smaller owing to the resistance in delivery from the convergent point O to the nipping point
A. Therefore, the friction between fibers is smaller, which easily meets the requirement that
F1 is greater than the strand draft force.

3. THE THEORETICAL ANALYSIS OF COMPLETE COVERAGE CONDITIONS

The assumption is proposed that the cross section of core yarn is a circle with radius R and
that the cross section of wrapping yarn is an ellipse with the long half axis a and the short
axis b. In an ideal state, the wrapping yarn wraps one circle when the core yarn rotates one
circle, as shown in Figure 5(a), and the axis of wrapping yarn forms a spiral. The two adjacent
spirals are shown in Figure 5(b). The pitch is h, which is the output length when the core
yarn rotates one circle. The spiral angle is β and the distance between the two spirals is L.
The distance L should be 2a if the core yarn is covered completely.

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 Figure 5: (a) The schematic diagram of core-spun yarn (b) The unfolded drawing of spiral lines

According to the Figure5: (a)and (b),

2a
sinβ （11）
h

( R  b)
2π　
tanβ （12）
h

Based on the Formula (11) and Formula (12),

2aπ( R  b)
h
π　 2
( R  b) 2  a 2
(13)

The core yarn twist should be that as followed,

1 π　2
( R  b) 2  a 2
T 
h 2aπ　 ( R  b) (14)

Formula (14) fits for the condition that R+b>a. When R+b<a, the wrapping yarn wraps all
round then the core yarn could be covered completely in any twists.

4. SPINNING EXPERIMENT
The spinning experiment is done in spinning lab at Tianjin Polytechnic University. The blend
ratio of core-spun yarn is terylene/cotton T/C 35/65. The core yarn is Terylene. The fineness
of core-spun yarn is 28 tex. The wrapping fibers is cotton fibers with 29.4mm in length, the
teylene fiber is staple fiber which is 1.67dtex and 32mm. The twist of spinning is 650twist/m.
The core-spun yarn obtained is shown in Figure7, and the performance index is shown in
Table 1.

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Figure 7: (a) the longitudinal microphotograph of the complete-covered polyester staple fiber/cotton
fiber core-spun yarn (b) The SEM photograph of cross section of the complete-covered polyester
staple fiber/cotton fiber core-spun yarn

Table 1. The performances of the core-spun yarn

Blending ratio strength Evenness hairiness(>3mm)
（T/C） （CN/tex） （CV/%） （number /mm）
35/65 16.84 15.9 25.44

Figure 7(a) shows that the red cotton fibers wrap the white teylene fibers completely and
Figure7 (b) shows that teylene fibers are covered all around by cotton fibers and are at the
center of core-spun yarn.

5. CONCLUSIONS
As a new type of composite yarns, staple fiber/staple fiber core-spun yarns can make best
use of the original excellent performances in two materials and overcome shortcomings of
the filament core-spun yarn. Moreover, the wrapping fiber and the core fiber could all be the
natural staple fibers, which enlarge the application scope of staple fibers. Characteristic
combinations of different fibers are adopted to develop series of productions which are of
various styles, special structural and widely used.
This paper analyzed the spinning theory of staple fiber/ staple fiber core-spun yarn and tested
the the characteristics of the yarn, Conclusions are obtained as follows:
(1) The fourth roller and the circumferential grooved top roller are added to the three-roller
drafting mechanism. The paths from the convergent point to the nipping point of the two
fiber strands are not equal. Therefore, the controlled states of two fiber strands are different.
The angles of two fiber strands are not equal between the fiber strand and the spinning axis.
Then there is a triangle at the combination point to the delivery point, in which the core yarn
is the shorter side and the wrapping yarn is the longer side. At the combination point, the
outer wrapping yarn wraps the core yarn to form the core-spun yarn.
(2) The draw ratio of the outer wrapping yarn is related to the twist, The greater the twist,
the larger the draw ratio, The twist can be theoretically calculated when the core yarn with
a certain yarn count and weight ratio is completely covered.
(3) The yarn produced is terylene/cotton T/C 35/65. The core yarn is terylene. The fineness
of core-spun yarn is 28 tex. The coverage effect and performance index of core-spun yarn
are well.

Page 149 of 150

REFERENCES
[1]Sawhney A.P.S. ， Ruppenicker G.F..Comparison of Filament-Core Spun Yarns
Produced by New and Conventional Methods[J]. Textile Research Journal ， 1992,
62(2)67. [2]Sawhney A.P.S ，Ruppenicker G.F..Special Purpose Fabrics Made with
Core-spun Yarns[J]. Indian Journal of Fiber & Textile Research，1997，22(4)：246-
254.
[3]Adlrich D.V. ， Grobler A. Some tensile properties of Wool Core-Spun Yarns [J].
SAWTRJ Bulletin，1973，7 (1)：26-35 .
[4]Tarafder N.，Chatterjee S.M.. Effect of Pre-tension of the Filament Core on the Relative
Strength Contribution of Core and Sheath Portions of Nylon/Cotton Core-spun Yarns at
Different Twist Factor Levels[J].Man made Textiles (India)，1989，32 (7)：264-267.
[5]Ruppenicker G.E.，A.P.S. Sawhney，Comparison of Cotton/Polyester Core and Staple
Blend Yarns and Fabrics[J]. Textile Research，1989，62 (2)：35-36.
[6]Li Zheping , Chu Catyuan . Mechanical properties of cotton/polyurethane core-spun
yarn[J] . Journal of China textile university ,1997,23(4):101-105.
[7]A.P.S. Sawhney，C.L.Folk. Improved Method of Producing Cotton-covered Polyester
Staple-core yarn on a Ring Spinning Frame[J]. Textile Research，1992，62 (1)：21-
25.
[8]Dong Weiguo,et al, An apparatus and method for spinning core spun yarn[P],China,
CN200710061243.6，2008.

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