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Polymer Nanocomposite Materials
Polymer Nanocomposite Materials
Applications in Integrated Electronic Devices
Edited by
Ye Zhou
Guanglong Ding
Editors All books published by Wiley-VCH
are carefully produced. Nevertheless,
Ye Zhou authors, editors, and publisher do not
Shenzhen University warrant the information contained in
Institute for Advanced Study these books, including this book, to
Room 358, Administration Building be free of errors. Readers are advised
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items may inadvertently be inaccurate.
Guanglong Ding
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Print ISBN: 978-3-527-34744-5

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Printed on acid-free paper
10 9 8 7 6 5 4 3 2 1
v
Contents
Preface xi
1 Introduction of Polymer Nanocomposites 1

Teng Li, Guanglong Ding, Su-Ting Han, and Ye Zhou
1.1 Introduction 1
1.2 The Advantage of Nanocomposites 3
1.3 Classification of Nanoscale Fillers 5
1.3.1 One-Dimensional Nanofillers 5
1.3.2 Two-Dimensional Nanofillers 6
1.3.3 Three-Dimensional Nanofillers 6
1.4 The Properties of Polymer Nanocomposites 6
1.5 Synthesis of Polymer Nanocomposites 7
1.5.1 Ultrasonication-assisted Solution Mixing 8
1.5.2 Shear Mixing 9
1.5.3 Three Roll Milling 9
1.5.4 Ball Milling 10
1.5.5 Double-screw Extrusion 10
1.5.6 In Situ Synthesis 10
1.6 Conclusions and Future Outlook 11
References 11
2 Fabrication of Conductive Polymer Composites and Their

Applications in Sensors 21
Jiefeng Gao
2.1 Introduction 21
2.2 Fabrication Methods for CPCs 22
2.2.1 Melt Blending 23
2.2.2 Solution Blending 25
2.2.3 In Situ Polymerization 27
2.3 Morphologies 27
2.3.1 Random Dispersion of Nanofiller in the Polymer Matrix 27
2.3.2 Selective Distribution of Nanofillers on the Interface 29
2.3.2.1 Segregated Structure 29
vi Contents
2.3.2.2 Surface Coating 31

2.4 Application in Sensors 32
2.4.1 Strain Sensor 33
2.4.2 Piezoresistive Sensor 33
2.4.3 Gas Sensor 35
2.4.4 Temperature Sensor 38
2.5 Conclusion 40
References 41
3 Biodegradable Polymer Nanocomposites for Electronics 53

Wei Wu
3.1 Introduction 53
3.2 Biodegradable Polymer Nanocomposites in Electronics 55
3.2.1 Polylactide 55
3.2.2 PCL 58
3.2.3 PVA 59
3.2.4 PVP 61
3.2.5 Cellulose 62
3.2.6 Chitosan 64
3.2.7 Silk 65
3.3 Challenges and Prospects 66
List of Abbreviations 67
References 67
4 Polymer Nanocomposites for Photodetectors 77

Raj Wali Khan, Zheng Wen, and Zhenhua Sun
4.1 Introduction 77
4.2 Photodetector Brief 79
4.2.1 Photodiode 80
4.2.2 Photoconductor 80
4.3 Photodetectors Based on Novel Semiconductors 82
4.4 Photodetectors Based on Polymer Nanocomposites 87
4.4.1 Polymer–Polymer Nanocomposite 88
4.4.2 Polymer–Small Molecular Organic Nanocomposite 98
4.4.2.1 MEH-PPV–Small Molecular Organic Nanocomposite 98
4.4.2.2 P3HT-Small Molecular Organic Nanocomposite 99
4.4.3 Polymer–Polymer–Small Molecular Organic Nanocomposite 107
4.4.4 Polymer–Small Molecular Organic–Small Molecular Organic
Nanocomposite 110
4.4.5 Polymer–Inorganic Nanocrystals Nanocomposite 112
4.4.5.1 MEH-PPV–Inorganic Nanocrystals Nanocomposite 112
4.4.5.2 P3HT–Inorganic Nanocrystals Nanocomposite 115
4.4.6 Polymer–Small Molecular Organic–Inorganic Nanocrystals
Nanocomposite 120
4.5 Outlook 123
Contents vii
List of Abbreviations 123

References 124
5 Polymer Nanocomposites for Pressure Sensors 131

Qi-Jun Sun and Xin-Hua Zhao
5.1 Introduction 131
5.2 Parameters for Pressure Sensors 132
5.2.1 Pressure Sensitivity 132
5.2.2 Linear Sensing Range 134
5.2.3 LOD and Response Speed 134
5.2.4 Reliability 134
5.3 Working Principles and Examples of Polymer Nanocomposite Based
Pressure Sensors 135
5.3.1 Capacitive Pressure Sensors 135
5.3.2 Piezoresistive Pressure Sensors 137
5.3.3 Piezoelectric and Triboelectric Tactile Sensors Based on Polymer
Nanocomposites 143
5.4 Applications of the Polymer Nanocomposite Based Pressure
Sensors 148
5.4.1 Human Wrist Pulse Detection 148
5.4.2 Subtle Human Motion Detection 149
5.4.3 Texture Roughness Detection 151
5.4.4 E-skin Application 152
5.5 Performance of Pressure Sensors with the Polymer Nanocomposites
Reported Over the Past Decade 153
5.6 Conclusion 154
References 154
6 The Application of Polymer Nanocomposites in Energy

Storage Devices 157
Ningyuan Nie, Mengmeng Hu, Jie Liu, Jiangqi Wang, Panpan Wang,
Hua Wang, Zhenyuan Ji, Zhe Chen, and Yan Huang
6.2 Electrodes 158
6.2.1 For Battery 158
6.2.1.1 Polymer–Graphene/Carbon Nanotube 158
6.2.1.2 Polymer Inorganic 161
6.2.1.3 Polymer–Organic Salt Graphene 163
6.2.2 For Supercapacitor 164
6.2.2.1 Polymer–Metal Oxide 165
6.2.2.2 Polymer–Graphene/Carbon Nanotube 165
6.2.2.3 Polymer–Metal Oxide–Graphene/Carbon Nanotubes 169
6.3 Electrolytes 171
6.3.2 For Supercapacitor 172
viii Contents
6.4 Separator 174

6.4.2 For Supercapacitors 175
6.5 Conclusion 176
References 177
7 Functional Polymer Nanocomposite for Triboelectric

Nanogenerators 189
Xingyi Dai, Jiancheng Han, Qiuqun Zheng, Cheng-Han Zhao, and
Long-Biao Huang
7.2 Triboelectric Nanogenerators 190
7.3 Functional Polymer Nanocomposite 194
7.4 Self-healing Triboelectric Nanogenerators 197
7.5 Shape Memory Triboelectric Nanogenerators 201
7.6 Biodegradable Triboelectric Nanogenerators 204
7.7 Conclusion 208
References 208
8 Polymer Nanocomposites for Resistive Switching

Memory 211
Qazi Muhammad Saqib, Muhammad Umair Khan, and Jinho Bae
8.2 Resistive Switching Memory for Polymer Nanocomposite 213
8.2.1 Resistive Switching 213
8.2.2 Resistive Switching Memory Operating Mechanism 214
8.2.2.1 Formation and Rupture of Conductive Filaments 214
8.2.2.2 Cations and Anions Migration 216
8.2.2.3 Electrons Trapping and De-tapping 216
8.2.2.4 Other Conduction Mechanisms 216
8.2.3 Fabrication Techniques 217
8.2.4 Polymer Nanocomposite Materials 218
8.3 Polymer Nanocomposite Based RSM Devices 218
8.3.1 Oxide Based Polymer Nanocomposite RSM 218
8.3.2 Metal Based Nanoparticles for Polymer Nanocomposite RSM 222
8.3.3 Graphene Based Polymer Nanocomposite RSM 224
8.3.4 Quantum Dot Based Polymer Nanocomposite RSM 227
8.3.5 Polymer Based Nanocomposites for RSM 229
8.3.6 2D Material Based Polymer Nanocomposites RSM 231
8.3.7 Other Materials Used for Polymer Nanocomposite Based RSM 232
8.4 Concluding Remarks 233
Acknowledgments 234
References 234
8.A Performance Comparison According to Device Material and
Structure 243
Contents ix
9 Polymer Nanocomposites for Temperature Sensing and

Self-regulating Heating Devices 247
Yi Liu, Han Zhang, and Emiliano Bilotti
9.2 Conducting Mechanism and Percolation Theory 248
9.3 PTC Theory 249
9.4 Main Factors Influencing the PTC Effect 250
9.4.1 Effect of Filler Size and Shape 250
9.4.2 Effect of Filler Dispersion and Distribution 253
9.4.3 Effect of Mixed Filler 254
9.4.4 Effect of Polymer Thermal Expansion and Crystallinity 255
9.4.5 Effect of Polymer Transition Temperature 257
9.4.6 Effect of Polymer Blend 257
9.5 Temperature Sensors 259
9.6 Self-regulating Heating Devices 259
9.7 Conclusions 262
References 263
10 Polymer Nanocomposites for EMI Shielding Application 267

Ajitha A. Ramachandran and Sabu Thomas
10.2 Mechanism of EMI Shielding of Polymer Composites 268
10.2.1 Materials for EMI Shielding 269
10.3 Polymer Nanocomposites for EMI Shielding Application 270
10.3.1 Nanofiller Incorporated Conducting Polymer Composites 270
10.3.2 Polymer Blend Nanocomposites for Electromagnetic Interference (EMI)
Shielding 271
10.3.3 Conducting Polymers for EMI Shielding Application 272
10.4 Characterization Techniques Used for the Electrical Studies of Polymer
Composites 274
10.4.1 Conductivity Studies of Polymer Composites 274
10.4.2 Electromagnetic Interference (EMI) Shielding Studies 276
10.5 Conclusion 278
References 279
Index 285
xi
Preface
Polymer nanocomposites combining the merits of polymers (e.g. light weight,

flexibility, low cost) and functional properties of nanomaterials caused by small
size effect, quantum size effect, and surface/boundary effect show adjustable
optical, electrical, biological, and mechanical characteristics and attract extensive
researches. Various polymer nanocomposites with amazing performances have
been prepared and utilized for developing integrated electronic devices in a number
of emerging areas and exhibit huge commercial value, thanks to their simple
preparation techniques and countless combinations. This book highlights the
recent researches about the basic conceptions, preparation/characterization tech-
niques, properties, device design strategies, and intriguing applications of polymer
nanocomposites. The existing/potential application prospects and challenges for
the polymer nanocomposites are also discussed. We expect that this book can
offer a well-timed assistance to the academic researchers in the rapidly expanding
applications including environment, sensor, energy conversion/storage, biology,
and information storage as a simple and convenience instrument.
Herein, we would like to thank all the authors who have made contributions in
this book. We want to express our sincerest appreciation and respect to Ms. Kather-
ine Wong, Dr. Shaoyu Qian, Ms. Pinky Sathishkumar, Mathangi Balasubramanian
and other editors at Wiley for all the help offered during the whole book editing
process. We also want to thank all the readers interested in this book. In this book,
we have introduced the concepts, properties, and mechanisms of polymer nanocom-
posites and summarized their recent applications in some hottest fields. The applica-
tion challenges, commercial prospects, and potential research directions of polymer
nanocomposites are also pointed out and discussed. We aim to provide a comprehen-
sive, popular, and up-to-date book for the researchers. Although we have done our
best to make this book better, there still inevitably are some omissions and mistakes.
Please grant your criticisms and instructions.
We hope that this book can provide references and guides for researchers in poly-
mer nanocomposites based electron devices, as well as promote the interests of the
students to this field.
01 June 2020 Ye Zhou

