Negative Poisson S Ratio Composites - Finite Element Modeling and Experiments

A Thesis
entitled
Negative Poissons Ratio Composites - Finite Element Modeling and Experiments
by
Sharmila Jayanty
Submitted to the Graduate Faculty as partial fulfillment of the requirements for the
Master of Science degree in Mechanical Engineering
_______________________________________
Dr. Lesley M. Berhan, Committee Chair
________________________________________
Dr. Maria Coleman , Committee Member
________________________________________
Dr. Yong X. Gan, Committee Member
________________________________________
Dr. Patricia R. Komuniecki, Dean
College of Graduate Studies
The University of Toledo

December 2010
Copyright 2010, Sharmila Jayanty

This document is copyrighted material. Under copyright law, no parts of this document
may be reproduced without the expressed permission of the author.
An Abstract of
Negative Poissons Ratio Composites - Finite Element Modeling and Experiments
by
Sharmila Jayanty
Submitted to the Graduate Faculty in partial fulfillment of the requirement for the
Master of Science Degree in Mechanical Engineering
The University of Toledo
December 2010
Auxetic or negative Poissons ratio materials are of great research interest as they
exhibit improved mechanical properties such as impact resistance, fracture toughness,
hardness and shear modulus over conventional materials with a positive Poissons ratio
and same stiffness. Most auxetic materials manufactured to date are porous, and the
major hindrance of using these materials in structural applications is their low strength. In
this research a new approach for manufacturing auxetic fiber-reinforced composites by
embedding an auxetic fibrous network in a conventional polymer matrix is investigated
using numerical and experimental methods.
iii
In this project, a finite element model was developed to investigate the proposed
hypothesis of manufacturing an auxetic composite. Compressed mats of sintered stainless
steel fibers are known to have negative Poissons ratio out-of-plane. It is hypothesized
that their auxetic behavior is from the arrangement of fibers within the matrix, relative
stiffness of the matrix and network of reinforcement. First, tension tests were performed
on the compressed sintered mats and the experimental results have shown that Poissons
ratio for all metal mat specimens is negative in transverse direction. Next, mechanical
tests were performed and microscopic images were taken of the composite samples made
by embedding the stainless steel mats with silanol terminated polydimethoxysiloxane
(PDMS) polymer. Finally, polymer nanocomposites were made through the inclusion of
high loading carbon nanofibers in the polymer matrix (PDMS). The experimental results
of both the composite mats and nanocomposites confirm the feasibility of manufacturing
an auxetic composite by embedding an auxetic network in a conventional polymer. The
auxetic behavior in the composite mats is due to the arrangement of fibers in the network
and compression of stainless steel mats during fabrication process. It was assumed that
the auxetic behavior of the nanocomposites is due to effective network formation of
nanofibers and the compression of the sample during preparation process.
iv
Dedicated to my parents Raghu Jayanty (late) and Surya Kumari Jayanty.
Acknowledgements
I would like to express my sincere gratitude to my advisor, Dr. Lesley M. Berhan,
for her invaluable support, guidance and encouragement during the course of this thesis
project and throughout my study at The University of Toledo. Her moral support and
continuous guidance enabled me to complete my work successfully. I am thankful to her
for giving me the opportunity to work in this project.
I would like to thank my committee members Dr. Maria R. Coleman and Dr.
Yong Gan, for their valuable suggestions and support throughout this study. I sincerely
thank Mehmet Tatlier and Jason Crowe for their help in the research lab. I truly
appreciate all the time and suggestions given by them. I would like to specially
acknowledge Nima Hakim-elahis for his help in membrane materials characterization
lab.
I sincerely thank all the faculty members in the Department of Mechanical,
Industrial and Manufacturing Engineering for their help during my Masters program. I
would also like to express my gratitude to all the staff members at the College of
Engineering. I would like to thank all my lab mates Azita Belashi, Julie Matheny, Greg
Tilton and Carrie Baker. I would like to thank my roommates and all my friends for their
help and support during my stay in Toledo.
vi
Contents
Abstract ........................................................................................................................... iii

Acknowledgements .......................................................................................................... vi
Contentsvii
List of Tables ......................................................................................................................x
List of Figures .................................................................................................................. xii
List of Symbols .................................................................................................................xv
1.Introduction .....................................................................................................................1
1.1
General Overview ................................................................................................ 1
1.2 Properties of Auxetic Materials................................................................................. 3

1.3 Potential Applications ............................................................................................... 5
1.4 Types of Auxetic Materials ....................................................................................... 6
1.4.1 Natural Auxetic Materials .................................................................................. 6
1.4.2 Man Made Auxetic Materials ............................................................................. 6
1.5 Objectives ................................................................................................................ 10
2. Finite Element Modeling .............................................................................................12
2.1 Network Generation and Modeling ......................................................................... 14
2.2 Simulation Procedure .............................................................................................. 17
2.3 Results and Discussion ............................................................................................ 17
2.3.1 Effect of Strain and Network Geometry on Poissons Ratio ............................ 18
2.2.3 Effect of Youngs Modulus on Poissons Ratio ............................................... 20
vii
3. Sintered Stainless Steel Fiber Mats ............................................................................26

3.1 Fabrication and Specifications of the Specimen ..................................................... 27
3.2 Specimen Shape ...................................................................................................... 28
3.3 Testing Procedure .................................................................................................... 30
3.4 Testing Results ........................................................................................................ 33
3.5 Discussion ............................................................................................................... 35
4. Composite Mats ............................................................................................................37
4.1 Sample Preparation Procedure ................................................................................ 38
4.1.1 Plain PDMS ...................................................................................................... 38
4.1.2 Composite Mat ................................................................................................. 39
4.2 Scanning Electron Microscope Image Analysis...................................................... 41
4.3 Weight Measurement Analysis ............................................................................... 50
4.4. Testing Results ....................................................................................................... 51
4.4.1 Plain PDMS .......................................................................................................... 51
4.4.2 Composite Mats ................................................................................................ 53
4.3 Discussion ............................................................................................................... 54
5. Nanocomposites ............................................................................................................56
5.1 General Overview and Motivation .......................................................................... 56
5.2 Introduction ............................................................................................................. 58
5.3 Purification of Oxidized Carbon Nanofibers .......................................................... 59
5.3.1 Sonication ......................................................................................................... 59
5.3.2 Purification ....................................................................................................... 60
5.3.3 Filtration ........................................................................................................... 62
5.4 Nanocomposites Sample Preparation ...................................................................... 63
5.5 Testing Results ........................................................................................................ 67
5.5.1 Pristine Fibers ................................................................................................... 68
5.5.2 Oxidized Fibers................................................................................................. 69
5.5.3 Functionalized Fibers ....................................................................................... 71
5.6 Discussion ............................................................................................................... 71
viii
5.6.1 Effect of Nanofiber Type ..................................................................................... 71

5.6.2 Effect of Nanofiber Loading............................................................................. 73
5.6.3 Effect of Compression ...................................................................................... 76
6. Conclusion and Future Work .....................................................................................78
6.1 Conclusion............................................................................................................... 78
6.2 Future Work ............................................................................................................ 79
References .........................................................................................................................80
ix
List of Tables
Table 2.1: Different Cell Geometries................................................................................ 15
Table 2.2: Effect of strain rate on Poissons ratio ............................................................. 19
Table 2.3: Effect of Youngs modulus on Poissons ratio ................................................ 21
Table 3.1: Average values of Youngs modulus and Poissons ratio for sintered mats ... 34
Table 4.1: Mixture of chemicals ....................................................................................... 38
Table 4.2: Weight fraction of fiber and polymer in composite mat for different porosities
........................................................................................................................................... 51
Table 4.3: Average values of Youngs modulus and Poissons ratio for plain PDMS ..... 51
Table 4.4: Comparison of Youngs modulus and Poissons ratio for composite and
sintered mats ..................................................................................................................... 53
Table 4.5: Variation in thickness for sintered and composite mats .................................. 53
Table 5.1: Fiber loading ratios .......................................................................................... 63
Table 5.2: Youngs modulus and Poissons ratio for 15% fiber loading of pristine fibers
........................................................................................................................................... 68
........................................................................................................................................... 68
........................................................................................................................................... 69
Table 5.5: Youngs modulus and Poissons ratio for 15% fiber loading of oxidized fibers
........................................................................................................................................... 69
........................................................................................................................................... 70
........................................................................................................................................... 70
Table 5.8: Youngs modulus and Poissons ratio for 20% fiber loading of functionalized
fibers ................................................................................................................................. 71
Table 5.9: Volume fraction of fiber and polymer for 15% fiber loading ......................... 75
Table 5.10: Volume fraction of fiber and polymer for 20% fiber loading ....................... 75
Table 5.11: Volume fraction of fiber and polymer for 25% fiber loading ....................... 75
xi
List of Figures
Figure 1-1: Schematic diagram of positive Poissons ratio deformation when a tensile
load is applied in the longitudinal direction, initially undeformed material (thin line)
undergoes longitudinal extension and lateral contraction (solid line) ................................ 2
Figure 1-2: Schematic diagram of negative Poissons ratio deformation when a tensile
load is applied in the longitudinal direction, initially undeformed material (thin line)
undergoes longitudinal and lateral extension (solid line) ................................................... 2
Figure 1-3: Deformation mechanisms in re-entrant and conventional honeycomb ............ 7
Figure 1-4: Pore structures of non auxetic and auxetic foam ............................................. 8
Figure 2-1: Fiber network model similar to random fiber network model before
compression ...................................................................................................................... 13
Figure 2-2: Fiber network model similar to random fiber network model after
compression ..................................................................................................................... 13
Figure 2-3: Dimensions of a re-entrant honey comb structure (unit cell)......................... 15
Figure 2-4: Boundary conditions for plane stress and beam elements ............................. 16
Figure 2-5: Deformed fibrous network model .................................................................. 17
Figure 2-6: Poissons ratio versus strain for re-entrant honeycomb network ................... 20
Figure 2-7: Poissons ratio versus effective stiffness ratio for re-entrant honeycomb ..... 21
Figure 2-8: Compliant matrix ........................................................................................... 23
Figure 2-9: Stiff matrix ..................................................................................................... 24
xii
Figure 2-10: Effect of change in Poissons ratio on matrix material ................................ 25

