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C
for 2 hours. The stirring speed was reduced for
higher concentrations as the pellet started
wobbling. The PVA solution was prepared
using distilled water (DW) and stirred until
complete dissolution of polymer occurred. The
polymer solution was also sonicated for at least
one hour and the polymer solution was found to
be uniform after the sonication.
3.3 Equipments used:
The set up used for the study is shown in
Figure 1. The electrospinning equipment
3
consists of a high voltage supply, a feed pump,
nozzles of different diameter and a collector
plate. The equipment is housed in a glass
enclosure as shown in the photograph.
3.4 Preliminary Experimentation:
Preliminary experiments were carried out
to determine the range of the parameters within
which the nanofibres are produced. Solutions of
concentration of 4%, 6%, 8%, 10% and 12% by
weight were prepared. The nozzle sizes chosen
were 18, 20 and 21 gauges. The polymer feed
rate was tried between 0.1 ml to 1.5 ml/hr. The
distance between the nozzle tip and the collector
was altered between 8 cm to 20 cm. The voltage
was varied from 0 to 27 KV.
3.5 TAGUCHIS ORTHOGONAL ARRAY:
The experimental design proposed by
Taguchi involves using orthogonal arrays to
organize the parameters affecting the process
and the levels at which they should be varied.
Instead of having to test all possible
combinations like the factorial design, the
Taguchi method tests pairs of combinations.
This allows for the collection of the necessary
data to determine which factors most affect
product quality with a minimum amount of
experimentation, thus saving time and
resources
xi
. The Taguchi method is best used
when there are an intermediate number of
variables (3 to 50), few interactions between
variables, and when only a few variables
contribute significantly.
Out of the spinning variables for the
electrospinning experiment, it was found that
satisfactory electrospinning was possible only
between the following ranges of conditions.
i. Voltage (V) range in which the fibres were
satisfactory - 16 to 27 KV.
ii. Concentration (C) of the spinning solution -
7% to 12%
iii. Feed rate (FR) - 0.4 ml to 1.0 ml/hr
iv. Collector Distance (D) - 10 cm to 20 cm
v. Nozzle diameter(ND) - 20 and 18 gauges
Based on the Taguchis design of
experiments, the lower and higher levels in
which the satisfactory spinning was possible
formed the two levels. 2 levels and L8
experiment design was used i.e. two limits and
8 experiments.
The two levels are
1. -1 ------------- Low Level
2. +1 ------------- High Level
4. RESULTS AND DISCUSSION
4.1 Characterization of electrospun PVA
Nanofibers
The nanofibres were characterized using
transmission electron microscopy (HRTEM).
The measured mean diameter of the fibres in for
the eight experiments is shown in Table-1. It was
found that for all the experiments carried out at
lower polymer concentrations, bead like
structures (Fig 2) were present. The beads were
found to decrease in number at higher voltage,
collector distance and at lower flow rate. At the
higher polymer concentration, the fibres were
found to be uniform, but the diameter of the
fibres increased considerably. Finest diameter
was spun when the voltage and collector distance
are the highest, using the smaller nozzle
diameter.
Table 1 TAGUCHIS ORTHOGONAL ARRAY
E
x
p
t
.
N
o
.
Col. Number &
Factor Assigned
Mean
Fibre Dia ()
in nm
V C F
R
D N
D
1 - 1 - 1 - 1 - 1 - 1 1 = 1 8 6
2 - 1 - 1 - 1 1 1 2 = 1 3 5
3 - 1 1 1 - 1 - 1 3 = 2 3 9
4 - 1 1 1 1 1 4 = 2 6 7
5 1 - 1 1 - 1 1 5 = 1 3 5
6 1 - 1 1 1 - 1 6 = 1 2 3
7 1 1 - 1 - 1 1 7 = 2 6 0
8 1 1 - 1 1 - 1 8 = 2 3 1
Fig. 2 Beaded and smooth fibres
The data were evaluated using Qualitek-4
software, which is a tool designed especially for
Taguchis design of experiments. The software
Fig.1 Electrospinning Equipment
4
is quite powerful in analysing the experimental
data and presenting the results in the desired
form, both graphically and numerically.
Fig 3Diameter of fibres from L8 experiments
4.2 The ANOVA analysis:
ANOVA analysis for averages and S/N ratio
(signal to noise ratio) carried out using the
software is presented in Tables 2 and 3. By
analysing the data, the following inferences
were arrived at:
Polymer concentration is the single most
contributing factor to effect a change in the fibre
diameter, contributing to nearly 55% (78%
based on S/N) of the total contribution (all
parameters put together).
In the interactions, voltage vs. flow rate, flow
rate vs. collector distance, flow rate, collector
distance & voltage vs. nozzle diameter showed
higher level interactions.
ANOVA analysis identified presence of
external factors that influenced the fibre
diameter. These factors need to be identified
and analysed carefully.
At lower polymer concentrations, all the
variables show good influence on fibre
diameter. However, when ANOVA analysis is
done for the whole set of experiments together;
the above inference cannot be arrived at.
Table 2: ANOVA- Based on Averages
Factor Sum of
squares
DO
F
Varianc
e
F
calc
ulat
ed
Pure
sum of
squares
%
cont
ribu
tion
Infe
renc
e
V 22234 1 22234 10.8
3
201809 1.7 NS
C 657098 1 657098 320.