Guanglong Ding
1
Introduction of Polymer Nanocomposites

Teng Li 1 , Guanglong Ding 2 , Su-Ting Han 1 , and Ye Zhou 2
1
Shenzhen University, Institute of Microscale Optoelectronics, Room 909, Shenzhen, Guangdong 518060,
China
2
Shenzhen University, Institute for Advanced Study, Room 358, Shenzhen, Guangdong 518060, China
1.1 Introduction
Polymers have been one of the most important components in almost every area of
human activity today. Nowadays, polymers as multifunctional materials gradually
replace metals, glass, paper, and other traditional materials in various applications
due to its lightweight, flexibility, and low cost [1]. In most of their applications,
the applied materials are not composed of a single chemical component but
mixture systems of multiple components with polymers and other additives. By
incorporating different additives, such as metal, minerals, or even air, a wide variety
of materials with unique physical properties and competitive production costs can
be produced. For example, glass fiber-reinforced plastics are composite materials
manufactured by laminating unsaturated polyester resin with glass fiber and filler,
which can increase mechanical strength and heat resistance [2].
In addition, scientific research shows that the size of filling material in fiber rein-
forced composites has a great influence on the material properties, since the size of
the filling particles largely determines the surface interactions of adhesion, particle
movement, dispersion, and bonding between the surface and matrix [3]. With the
particle size of the filler that gradually reduces to the nanoscale, some properties
depending on the interface have undergone great changes, such as gas adsorption,
chemical activity, electrical properties, and catalytic activity. Examples of different
sizes of materials are shown in Figure 1.1, and a hydrogen atom is about 0.1 nm
in size, while a human hair is 104 nm in diameter. Among them, nanomaterials
are employed to describe the materials that have at least one dimension in the size
range from approximately 1 to 100 nm [4]. Different from the bulk and microscale
materials, nanomaterials are unique in that they have many unusual, useful, and
interesting properties. For example, bulk gold is a very stable precious metal in
golden color, which can be kept for a long time under atmospheric environment,
so it is used as the initial currency by people. Unlike bulk gold, gold nanoparticles
dispersed in water will show different colors according to the size of nanoparticles,
Polymer Nanocomposite Materials: Applications in Integrated Electronic Devices, First Edition.
Edited by Ye Zhou and Guanglong Ding.
© 2021 WILEY-VCH GmbH. Published 2021 by WILEY-VCH GmbH.
2 1 Introduction of Polymer Nanocomposites
0.1 nm 5 nm 100 nm 10 000 nm 1 000 000 nm
0.5 nm 10 nm 1000 nm 100 000 nm 10 000 000 nm
. Quantum confinement
. Quantum tunneling
. Electromagnetic behavior
. Quantization of energy
. Molecular motion
. Large surface to volume ratio Governed by physical laws, gravitational forces,
and macromechanics
Increased
. Chemical reactivity . Light scattering
. Interfacial area . Tunneling effects
. Catalysis . Strain forces
. Adhesion forces . Purity
. Adsorption . Supramagnetic effects
. Light scattering . Conductivity
Figure 1.1 Nanomaterials peculiarities of size scale.
and they have high reactivity that can even be used as catalyst at low temperature
[5]. Since most of the properties of nanomaterials depend on their size, shape,
and surface structure, their ultrafine size always tends nanomaterials to aggregate
into bulk materials, especially without proper stabilization in their formation and
application [6]. This is because the agglomeration process makes the high surface
energy and activity of nanomaterials decrease to a more stable state. Therefore, in
order to preserve the properties of nanomaterials, it is necessary to distribute them
uniformly in matrices to prevent from aggregating into bulk materials [7].
Polymer nanocomposites (PNCs) are the mixture of polymers and nanomaterials,
having at least one-dimensional structure and one component material in the
nanometer regime of less than 100 nm. Combining nanomaterials into the polymer
matrix not only makes it possible to produce a new class of properties provided
by uniformly dispersed nanomaterials, but also greatly improves most of expected
properties of the original polymer, such as mechanical properties, heat resistance,
biodegradability, and so on [8]. As early as 1970, the term “nanocomposites” was
first proposed by Theng [9], and PNCs began to develop in commercial research
institutions and academic laboratories in the late 1980s [10, 11]. Over the past
decade, PNCs have made great progress in various fields, which is reflected by
the exponential growth of publications from their inception (Figure 1.2). The
existence of nanomaterials in polymer matrix changes the surface chemical and
physicochemical properties of PNCs, where the geometry, surface chemistry,
aspect ratio, and size of nanomaterials are the key parameters to regulate these
performances. Therefore, PNCs are a new class of materials with unique properties,
which are far superior to traditional doped and composite polymer systems. The
large interface interaction between nanomaterials and polymer matrix surfaces and
the difference of nanoscale fundamentally distinguish PNCs from the traditional
system. The development of nanomaterials and polymer science and technology
1.2 The Advantage of Nanocomposites 3
20 000
Nanomaterial
Nanocomposite
16 000 Polymer nanocomposite
Number of publications
12 000
8000
4000
0
1990 1995 2000 2005 2010 2015 2020
Year
Figure 1.2 Number of publications per year on “nanomaterials,” “nanocomposites,” and

“polymer nanocomposites,” according to SciFinder Scholar on 30 April 2020.
has promoted many applications of PNCs, which cover almost all fields of polymer
material application fields, such as microelectronics, magnetic electronics, biologi-
cal materials, sensor, energy storage, and so on [12]. Therefore, the chapters include
unique perspectives of different experts with their knowledge and understanding of
PNCs in this book.
1.2 The Advantage of Nanocomposites
Since the fillers of nanocomposites are nanoscale, the performances of nanocom-

posites can be improved by the advantages of the reduction of filler size and the
increased surface area. In terms of size, the filler is 3 orders of magnitude smaller
than the traditional substitute. In addition, the quantum confinement effects caused
by the nanomaterials will lead to new physical phenomena, which can be applied
in electrical and optical research. Many of these properties are related to the size
of the polymer chain, and the polymer chain close to the fillers is affected by the
interaction between the packing surface and the polymer matrix, which is differ-
ent from the polymer chain far away from the interface. The size of polymer chain
can be reflected the radius of gyration Rg , and the thickness of the interface regions
(t) around the particle is independent of the particle size. Therefore, the volume of
interface material (V interface ) relative to the volume of particle (V particle ) will increase
with the decrease of particle size.
Figure 1.3 shows the functional relationship between the V interface /V particle varies
and the aspect ratio of particles [13]. The aspect ratio reflects the shape of the
10 000
Plates Spheres Rods

1000
2r
2r
100
l
10 Rod, 2r < l
Vinterface/Vparticle
δ = 10
Sphere, r Aspect ratio = 1/2r > 1
Nanoparticles
Aspect ratio = 1 δ = t/r
1 δ = t/r
δ=1
0.1 2r
Plate, 2r > h
δ = 0.1
h Aspect ratio = 1/2r < 1
δ = 2t/h
0.01
δ = 0.01
Macroparticles
0.001
0.00 0.01 0.1 1 10 100 1000
Aspect ratio (as defined in figure)
Figure 1.3 The graph on the left shows the function relationship between the ratio of
interfacial volume to the particle volume (V interface /V particle ) and the particle aspect ratio.
The red shell represents the interface of particle, where the blue nucleus represents the
particle. The graph on the right defines the particle aspect ratio and the ratio of the
interfacial thickness to the particle size (𝛿) with different shapes (r is radius, I is length, h is
height). The interface thickness (t) is considered to be independent of particle size. When
the particle size is reduced to less than 100 nm, the physical properties can be controlled
by the volume of the interface around the particle, which is especially obvious for the
sphere and rod. Source: Winey and Vaia [13].
particles, which can be divided to plate (aspect ratio <1), sphere (aspect ratio = 1),
and rod (aspect ratio >1). 𝛿 represents the size of the filler, that is, the ratio of the
interface thickness t to the minimum dimension size of the particle. For spherical
and rod-shaped particles, 𝛿 is equal to the t/r, but 𝛿 is 2t/h in plate-shaped particles.
When the particle is microscale, 𝛿 is approximately equal to 0.01, and the particle
volume exceeds the volume of the interface region in all shapes. As the particle
size decreases, V interface /V particle values gradually increases. When 𝛿 goes above
one, V interface is going to exceed V particle . When the particles reach the nanoscale
(𝛿 = 10), the interface volume is more than 10 times that of the particle. Moreover,
particles with different shapes have different V interface /V particle in the same 𝛿. The
three-dimension sphere has the highest value, followed by the two-dimensional rod
and the one-dimensional plate. With the decrease of particle size, the gap becomes
more obvious, and even the V interface /V particle of spherical particles is 2 orders of
magnitude larger than that of plate-shaped particles. Therefore, the addition of
nanoscale fillers has a great impact on the performance of polymer in PNCs. Even
if the volume fraction of fillers is very small, the resulting interface region volume
will be very large.
As the interaction between polymer and particle is strengthened in PNCs, the
interparticle interface and coordination will be reflected in the macroscopic prop-
erties. Due to the nanoscale of particles, the secondary forming constituents have a
very high aspect ratio of over 100. When the volume fraction is 1–5%, these fillers
1.3 Classification of Nanoscale Fillers 5
can reach the percolation thresholds, which refer to the critical value of the volume
fraction of the packed particles that can mutate a certain physical property of the
composite material system. Therefore, the mechanical and transport performances
of PNCs can be greatly improved under the condition of low load nanoparticles.
Especially for the conductive particles, when the volume fraction of these parti-
cles increases to a certain critical value in polymer, conductivity of the polymer
suddenly increases sharply from insulator to conductor, and the change range is up
to 10 orders of magnitude.
1.3 Classification of Nanoscale Fillers
So far, various types of nanomaterials have been found to be able to form PNCs
with polymers. According to different applications, nanoparticles with correspond-
ing properties can be selected into the polymer system to achieve the expected
performance. In general, these nanofillers suitable for PNC applications can be
mainly divided into one-, two-, and three-dimensional materials according to their
different dimensions (Table 1.1).
1.3.1 One-Dimensional Nanofillers

One-dimensional nanofillers are plate-like materials with one-dimensional dimen-
sions less than 100 nm, which are usually a few nanometers thick and relatively
long sheets [14]. Most one-dimensional nanofillers have unique morphology
Table 1.1 Overview of nanomaterials classified by their nanoscale dimensions.
Plate Rod Sphere
L
D D1
D1
L L
D2
D3
• Montmorillonite clays • Carbon nanofibers (CNFs) • Nano-silica (n-silica)

(MMT)
• Nanographene platelets • Carbon nanotubes (CNTs) • Nano-alumina (n-Al2 O3 )
(NGPs)
• Layered double • Halloysite nanotubes • Nano-silver (n-Ag)
hydroxide (LDHs) (HNTs)
• Nickel nanostrands (NiNs) • Nano-titanium dioxide
(n-TiO2 )
• Aluminum oxide nanofibers • Nano-silicon carbide (n-SiC)
(Nafen)
• Nano-zinc oxide (n-ZnO)
• POSS
characteristics, such as nanoplate [15], nano-disk [16], nano-wall [17–23], etc.,

which play an important role in functional nano-devices [24, 25]. Recently, the
widely studied materials are montmorillonite clays (MMT) [26], nanographene
platelets (NGPs) [27, 28], ZnO nanosheets [29–31], Fe3 O4 nanosheets [30], and
so on, which have excellent electrical, optical, and magnetic properties [32], and
are widely used in the fields of micro–nano electronics, biosensors, and chemical
engineering [33]. The one-dimensional nanofillers are common nanomaterials in
electronic and thermal devices due to their shape characteristics.
1.3.2 Two-Dimensional Nanofillers

Two-dimensional fillers are the materials with two dimensions less than 100 nm,
and they are mostly in the form of rods [14]. The typical two-dimensional nano-
materials are carbon nanofibers (CNFs), carbon nanotubes (CNTs), halloysite
nanotubes (HNTs), nickel nanostrands (NiNS ), and aluminum oxide nanofibers
(Nafen). In addition, the most common two-dimensional nanofillers in PNCs
are nanotubes [34], plant fibers [35–39], nanowires [40], carbon fibers [41–44],
oxides [45–55], graphene [56, 57], molybdenum disulfide (MoS2 ) [58], and hexagon
boron nitride (h-BN) [59]. Compared with one- and three-dimensional fillers,
two-dimensional fillers have better flame retardancy and striped characteristic,
resulting in wide applications in the fields of catalysis, electronics, optics, sensing,
and energy [3, 26, 60–62].
1.3.3 Three-Dimensional Nanofillers