Figure 3-1: Cutting die ...................................................................................................... 28
Figure 3-2: Manual press .................................................................................................. 29
Figure 3-3: Dog- bone shaped stainless steel fiber mat .................................................... 29
Figure 3-4: Laser extensometer ........................................................................................ 30
Figure 3-5: Instron tensile testing machine ....................................................................... 31
Figure 3-6: Electronic vernier caliper used for width calculation .................................... 31
Figure 3-7: Stress vs. strain graphs for sintered mats of different porosities ................... 34
Figure 3-8: Lateral strain vs. longitudinal strain graphs for sintered mats of different
porosities ........................................................................................................................... 35
Figure 4-1: Preparation of Plain PDMS sample ............................................................... 39
Figure 4-2: Sample preparation procedure for a composite mat....................................... 40
Figure 4-3: 60% porosity mat ........................................................................................... 42
Figure 4-6: 60% porosity composite mat .......................................................................... 45
Figure 4-9: 60% porosity composite mat at fractured surface .......................................... 48
Figure 4-10: 70% porosity composite mat at fractured surface ........................................ 49
Figure 4-11: 80% porosity composite mat at fractured surface ........................................ 50
Figure 4-12: Stress vs. strain graphs for plain PDMS ...................................................... 52
Figure 4-13: Lateral strain vs. longitudinal strain graphs for plain PDMS ...................... 52
xiii
Figure 4-14: Lateral strain vs. longitudinal strain graphs for composite mats ................ 54
Figure 5-1: Sonication process.......................................................................................... 60
Figure 5-2: Experimental setup for purification of oxidized carbon nanofibers .............. 61
Figure 5-3: Filtration process ............................................................................................ 62
Figure 5-4:: Schematic procedure for nanocomposite preparation ................................... 65
Figure 5-5: OCNF- 2 roll mill procedure (20% fiber loading) ......................................... 66
Figure 5-6: OCNF- manual press with weight during curing procedure (20% fiber
loading) ............................................................................................................................. 66
Figure 5-7: OCNF- manual press with weight during curing procedure(20% fiber
loading) ............................................................................................................................. 67
Figure 5-8: Stress vs. strain graphs for different nanocomposites of 20% fiber loading.. 72
Figure 5-9: Stress vs. strain graphs for different nanocomposites of 20% fiber loading
(elastic range) .................................................................................................................... 72
Figure 5-10: Lateral strain vs. longitudinal strain graphs for nanocomposite samples at
20% fiber loading .............................................................................................................. 73
Figure 5-11: Lateral strain vs. longitudinal strain graphs for different fiber loading of
pristine fibers .................................................................................................................... 74
Figure 5-12: Stress vs. strain curves for nanocomposite samples with pristine nanofibers
........................................................................................................................................... 74
Figure 5-13: Lateral strain vs. longitudinal strain for 20% fiber loading of pristine fibers
........................................................................................................................................... 77
xiv
List of Symbols
Poissons ratio
x ..Transverse strain
y ...Longitudinal strain
E.Youngs modulus
K.Bulk modulus
H.Hardness
P..Load
A0.Initial cross section
l ...Change in length
l0.Initial Length
.........Stress
t .....Change in thickness
t0...Initial thickness
xv
Chapter 1
Introduction
1.1 General Overview

When a material is stretched in one direction, it expands in the direction of
applied force and contracts in the direction perpendicular to the applied force. Similarly,
a material when compressed in the longitudinal direction usually expands in the
transverse direction. This behavior of the material under deformation is governed by one
of the four fundamental properties of materials, called Poissons ratio. Poissons ratio is
defined as the ratio of change in strain in the transverse direction to the change in strain
in the longitudinal direction in the direction of stretching force, as shown by the formula
given below,
xy
x
(x / x)
,
y
(y / y )
(1)
where
= Poissons ratio
x = Transverse strain
1
y = Longitudinal strain
In Equation (1), there is a negative sign so that the Poissons ratio is positive as most of
the materials contract in the transverse direction due to an applied tensile load. Figure 1-1
shows a schematic diagram of positive Poissons ratio materials.
Figure 1-1: Schematic diagram of positive Poissons ratio deformation when a

tensile load is applied in the longitudinal direction, initially undeformed material
(thin line) undergoes longitudinal extension and lateral contraction (solid line)
However, some materials undergo lateral expansion when stretched longitudinally and
become thinner when compressed as shown in Figure 1-2. This results in negative values
of Poissons ratio. Materials with negative Poissons ratio are called auxetic materials.
Figure 1-2: Schematic diagram of negative Poissons ratio deformation when a

tensile load is applied in the longitudinal direction, initially undeformed material
(thin line) undergoes longitudinal and lateral extension (solid line)
Lakes first synthesized auxetic polyurethane (PU) foams with re-entrant structures
in 1987 [1]. Later Evens designated these negative Poissons ratio materials as
Auxetics in 1991 [2]. Negative Poissons ratio materials are also known as anti-rubber
because when stretched they become fatter in cross-sectional area, while rubber becomes
thinner [3]. These materials are also known as dilatational materials as they undergo
volumetric change instead of shape change [4].
1.2 Properties of Auxetic Materials

In theory, negative Poissons ratio materials have improved mechanical properties
such as shear modulus [5], fracture toughness [6, 7], indentation resistance [8] and
acoustic response compared to conventional materials with same Youngs modulus. In
the following section, some of these properties are discussed.
Generally for an isotropic material, the four elastic constants used to describe the
materials properties are Youngs modulus (E), Shear modulus (G), Bulk modulus
(K) and Poissons ratio (). The first three constants are a measure of stiffness,
rigidity and compressibility of a material. The equations relating these four
constants are given as follows [9].
E
2(1 v)
(2)
E
31 2
(3)
According to Equations (2) and (3), its clear that when Poissons ratio
approaches -1, the shear modulus approaches infinity. Therefore a very high shear
3
modulus relative to bulk modulus is obtained for auxetic materials when

compared to conventional materials.
According to classical theory of elasticity, the relationship between indentation

resistance or hardness and Poissons ratio is shown in the following equation
E
,
H
2
1
where H is hardness and 1 is for uniform pressure distribution and
(4)
2
for
3
Hertzian indentation. According to Equation (4) as approaches 1 or -1, the

indentation resistance becomes infinitely large. However cannot exceed 0.5
because in isotropic materials, the value of Poissons ratio lies in the range
of 1 0.5 . Therefore indentation resistance of a material can be improved
only when is in the range of -0.5 to -1. When a compressive force is exerted on
an auxetic material, the material effectively flows to the vicinity of the impact.
This develops an area of denser material, which has high indentation resistance.
Auxetic materials also show remarkable damping and absorption properties. The
damping capacity of high compressive pre-strained auxetic foam is greater than
that of the conventional foam. This effect is due to the abrasion inwardly buckled
cell ribs of the auxetic foam [10]. It is reported that the absorption of sound at all
frequencies by auxetic foam is superior to conventional foams [11, 12].
1.3 Potential Applications