04
6550451 55.2
4
S
FR 9152 1 9152 4.46 70992 0.6 NS
D 15617 1 15617 7.61 135635 1.14 NS
ND 1252 1 1252 0.61 0 0 NS
ERR 480447 234 2053
TOTAL 1185800 239
Table 3: ANOVA- Based on Signal/Noise Ratio
Factor Sum of
squares
DO
F
Varianc
e
F
calc
ulat
ed
Pure
sum of
squares
%
cont
ribu
tion
Infe
renc
e
V 2.4 1 2.4 1.29 0.55 0.99 NS
C 45.3 1 45.3 24.0
7
43.47 78.9 S
FR 1.5 1 1.5 0.81 0 0 NS
D 1.99 1 1.99 1.06 0.114 0.21 NS
ND 0.004 1 0.004 0.02 0 0 NS
ERR 3.767 2 1.883
TOTAL 55.078 7
4.3 Further analysis:
When the data is analysed taking the
concentration as the primary parameter and its
interaction with other parameters at both levels,
we can appreciate the contribution of the
individual parameters. Annexure 1 shows the
interaction between other variables and
concentration. It can be observed from the table
that the changes in fibre diameters are
insignificant at the higher concentration (12%). It
is only at the lower concentration that maximum
changes are apparent. A generalised ANOVA
test does not lead to this conclusion. At lower
concentration, the fibre diameter decreases for
the larger nozzle diameter and also at the higher
flow rate (contrary to the expectations) indicating
that electrospinning is a complex process that
entails careful experimentation in identifying the
variable interactions in order to optimise the
spinning parameters.
5. CONCLUSIONS
Based on the above results, it can be
confidently concluded that Taguchis design is a
5
good starting point for the optimisation of
electrospinning of polymers. Obviously, this
means the amount of experimental work, time
and associated costs can be reduced. The
conclusions arrived at in the present investigation
are listed below.
1. Polymer concentration was found to be the most
significant parameter influencing the diameter of
the nanofibres.
2. Voltage and collector distance are also important
factors influencing the fibre diameter. Higher
voltage and higher collector distance resulted in
finer fibres. These two observations are in
agreement with the findings of the previous study
on PVA electrospinning
viii
.
3. The influence of nozzle diameter and the
polymer flow rate show a complex interaction in
determining the diameter of fibres and require
further experimentation.
4. In the interactions, flow rate showed higher level
interactions with voltage, collector distance and
nozzle diameter. Similarly, voltage and collector
distance also exhibited higher level interactions
with nozzle diameter.
5. Little interaction was observed between voltage
and collector distance, voltage and concentration
and also concentration with collector distance.
6. It was possible to produce finer fibres of 123 nm
(Experiment 6) by adopting Taguchi design. Our
next set of experiments would focus on
optimising the concentration in order to eliminate
bead formation and optimising the factors like
needle diameter and collector distance.
Acknowledgements:
The authors wish to acknowledge the help
of Dr. Biji Manoj and Mr. K.K. Karthikeyan
in carrying out the experimental work and for
the useful inputs in planning the experimental
work.
7. REFERENCES
i
Seeram Ramakrishna et al. An introduction
to electrospinning, 2005, World Scientific
Publish Co, Singapore.
ii
Hai-Sheng Wang et al., Functional
Polymeric Nanofibres from Electrospinning,
Recent Patents on Nanotechnology, 2009, 3, 21-
31.
iii
Website:http://www.zeusinc.com/technicalser
vices/technicalbulletins/technicalnewsletters.as
px
iv
Darrel H Reneker and Iskoo Chun.
Nanometre diameter fibres of polymer,
produced by electrospinning, Nanotechnology,
1996, 7, 216223.
v
Wen Ji Jin et al. Preparation of Polymer
Nanofibers Containing Silver Nanoparticles by
using Poly(N-vinylpyrrolidone),
Macromolecular Rapid Communications, 2005,
Volume 26, Issue 24, pages 19031907.
vi
C. L. E. Carraher and J. Moore,
Modification of Polymers, Plenum, New York,
1983.
vii
Bin Ding et al. Preparation and
Characterization of Nanoscaled Poly(vinyl
alcohol)Fibers via Electrospinning, Fibers and
Polymers, 2002, 3 (2), 73-79.
viii
A.Koski et al. Effect of molecular weight
on fibrous PVA produced by electrospinning,
Materials Letters, 2004, 58 (3-4), 493-497.
ix
Chunxue Zhang et al. Study on
morphology of electrospun poly(vinyl alcohol)
mats, European Polymer Journal, 2005, 41(3),
423-432.
x
Qiang Li et al. Preparation and Properties
of Poly (vinyl alcohol) Nanofibers by
Electrospinning, Proceedings on the
International Conference on Solid Dielectrics,
UK, 2007, 215-218.
xi
Website:http://controls.engin.umich.edu/wiki/
index.php/Design_of_experiments. _
Annexure 1: Interaction of other
parameters with concentration change
INTERACTION OF OTHER PARAMETERS WITH CONCENTRATION
VOLTAGE
(KV) 7 % 12 %
COLLECTOR
DISTANCE
(CM)
7 % 12
%
Chan
ge
In
Dia
(nm)
Chan
ge
In
Dia
(nm)
LEVEL
1
1
6
160
.5
252.
8 92.4
LEVEL
1 10 160.6
249.
5 88.8
LEVEL
2
2
7
128
.8
245.
9 117
LEVEL
2 20 128.7
249.
2 120.6
Change in dia
(nm)
31.
6 7
Change in dia
(nm) 32 0.2
NEEDLE
DIA (G) 7 % 12 %
Chan
ge
In
Dia
(nm)
FLOW
RATE
(ml/hr)
7 % 12
%
Chan
ge
In
Dia
(nm)
LEVEL
1
2
1
15
4.5
234.
9 80.4
LEVEL
1 0.4 160.5
245.
9 85.4
LEVEL
2
1
8
13
4.8
263.
8 129
LEVEL
2 1.0 128.8
252.
8 124
Change in dia
(nm)
19.
7 28.9
Change in dia
(nm) 31.5 7