Three-dimensional nanofillers are nanomaterials with three dimensions on the
nanometer scale, so they are mostly spherical or cube-shaped [63], which is
also commonly referred to zero-dimensional particles. The most common three-
dimensional fillers are polyhedral oligomeric silsesquioxane (POSS), nanosilicon,
nanometal particles, nanometal oxides, and quantum dots (QDs) [33, 64]. Among
them, metals and metal oxide nanoparticles have the advantages of high stability,
catalytic activity, and easy preparation, and they are often used in the fields of
catalysis [65], purification [66–69], coatings [70–74], and biological fields [75, 76],
together with various polymers. One-, two-, and three-dimensional nanofillers
all have various special properties, and will ultimately promote the remarkable
performance of PNCs by loading in compatible polymers.
1.4 The Properties of Polymer Nanocomposites
In PNCs, many properties of the original polymer can be greatly improved, as well as
new properties resulting from the addition of nanoparticles. As shown in Figure 1.4,
the main properties of PNCs are listed, covering physical, chemical, and biologi-
cal areas. In general, the improvement level of properties is determined by the size,
Optical
activity
Lightweight Conductivity
Thermal
Toughness
stability
Polymer
nanocomposite
Catalytic Mechanical
activity strength
Biological Sensing
activity activity
Figure 1.4 Significant properties of polymer nanocomposites.
loading capacity, aspect ratio, dispersion uniformity, and interface interactions of the
nanofillers with polymer matrix [4].
For example, most polymers don’t possess conductivity except some conducting
polymers, which is due to the covalent bonding of polymers and the lack of electron
channels or ion migration. Interestingly, new PNCs formed by adding conductive
nanofillers to insulating polymers exhibit many electrical properties. As early as
1994, Ajayan et al. used CNTs as reinforcement materials to prepare PNCs [77].
Since then, there have been a lot of researches on using CNTs as fillers to improve
the electrical properties of PNCs. Only a small volume fraction of such fillers is
needed to improve the electrical properties of polymers by several orders of mag-
nitude effectively [78].
1.5 Synthesis of Polymer Nanocomposites

In the synthesis of PNCs, it is necessary to uniformly distribute the fillers into matrix
in order to realize the functions of fillers. However, due to the fact that the fillers
are nanoscale, the uniform dispersion is much different from that of the microscale
fillers, which is mainly manifested in the following aspects. First, if the filling
operation is carried out according to the volume fraction, much more nanometer
fillers than the microfillers are required at the same volume fraction. Therefore,
the nanoparticles in matrix are very crowded with greater van der Waals and elec-
trostatic interactions between the particles, making it difficult to distribute evenly.
Second, the anisotropic nanofillers have a very high aspect ratio, which makes them
Table 1.2 Summary of common methods for synthesis of polymer nanocomposites.
Technique Suitable filler Suitable matrix Solvent Controlling factors
Ultrasonication- All types Liquid or viscous Required Sonication

assisted monomers or power and time
solution mixing oligomers of
thermosets
Shear mixing Nanosheets Liquid or viscous Required Shapes of the
monomers or rotor blades,
oligomers of rotating speed
thermosets and time
Three roll Nanosheets Liquid or viscous Not Speed of roller,
milling and nanotubes monomers or required gap between
oligomers of adjacent roller
thermosets
Ball milling All types Liquid or solid Not Time of milling,
thermoplastics and required ball size,
thermosets rotating speed,
ball/nanofiller
ratio
Double-screw All types Solid Not Processing
extrusion thermoplastics required temperature,
screw
configuration,
rotation speed
In situ synthesis All types Liquid or viscous Required Chemical
monomers or reaction
oligomers of conditions,
thermosets temperature,
condensation
rate
more prone to agglomerate. For example, monolayer graphene has aspect ratio of
about 104 , so they tend to reduce their surface energy by π–π stacking. Third, a
large amount of nanofillers with huge surface area is loaded in the polymer matrix,
which will produce a large interface area and change the overall performances
of the PNC. Therefore, the decisive step in the synthesis of PNCs is the uniform
dispersion of nanofillers in polymer matrix. As shown in Table 1.2, the common
methods to disperse nanofillers and prevent the aggregation of nanoparticles by
using external energy are summarized.
1.5.1 Ultrasonication-assisted Solution Mixing

The most widely used approach to produce PNCs is ultrasonication-assisted solution
mixing [79–83]. In this method, the nanofillers and polymer are initially dissolved
in a solution. Then the nanofillers are evenly distributed in the matrix in assistant
of the ultrasound. Afterwards, the PNCs are obtained by evaporation of the solvent.
The nanoparticles are separated from the agglomeration state to the smaller units
by the ultrasonic energy, which is higher than the energy of interaction between
the nanomaterials in the aggregates. With the increase of ultrasonic time, the aggre-
gates of nanofillers are broken down into smaller ones, and even become individual
nanoparticles independent of other nanoparticles in the polymer. In addition, this
process often occurs at a high temperature, which can initiate in situ polymerization
of reactive monomers or their soluble prepolymers with nanomaterials to enhance
interfacial interactions [84].
Due to the simple operation and stable performance, the ultrasonic-assisted
solution mixing method has been widely used in the researches of new nanocom-
posites. However, due to the poor effect of ultrasound in high viscosity solution,
most of the polymers need to be dissolved in a high boiling point solvent and
maintain a low concentration, which will affect the process of solvent removal and
ultimately reduce the quality of the nanocomposites. Therefore, when using this
method, it is important to pay attention to the choice of solvent.
1.5.2 Shear Mixing

Compared with the ultrasonic-assisted method, shear mixing is a much more
common and simple method, which only requires the stirring process and has the
potential for industrial mass production [85]. In the process of stirring, the shear
force generated by stirrer rotating is used to separate the aggregates of nanofillers.
Due to the low strength of the shear force, the nanoparticles will be separated
under stirring and then aggregated again, so it is generally necessary to increase the
speed of the agitator to complete the separation. This method generally does not
destroy the structure of nanofillers; therefore it is suitable not only for separating
loosely bound nanoaggregates, but also for stripping off some layered nanosheets.
In addition, this method needs to be carried out in low viscosity solvent just like
ultrasonic assisted method.
1.5.3 Three Roll Milling

Three roller milling is a method of dispersing nanofillers by the shearing force
between rolls in high viscosity matrix, such as ink, paste material, coating, etc. The
machine of three roll milling is composed of three cylindrical rollers with different
rotating speeds, and the adjacent rollers rotate in the opposite direction. The particle
size distribution and uniformity of the packing can be well controlled as the speeds
of the rollers and the gap between them are adjustable. In addition, the shearing
force generated between the rollers is higher than that generated by stirring, so
the method can be applied to high viscosity materials, and carried out under the
condition of little or no solvent. Therefore, this method is often used to disperse
some anisotropic nanofillers, such as CNTs [86–89], graphene nanosheets [90–92],
nanoclays [93–95], and so on.
However, it should be noted that the distance between adjacent rollers should be at
least 1 μm, so the dispersion effect of nanospheres with three-dimensional direction
less than 100 nm will not be good. The aggregates of nanospheres can only be turned
into smaller units, not broken into individual particle. On the other hand, the rota-
tion of the roller requires the addition of viscous materials, and nanofillers can only
be dispersed in the thermosetting matrix but not in the thermoplastic matrix.
1.5.4 Ball Milling

Ball milling is widely used in metallurgy and mineral processing industry [96]. The
principle of ball milling is to grind and mix powders in a closed space by using
the huge shear force and compression force produced by hard ball collision. In the
synthesis of PNCs, this method can disperse CNTs [97], graphene nanoparticles
[98–101], silica nanoparticles [102], and BNs [103, 104] into thermoplastic and
thermosetting polymers. The high shear force produced by ball milling can peel
off some two-dimensional nanostructures, such as graphene, MoS2 , and BNs, but
may not separate the interlayer structure connected by ionic bonding [105–110].
In addition, ball milling is not only suitable for solvent-free conditions but also
solvent-free conditions, so nanofillers can be directly dispersed in some solid
thermoplastic matrix, such as polyethylene (PE) [101, 111], polyphenylene sulfide
[104, 112], and polymethyl methacrylate (PMMA) [102].
1.5.5 Double-screw Extrusion

Double-screw extrusion disperses nanofillers in thermoplastic matrix by huge
shear force generated by high speed rotation of double-screw at high temperature
[113, 114]. This method has been widely used in industry due to the advantages of
solvent-free and environment-friendly technology. With this method, the fillers can
be dispersed into the polymer in a high content way to achieve the well-controlled
performance, and applied to different sizes of nanoparticles, such as graphene
sheets [115], CNTs [116], and silicon dioxide [117]. This method needs higher
temperature, which is helpful to reduce the viscosity of polymer and load more
nanofillers, but also has the risk of decomposing polymers and nanofillers. The
reason is owing to the existence of low thermal stability functional groups in the
materials. When the temperature is too high, the fracture will occur, resulting in
the deterioration of the performance of PNCs [118]. Moreover, the gap between the
screws is too large to keep some aggregates of nanofillers evenly, which will not
achieve the uniform monodispersing of nanofillers. So, it is necessary to combine
other technologies to further improve the performance [119, 120].
1.5.6 In Situ Synthesis

In addition to the aforementioned methods of dispersing prepared nanofillers into
polymers, another important synthesis strategy is in situ synthesis, which directly
generates nanoparticles in polymers through molecular precursors [121]. This
method can be divided into chemical and physical in situ synthesis [122]. Chemical
in situ synthesis is used to synthesize nanoscale fillers by chemical reaction, such
References 11
as the hydrothermal method and sol–gel method [123, 124]. The physical in situ
synthesis is transforming the precursor of gas phase into inorganic nanoparticles
through plasma action, and then condensing the organic compounds on the surface
of inorganic particles to cover the polymer shell to form PNCs [125].
1.6 Conclusions and Future Outlook

In this chapter, the basic principles, properties, and synthesis methods of PNCs are
clearly described. The composite material has unique structure and performance,
and has a wide range of applications in many fields. The particle size, orientation,
shape, dispersion, and volume dispersion of nanofillers affect the properties of
PNCs. Most of the physical, chemical, and mechanical properties of PNCs depend
on the interface interaction between the filler and the matrix. Therefore, the uni-
form dispersion of nanofillers is the most important consideration in the synthesis
of PNCs. PNCs have recently become part of modern technology, but these areas
are still in the early stage of development. With more and more scientists and
engineers contributing to the understanding of PNCs, these functional materials
will be applied in more and more fields.
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21
Fabrication of Conductive Polymer Composites and Their

Applications in Sensors
Jiefeng Gao
Yangzhou University, School of Chemistry and Chemical Engineering, No 180, Road Siwangting, Yangzhou,
Jiangsu 225002, China
2.1 Introduction
Compared with traditional conductive materials like metals, conductive polymers

(CPs) exhibit excellent flexibility, light weight, low cost, and easy processing
characteristics. Therefore, CPs have become the research hotspot in recent decade
and been widely used in many fields such as electromagnetic interference (EMI)
shielding, sensors, and wearable electronics [1–3]. Generally, CPs can be divided
into two categories: (i) structural (intrinsic) structural conductive polymers (SCPs)
and (ii) conductive polymers composites (CPCs).
SCPs refer to a material possessing inherent conductivity provided by the
structure carrier. The SCPs were firstly discovered in the 1970s, which aroused
the attention of researchers on the chemical structure and the electrical properties
of polymers [4, 5]. The common types of SCPs possessing conjugated bonds
are polyacetylene, polypyrrole (PPy), polyaniline (PANI), polyphenylacetylene
(PPA), and their derivatives. However, the value of electrical conductivity for the
conjugated polymer materials is relatively small, usually ranging from 10−10 to
10−5 S cm−1 . The electrical conductivity of polymer materials can be enhanced
by 104 S cm−1 by doping various molecules like salt ions, hyaluronic acid, and
peptides [6, 7]. The doped SCPs show both electrical conducting property from
metallic material and many merits like flexibility, lightweight, etc., from polymer
material. Therefore, The SCPs have demonstrated their potential applications in
flexible electronics, sensors, and EMI shielding [8–10]. However, the SCPs have
their inherent deficiencies including poor solubility, mechanical properties, and
high cost. Usually, further modification or compounding with other polymers is
needed to improve their overall performance [11].
CPCs refer to one kind of electrically conductive polymer composite materials
fabricated by incorporating the conductive fillers [carbon black (CB), carbon
nanotubes (CNTs), graphene, etc.] into insulating polymer matrix [12–14]. The
electrical conductivity of CPCs is highly related with the percolated conductive
Polymer Nanocomposite Materials: Applications in Integrated Electronic Devices, First Edition.
Edited by Ye Zhou and Guanglong Ding.
© 2021 WILEY-VCH GmbH. Published 2021 by WILEY-VCH GmbH.
22 2 Fabrication of Conductive Polymer Composites and Their Applications in Sensors
network constructed by different conductive nanofillers. It is believed that most of

the resistance comes from tunneling between adjacent conductive fillers dispersed
in polymer matrix [15]. CPCs based on non-conductive polymer elastomers and
conductive fillers have caused wide concern of both academic and industrial group
and become a hot topic of polymer composites due to its easy preparation, control-
lable electrical property, excellent flexibility, and stretchability. In this chapter, we
systematically introduce the development and prospect of CPCs through several
parts including the fabrication method of CPCs, morphology, and microstructure of
CPCs and their application as sensors.
2.2 Fabrication Methods for CPCs