Auxetic materials have immense potential applications in aerospace engineering,
automobile industry, construction industry, biomedical industry and military applications.
Some of these applications are discussed below
Auxetic materials undergo synclastic or double curvature deformation when they

are subjected to bending moments. This unique behavior of such materials have
wide reported applications in industries as they require less machining time,
effective cost reduction and flawless structures during manufacturing process. For
example in aerospace industry auxetic materials can be incorporated in
manufacturing of airplane nose-cones, sandwich panels and duct liners wings [13,
14].
In biomedical field auxetic materials have numerous potential applications like

prosthetic materials, surgical implants, suture/muscle/ligament anchors. For
instance vessel rupture resulting in decrease of wall thickness because of blood
flow in artificial blood vessels made of conventional materials could be avoided
by using auxetic materials. [15].
Auxetic materials have been proposed for potential military applications like
bullet-proof or projectile resistant vests, body armors, crash helmets, and
bandages or wound pressure pads [16].
Auxetic materials have applications in nuclear reactor construction. For example,

moderators of magnox nuclear reactors are designed with Negative Poissons ratio
to have maximum shear modulus so that loads that might be caused by
earthquakes can be resisted [13].
5
Auxetic materials could be used for the construction of wear resistant machine
components as they have improved hardness. For instance press-fit fasteners with
negative Poissons ratio during compression, undergo lateral contraction which
assists the insertion of the fastener [17, 18].
1.4 Types of Auxetic Materials

Auxetic materials are divided into two main groups namely, natural and manmade auxetic materials. These are discussed in detail in the following section.
1.4.1 Natural Auxetic Materials

Natural auxetic materials are classified into natural molecular auxetic materials
and biomaterials. Some examples of natural molecular auxetic materials are iron pyrites
[19], single crystalline materials such as arsenic [20], cadmium [21] and silicate cristobalite [22]. Since all these materials are inorganic in nature and possess unique
molecular structure they are known as natural molecular auxetic materials. Auxetic
biomaterials such as cow teat [23] and salamander skin [24] exhibit negative Poissons
ratio. The negative Poissons ratio is presumed to be due to complicated micro structural
fibrous network in their skins.
1.4.2 Man Made Auxetic Materials
1.4.2.1 Auxetic Cellular Solids
Two dimensional silicon rubber or aluminum honey combs were the large scale
auxetic cellular structures first developed in 1982. The deformation mechanism in these
structures is shown in Figure 1-3 which is due to flexure of diagonal ribs under applied
tensile loads [25, 26]. These honeycomb structures are used in filtration media as they
sustain pressure across the filter when load is applied. However, to take full advantage of
these structures the cell size must be reduced below 1mm. Techniques used for this
purpose are molecular self-assembly [27], LIGA technology, silicon surface
micromachining techniques [28], laser stereo lithography [27] and nanomaterials
fabrication processes [29]. Honeycomb structures reduced to a scale of 50m have
potential applications in nano-technology and MEMS [30].
Figure 1-3: Deformation mechanisms in re-entrant and conventional honeycomb

7
Auxetic polyurethane foams developed by Roderick Lakes in 1987 were an

important discovery in auxetic research [1]. Metallic and polymeric foams were made
with Poissons ratio of = -0.8 [6] and = -0.7 [31], respectively. While conventional
foams contained convex polyhedral cells these new auxetic foams featured convoluted
cell structures. Figure 1-4 shows scanning electron images of conventional and auxetic
foams. The conventional foam when subjected to tensile loading shrinks laterally because
of normal cell structure whereas the auxetic foam extends in lateral dimension when
subjected to tensile loading as the re-entrant cell structures transform from convolute to
convex geometry. Auxetic foams have shown enhancement in properties such as fracture
toughness [6], shear resistance [32, 33], indentation resistance [34, 35], sound and
vibration absorptions [36, 37] and synclastic deformation [31]. Auxetic foams have
various applications in air filtration, packaging, sound insulation, press-fit fastener and
shock absorption.
Figure 1-4: Pore structures of non auxetic and auxetic foam
1.4.2.2 Micro Porous Polymers

Brian Caddock and Evans observed auxetic behavior in expanded form of
microporous polytetrafluoroethylene (PTFE) [38]. Their study showed that nodules and
fibrils microstructure arrangement was responsible for the auxetic behavior in PTFE [39,
40]. Evans and Kim Alderson later developed an auxetic ultra-high molecular weight
polyethylene (UHMWPE) [41] resembling a nodulefibril microstructure. Development
of UHMWPE has increased stiffness and indentation resistance [42] and attenuation of
ultrasonic signals [43].
1.4.2.3 Auxetic Composites

Composite materials consist of two or more individual materials combined in a
macroscopic structural unit, which are formed from different combinations of other two
materials. Composite materials are developed to get desirable combination of properties.
Composites are classified based on matrix material and reinforcement geometry. Two
different types of structural reinforcement geometry laminates or sandwich panels are
more significant. These composites are now widely used in various components of
automotive, aerospace, marine and architectural structures apart from consumer products
like tennis rackets, golf clubs and skis as they have high strength and high stiffness to
weight ratio [44].
Development of auxetic composites in industries will also take advantage of
auxetic behavior of materials in addition to non-auxetic composites which have high
strength and stiffness to weight ratio. Current research on auxetic composites is mainly
focused on various methods to manufacture auxetic composites. Sequential piling of
9
angle-ply reinforced laminates and the development of composites which have one or
more auxetic phases are the two primary techniques used in the design of auxetic
composites.
One approach to manufacturing auxetic composites by laminated angle ply
method was proposed by G. Milton in 1992 [45]. Later this approach was proposed and
validated through experiments by stacking unidirectional layers of carbon fiber reinforced
epoxy in a special sequence which gives rise to negative Poissons ratio in-plane and outof-plane direction [46-49]. This type of development has predicted an improvement in
mechanical properties such as static indentation resistance and low velocity impact
testing [50].
A second approach to manufacturing auxetic composites is using one or more
auxetic components as reinforcement material or the matrix. For instance, re-entrant
copper foam was used as matrix material with viscoelastic polymer, solder and, indium as
filler material in the fabrication of auxetic composite [51]. Recent developments made in
using different auxetic fibers as reinforcement in conventional matrices motivated interest
in fiber reinforced composites [ 52,53,54]. Use of auxetic fibers is proposed to enhance
pull-out performance as these auxetic fibers maintain an interface between the matrix and
the fiber. Experimental results reported that the energy used to pull out the auxetic fiber is
three times greater than a conventional fiber.
1.5 Objectives
Deformation mechanisms in re-entrant honey comb structures, auxetic foams,
liquid crystal polymers are well understood because of their common periodic micro
10
structures but there is limited knowledge of how the auxetic effect arises in non-periodic
microstructures. In order to understand the auxetic effect in these disordered and random
fiber networks, linear 2D and 3D fiber network models were developed by Tatlier and
Berhan [55]. They investigated the effect of compression ratio, fiber density, anisotropy
of fiber mats, applied strain, and aspect ratio on mechanical properties such as Poissons
ratio and effective modulus. Simulation results showed that compression of random fiber
networks is one of the key parameters in determination of auxetic behavior.
The goal of the project is divided into two parts. First, to experimentally validate
the numerical model developed by Tatlier and Berhan by conducting tensile tests on
compressed mats of sintered stainless steel fibers which are known to exhibit negative
Poissons ratio out-of-plane. Second, to test the hypothesis whether an auxetic composite
can be manufactured by embedding a random fibrous network with a negative Poissons
ratio in a conventional matrix material provided the modulus of the reinforcing fibers is
sufficiently high compared to the matrix material. To validate the hypothesis, two
dimensional finite element analysis and experiments on composite mats (sintered
stainless steel mats as random fibers and PDMS polymer as conventional matrix) and
nanocomposites (high loading carbon nanofibers in PDMS polymer matrix) were
performed.
11
Chapter 2
Finite Element Modeling
Mechanism of the auxetic behavior in fibrous network was studied by Tatlier and
Berhan [56] which showed resemblance between re-entrant honey comb or inverted cell
structures and random fiber networks. Their study proposed that compression is the
critical factor which resulted in similarities between the deformation mechanism of reentrant honeycomb structure and random fiber networks. Figure 2-1 shows the fiber
network model which is similar to random fiber network before compression where the
contact points are considered to be rigid and Figure 2-2 shows fiber network model which
is similar to random fiber network after compression. From these figures it is clear that
compression on the random fiber mats resulted in a geometrical structure equivalent to
geometry of re-entrant honeycombs.
12
Figure 2-1: Fiber network model similar to random fiber network model before
compression[56]
Figure 2-2: Fiber network model similar to random fiber network model after
compression[56]
13
The modeling discussed in this chapter includes a two dimensional multiphysics

finite element network model. Comsol Multiphysics, finite element analysis software was
used to generate the theoretical composite. In this study feasibility of producing an
auxetic composite by embedding auxetic network within a flexible matrix was
investigated. Re-entrant honey comb structure of beam elements was used as
reinforcement since deformation mechanism shown by random fibrous networks and reentrant honey comb is similar; plane stress elements were used to model the matrix.
2.1 Network Generation and Modeling