As known, conductive fillers, especially nano-sized conductive particles, are easy
to aggregate in the polymer due to their high-aspect-ratio, resulting in uneven
distribution, which may deteriorate the comprehensive performance of CPCs [16].
Therefore, surface modification of nanofillers and special processing technique
are required to enhance the dispersion of conductive nanofillers in the polymer,
which mainly includes the following methods: (i) The physical blending [17].
The conductive particles are uniformly dispersed into the polymer melt matrix or
polymer solution under the ultra-strong external field forces (shear, tensile, etc.).
(ii) In situ polymerization [18]. The conductive particles were firstly dispersed in
the organic solvent containing the polymer monomer. After the polymerization
reaction, the previously evenly dispersed conductive particles were anchored in the
polymer matrix in situ. (iii) Chemical modification of conductive filler [19]. After
the chemical reaction, the surface of conductive particles is grafted with functional
groups such as hydroxyl group, carboxyl group, amino group, etc. These groups
have good interactions with the polymer, such as covalent bond and hydrogen
bond, which can effectively avoid the nanofillers aggregation and hence improve
their dispersion in the polymer matrix. (iv) Introduction of surfactant [20]. The
surfactant will wrap around the conductive particles, increasing their compatibility
in polymer solution or melt, thus improving the dispersion of the fillers.
For CPCs, the electrical conductivity is depended on the transportation of charge
carriers (current) along the conductive network constructed by conductive fillers in
the polymer matrix. Generally, a sudden increase of several orders of magnitude in
conductivity (transition from insulator to conductor) can be found as the concen-
tration of conducting phase reaches a critical value in the polymer matrix, which is
defined as the percolation threshold. Above this threshold, the concentration depen-
dence of the conductivity of the CPCs (σ) can be described by a scaling law
𝜎 = 𝜎0 [(𝜑 − 𝜑c )]t
where σ0 represents the intrinsic conductivity of the fillers, t represents the
electrical conductivity exponent, 𝜑 represents the volume fraction of conductive
particles, and 𝜑c represents the volume fraction at percolation transition [21]. In a
random conducting network, the exponent t only depends on the dimensionality
of the network [22], which is called universal percolation behavior. Theoretical

calculation suggests that t = 1–1.3 corresponds to two-dimensional networks, while
t = 2.0 represents a three-dimensional network. The percolation threshold and
electrically conductivity are affected by many factors such as nanofiller dimension
and microstructure of the CPCs. For example, conductive nanofillers with a large
aspect ratio (CNTs, graphene nanosheet) could form well connected conductive
network, which is beneficial to a low percolation threshold in CPCs [23–25]. It is
also reported that nanofiller filled CPCs exhibit better electrical and mechanical
properties than CPCs incorporated with microsized fillers [26, 27]. Also, the
electrically conductive behavior of CPCs has strong relationship with the structure
of conductive network in the polymer matrix. The perfect interconnection between
conductive nanofillers and formation of 3D continuous pathway in the polymer
matrix are regarded as the key factor for construction of the conductive network
[28]. As a result, the morphology and distribution of nanofiller in the polymer
matrix play an important role determining the electrical conductivity of CPCs.
The fabrication process and parameters can greatly influence the morphology of
conductive network in polymer matrix and thus their electrical properties. There
are many methods for fabrication of CPCs have been reported, among which melt
blending, solution mixing and in situ polymerization are regarded as three major
methods. However, it still remains challenge to prepare high performance CPCs
with low percolation threshold while high conductivity [29, 30].
2.2.1 Melt Blending

Melt blending is processed by using kneading machine, molding machine, internal
mixer or double screw extruder, etc. [31, 32] to evenly mix the polymer matrix
and conductive fillers with the processing temperature above the melting point of
polymer. Thus, high temperature and high shear force are needed in melt blending
process to ensure the homogeneous dispersion of the conductive nanofiller in the
melting polymer matrix. During the melting blending, the nanofillers are forced
to disperse by the mechanical shear force and at the same time prevented from
re-aggregation by the viscous polymer matrix. After the masterbatch is obtained,
the final CPCs can be prepared by using different polymer processing technolo-
gies like spinning, hot press, and injection molding [33–35]. Melt blending is an
environmental-friendly process method and is feasible for large-scale industrial
production of the CPCs. Many recent studies have investigated the effect of fillers
introduction, dispersion state, and processing factors on the physical and electrical
properties of the CPCs prepared by the melt blending [36].
Kim [37] studied the influence of the CNTs concentration and dispersion state on
thermal, rheological, and mechanical properties of the polybutylene terephthalate
(PBT) nanocomposites. It was found that the storage and loss moduli of the com-
posite increased with the increase of the CNTs content. The interaction between
nanotube–nanotube and polymer–nanotube was regarded as the main cause for
the nonterminal behavior of the PBT nanocomposites. Besides, it can be found that
the heat distortion temperature and the thermal stability of the composite were
High shear forces

Graphene sheets
0 min 5 min 10 min 30 min 60 min PS chain
The formation of The π orbitals between PS and graphene reached

intercalated structure a specified distance, which was essential for the
formation of π–π stacking
π–π stacking
The formation of
π–π stacking
(a) (b)
10–1
10–2
10–3
Conductivity (S cm–1)
–4
10
10–5
10–6
–7
10
MWCNTs/PP
10–8 MWCNTs/PP-g-MA/PP
Acid treated MWCNTs/PP
–9 Acid treated MWCNTs
10
/PP-g-MA/PP
–10
10
0 2 4 6 8 10
50 μm 50 μm
MWCNTs loading (wt%)
(c) (d) (e)
Figure 2.1 (a) Photographs of the PS/graphene/toluene suspension prepared by

centrifuged at 8000 rpm for 30 minutes. (b) Schematic illustration for the formation of π–π
stacking between graphene and PS in melt blending process. Source: (a)–(b) Reproduced
with permission. [38] Copyright 2011, American Chemical Society. Microscopic morphology
of (c) 1% pristine MWCNTs/PP; (d) 1% pristine MWCNTs/PP-g-MA/PP. (e) Electrical
conductivity of various PP composites. Source: (c)–(e) Reproduced with permission. [39]
Copyright 2009, Elsevier Ltd.
substantially enhanced at a low CNTs concentration. During the melt blending,

the interaction between conductive fillers and polymer matrix greatly influences
the dispersion state of the filler. For example, due to the interaction of π–π stacking
between graphene and polystyrene (PS), the graphene could be easily dispersed
in PS matrix during the melt blending [38]. It can be seen in Figure 2.1a that the
suspension of PS/graphene without melting blending is transparent, suggesting
the absence of graphene in the suspension. However, the solubility of graphene in
toluene is greatly enhanced by prolong the melt blending time (5–60 minutes). This
dark-colored suspension keeps stable and homogeneous even after three months
or longer. The forming of π–π stacking between PS and graphene sheet in melt
blending process is schematically demonstrated in Figure 2.1b. In melt blending,
the PS chains were stretched by shear forces, forming some closely aligned aromatic
rings parallel to the graphene sheet. Therefore, the interaction between PS and
graphene was enhanced.
But mostly graphene and CNTs tend to aggregate in the polymer matrix
[polymethyl methacrylate (PMMA), polystyrene-block-poly(ethylene-co-butylene)-
block-polystyrene (SEBS), polypropylene (PP)] [40, 41]. To solve this problem, com-
patibilizers, chemical modification, or surfactants have often been used to improve
the interaction between the filler and the nonpolar polymer matrix [42–44]. Pan
et al. [39] studied the correlation between the dispersion state of multiwalled carbon
nanotubes (MWCNTs) in PP and electrical conductivity of its composite. They
adopted two methods to achieve the uniform dispersion of MWCNTs in PP matrix.
One is chemical modification of MWCNTs and another one is incorporation of a
master batch [polypropylene-grafted-maleic anhydride (PP-g-MA)] as a compatibi-

lizer followed by simple melt blending. Through comparing the optical microscopic
images of MWCNTs dispersion in PP in Figure 2.1c,d, we can get that the addition
of compatibilizer could largely enhance the uniform dispersion of MWCNTs in
PP matrix. Although the interfacial interaction between MWCNTs and PP could
enhance the dispersion of MWCNTs, it may cause the reduction of the electrical
conductivity of the composites (Figure 2.1e). Meanwhile, post-heat treatment can
improve the connection of MWCNTs in the composite, leading to the increase of
the electrical conductivity. Herein, a balance between uniform dispersion of CNTs
and construction of conductive networks is vital to the enhancement of electrical
conductivity for composites.
In short, melt blending is a simple method to fabricate CPCs. The electrical
properties of the CPCs are strongly dependent on the processing parameters like
mixing time, shear stress, and temperature as well as the surface modification and
introduction of compatibilizers.
2.2.2 Solution Blending

Although melt blending is a useful and feasible processing method for the large-scale
industrial production of the CPCs, the volume concentration of conductive parti-
cles is usually higher than 5% to obtain the composite with a high conductivity [45].
Such a high content of fillers would largely increase the melt viscosity [46, 47] and
thus make the processing less smooth and also increase the cost of the material fab-
rication. As an alternative, solution mixing method can tackle this issue, because the
nanofillers can be diluted in solvent to achieve relatively good dispersion [48, 49].
Solution mixing refers to a process for preparation of CPCs through mixing con-
ductive elements and polymer matrix in a solvent, followed by cooling and solvent
removal. Generally, this fabrication process contains three key steps: (i) preparation
of filler suspension in a suitable solvent, (ii) mixing filler suspension with polymer,
and (iii) precipitation or solvent evaporation of the mixed solution. While the major-
ity of conductive fillers, especially carbon-based fillers (e.g. CNTs, graphene, and
carbon black) show undesired dispersion in organic solvent due to their large spe-
cific surface area and high degree of graphitization thus low surface energy. Herein,
it is difficult to get a uniformly dispersed suspension of carbon-based fillers just by
mechanical stirring. Thus, powerful ultrasonication is often adopted to assist the
nanofiller dispersion in a polymer solution [50–52]. In many cases, chemical mod-
ification or the dispersant is required. For instance, acid (such as sulfuric and/or
nitric) is often used to modify the CNTs, and the graphitized structure of the CNTs
is partially damaged and oxygen containing functional groups can be grafted onto
the filler surface through covalent bonding [53, 54]. These functional groups can
effectively promote the nanofiller dispersion in the solution due to the interaction
(e.g. hydrogen bond) between fillers and solvent [16, 55].
Although covalent bonding is permanent and mechanically stable, chemical
reaction can also, to a large degree, damage the sp2 conformation of the carbon
atom, thereby disrupting the conjugation of the CNT wall. As a result, thermal,
0.20
(a) PEO/DNA/CNT = (b) PEO/DNA/CNT = (c) PEO/DNA/DWNT5%
80/15/5 70/25/5 0.15 PEO/DNA/DWNT1%
Strain (MPa)
PEO
0.10
0.05
PEO/DNA
0.00
2 μm 2 μm 0 5 10 15 20 25 30
Strain (%)
Figure 2.2 (a, b) The PEO/DNA nanofiber webs containing 5% DNA-dispersed DWNTs.
(c) Stress–strain curves for nanofiber webs of pure PEO, PEO/DNA, and PEO/DNA/DWNT.
Source: (a)–(c) Reproduced with permission. [57] Copyright 2013, American Chemical
Society.
electrical, and mechanical properties of the chemically modified CNTs decreased

dramatically, as compared with the pristine nanotubes [56]. To preserve the
integrity of CNT microstructure while at the same time improve CNT dispersity,
the noncovalent method to functionalize CNTs has received increasing attention,
because the surface structure of the nanofillers is preserved and thus the physical
and electrical properties of the nanofillers are preserved [19, 57]. Generally, the
surfactants with perfect solubility with the solvent are usually used in noncovalent
method, and these molecules are able to wrap CNTs, and the affinity between CNTs
and the solvent is thus enhanced [58].
In recent years, amphiphilic molecules like polymers are non-covalently attached
on the surface of nanofillers to overcome their aggregation [59, 60]. For example,
poly(vinylpyrrolidone) (PVP) and polystyrene sulfonate (PSS) were used to improve
the solubility of CNT in water and thus the CNT dispersion in polymer matrix
[e.g. polyvinyl alcohol (PVA) and polyethylene oxide (PEO)] [61, 62]. Lee et al. [63]
successfully dispersed MWCNTs with the concentration as high as 6.7 wt% in a
PEO solution by attaching the amphiphilic poly(styrenesulfonic acid-graft-aniline)
(PSS-g-ANI) to the surface of MWCNTs. The attachment of PSS-g-ANI has dramat-
ically enhanced the dispersion of MWCNTs and dispersion of 1%, 10%, 20%, 30%,
and 40% MWCNT/PEO solutions still remains homogeneous even after three days.
Deoxyribonucleic acid (DNA) as a representative biopolymer has now also been
considered as a powerful dispersing agent to disentangle strongly bundled CNTs
in an aqueous solution, resulting from DNA’s strong ability to wrap around the
sidewalls of CNTs [64, 65]. It was reported that CNTs were individually dispersed
in the DNA solution, and the uniform dispersion could be preserved in the poly-
mer/CNTs/solvent ternary solution [65]. In PEO nanofiber composite, under the
DNA assistant dispersion, double-walled carbon nanotubes (DCNTs) were finally
trapped along the axis of the PEO nanofiber and acted as mechanically reinforcing
filler and an electrical conductor [57]. The morphology of PEO nanofiber web con-
sisting of long, homogeneous nanofibers with a diameter of <100 nm was obtained
even with the content of 5% DNA-dispersed double-walled carbon nanotubes
(DWNTs) shown in Figure 2.2a,b. Also, the modulus and tensile strength were
largely improved by adding individually DNA dispersed DWNTs (Figure 2.2c).
2.3 Morphologies 27
2.2.3 In Situ Polymerization