In order to generate the auxetic network, re-entrant honeycomb structures were
considered as unit cells. These unit cells were taken as beam elements and variables used
for construction of this unit cell are cell geometries (length, width and thickness) as
shown in Figure 2-3 and different cell geometries used are given in Table 2.1.
Sub-domain settings were assigned to plane stress elements such as material
property (isotropic material), dimensions (thickness and cross sectional area) and
stiffness. Boundary settings were prescribed on all four edges of the matrix where a
uniform displacement (0.1m) in y-direction was applied to each node on the top edge,
rollers on bottom and left edges constraining their movement in x and y planes
respectively and the right edge is left free. Similar boundary settings were given to beam
elements as that of plane stress elements but the thickness of the plane stress elements
(0.01m) is ten times larger than that of the beam elements (0.001m). Figure 2-4 shows the
boundary settings for plane stress and beam elements.
14
Figure 2-3: Dimensions of a re-entrant honey comb structure (unit cell)
Table 2.1: Different Cell Geometries

Cell geometries
1
3.8
9.2
7.8
9.2
12.2
10.6
3.2
9.6
8.4
0.6
1.2
0.6
1.2
0.6
0.4
0.8
0.4
1.2
1.2
0.2
0.8
0.2
0.8
0.6
0.6
15
Figure 2-4: Boundary conditions for plane stress and beam elements
16
2.2 Simulation Procedure

The geometries of beam elements and plane stress elements were created, and
simulations were carried with prescribed sub-domain and boundary settings by internal
solver in Comsol Multiphysics. The average displacements x of the points on the right
edge were exported to a text file and effective Poissons ratio of the model was calculated
using Equation 1, the deformed model is shown in Figure 2-5.
Figure 2-5: Deformed fibrous network model

17
2.3 Results and Discussion

In this section, results obtained from simulation of finite element model are
presented. Simulations were run for calculation of Poissons ratio considering the strain
and Youngs modulus as parameters.
2.3.1 Effect of Strain and Network Geometry on Poissons Ratio

To investigate the effect of increased strain rate on the model, simulations were
run by changing the amount of displacement on the top edge for both plane stress and
beam elements for the calculation of Poissons ratio. The simulation results are listed in
Table 2.2 and Table 2.3 for model geometry of a = 0.6, b = 0.8, c = 0.2, x = 7.8, and y =
8.
18
Table 2.2 Effect of strain rate on Poissons ratio

Displacement on top
edge
Strain
Poisson's ratio
0.001
0.0001
0.12
0.005
0.0006
0.12
0.009
0.0011
0.12
0.03
0.0037
0.12
0.07
0.0087
0.12
0.1
0.0125
0.12
0.5
0.0625
0.12
0.9
0.1125
0.12
0.125
0.12
1.5
0.1875
0.12
1.9
0.2375
0.12
19
Figure 2-6: Poissons ratio versus strain for re-entrant honeycomb network
From the above results, it can be observed that the variation in strain i.e. displacement on
the top edge, does not affect the Poissons ratio. It was observed that Poissons ratio was
not affected significantly either by change in cell geometry or number of cells for the
various combinations listed in Table 2.1.
2.2.3 Effect of Youngs Modulus on Poissons Ratio

To investigate the effect of Youngs modulus, simulations were run by changing
the sub domain settings of plane stress elements. Stiffness is kept constant for the beam
elements and varied for plane stress elements. Simulations were run in Comsol and the
results are tabulated in Table 2.3.
20
Table 2.3: Effect of Youngs modulus on Poissons ratio

Effective stiffness ratio (beam
elements / plane stress elements)
Poissons ratio
2.97E-08
0.33
2.97E-07
0.3299
2.97E-05
0.3196
2.97E-04
0.127
2.97E-02
-1.3799
2.97E+00
-1.55099
Figure 2-7: Poissons ratio versus effective stiffness ratio for re-entrant honeycomb
A significant change in the Poissons ratio was observed with the variation in
Youngs modulus. The deformation of auxetic network (beam elements embedded in
21
compliant plane stress elements) is shown in Figure 2-8 where the lateral dimension
increases with the application of longitudinal displacement. In Figure 2-9 conventional
network (beam elements were embedded in stiffer plane stress elements) is shown where
the lateral dimension decreases with longitudinal displacement. Stiffness ratio of beam to
plane stress elements for compliant matrix was 5.93, for stiffer matrix the ratio was 5.93
x 10-8. Thus the effective Poissons ratio of the network changes from negative to
positive when the matrix material (plane stress elements) changes from a compliant
matrix to a stiffer matrix as shown in Figure 2-10. The obtained finite element simulation
results validate the hypothesis of manufacturing an auxetic composite by embedding an
auxetic network in a conventional matrix where the auxetic network is much stiffer than
the conventional matrix.
22
Figure 2-8: Compliant matrix
23
Figure 2-9: Stiff matrix
24
Figure 2-10: Effect of change in Poissons ratio on matrix material
25
Chapter 3
Sintered Stainless Steel Fiber Mats

In this chapter the experimental methodology and test results performed on
sintered stainless steel mats, known to have negative Poissons ratio out of plane [61, 62],
are discussed to validate the finite element model in Chapter 2. Details of the fabrication
procedure, specifications of the specimen, specimen shape, testing procedure are
provided along with the results and discussion.
Tension test is a method used to determine the behavior of materials under axial
loading. It is the most fundamental mechanical test performed on a material. Tension test
is extensively used to perform analysis on strength, elastic and plastic properties of a
material. For many structural metals, stress-strain curves help to define various properties
of a material such as ultimate tensile strength which is significant for safe design. In
general, engineering stress-strain graphs are used for the calculation of mechanical
properties of a material. Engineering stress ( ) is defined as the ratio of load (P) to the
initial cross section area of the specimen ( A0 )
P
A0
26
(7)
Engineering strain ( ) is defined as the ratio of change in length ( l ) to the initial length
of the specimen ( l0 )
l
l0
(8)
3.1 Fabrication and Specifications of the Specimen

The compressed sintered metal fiber mats were purchased from N.V. Bekaert
Fiber Technologies. These mats were made of stainless steel AISI 316 L material.
Stainless steel fiber mats are the most reliable filtration media. The mats were fabricated
by dispersion of metal fibers into a viscous solution of cellulose ether. These viscous
layers of metal fibers were compressed on the foraminous support by either vacuum
molding or pressurized with high viscous flow for the formation of fiber mat. Depending
on the requirement of porosity level of the fiber mat both vacuum molding (pressure of
14.7 psi) and pressurized filtration (pressure of 30 psi) could be used.
Excess amount of cellulose ether on the fiber mat were removed completely by
vacuum washing, forced washing or combustion. Washed fiber mats undergo sintering
process at elevated temperatures (below the melting point of fibers) till the fibers are
fused to each other [57, 58, 59, and 60]. These mats are monolayer with a constant fiber
diameter of 30 m. The compressed mats differ in porosities from 60%, 70% and 80%
depending on different degrees of compression in the manufacturing process. As the
compression on the mat increases the porosity decreases.
27
3.2 Specimen Shape

The metal mats were cut with the help of an ASTM 412 cutting die and a manual
press into a dog bone shape specimen, the shape is narrower at the center than at the ends.
The shape of the specimen is important to prevent breakage or fracture within the
gripping area. Standards have been established such that the dog bone shaped specimens
have a reduction in cross sectional area or the diameter all over the gauge length to make
sure it breaks in the narrow region. Reduction in the cross sectional area of the gauge
length increases the stress in the specimen as stress is inversely proportional to cross
sectional area under loading.
Figure 3-1, Figure 3-2 and Figure 3-3 show the cutting die, manual press and the
specimen respectively.
Figure 3-1: Cutting die

28
Figure 3-2: Manual press
Figure 3-3: Dog- bone shaped stainless steel fiber mat

29
3.3 Testing Procedure

Tensile tests on compressed stainless steel fiber mats were performed using a
universal testing machine (Instron 5560 series) which is mainly used for material testing,
product development testing and quality control by industrial users. It has a load capacity
of 100kN and a load accuracy of +/- 0.5% of indicated load. This machine is a dual
column model with a load cell and two pneumatic side action grips. Load (N) and the
extension in length (longitudinal strain) of the specimen were recorded by the Instron.
Laserlinc laser extensometer was mounted to the frame of the Instron machine as shown
in Figure 3-4 to record the lateral strain (thickness direction). This machine was
administered by Advance Bluehill2 software which generates a stress-strain curve. The
machine has a digital signal processor board which helps to export data to the computer.
Figure 3-5 shows the arrangement of the Instron machine.
Figure 3-4: Laser extensometer

30
Figure 3-5: Instron tensile testing machine
Figure 3-6: Electronic vernier caliper used for width calculation

31
The specimen was clamped vertically to the top grip and allowed to hang freely
for better alignment and then clamped to the bottom grip. Vertical alignment of the
specimen was important to avoid side loading or bending moments in the specimen. After
mounting the specimen, a small amount of load was applied with the help of jog up
switch in the Instron to ensure that it is stiff enough in between the grips. The laser
extensometer was adjusted horizontally such that the laser beam showed the minimum
thickness of the specimen in the Bluehill2 software.
The initial input parameters were gauge length, width and thicknesses of the
narrow cross sectional area. The gauge length and the width of the specimen were
measured with the help of Vernier calipers (Figure 3-6) and thickness was obtained from
the laser reading. The experiments were controlled at a constant strain rate of 1 mm/min
and the intervals at which the raw data points were collected were fixed by the system
using two channels load and time. The experimental procedure was performed on five
samples for each type of mat.
The raw data file obtained from the software after testing comprises of load,
tensile extension, tensile stress, tensile strain, and thickness value (laser reading).
Youngs modulus and Poissons ratio were calculated with the help of test results.
Youngs modulus was calculated as the slope of the line in the elastic region where stress
is proportional to strain obtained from the raw data files.
E /
(9)
E is the Youngs modulus, is the tensile stress and is the tensile strain. Poissons
ratio is the ratio of lateral strain to longitudinal strain with a negative sign. Since most
32
of the materials contract in the direction perpendicular to the applied load, negative sign
is included in the formula to make sure that the ratio is positive.
3
1
(10)
1 is longitudinal strain in the direction of the applied load and 3 is the lateral strain in
the direction perpendicular to the applied load. Later strain is calculated using laser
extensometer reading. Longitudinal strain is calculated from equation 8. l is the
longitudinal displacement of the specimen obtained from the software and l 0 is the initial
gauge length of the specimen. Lateral strain is calculated as the ratio of change in
thickness to the original thickness.
t
t0
(11)
t is the change in thickness of the specimen calculated from the laser extensometer
readings and t 0 is the initial thickness of the specimen.
3.4 Testing Results

Sintered mats of three different porosities were used for tensile testing. The
following table (Table 3.1) shows the average values of Youngs modulus and Poissons
ratio of sintered metal fiber mat of different porosities. Figure 3-7 and Figure 3-8
demonstrate longitudinal stress versus longitudinal strain graphs and lateral strain versus
longitudinal strain graphs for 60%, 70% and 80% porosity sintered metal fiber mat.
33
Table 3.1: Average values of Youngs modulus and Poissons ratio for sintered mats
Sintered mat
Young's modulus
Poissons ratio
(%Porosity)
(MPa)
80
923.51
-5.26
70
1197.12
-7.54
60
1283.52
-17.81
Figure 3-7: Stress vs. strain graphs for sintered mats of different porosities
34
Figure 3-8: Lateral strain vs. longitudinal strain graphs for sintered mats of
different porosities
3.5 Discussion
Sintered stainless steel fiber mats purchased from Bekaert are random metallic
fibrous networks. The porosity of the fiber mat is restrained by the application of pressure
either by vacuum molding or pressurized viscous flow as described in Section 3.1.
Compression of the fibrous mat is related to its porosity, as compression on the mat
increases porosity decreases. The experimental tests conducted by F. Delannay on
sintered mats of compressed steel fibers exhibited negative Poissons ratio out-of-plane
[61, 62]. The auxetic behavior in compressed random fibers was explained by the
deformation mechanism put forward by Tatlier and Berhan as discussed in Chapter 2 i.e.,
compression of random metal fibers results in a geometrical structure equivalent to
geometry of re-entrant honeycombs. Thus compressed sintered stainless steel mats were
35
of interest in order to experimentally validate the numerical model of random fiber

networks developed by Tatlier.
The experimental results (shown in Table 3.1) indicate that the Youngs modulus
of mats increases as the porosity decreases from 80%, 70% and 60 % (increasing
compression). This is because compression of mat decreases the cross sectional area for a
given strain. Since all the experiments were performed at a constant strain rate, increase
in stress results in an increase in effective stiffness of the mat. Simulation results also
show that Youngs modulus increases as compression increases.
From Table 3.1 all the specimens tested can be found to have a negative out-ofplane Poissons ratio. Auxetic effect of the mat increases as the porosity of the mat
decreases (compression increases) i.e. highest for 60% porosity mat and least for 80%
porosity mat. When a mat is compressed, volume decreases thus resulting in greater
deformation of the fibrous network as the number of fibers within the network are
constant. The experimental results also agree qualitatively but not quantitatively with the
numerical study. Thus compression plays a significant role in determining the auxetic
behavior of random fibrous networks.
36
Chapter 4
Composite Mats
Sintered stainless steel mats are highly porous in nature and are known to exhibit
negative Poissons ratio. The main limitation of these mats is their low strength because
of the porosity. Finite element model developed using Comsol Multiphysics discussed in
Chapter 2 validates the hypothesis of manufacturing an auxetic composite by embedding
an auxetic fibrous network with higher stiffness in a conventional matrix with lower
stiffness. To investigate the feasibility of manufacturing the hypothetical composite
model as real materials, experiments were conducted by infusing auxetic network
(compressed sintered stainless steel mats) in a polymer matrix whose stiffness is
significantly lower than that of the auxetic network. DMS- S21 Silanol-terminated
polydimethylsiloxane elastomer was used as the polymer matrix with PSI 021- Poly
(Diethoxysiloxane) as the cross-linker and SND-3260 Di-n-Butyldilauryl Tin as the
catalyst. PDMS is viscoelastic, acts like a viscous liquid at high temperatures, and like an
elastic solid at low temperatures. It is optically clear, and considered to be inert, nontoxic and non-flammable. The chemical formula of PDMS is CH3[Si(CH3)2O]nSi(CH3)3.
37
In the following section sample preparation procedure, experimental results and

scanning electron microscope image analysis for composite mats are discussed.
4.1 Sample Preparation Procedure

4.1.1 Plain PDMS
Appropriate amount of chemicals (Figure 4-2.a, 4-2.b, 4-2.c) as shown in Table
4.1 was taken in a plastic cup (Figure 4-2.d) and weighed on a microbalance. A pipette
tube was used to transfer the measured quantity of chemicals. The cup was placed in the
holder of the Flack Tek Inc Speed mixer (Figure 4-2.f) at the rate of 3500 rpm for about
20 seconds; this helped in improving the mixing of chemicals. Then the mixture was
poured into a plastic dish where it was allowed to cure for 24 hours. After the curing
process the sample was washed with ethanol to remove excess amount of catalyst on the
surface and dried in an oven at 60 degree centigrade overnight. Figure 4-1 shows a
picture of the PDMS sample when the mixture was poured into the plastic dish (left) and
the sample after curing process (right).
Table 4.1: Mixture of chemicals
3 gms sample
Oligomer
Cross linker
Oligomer/ Cross linker
Type -1
2.7
0.3
38
Figure 4-1: Preparation of Plain PDMS sample
4.1.2 Composite Mat

Dog bone shaped wire mesh sheets of different porosities (60%, 70% or 80%)
were placed on a wax paper and weighed initially before the PDMS mixture was added
(Figure 4-2.g). The PDMS mixture prepared as discussed in Section 4.1.1 was spread
evenly on the wire mesh sheets on both sides with the help of a spatula (Figure 4-2.h). A
second sheet of wax paper was placed on the sample and pressure was applied by setting
the 2- roll mill to a desired thickness and the specimen was run in between the rolls
(Figure 4-2.i). The sample was flipped and rotated by 1800. The process was repeated
about three to four times to obtain uniform distribution of PDMS on the sintered mat. The
excess amount of polymer was removed with the help of the spatula and the mat was
allowed to cure for 24 hours. After the curing process the metal wire strips were weighed
again. Thus the composite mat specimen was readied for tensile testing. The schematic
procedure for sample preparation is shown in Figure 4-2.
39
(a) Monomer
(b) Cross linker
(g) Stainless steel mat
(h) Polymer mixture on

steel mat
(c) Catalyst
(f) Speed mixer
(d) Plastic cup
(e) Cup holder
(i) 2- Roll mill
Figure 4-2: Sample preparation procedure for a composite mat
40
4.2 Scanning Electron Microscope Image Analysis