In situ polymerization was firstly proposed by Imai et al. where polyimide (PI)/CB
composite was obtained by dispersing the CB into the polymer salt monomer [66].
In fact, this is a unique solution based processing technology for preparing the
CPCs, and chemical reaction is usually involved during the polymerization [67, 68].
The efficient polymer-chain graft onto the filler surface could form a perfect
interface interaction between the filler and polymer matrices, which also improves
the homogeneous dispersion of the fillers in the polymer matrix and influences the
crystallization of polymer chains to some extent [69–71]. As a result, CPCs with a
high weight content of the nanofillers can be obtained by this method [69, 72].
Zhu and coworkers prepared reduced graphene oxide (r-GO)/PI composites with
different loadings of GO by in situ polymerization and the maximum content of
GO can reach 30 wt%. During polymerization, a relatively high temperature was set
to reduce GO into conductive r-GO in the polymer matrix. The electrical property
of the obtained r-GO/PI was greatly enhanced, because of the conductive network
formed by r-GO in the composite film and the conductivity could reach as high as
1.1 × 101 S m−1 , which is about 1014 times that of pure PI film [73]. The mechanical
properties of GO/PMMA composites fabricated by in situ polymerization were
also tested by Potts et al. [74]. It is found that the elastic modulus and tensile
strength of the GO/PMMA composites could be improved even with 1 wt% loading
of fillers.
2.3 Morphologies
Different fabrication techniques may lead to different morphologies of conductive

networks in CPCs, which significantly influence the electrical properties of these
composites [30]. Various morphologies including uniform dispersion of nanofiller in
the polymer matrix, segregated structure, and selective decoration of the nanofiller
on the skeleton of porous polymer materials are reported [75].
2.3.1 Random Dispersion of Nanofiller in the Polymer Matrix

The most straightforward and popular strategy to fabricate CPCs is the incorporation
of conductive fillers (e.g. graphene, CNTs) in the polymer matrix by either melting
or solution method. Naturally, the nanofillers are randomly located in the polymer
matrix, and some of them may be squeezed out to polymer surface in particular
at a high filler concentration [76]. The nanofillers can be uniformly distributed in
the fibers, film, and three-dimensional polymer materials, depending on the pro-
cessing technology used. Wet-spinning [77, 78] and electrospinning [75, 79] are two
most common means to prepare one dimensional CPCs. Yu et al. [80] have success-
fully prepared conductive poly(styrenebutadiene-styrene) (SBS)/CNT fiber through
wet-spinning the mixed solution of CNT and SBS elastomer. The schematic diagram
of the fabrication procedure of SBS/CNT and the pictures of flexible SBS composite
(a)
CNT, ultrasonication SBS, magnetic stirring

20 °C, 4 h CNT/THF Room temperature, 24 h Wet-spinning
THF 20 ml Suspension solution
Winding device
SBS/CNT fiber
Wet-spinning solution Ethanol coagulation bath
Pure SBS SBS/0.5CNT SBS/0.75CNT SBS/1CNT
(b) SBS/0.5CNT (c) SBS/0.75CNT (d)SBS/0.1CNT
200 nm 200 nm 200 nm
(e) 100 (f) (g) 100

10–1
σ (S m−1 g−1 cm−3)
PU-PEDOT:PSS(top) 80
Transmittance (%)
10–2 0.0
y = 1.1421x + 2.1531
SWCNT
60
R2 = 0.99696
10–3 –0.4
log (σ)
–0.8
10–4 –1.2
Experimental date
20
10–5 –1.6
Fit curve
–3.0 –2.8 –2.6 –2.4 –2.2 –2.0 PU-PEDOT:PSS(bottom)
log (p–p)
10–6 PDMS 0
400 500 600 700 800
0.0 0.2 0.4 0.6 0.8 1.0
CNT content (wt. %) Wavelength (nm)
Figure 2.3 (a) Schematic diagram illustrating the preparation procedure for SBS/CNT
fibers (SCFs) and photograph of SCFs with the various content of CNT. (b–d) The
cross-sectional morphologies of SBS/CNT fibers containing different content of CNT.
(e) The specific conductivities of SFCs as a function of different loading content of CNT.
Source: (a)–(e) Reproduced with permission. [80] Copyright 2018, Elsevier Ltd. (f) Schematic
illustration of the PU-PEDOT:PSS/SWCNT/PU-PEDOT:PSS with sandwiched structure on a
polydimethylsiloxane (PDMS) substrate. (g) Transmittance of the integrated composite in
the visible wavelength range from 350 to 700 nm. Source: (f)–(g) Reproduced with
permission. [81] Copyright 2015, American Chemical Society.
with different content of CNTs are shown in Figure 2.3a. Figure 2.3b–d show the
SEM micrographs of fracture SBS/CNT fibers with a content of 0.5%, 0.75%, and 1%,
respectively. Uniformly dispersed CNTs in SBS matrix can be observed even at a CNT
content of 1%. Also, the conductivity of the obtained 1-D conductive fiber composite
improves with the increase of CNT content (Figure 2.3e).
Thin film-like CPCs can be fabricated by facile casting or template mold-
ing [82, 83] or polymer encapsulation [81, 84–86]. A stretchable, transpar-
ent, patchable nanohybrid conductive polymer film was reported by Roh
et al. [81]. The CNTs were encapsulated in the interlayer of polyurethane
(PU)-poly(3,4-ethylenedioxythiophene) polystyrenesulfonate (PEDOT:PSS) form-
ing a sandwich-like structure, which is schematically illustrated in Figure 2.3f,
2.3 Morphologies 29
where the CNTs functioned like a bridge that connects the conductive PEDOT to
the PEDOT phases. The obtained sandwich-like composite with 5 mg ml−1 SWCNT
dispersion is optical transparent and shows the optical transmittance of 62% in the
visible range (Figure 2.3g).
In terms of three-dimensional composite, nanofillers are often distributed in a
foam composite that is usually obtained by freezing drying method [87, 88]. For
example, Huang et al. [87] fabricated a novel aligned porous CNT/thermoplastic
polyurethane (TPU) foam composite by using a directional-freezing method. During
the freezing–drying process, the solvent of the mixture would form directional crys-
tal due to the low temperature and then the ice crystal of the solvent would be
sublimated, leaving aligned interconnected pores.
2.3.2 Selective Distribution of Nanofillers on the Interface

To reduce the content of conductive fillers in polymer matrix and at the same
time maintain a relatively high conductivity of the CPCs, researchers try to locate
conductive fillers on the interfaces of the polymer granule (i.e. segregated structure)
or on the skeleton (surface coating) of the porous materials. Also, when used as
sensors, the specially distributed conductive paths are easier to destruct upon
external stress compared with conventional CPCs with relatively strong and dense
conductive paths.
2.3.2.1 Segregated Structure

The study about construction of segregated structure was first reported in 1971 [89],
and to date much work have been done on this topic [15, 30, 90]. In fact, segregated
structure is a unique dispersion state of the conductive fillers in the polymer matrix,
at which conductive fillers are dispersed at the interfaces between polymer particles.
Mechanical blending and hot compression molding technique is usually applied to
fabricate CPCs with a segregated structure [91, 92]. Generally, conductive fillers such
as CNTs and graphene were adsorbed to the surface of polymer microspheres by
chemical or physical methods, and then the temperature and pressure of hot pressing
were controlled, guaranteeing that the conductive fillers were only distributed at the
interface between polymer microspheres instead of evenly dispersed in the whole
polymer matrix [15, 93, 94].
For example, Wu et al. [95] added amino-functionalized PS microspheres suspen-
sion into the GO solution. Graphene was tightly coated on the surface of PS micro-
spheres after a series process of flocculation, filtration, washing, and hydroiodic acid
reduction. The composite with a low percolation value of 0.15 vol% was obtained
after hot press of the graphene coated PS microsphere. Also, the conductivity of the
composite could reach as high as 1024.8 S m−1 when the volume content of graphene
is 4.8%, which is much higher than that of PS/graphene and PS/CNT composite
made by solvent blending.
An ultralow percolation threshold of 0.047 vol% was achieved by Cui and
Zhou [92]. In their work, the conductive PS/graphene and PS/MWCNTs com-
posites with segregated structures were obtained by hot press surface sulfonated
PS microspheres and protonated triethylenetetramine functionalized perylene
SO H
3
(a) SO H
3
SO H
3 Sulfonated PS layer (b) (c)
SO H SO H
3 3
Nanocarbons
SO H
SO H 3
3
SO H
3
Silfonated PS microsphere Dispersion mixing Hot-press
PS matrix
+
2 μm 2 μm
Nanocarbons Sulfonated PS/nanocarbons Conductive composite
(d) (e) (f) 100
0.0
𝜙c = 0.09 vol %
Conductivity (Sm–1)
10–3
Log conductivity (Sm–1)

–0.2
t = 0.37 ± 0.02
–0.4
10–6
–0.6
1000 nm
–0.8
10–9
–1.0
–1.2
10–12
–1.4
–3.0 –2.5 –2.0 –1.5 –1.0 –0.5 0.0 0.5
Log (𝜙–𝜙c)
10–15
100 μm 100 μm 0.0 0.2 0.4 0.6 0.8 1.0 1.2
CNT content (vol %)
Figure 2.4 (a) The fabrication process of PS–nanocarbon composite with interconnected
networks. Cross-sectional SEM images of PS composites with (b) 0.94 vol% graphene sheets
and (c) 0.94 vol% MWCNTs. Source: (a)–(c) Reproduced with permission. [92] Copyright 2017,
The Royal Society of Chemistry. Morphologies of double-segregated (d) CNT/PMMA/
UHMWPE (0.2/7.8/92.0 by volume) and (e) CNT/PMMA/UHMWPE (0.5/16.2/83.3 by volume)
composites. The inset transmission electron micrograph (TEM) image in (e) shows the state
of the segregated CNT conductive network in the CNT/PMMA layers. (f) The variation of
electrical conductivity for the double segregated CNT/PMMA/UHMWPE composites with
different CNT content. Source: (d)–(f) Reproduced with permission. [96] Copyright 2013,
The Royal Society of Chemistry.
bisimide (HTAPBI)-stabilized nanocarbon. The formation of conductive PS com-

posites with a segregated network is schematically demonstrated in Figure 2.4a.
The SEM micrographs of the fracture surface of PS composites containing 0.94 vol%
graphene sheets and 0.94 vol% MWCNTs are displayed in Figure 2.4b,c, respectively.
Due to the strong electrostatic attraction between the negatively charged PS and
positively charged nanocarbon, the interconnected conductive pathways could
be preserved regardless of a high hot press temperature, leading to an ultralow
percolation threshold.
Pang et al. reported CPCs with double-segregated structure [96, 97]. CNTs
wrapped around the small-sized PMMA particles to form the first layer of segre-
gated structure, and CNTs/PMMA were distributed at the interface of the large-sized
ultrahigh molecular weight polyethylene (UHMWPE) particles to construct a sec-
ond layer of segregated conductive network throughout the whole system. The
optical micrographs of CNT/PMMA/UHMWPE composite with 0.2 and 0.5 vol%
CNTs are shown in Figure 2.4d,e, respectively, showing perfect double-segregated
structure. Figure 2.4f shows the electrical conductivity of CNT/PMMA/UHMWPE
composites as a function of CNT content. The percolation value of the CPC was
calculated to be only 0.09 vol% [96].
Another kind of segregated structure can be constructed by infiltration of flexible
elastomers into conductive foams. Carbon based foams (e.g. graphene and CNTs)
and carbonized polymer foams are usually selected as the conductive skeleton and
polydimethylsiloxane (PDMS) ink was impregnated in the foam to prepare the CPCs
[98–100].
2.3 Morphologies 31
2.3.2.2 Surface Coating