Scanning electron microscope images were taken using Hitachi S-4800 at the
Center for Materials and Sensor Characterization at The University of Toledo to visualize
the dispersion of the polymer in the metal mats. Comparison between sintered steel mats
and composite mats is illustrated in the following figures. Images of sintered mats with
60%, 70%, and 80% porosities are shown in Figures 4-3, 4-4, and 4-5, images of
composite mats are shown in Figures 4-6, 4-7, and 4-8, and images of composite mats at
fractured surfaces are shown in Figures 4-9, 4-10, and 4-11. From composite mat images
it was observed that an appreciable amount of polymer was well distributed in the pores
of the sintered steel mats of different porosities.
41
Figure 4-3: 60% porosity mat
42
43
44
Figure 4-6: 60% porosity composite mat
45
46
47
Figure 4-9: 60% porosity composite mat at fractured surface
48
49
4.3 Weight Measurement Analysis

The amount of polymer deposited on the composite mat can be estimated by the
weight measurement analysis. A microbalance was used to measure the weight of the
samples before and after the addition of the polymer. Weight fractions of fiber and
polymer of different porosities (60%, 70% and 80%) are shown in Table 4.2. Weight
fraction of the fiber is the ratio of weight of fiber to total weight and weight fraction of
polymer is weight of polymer to total weight where total weight is the sum of weights of
fiber and polymer. From these results it can be observed that a good amount of polymer
was deposited on the metal mats. As compression of mat increases, the amount of void
50
spaces in between the fibers decrease which result in decrease in amount of polymer
deposited on the fibrous mats. Deposition of polymer is least on 60% porosity composite
mat and highest on 80% porosity composite mat.
Table 4.2: Weight fraction of fiber and polymer in composite mat for different
porosities
Composite mat
Weight fraction
Porosity
Fiber
Polymer
60%
0.81
0.19
70%
0.77
0.22
80%
0.75
0.24
4.4. Testing Results

4.4.1 Plain PDMS
Plain PDMS polymer was tested using the same testing procedure as discussed in
Section 3.2 but the experiments were controlled at a constant strain rate of 0.5 mm/min
and raw data points were recorded at every 0.1 sec interval. Test results are shown in
Table 4.3. Figure 4-12 and Figure 4-13 show stress versus strain and lateral strain versus
longitudinal strain graphs.
Table 4.3: Average values of Youngs modulus and Poissons ratio for plain PDMS
Plain PDMS
Young's modulus(MPa)
Poissons ratio
Type-1
5.49
1.12
51
Figure 4-12: Stress vs. strain graphs for plain PDMS
Figure 4-13: Lateral strain vs. longitudinal strain graphs for plain PDMS
52
4.4.2 Composite Mats

Composite mats (60%, 70% and 80% porosity) were tested using the same testing
procedure as discussed in Section 3.2. Average values of Youngs modulus and Poissons
ratio are tabulated in Table 4.4. The graph of lateral strain versus longitudinal strain is
shown in Figure 4-14.
Table 4.4: Comparison of Youngs modulus and Poissons ratio for composite and
sintered mats
Mats
Composite Mats
Young's
modulus(MPa)
Composite
Mats Poissons
ratio
Sintered
Mats
Young's
modulus
(MPa)
60%
1371.7
-9.2
923.51
-5.26
70%
1325
-9.2
1197.12
-7.54
80%
1272.8
-4
1283.52
-17.81
Sintered
Mats
Poissons
ratio
Table 4.5: Variation in thickness for sintered and composite mats
Mat porosity
Sintered mat
thickness(mm)
Composite mat
thickness(mm)
Thickness
compressed
(mm)
60%
0.38
0.33
0.05
70%
0.42
0.35
0.07
80%
0.54
0.41
0.13
53
Figure 4-14: Lateral strain vs. longitudinal strain graphs for composite mats
4.3 Discussion
A considerable amount of deposited polymer was seen both from SEM image
analysis and weight measurement analysis as described in previous sections. From
Figure- 4-14 it can be observed that the Poissons ratio remains negative after auxetic
network is embedded in the polymer matrix. This can be associated with the fact that the
stiffness of the plain polymer (of order 5 MPa) as shown in Figure 4-12 is much lower
compared to the sintered metal fiber mat (of order 1100 MPa).
Experimental results from Table 4.4 exhibit a significant increase in stiffness of
the composite mats, formed by embedding an auxetic network in a polymer matrix,
compared to sintered metal mats. This increase of stiffness in composite mats can be
54
attributed to the compression when passed over 2-roll mill but not because of presence of
polymer whose stiffness is much lower than that of fibrous mats. Table 4.5 shows the
variation in thickness of the mat before and after passing through 2-roll mill. From the
table one can observe that 80% porosity composite mats were more compressed when
compared to 70% and 60% because these mats are highly porous and thicker.
Composite mats exhibit negative Poissons ratio which is shown in Table 4.4.
From this we can conclude that reinforcement of an auxetic network (sintered metal mat)
in a conventional matrix (polymer matrix) resulted in an auxetic composite. This
confirms the feasibility of the hypothetical composite discussed in Chapter 2. However,
the increase of stiffness observed in composite mats was mainly due to the compression
of mats during preparation process.
55
Chapter 5
Nanocomposites
5.1 General Overview and Motivation

Carbon materials have drawn immense attention from industrial and scientific
societies since the inventions of C60, carbon nanobers (CNFs) and carbon nanotubes
(CNTs) in the 1980s. Carbon nanofibers are cylindrical nanostructures with graphene
layers stacked in the form of cones or plates. Carbon nanofibers with graphene layers
wrapped into perfect cylinders are called carbon nanotubes. Carbon nanomaterials
possess extraordinary properties, such as tensile strength, elastic modulus, electrical and
thermal conductivity [63, 64]. They have very high aspect ratio and exhibit extremely
high Youngs modulus compared to steels [65, 66]. However, high material cost and the
difficulty in material handling are the two main reasons limiting the engineering
applications of carbon nanomaterials.
In order to take full advantage of carbon materials (carbon nanotubes and carbon
nanofibers) carbon-based polymer composites are normally synthesized either by directly
mixing the nanofillers with low viscosity polymer matrices [67, 68, 69] or through the
56
introduction of in situ polymerization [70, 71]. The effective utilization of carbon

nanofibers in composite applications depends considerably on the ability to disperse and
functionalize them. Good interfacial bonding is required to attain high load transfer
across the nanofiber-matrix interface, in order to improve the mechanical properties of
polymer composites.
Evans first developed a numerical model, considering periodic arrangement of reentrant structures as reinforcing elements in a matrix, to manufacture an auxetic
composite by embedding an auxetic network in a conventional matrix. In this study it was
found that the model exhibited auxetic behavior when the stiffness of the matrix material
is significantly lower than that of the reinforcing network [72]. The possibility of auxetic
behavior in carbon fiber composites was also proposed in the same study. This was the
motivation for our research to manufacture nanocomposites and investigate their auxetic
behavior. The in-plane auxetic behavior in nanotube networks was recently reported [73].
The focus of present study is to investigate the out-of-plane auxetic behavior of
nanocomposites. The cost effective carbon nanofibers were selected instead of carbon
nanotubes.
The mechanism of compressed random fiber network was best understood from
the numerical model created by Tatlier and Berhan [55]. They proposed that the amount
of compression and the mat anisotropy were the critical parameters in determination of
the auxetic behavior in out-of-plane direction. Experiments were conducted to validate
the proposed numerical model and to investigate the feasibility of manufacturing an
auxetic nanocomposite by embedding an auxetic fiber network (high loading of
nanofibers) in a supporting matrix (polymer matrix). The effect of several parameters
57
such as nanofiber loading, nanofiber functionalization and matrix material were

considered.
5.2 Introduction
In this section purification and preparation methods of high strength and flexible
carbon
nanofiber
elastomer
composites
are
discussed.
Silanol
terminated
polydimethlsiloxane (PDMS), because of its flexibility, moldability and mechanical

stability, was used as the elastomer in the preparation method of nanocomposites. PDMS
acts as an elastic solid at room temperature and as a high viscous liquid at high
temperatures. Poly (Diethoxysiloxane) and di-n-Butyldilaurylin were used as cross linker
and catalyst respectively. The function of a cross linker is to cross link one polymer chain
to the other by strong covalent bond and the catalyst helps to speed up the polymeric
reaction between silicon molecules. These chemicals were supplied by Gelest, Inc. The
three different types of fibers used were pristine, oxidized and functionalized carbon
nanofibers. Pristine fibers, produced by Pyrograf Products Inc, were directly used in
nanocomposite sample preparation, but oxidized carbon nano fibers purchased were
purified from impurities before being used. Carbon nanofibers were functionalized with
PDMS-NH2 by Dr. Javed Mapker, who was a Ph.D. student in CHEE Department, at The
University of Toledo. Functionalization of carbon nanofibers is to improve interface
between the fiber and the polymer there by enhancing the properties of the
nanocomposite.
58
5.3 Purification of Oxidized Carbon Nanofibers