To prepare CPCs with a low percolation, a high conductivity at a low filler content,
and meanwhile no evident fillers aggregation in polymer matrix, decoration of con-
ductive nanofillers on the skeleton (out surface) of the polymer material tends to be
an effective solution, which includes dip coating [101, 102], spray coating [103, 104],
and ultrasonication [105, 106]. Note that the polymer materials usually possess a
porous structure (e.g. fabric and foam), which facilitates the nanofillers penetration
into the interior of the material during the surface coating.
In dip coating, the polymer scaffold was immersed into the ink of conductive fillers
(graphene, CNTs, AgNWs) [102, 107, 108] or the precursor solution [109, 110] fol-
lowed by drying or in situ reduction and drying. Cui and coworkers [108] produced
highly conductive textiles with conductivity reaching 125 S cm−1 by immersing tex-
tile into single-walled carbon nanotube (SWNT) ink (Figure 2.5a). The color of the
textile becomes black after immersed in SWNT ink (Figure 2.5b), suggesting that
the SWNT has been successfully decorated on the surface of textile fibers. Also,
SWNT can be observed on the surface of textile from SEM image in Figure 2.5c.
The interaction of van der Waals forces and hydrogen bonding guarantees the tightly
binding of single walled CNTs to the cellulose. A conductive multifilament fiber with
conductive Ag shell and elastomer polymer core was reported by Lee et al. [111].
The multifilament elastomer fiber was first dipped in the AgCF3 COO solution to
adsorb Ag precursor through ion–dipole interaction. Then the Ag+ ions absorbed
in the fibers was in situ reduced by the reduction solution. The microstructure of
the core–shell structure can be observed in Figure 2.5d,e. The interfacial interactions
like electrostatic interaction [111], hydrophobic interaction, and hydrogen bonding
[108, 114] are considered to be the leading driving force for the successful decoration
of conductive nanofillers on the polymer substrate surface.
In addition to the aforementioned interfacial interaction, ultrasonication induced
nanofiller anchored onto the nanofiber surface or the skeleton of the foam is wildly
used to prepare conductive polymer sponge [106, 115] or nanofiber [116] composite.
Its working mechanism is as follows: under ultrasonication, a large number of cav-
itation bubbles will be generated in the solution, and these cavitation bubbles will
be blasted generating micro-jets [117], which will break up the nanofiller aggregates
in the solution, and at the same time, the dispersed nanofillers can rush to polymer
scaffold at high speed. The viscoelastic elastomer at the interface between fiber and
CNTs would be soften or even partially melt under the instantaneous high temper-
ature and high pressure. At this point, the well dispersed nanofillers under ultra-
sonication would be anchored in situ on the surface of elastomer surface. Gao et al.
[118] first reported this technique to prepare the CNTs decorated TPU nanofiber
composite. Recently, they [112] prepared multifunctional nanofiber composite by
dip coating one PDMS layer onto the CNTs/TPU surface. The fluffy CNTs forms
conductive shell on the fiber surface as shown in Figure 2.5f,g. The PDMS layer acts
not only as adhesion promoter enhancing the interfacial interaction but also as low
surface energy material endowing the CPCs surface with low surface energy. CPCs
with dual conductive networks are also reported by Gao and his coworkers by com-
bination of ultrasonication and dip-coating [113]. The acidified carbon nanotubes
2 cm 5 cm 100 nm
(a) (b) (c)
Ag-rich shell Composite
50 μm 20 μm 1 µm
(d) (e) (f)
200nm
1 µm 1 µm 1 µm
(g) (h) (i)
Figure 2.5 (a) Conductive textiles fabricated by dipping coating aqueous SWNT ink.
(b) Picture of obtained conductive textile. (c) SEM image showing SWNT coating on the
surface of fabric fibers. Source: (a)–(c) Reproduced with permission. [108] Copyright 2010,
American Chemical Society. (d) Cross-sectional SEM images of the electrically conductive
elastomer fiber composite. (e) Magnified SEM image of (d) showing the conductive Ag-rich
shell on the outer surface of elastomer fiber. Source: (d)–(e) Reproduced with permission.
[111] Copyright 2018, American Chemical Society. (f) Cross sectional SEM image and (g)
TEM image of the TPU/CNTs/PDMS nanofiber composite. SEM images of the nanofiber
composite at different strain during stretching, Source: (f)–(g) Reproduced with permission.
[112] Copyright 2019, Elsevier B.V. (h) 𝜀 = 10%, (i) 𝜀 = 70%. Source: (h)–(i) Reproduced with
permission. [113] Copyright 2019, Elsevier B.V.
(ACNTs) decorated nanofiber composite was immersed in Ag precursor solution,

and then AgNPs were generated after the precursor was reduced. PDMS was also
used to improve the interfacial adhesion between the AgNPs. The dual conductive
structures on the fiber surface can be observed in Figure 2.5h. The outer surface of
the CPC is surrounded by silver nanoparticles, and ACNTs in the interlayer could
be observed after stretching the fiber composite as shown in Figure 2.5i.
2.4 Application in Sensors

CPCs have been widely used for different sensors, due to its light weight, porta-
bility, flexibility, and low cost [90, 119]. The sensing mechanism of CPC sensors is
based on the resistance variation of CPCs when experiencing external stimulus like
mechanical deformation [120, 121], temperature variation [122, 123], and adsorp-
tion of vapors or organic solvent [124, 125]. The resistance of CPCs is affected by
the evolution of conductive network under external stimulus [5]. These transient
resistance change can be detected as a signal for sensing purpose.
2.4.1 Strain Sensor

As a device for detecting object deformation, CPC based strain sensors have been
widely used for health monitoring, electronic skin, wearable electronics, etc. For the
purpose of monitoring, the resistance (conductive networks) should response upon
external strain/stress [119]. Thus, CPCs should possess excellent resilience such that
the material could be elongated under external strain (destruction of conductive
networks) and recovered immediately after the removal of the stress (reconstruction
of conductive networks).
Conductive natural rubber/elastomer composites decorated with different con-
ductive nanofillers are explored as promising candidates of wearable strain sensors
[110, 126, 127]. The sensors show broad workable sensing range, high sensitivity,
and excellent recoverability. Among these materials, conductive fabric composite
strain sensors have shown promising applications in wearable electronics, thanks
to their breathability, skin affinity, and so on [128, 129]. For example, they can be
incorporated into clothing or gloves to detect human body motions [111, 114] and
detect the motions of human body as shown in Figure 2.6. Figure 2.6a–d demon-
strate that the fiber strain sensor could be used for human–machine interfaces by
simply incorporating the fiber composites onto a glove, demonstrating the potential
application in remote control of hand robot. Figure 2.6e–j show sensing performance
of the smart integrated glove in monitoring motions like head-forward, shoulder
imbalance, kyphosis, etc. In order to improve the environmental suitability of the
sensors, self-protective CPCs with superhydrophobicity have attracted great inter-
ests [128, 130] from the academia. This superhydrophobicity endows the sensor with
self-cleaning behavior and can prevent the water or even corrosive solution diffusion
into the materials, which can extend their applications in some harsh conditions.
To reveal the strain sensing mechanism, the evolution of conductive network of the
CPC under different strains is observed by using the SEM [126].
Hydrogel as a new type of conductive polymer composite demonstrating prefer-
able bio-compatibility, self-healing, and self-adhesiveness is an ideal material
for strain sensing usage [131, 132]. Zhang et al. [133] developed a MXene
(Ti3 C2 Tx )/PVA hydrogel sensor with outstanding sensing performance by mixing
MXene nanosheet with PVA hydrogel. The hydrogel composite shows outstanding
stretchability, self-healing property, and strong adhesiveness to skin, which can
adhere to human skin without the assistance of bonding materials to detect subtle
motions including facial expression, vocal signals, handwriting, and finger bending,
demonstrating high accuracy and sensitivity.
2.4.2 Piezoresistive Sensor

In recent years, CPC based pressure sensors as a branch of smart material, which
could respond to compressive deformation and transform mechanical forces into
Thumb
Index finger
Relative resistance (ΔR/R0)

Ring finger
(a) Middle finger

Relative resistance (ΔR/R0)
20
15
Ring finger
Ring finger + little finger
10
0
0 10 20 30 40 50 60 70 80 90 0 10 20 30 40 50
All finger
(b) Time (s) (c) Time (s) (d)
Head-forward Shoulder imbalence Kyphosis
ΔR/R0 (a.u.)
ΔR/R0 (a.u.)
ΔR/R0 (a.u.)
2
4
6
3
1 5
0 10 20 30 0 5 10 15 0 10 20 30
(e) Time (s) (f) Time (s) (g) Time (s)
35°
ΔR/R0 (a.u.)
ΔR/R0 (a.u.)
Little
25°
Ring
Middle 10° 15°
Index 0°
Thumb
0 4 8 12 14 0 20 40 60
Time (s) Time (s)
(h) (i) (j)
Figure 2.6 (a) Photograph showing the smart glove integrated with the fiber composites.
(b, c) Strain sensing behavior of the smart glove for (b) fingers bending and (c) a full
bending stimulation of each finger. (d) Photographs showing the hand robot operated by
the smart glove. Source: (a)–(d) Reproduced with permission. [111] Copyright 2018,
American Chemical Society. Relative resistance change of the sensor responding to various
postures: (e) head-forward, (f) shoulder imbalance, and (g) kyphosis, respectively. (h) Photos
showing a smart glove incorporated with fiber composite. Strain sensing behavior of the
smart glove for (i) different gestures of the five fingers and (j) different bending angels of
the wrist. Source: (e)–(j) Reproduced with permission. [114] Copyright 2019, The Royal
Society of Chemistry.
electrical signals, have been extensively developed [134]. To meet the demands
of different applications, innovated material structures and fabrication strategies
are developed to prepare flexible and wearable pressure sensors with excellent
sensing performance. CPCs containing an elastic matrix and conductive nanofillers
are the most popular candidates of the piezoresistive sensor [135]. Textiles with
fiber networks are often used as flexible scaffolds of piezoresistive sensors by
carbonization or coating conductive fillers onto the fiber surface [136, 137]. Li
et al. [137] fabricated flexible and electrically conductive carbon cotton (CC)/PDMS
composites by infiltrating PDMS glue into the CC scaffold. The CC/PDMS demon-
strates a sensitivity of 6.04 kPa−1 , a working pressure of 700 kPa and durability over
1000 cycles. CPCs with a porous structure (foam, aerogels) are another ideal active
materials of piezoresistive sensors because of their highly reversibility and hence
reusability after large-deformation cycles [138, 139]. Zhong and coworkers [140]
successfully fabricated lightweight MXene (Ti3 C2 ) aerogel with ultra-stable lamel-
lar structure by freeze drying the mixture of bacterial cellulose fiber and MXene
nanosheets. The carbon aerogel used for pressure sensor demonstrates ultrahigh
compressibility and superelasticity, a wide linear range and low detection limits.
To enhance the response intensity and low detection limit, CPCs with delicate
structures like fingerprint pattern [141, 142], microdome or micropillar array
[143, 144], hair of human skin [145], plant leaves [146, 147], hollow spheres [148],
etc. were studied. Park et al. [149] have reported flexible piezoresistive sensor by
building interlocked microdome arrays on the elastomer composite film. The flexible
film with regular microdome arrays can be observed by SEM as shown in Figure 2.7a.
The inset picture demonstrates its excellent flexibility. The schematic diagram (top)
and SEM image (bottom) of the fracture surface for the composite films are shown in
Figure 2.7b, and an interlocked structure can be observed. The operating principle
of the sensing device is also schematically illustrated in Figure 2.7c. Under the stress
of external pressure, the microdomes would deform and the contact area between
interlocked microdomes was increased, which in turn influenced the tunneling
resistance of the sensor. Figure 2.7d shows the pressure sensing performance
(relative electrical resistance (R/R0 )) of composite film with different structures. The
film with interlocked microdomes demonstrates a sharp decrease in R/R0 when the
applied pressure increases from 0 to 10 kPa, while the sensing signals for films with
single microdome arrays and planar structure are much weaker. Also, the sensing
curve (log–log plot) of R/R0 vs. pressure demonstrates a high linearity (Figure 2.7e),
indicating an exponential dependence of resistance on the applied pressure.
Bae et al. [144] prepared highly linear and sensitive graphene/PDMS composite
films with microdome structures. They found that pressure sensor made of hierar-
chical graphene/PDMS array with wrinkles on the surface of the microdome was
more sensitive to external stimuli than sensor made of smooth-dome graphene/
PDMS array. This novel type of pressure sensor exhibits a superb endurance of
10 000 cycles and a low detection limit of 1 Pa.
2.4.3 Gas Sensor

CPCs based gas sensors have also aroused tremendous attention for application
in detecting or quantifying organic vapors or liquids chemicals [150, 151]. The
electrical resistance of the CPC usually undergoes change when the sensor is
exposed to organic vapor or liquid. The sensing mechanism of the gas sensor can
be discussed on the basis of percolation theory. Upon exposure to vapor or liquid,
the interaction between polymer matrix and gas would cause polymer expansion,
resulting in the redistribution of the conductive nanofillers hence change of resis-
tivity. Once the sensor is removed from the vapor stimuli, the resistance of the CPC
recovers to its original value due to the desorption of vapor [152, 153]. Li et al. [154]
proved a schematic illustration of the conductive networks formed by different fillers
(a) (b)
Pressure
Tunnel
Contact current
Pressure
e–
(c)
101
R1 100
100
10–1 10–1
10–2 10–2 ~0.2 Pa

R/R0
R/R0
R1
Planar
10–3 Rc 10–3
Singlee microdomes ~59 kPa
10–4 Interlocked microdomes 10–4
R1
10–5 Rc 10–5
R1
10–6
0 5 10 15 20 25 30 10–1 100 101 102 103 104 105
Pressure (kPa) Pressure (Pa)
(d) (e)
Figure 2.7 (a) SEM image showing the surface morphology of the composite elastomers
(scale bar: 10 μm); Inset photograph shows the flexibility of the film composite.
(b) Schematic diagram (top) and SEM image (bottom) of the fracture surface for the
composite films (scale bar: 5 μm). (c) Schematic illustration demonstrating the operation
principle of the film composite. (d) The pressure sensing performance of composite film
with different structures. (e) Relative resistance (R/R0 ) as a function of applied pressure
(log–log plot) for the sensor with interlocked microdome arrays (8 wt% CNTs). Source:
(a)–(e) Reproduced with permission. [149] Copyright 2014, American Chemical Society.
in sensing process shown in Figure 2.8a–d. It can be observed that the dispersion
state of conductive nanoparticles (CB, CNTs) in poly(lactic acid) (PLA) matrix
(Figure 2.8a,c) are quite different from that of ramie fiber (RF)/PLA (Figure 2.8b,d),
resulting in different sensing mechanism. They found the addition of RF greatly
tailored the vapor sensing behaviors of CB/PLA and CNTs/PLA composite.
Many efforts have been paid to modify the sensitivity, selectivity, and recoverability
of vapor sensors. Gao et al. [116] reported a superhydrophobic PU@SEBS/carbon
nanofiber (CNF) composite vapor sensor to improve water proof and corrosion
resistance. The superhydrophobic membrane could be easily wetted by different
solvents, corresponding to a rapid response time. The sensor is also sensitive to
Immersion Drying
(a)
Immersion Drying
(b)
Immersion Drying
(c)
Immersion Drying
(d)
Figure 2.8 Schematic illustration of conductive networks formed by carbonaceous filler in

PLA during immersion-drying runs. (a–d) Illustrating the evolution of conductive networks
in CB/PLA, CB/RF/PLA, CNTs/PLA, and CNTs/RF/PLA, respectively (the red lines and circles
suggest the changes of conductive paths). Source: (a)–(d) Reproduced with permission.
[154] Copyright 2015, Elsevier B.V.
both polar and non-polar vapors. It is obvious that the PU@SEBS/CNF composites
show different sensing behavior to tetrahydrofuran (THF), toluene, and heptane as
shown in Figure 2.9a–c.
Usually, CPCs with disordered dispersion of conductive nanofillers show poor
sensing repeatability, because the swelled conductive network can’t perfectly recover
when the materials is taken out from the vapor in most cases. To solve this prob-
lem, CPCs with segregated structures have become alternatives [156, 157], because
organic vapors or liquids could more easily be permeated in the CPC by the capillary
effect generated from the interfaces of polymer matrix.
Sensor that could detect both humidity and chemical vapors with high sensitivity
and low detection limit is reported by Huang et al. [155]. The obtained conductive
ACNT/PU nanofiber membrane shows excellent superhydrophilicity and underwa-
ter superoleophobicity, and it is sensitive to both humidity and chemical vapors.
The membrane composite can be integrated into masks to detect human respira-
tion showing potential usage in monitoring biomarker gases from human breath
(Figure 2.9d–f).
Another random document with
no related content on Scribd:
— Oui, c’est bien moi, Gérard… c’est moi !… Claude, ma petite
cousine, ma chère fiancée, nous ne rêvons ni l’un ni l’autre… et j’en
ai la preuve ! Notre union était si bien voulue que le ciel a fait un
miracle pour nous rapprocher…
Claude ne demandait pas qu’on lui expliquât le miracle ; elle y
croyait de tout son cœur et cela suffisait à sa raison. Elle était un
peu étourdie de la soudaineté de son bonheur, mais elle était à
peine étonnée d’apprendre que le prince Charmant entrevu dans
son rêve se trouvât être Gérard de Chanteraine, ce fiancé que l’aïeul
lui avait toujours destiné et qui devait apparaître à l’heure dite.
— J’avais deviné… j’avais deviné… quelque chose m’avait dit
que c’était vous… répétait-elle comme en rêve.
Et ses yeux rayonnaient et ses lèvres souriaient, et toute son
âme était dans ce regard, dans ce sourire.
Ce fut seulement quand Pierre, assis près d’elle, lui eut montré le
petit coffre d’émail tout pareil au sien, la chaîne de Gérard, la clé
ciselée, qu’une curiosité lui vint de connaître les détails de la
merveilleuse odyssée à la suite de laquelle le colonel Fargeot se
retrouvait à ses genoux métamorphosé en duc de Chanteraine, ou
plutôt de savoir comment il avait pu se faire que Gérard de
Chanteraine, l’homme qu’elle aimait, qu’elle avait aimé tout de suite
et dès qu’il lui était apparu, lui fût apparu pour la première fois sous
le nom de Pierre Fargeot.
II
LA VENGEANCE D’ANTONIN FARGEOT
Pierre ou Gérard en avait long à dire. Il commença son récit en