Oxidized carbon nanofibers were purchased from Pyrograf Products Inc., Ohio.
Oxidized fibers comprise of carbon fiber (>98 wt %), iron (1.4 wt %), sulfur (<0.8 wt %),
mineral content (1% from H2O) and oxygen (10-14 atom %) according to the companys
material technical data sheet. The impurities present in these fibers were purified with
nitric acid and distilled water. The purification procedure can be divided into three
phases: sonication, purification and filtration. Each of these is discussed in detail in the
following sections.
5.3.1 Sonication
14 grams of oxidized fibers were taken and crushed in the mortar with the help of
a pestle to disperse agglomerated carbon fibers. They were weighed with the weight
balance and transferred to a round bottle flask. Nanofibers were mixed with diluted nitric
acid (For 110 ml of nitric acid 590 ml of distilled water was used for dilution) and
sonicated in the sonicator for about 2 hours. Sonication, the process of applying ultra
sound waves to agitate carbon fiber particles in the liquid solvent, also helps in
evacuating dissolved gases from liquid under vacuum. The sonication process is shown in
Figure 5-1.
59
Figure 5-1: Sonication process
5.3.2 Purification
Experimental setup for purification process is shown in the Figure 5-2. This
consists of an electric heater to maintain a constant temperature of 110 degrees centigrade
throughout the experiment. Heat is conducted from the electric heater by a sand bath
placed on it to the round bottle flask which contains sonicated carbon nanofibers. A
thermometer was placed in the sand bath for measurement of temperature. A refluxor was
placed on top of the round bottle flask to facilitate the back flow of heated nitric acid in to
the round bottle flask. Condenser was attached to the refluxor to help in cooling the acid
60
vapors. Two outlets were provided to the condenser for tap water flow throughout the
process. Entire experimental setup was placed in a hood and was heated for about 48
hours. Then heat was removed and the setup was cooled down to room temperature.
Carbon fibers were then separated from nitric acid solution by filtration procedure.
Figure 5-2: Experimental setup for purification of oxidized carbon nanofibers

61
5.3.3 Filtration
Experimental setup for filtration process is shown in Figure 5-3. The apparatus
consists of a conical filtration flask, funnel and a vacuum pump. Filter papers were placed
in the funnel and then cooled carbon fibers, nitric acid solution were poured. Nitric acid
was collected in to the conical flask, with an outlet to the vacuum pump. Carbon fibers
were collected on the filter paper. Vacuum was applied to speed up the separation of
nitric acid from fibers with the help of vacuum pump. The fibers were washed about 8 to
10 times with distilled water to completely remove nitric acid. Moist carbon fibers were
carefully transformed into a plastic dish to dry at 60 degree centigrade overnight in the
oven. This lump of carbon fibers was crushed in a mortar and used for nanocomposite
preparation.
Figure 5-3: Filtration process

62
5.4 Nanocomposites Sample Preparation

Pristine, oxidized and functionalized carbon nanocomposites were prepared by the
following method. The schematic method followed in preparation of nanocomposites is
shown in the Figure 5-4. The amounts of carbon fibers and chemicals used for sample
preparation are shown in Table 5.1. Silanol terminated polydimethyl siloxane (PDMS)
elastomer was used as the polymer matrix to make nanocomposite. Poly (Diethoxy
siloxane) was used as cross linker and di-n-Butyldilaurylin as catalyst.
Table 5.1: Fiber loading ratios

Loading
(%)
15
Carbon
nanofibers
(Grams)
0.45
Oligomer
(Grams)
2.295
Cross linker
(Grams)
0.255
Catalyst
(Grams)
0.255
20
0.6
2.16
0.24
0.24
25
0.75
2.025
0.225
0.225
Carbon nanofibers were taken into mortar and crushed with the help of pestle.
Desired amount of fibers (Table 5.1) were weighed in a plastic cup with weight balance.
Required amount of oligomer was added to the fibers with plastic filler. The plastic cup
was placed in the holder of the speed mixer. The purpose of the speed mixer is for better
dispersion of carbon fibers in the elastomer. The speed mixer was programmed to mix for
20 seconds at 3500 rpm. The process was repeated by adding cross linker and catalyst to
the mixture. Lump of carbon fiber and elastomer obtained was removed and placed in
63
between two wax sheets with a spatula. One of the three different methods was followed
in the curing process of the sample.
(a) In 2- roll mill procedure the roller was set to desired thickness and the mixture
obtained was run in between the rolls. The sample was flipped and rotated to 180
degrees. The process was repeated for about three to four times. Now the sample was
left to cure for about 24 hours. The 2- roll mill procedure gives a uniform thickness
throughout the sample.
(b)
In manual press with no weight procedure the lump of carbon fiber mixture was
pressed with the help of glass cap uniformly and left to cure for 24 hours.
(c) In manual press with heavy weight procedure the lump of carbon fiber mixture was
pressed with the help of glass cap uniformly and a heavy weight was placed on the
glass cap during the curing process of 24 hours.
After curing the sample, they were washed with ethanol to remove excess catalyst
formed on the surface of the nanocomposite and dried in an oven at 60 degree centigrade
for about 24 hours. The sample was later cooled down to room temperature and was
tested on the Instron machine to find strength and Poissons ratio. Scanning electron
microscope images of 20% fiber loading oxidized carbon nanocomposites prepared by all
three procedures were taken as shown in Figures 5-5, 5-6 and 5-7.
64
Figure 5-4: Schematic procedure for nanocomposite preparation
65
Figure 5-5: OCNF- 2 roll mill procedure (20% fiber loading)
Figure 5-6: OCNF- manual press with weight during curing procedure
(20% fiber loading)
66
Figure 5-7: OCNF- manual press with weight during curing procedure
(20% fiber loading)
5.5 Test Results

Different nanocomposite samples of pristine, oxidized and functionalized fibers
prepared were tested using the same testing procedure as discussed in Section 3.2 but the
specimens were cut in to 5mm wide strips instead of dog bone shape. The gauge length of
the specimen in between the grips was measured with electronic vernier caliper. The
experiments were controlled at a constant strain rate of 0.5mm/min and raw data points
were collected at every 0.1 sec. Results of Youngs modulus and Poissons ratio for all
types of nanofibers with different fiber loadings were presented in the following tables.
67
5.5.1 Pristine Fibers

Table 5.2: Youngs modulus and Poissons ratio for 15% fiber loading of pristine
fibers
Young's modulus (MPa)
Poisson's ratio
15% Fiber loading
R1
R2
R3
R1
R2
R3
2Roll mill
13.33
10.97
8.32
0.15
0.17
2.73
Manual pressweight used
21.03
18.15
13.99
3.09
0.168
-0.2
Manual press-no
weight
11.36
10.77
12.24
-2.95
-0.58
-2.27
fibers
Poisson's ratio
20% Fiber loading
R1
R2
R3
R1
R2
R3
2Roll mill
12.46
11.26
12.57
-0.74
3.44
0.83
Manual pressweight used
11.41
12.37
8.75
-1.43
-0.32
-0.77
Manual press-no
weight
13.41
12.69
12.6
-2.96
-6.4
0.35
68
fibers
25% Fiber
loading
2Roll mill
Manual
press-no
weight
Poisson's ratio
R1
R2
R1
R2
5.09
5.02
-2.23
5.9
8.88
11.8
-1.67
-1.96
5.5.2 Oxidized Fibers

Table 5.5: Youngs modulus and Poissons ratio for 15% fiber loading of oxidized
fibers
Young's
modulus
Poisson's ratio
(MPa)
15% Fiber loading
R1
R2
R3
R1
R2
R3
2Roll mill
12.68
13.48
11.27
-3.15
2.81
-2.13
11.78
9.78
10.11
0.38
-1.72
0.29
Manual pressweight

used
69
fibers
Young's modulus
(MPa)
20% Fiber loading
Poisson's ratio
R1
R2
R3
R1
R2
R3
22.27
18.21
18.31
-3.04
-5.58
-6.64
used
17.34
16
-3.29
0.43
Manual press-no weight
15.85
19.67
-0.8
0.84
2Roll mill
15.99
-0.35
fibers
Young's modulus
(MPa)
Poisson's ratio
25% Fiber loading
R1
R2
R3
R1
R2
R3
2Roll mill
18.72
15.49
16.53
3.2
-4.9
-4.1
12.56
14.83
16.05
-0.39
1.27
4.03

used
70
5.5.3 Functionalized Fibers

Table 5.8: Youngs modulus and Poissons ratio for 20% fiber loading of
functionalized fibers
Youngs
modulus(MPa)
20% Fiber loading
Poissons ratio
R1
R2
R3
R1
R2
R3
36.26
34.47
24.6
-1.39
0.61
0.98

used
5.6 Discussion
5.6.1 Effect of Nanofiber Type
Nanocomposite made of different types of nanofibers, i.e. pristine, oxidized and
functionalized showed a significant increase in stiffness respectively. From Figures 5-8
and 5-9, it can be observed that PDMS functionalized fibers exhibit better stiffness
compared to oxidized and pristine fibers. The -NH2 link is highly reactive when
compared to OH resulting in good dispersion of CNF-PDMS-NH2 in PDMS matrix. The
functionalized fibers also improve wetting, as they are cross linked and covalently
attached to the bulk polymer, enhance interfacial adhesion. The pristine nanocomposites
have poor dispersion and wetting compared to oxidized and functionalized composites as
they are not attached with any functionalized group on their surface. Test results of 20%
fiber loading of pristine, oxidized and functionalized nanocomposites tabulated in Table
5.3, Table 5.6 and Table 5.8 respectively exhibited auxetic behavior for most of the runs.
From the Figure 5-10 it can be observed that there is no significant effect on Poissons
71
ratio based on surface treatment methods. They have similar values of Poissons ratio for
all types of fiber.
Figure 5-8: Stress vs. strain graphs for different nanocomposites of 20% fiber
loading
Figure 5-9: Stress vs. strain graphs for different nanocomposites of 20% fiber
loading (elastic range)
72
Figure 5-10: Lateral strain vs. longitudinal strain graphs for nanocomposite samples
at 20% fiber loading
5.6.2 Effect of Nanofiber Loading

Pristine fibers made of 15%, 20%, and 25%
fiber loading showed a little
variation in the slope of the elastic portion of lateral strain versus longitudinal strain as
shown in Figure 5-11. Figure 5-12 shows the elastic portion of stress versus strain graph
for pristine fibers. It can be observed from these results that as the fiber loading increases
stiffness decreases. This is because if fiber loading increases mixing and dispersion of
fibers in the polymer matrix become difficult. From Table 5.9, Table 5.10 and Table 5.11
one can observe that as fiber loading increases the amount of cross linker decreses which
effects the dispersion of these fibers in the polymer matrix.
73
Figure 5-11: Lateral strain vs. longitudinal strain graphs for different fiber loading
of pristine fibers
Figure 5-12: Stress vs. strain curves for nanocomposite samples with pristine
nanofibers
74
Table 5.9: Volume fraction of fiber and polymer for 15% fiber loading
Nanocomposite
sample
Weight
Density(g/cm )
percentage
Volume fraction
Fiber
1.95
15%
.0813
PDMS
0.97
77%
.8339
Cross linker
1.05-1.07
9%
.0848
Nanocomposite
Density(g/cm3)
Weight percentage
Volume fraction
Fiber
1.95
20%
.1114
PDMS
0.97
72%
.8065
Cross linker
1.05-1.07
8%
.0820
sample
Nanocomposite
Weight
3
sample
Density(g/cm )
percentage
Volume fraction
Fiber
1.95
25%
.1433
PDMS
0.97
68%
.7777
Cross linker
1.05-1.07
8%
.0791
75
5.6.3 Effect of Compression

Nanocomposite sheets made by different procedures were tested. It is observed
from most of the results that preparation of nanocomposite with 2 roll mill method
showed greater auxetic effect. The nanocomposite sample is assumed to be auxetic,
because of the subjected compression while passing through 2 roll mill, similar to the
auxetic nature developed due to compression in both fused networks of the numerical
model and stainless steel mats.
In order to increase the auxetic nature, nanocomposite samples were produced by
compressing with heavy weight during curing process. However, results have shown that
these samples have almost positive Poissons ratio. This suggests that the excessive
compression in-spite of increasing auxetic behavior has compromised the structural
integrity on embedded nanofiber network. These results show that compression plays a
key role in determination of auxetic behavior of nanocomposite similar to fibrous
networks. Figure 5-13 shows lateral strain verses longitudinal strain for 20% fiber
loading of pristine fibers.
76
Figure 5-13: Lateral strain vs. longitudinal strain for 20% fiber loading of pristine
fibers
Thus nanocomposite sheets prepared as discussed show auxetic behavior and
support the central hypothesis of the project and also validate the random fiber network
model where compression is the key parameter in auxetic behavior of both fiber networks
and their composites. However, auxetic behavior is not observed in nanocomposite if the
compression is too high.
77
Chapter 6
Conclusion and Future Work
6.1 Conclusion
The two dimensional finite element model created confirms the hypothesis of
manufacturing an auxetic composite by embedding an auxetic fibrous network in a
conventional matrix material. Experiments conducted on sintered stainless steel mats
validated the simulations of numerical model qualitatively but not quantitatively and
those on composite mats confirmed the feasibility of manufacturing auxetic composites.
The amount of compression during mat formation was found to be significant in
determination of auxetic behavior.
Experimental results confirm that the auxetic nanocomposite can be
manufactured. From the results, at high carbon fiber loading it is assumed that the
embedded nanofibers, even not fused or sintered, form an effectively connected network
within a polymer matrix. Compression during the preparation of nanocomposite sheets
plays a key role in determining auxetic behavior.
Poissons ratio is found to decrease with increasing compression for both sintered
mats and nanocomposites. However excessive compression seems to compromise the
78
auxetic network and also the auxetic behavior in nanocomposites is not seen if the
compression is too high.
6.2 Future Work

A best practice should be implemented for recording minimum initial thickness to
minimize experimental errors that might have occurred while mounting the laser
extensometer on the Instron. Preliminary results showed that presence of Epon resin
polymer increased the stiffness and strength of the composite mat. Thus, further
investigation of methods to increase the stiffness of the composite mats should be
explored. Further experiments on nanocomposite samples should be conducted for a
better understanding the effect of compression, type of fiber and fiber loading on auxetic
behavior.
79
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87

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A Thesis

The University of Toledo

Copyright 2010, Sharmila Jayanty

Dedicated to my parents Raghu Jayanty (late) and Surya Kumari Jayanty.

Abstract ........................................................................................................................... iii

General Overview ................................................................................................ 1

1.2 Properties of Auxetic Materials................................................................................. 3

3. Sintered Stainless Steel Fiber Mats ............................................................................26

5.6.1 Effect of Nanofiber Type ..................................................................................... 71

Figure 2-10: Effect of change in Poissons ratio on matrix material ................................ 25

1.1 General Overview

Figure 1-1: Schematic diagram of positive Poissons ratio deformation when a

Figure 1-2: Schematic diagram of negative Poissons ratio deformation when a

1.2 Properties of Auxetic Materials

modulus relative to bulk modulus is obtained for auxetic materials when

According to classical theory of elasticity, the relationship between indentation

where H is hardness and 1 is for uniform pressure distribution and

Hertzian indentation. According to Equation (4) as approaches 1 or -1, the

1.3 Potential Applications

Auxetic materials undergo synclastic or double curvature deformation when they

In biomedical field auxetic materials have numerous potential applications like

Auxetic materials have applications in nuclear reactor construction. For example,

1.4 Types of Auxetic Materials

1.4.1 Natural Auxetic Materials

1.4.2 Man Made Auxetic Materials

1.4.2.1 Auxetic Cellular Solids

Figure 1-3: Deformation mechanisms in re-entrant and conventional honeycomb

Auxetic polyurethane foams developed by Roderick Lakes in 1987 were an

Figure 1-4: Pore structures of non auxetic and auxetic foam

1.4.2.2 Micro Porous Polymers

1.4.2.3 Auxetic Composites

Finite Element Modeling

The modeling discussed in this chapter includes a two dimensional multiphysics

2.1 Network Generation and Modeling

Figure 2-3: Dimensions of a re-entrant honey comb structure (unit cell)

Table 2.1: Different Cell Geometries

2.2 Simulation Procedure

Figure 2-5: Deformed fibrous network model

2.3 Results and Discussion

2.3.1 Effect of Strain and Network Geometry on Poissons Ratio

Table 2.2 Effect of strain rate on Poissons ratio

2.2.3 Effect of Youngs Modulus on Poissons Ratio

Table 2.3: Effect of Youngs modulus on Poissons ratio

Figure 2-8: Compliant matrix

Figure 2-9: Stiff matrix

Figure 2-10: Effect of change in Poissons ratio on matrix material

Sintered Stainless Steel Fiber Mats

3.1 Fabrication and Specifications of the Specimen

3.2 Specimen Shape

Figure 3-1: Cutting die

Figure 3-2: Manual press

Figure 3-3: Dog- bone shaped stainless steel fiber mat

3.3 Testing Procedure

Figure 3-4: Laser extensometer

Figure 3-5: Instron tensile testing machine

Figure 3-6: Electronic vernier caliper used for width calculation

readings and t 0 is the initial thickness of the specimen.

3.4 Testing Results

of interest in order to experimentally validate the numerical model of random fiber

In the following section sample preparation procedure, experimental results and

4.1 Sample Preparation Procedure

Oligomer/ Cross linker

Figure 4-1: Preparation of Plain PDMS sample