parlant à la jeune fille de la mort d’Antonin Fargeot, des paroles que
le malheureux avait prononcées à l’heure suprême, des doutes et
des soupçons engendrés par cette confession incohérente… Puis il
entreprit l’histoire du passé telle qu’il la connaissait maintenant, telle
que tante Manon la lui avait racontée, lorsque après la découverte
du coffret d’émail, elle avait enfin développé et complété les vagues
révélations qu’il avait fallu auparavant arracher une à une à son
angoisse.
Comme l’officier s’étendait malgré lui sur le douloureux roman
d’Antonin Fargeot, comme il s’apitoyait sur les tristesses de cette vie
sacrifiée, Claude eut un petit mouvement de surprise et de révolte.
— Ce méchant homme vous a pris à nous ! objecta-t-elle.
Avec une grande douceur, une profonde tendresse, Pierre attira
Claude contre sa poitrine et la gardant ainsi étroitement enfermée
dans ses bras comme pour se bien persuader, à cette minute,
qu’elle était à lui maintenant et qu’aucune puissance, aucun préjugé
humain ne pouvait plus la lui prendre :
— Ma fiancée, ma Claude adorée, fit-il, il ne vous est pas
possible de concevoir ce que cet homme, ce « méchant homme »,
comme vous dites, a souffert !… Ah ! si vous saviez !… Aimer une
jeune fille de toutes les forces de son être, assez passionnément,
assez exclusivement pour ne plus pouvoir se figurer une vie où on
ne la verrait pas et dont elle ne serait pas le but et la raison d’être ;
se juger digne d’elle ou capable de le devenir, sentir qu’aimé d’elle
on lutterait sans faiblesse, on triompherait de toutes les difficultés…
Et cependant n’avoir pas le droit d’espérer que tant d’amour puisse
éveiller jamais dans l’âme de la bien-aimée autre chose qu’un
profond dédain ou — si elle est généreuse — une vague pitié !
N’être après tout séparé d’une femme chérie que par un préjugé, et
avoir la certitude que ce préjugé constitue le plus terrible, le plus
infranchissable des abîmes, un abîme que rien au monde ne saurait
combler… Mais, y avez-vous songé ? c’est, pour un cœur aimant et
fier, une torture dont l’horreur est inexprimable !… Cette torture, il l’a
connue dans ses plus atroces raffinements, le malheureux Antonin
Fargeot !… Bien plus, il a été insulté, traité comme le dernier des
lâches… bâtonné, devant celle qu’il aimait !… Ah ! mon Dieu ! mon
Dieu ! comment voulez-vous, quand il a souffert cela, que je refuse
de pardonner, moi, moi ?… Mais s’il avait tué, s’il… ma bien-aimée,
s’il avait tué l’homme qui cherchait à l’avilir, je crois que je
pardonnerais encore.
Emporté par la violence du sentiment qu’il défendait et qu’il avait
fait sien, Pierre s’était levé, le front pâle, les yeux enflammés.
— Comme vous avez l’air méchant, quand vous parlez ainsi ! fit
Claude en secouant la tête.
Mais elle souriait, presque convaincue, car elle savait qu’il y avait
beaucoup d’amour pour elle dans ce pardon accordé à Antonin
Fargeot.
— Vous n’avez pas peur de moi, pourtant ? demanda doucement
l’officier, en se rasseyant auprès d’elle.
— Non, soupira-t-elle, non… tout de suite, j’ai eu en vous une
confiance… très folle… que rien, je crois, ne pourrait plus ébranler. Il
me semble que vous devez mieux que moi juger de toutes choses…
Et, cependant, quelle excuse trouver au rapt d’un enfant sans
défense…
— Ce rapt qu’Antonin Fargeot s’est reproché comme un crime,
sur son lit de mort, n’a pas été commis de propos délibéré, fit le
jeune homme. Tout à l’heure, je vous ai raconté comment le pauvre
maître de poésie avait renoncé à se faire justice lui-même aussi bien
qu’à obtenir justice des autorités… Un grand découragement avait
anéanti en lui toute énergie, toute ambition… Ses chers travaux de
littérature et de philosophie ne lui paraissant plus que vains et sans
portée, il les avait délaissés… Là n’était pourtant pas encore le
terme de ses épreuves. Quelque temps après le mariage de… —
c’est par vous que je connais, vous le savez, les noms mystérieux
de cette étrange histoire — quelque temps après le mariage de
mademoiselle Irène de Champierre, Antonin s’était senti si seul… et
si malheureux dans sa solitude qu’il avait essayé de se créer de
nouvelles affections, de nouveaux devoirs. Il avait épousé une jeune
fille qui lui était inférieure, sans doute, sous le rapport de
l’intelligence et de l’éducation, mais dont la bonté, l’honnêteté, le
courage avaient attiré son estime… Bientôt, il perdit sa femme, puis
l’enfant qui lui était resté de ce demi-bonheur trop court… Quelques
jours après ce dernier deuil, comme il errait au hasard de sa
songerie dans cette grande ville de Paris où il vivait seul,
maintenant, d’hôtellerie en hôtellerie, très ignoré, très silencieux, ne
se plaisant en aucun logis, ne recherchant la société de ses
semblables qu’autant que l’exigeait la nécessité de pourvoir à sa
subsistance, il oublia l’heure et minuit sonna avant qu’il eût pensé à
la retraite… Sa songerie l’avait conduit, comme bien souvent sans
doute, dans les parages de cet hôtel de Chanteraine-Champierre qui
abritait la nouvelle existence de la bien-aimée d’autrefois, d’Irène,
heureuse épouse, heureuse mère… Mais, ce soir-là, malgré l’heure
tardive, un grand nombre de personnes couraient affolées suivant la
même direction qu’Antonin Fargeot… L’hôtel de Chanteraine-
Champierre était en flammes !… Bientôt le pauvre homme se
précipita vers le lieu du sinistre et, arrivé là, il apprit simultanément
qu’on venait de retirer de l’édifice incendié le cadavre du marquis de
Chanteraine, puis celui de sa femme… et qu’on ignorait le sort de
leur fils, un enfant de deux ans… Les secours étaient venus trop
tard, les escaliers menaçaient de s’écrouler… Tout espoir était
perdu… Antonin n’en demanda pas plus. Comme un fou, un
halluciné, il s’élança dans la fournaise, ne sachant pas s’il souhaitait
de mourir lui-même, parce qu’Irène était morte, ou de sauver l’enfant
de celle qu’il avait tant aimée… Plus tard, il ne se rappela
qu’imparfaitement ce qui s’était alors passé… La nourrice
épouvantée avait quitté sa chambre à coucher en emportant le petit
Gérard de Chanteraine et courait éperdument à travers l’hôtel, sans
plus savoir trouver d’issue ; elle rencontra un homme qui semblait
braver les flammes ou les ignorer, et elle lui confia précipitamment,
avec l’enfant que ses bras ne pouvaient plus soutenir, un petit coffret
d’émail, qu’elle avait pu sauver et qu’elle savait précieux…
— Oh ! Pierre, s’écria Claude, cette impression d’une grande
terreur ressentie dans une maison en flammes, ce rêve qui troublait
vos nuits d’enfant, c’était un souvenir !
— C’était un souvenir, oui, répéta Pierre.
Puis il reprit, continuant son récit :
— Antonin saisit l’enfant et le coffret et se jeta au hasard dans un
couloir que le feu avait épargné ; bientôt, il s’aperçut que, malgré ses
recommandations expresses, la nourrice ne l’avait pas suivi… Avait-
elle tout à coup manqué de force ? était-elle retournée en arrière,
follement, pour chercher un objet oublié ? Il ne le sut jamais. Il ignora
toujours aussi, par quel prodige, à l’instant où l’immense escalier
s’effondrait aux cris d’horreur de la foule, il avait pu, lui, le sauveteur
inconscient, sortir de l’hôtel par une petite porte de service. Mais le
même instinct qui l’avait dirigé, à travers tous les obstacles et tous
les périls, vers l’air respirable, lui interdit alors de s’arrêter, et sa fuite
éperdue ne prit fin que lorsqu’il eut atteint, loin de l’incendie, la
fraîcheur d’une rue sombre et déserte… Là, une émotion terrible
l’attendait encore… En se penchant sur l’orphelin qu’il avait sauvé et
qui se cramponnait à lui, muet, sans larmes, Antonin Fargeot crut
rencontrer des yeux déjà vus… les yeux de cette Irène de
Champierre qui n’était morte pour le monde que depuis une heure,
mais qu’il pleurait, lui, depuis longtemps. Une ressemblance qui lui
parut frappante, chez cet enfant de deux ans…
— C’est vrai, murmura mademoiselle de Chanteraine… Vous
avez les yeux de votre mère, vous avez aussi son sourire… Cette
ressemblance, je l’ai vue tout de suite… D’abord, je ne me rendais
pas compte… puis, brusquement, quand vous avez regardé le
portrait de ma pauvre tante, j’ai été saisie… Et vous, vous avez aimé
ce cher portrait, sans rien savoir, sans rien prévoir de la vérité !
— Oh ! Claude, c’était le portrait de ma mère… de ma mère à
moi ! Comme je l’eusse aimée ma mère, Claude ?… Et mon père,
vous ne m’en avez rien dit… vous me parlerez de lui ?…
— Oui, je vous le promets, répondit la jeune fille. Que de choses
nous avons à nous dire ! mais continuez votre récit, mon cher, cher
ami… Cette ressemblance ?…
— … Cette ressemblance qui n’est pas illusoire, puisque, vous
aussi, vous l’avez observée, provoqua chez Antonin Fargeot une
sorte de détente… Et le pauvre homme se mit à pleurer… Il pleurait
sur la mort affreuse d’Irène, sur sa propre misère, sur le sort du petit
enfant sans père ni mère qu’il tenait entre ses bras… et, le petit
enfant, sentant confusément, sans doute, que cet homme au visage
de douceur et de tristesse était bon et qu’il souffrait… l’embrassa
soudain et le caressa pour le consoler… Alors, au milieu de tant de
douleur, à l’heure même où la femme aimée venait de mourir,
Antonin Fargeot eut un moment d’ineffable joie et le courage lui
manqua pour se séparer aussitôt de l’orphelin, de ce fils d’Irène qui
ne connaissait pas encore les distances sociales et qui baisait
doucement de sa bouche innocente le « philosophe » que les laquais
de son grand-père avaient chassé… Personne dans la foule terrifiée
n’avait pu remarquer au milieu des flammes et de la fumée tandis
que l’escalier s’écroulait et bientôt, avec lui, toute une partie de
l’hôtel, le passage d’un homme qui s’était enfui, en courant, comme
beaucoup d’autres à cette minute d’épouvante ; personne ne savait
que Gérard de Chanteraine eût échappé à la mort… Antonin
l’emporta à l’autre bout de Paris, dans une auberge où il se présenta
vers le matin, comme un voyageur quelconque… Mais l’enfant, en
proie à une fièvre ardente, semblait maintenant anéanti… comme s’il
n’eût plus su trouver les quelques mots qu’il devait déjà connaître, il
bégayait de temps à autre des sons inarticulés, de vagues syllabes
qui n’avaient point de sens… Une grave maladie se déclara.
Pendant plusieurs jours, la vie et la mort se disputèrent Gérard de
Chanteraine, et quand la vie eut enfin triomphé, Antonin sentit qu’en
rendant ce petit être à ceux qui le croyaient mort, à M. de
Champierre peut-être, il allait perdre Irène encore une fois… Mais il
ne trouva pas la force d’accepter ce nouveau déchirement… Et,
après une suprême lutte, il consomma sa faute ; il la consomma en
la raisonnant sans doute et je crois comprendre le travail qui put se
faire dans son esprit.
» Rien du passé ne subsistait plus, après l’horrible crise, dans le
cerveau de l’enfant. On eût dit que, revenant à la santé, Gérard avait
recommencé une autre vie. Il avait fallu lui apprendre à marcher, il
faudrait lui apprendre à parler…
» Antonin Fargeot garderait auprès de lui l’héritier des
Chanteraine, l’élèverait comme il eût élevé le fils qu’il venait de
perdre, il le doterait de tout le savoir qu’il avait lui-même amassé au
cours de sa douloureuse jeunesse ; il le mettrait à l’abri des préjugés
de race, il développerait en ce cœur vierge les instincts généreux et
purs de l’être que la corruption sociale n’a pas encore touché, puis,
quand il aurait fait de ce fils de noble un homme libre, conscient et
respectueux de la dignité humaine, il le rendrait au comte de
Champierre. Telle serait la revanche de l’amoureux bafoué ! Un jour,
le grand seigneur avait jeté comme une injure à la face d’Antonin
Fargeot le mot de philosophe ; ce serait bien en philosophe
qu’Antonin Fargeot se vengerait du grand seigneur… »
» Mais les événements publics vinrent modifier ces projets. Il y
eut un jour où Antonin put penser avec raison qu’étant donné l’état
des choses, il était meilleur et moins périlleux pour l’enfant enlevé de
s’appeler Pierre Fargeot que Gérard de Chanteraine… Vous
connaissez la fin de cette étrange histoire. Je serais resté toujours
Pierre Fargeot, non seulement si mon père adoptif n’avait pas été
pris de remords à l’heure de quitter cette vie, mais encore si le plus
extraordinaire des hasards ne m’avait permis de deviner, par
déduction, un nom que la vue des objets impersonnels contenus
dans ce coffret, n’eût pas suffi à me révéler… Mais, je vous ai
connue, je vous ai aimée, mon ange, mon trésor !… Et il semble
vraiment qu’en mourant, celui qui m’a élevé — oh ! si tendrement,
Claude, avec tant de dévouement — ait pressenti, lui aussi, quelque
chose de l’avenir quand il m’a dit : « Tu me pardonneras, peut-être,
quand tu auras aimé… » Vous lui pardonnerez comme moi, n’est-ce
pas, Claude ?
— Si vous voulez, concéda mademoiselle de Chanteraine. Il me
semble que je ne sais plus haïr… Et pourtant, mon grand-père le
duc de Chanteraine a pleuré amèrement la mort de son petit-fils, et
pourtant si cet homme ne vous avait pas enlevé à votre famille, vous
ne seriez pas…
— Qui sait ce que je serais ?… Rougissez-vous donc de ce que
je suis ?
— Rougir de vous ! oh ! Pierre !
— Vous m’appelez encore Pierre ?
Claude sourit, et très bas :
— Je crois que pour moi vous serez toujours Pierre.
— Et cependant, si j’étais resté Pierre pour tous, si je n’avais eu
droit que… qu’au seul titre en somme, ma pauvre bien-aimée, qui
vaille qu’on m’en sache gré, parce que je l’ai moi-même conquis ; si
je n’avais été enfin qu’un pauvre officier de l’armée d’Italie… vous
n’auriez jamais été ni ma fiancée ni ma femme. Et si Gérard, un
autre Gérard était venu…
Mademoiselle de Chanteraine le regarda avec reproche.
— Vous m’avez fait espérer, lors de notre tout premier entretien,
dit-elle, que Bonaparte n’était point ennemi de la foi et que, par lui,
les églises seraient rouvertes aux âmes pieuses. Ne me croirez-vous
pas, si je vous jure que depuis, cette idée m’a hantée : « Les cloîtres
aussi nous seront-ils rendus ? »… Car, si je restais la fiancée fidèle
de Gérard de Chanteraine, c’était bien, néanmoins — oh ! mon ami,
soyez-en sûr — c’était bien à Pierre Fargeot que mon âme s’était
donnée… Et je n’aurais pu la lui reprendre que pour l’offrir à Dieu.
III
LA CLÉ D’ARGENT
Il fallut bien pourtant se rappeler que Claude n’était ni la seule

survivante de la famille de Chanteraine, ni la seule habitante du
château…
Deux jours avant, obsédée par une pensée qui ne lui avait pas
laissé de repos depuis qu’elle avait vu la bague du vieux duc de
Chanteraine entre les mains de Pierre Fargeot, la jeune fille s’était
décidée à prendre un parti qui lui coûtait beaucoup. Elle avait parlé à
sa tante des choses qu’elle avait si longtemps tues pour obéir au
désir de son grand-père et des événements plus récents qui avaient
jeté le trouble dans sa vie et lui paraissaient trop merveilleux pour
qu’elle n’y vît pas la manifestation d’une volonté providentielle.
La tante de Chanteraine et les cousins de Plouvarais n’avaient
pas été éloignés de croire tout d’abord que, prise de folie, Claude
leur faisait ouïr le plus étrange de ses « contes de fées » ; mais la
jeune fille leur avait révélé au moyen des deux devises, le secret de
l’armoire de fer et, ayant pour ainsi dire touché du doigt le mystère
dont ils étaient prêts à rire, les vieux portraits s’étaient trouvés forcés
d’avouer que le conte offrait, tout au moins, les apparences d’une
histoire vraie.
Claude avait espéré décider ainsi sa tante à se mettre sous la
protection des autorités nouvelles, pour reparaître dans le monde
des vivants et obtenir ensuite que des recherches fussent faites —
elle eût été bien en peine de dire lesquelles — sur les origines de ce
Pierre Fargeot qui ressemblait si singulièrement à la marquise Irène
de Chanteraine.
Mais, quoique fort surprise et même réellement intriguée,
mademoiselle Charlotte avait déclaré qu’elle ne voulait à aucun prix
s’exalter sur des faits aussi peu vraisemblables… Ah ! si ce petit
républicain avait apporté, avec la bague, la chaîne de Gérard et la
seconde clé du coffre de fer, peut-être eût-il été nécessaire
d’envisager plus sérieusement les choses, mais la bague pouvait,
après tout, avoir été achetée chez un antiquaire quelconque par le
père Fargeot… Conclusion : Claude avait l’imagination de son
grand-père !
Quant à M. de Plouvarais, il avait remarqué tout haut que, sur un
tel thème, l’imagination la plus calme eût trouvé, cette fois, prétexte
à broderies.
Et Fridolin avait hoché la tête sans rien dire.
Les choses en étaient restées là.
— Comme la première fois, j’irai vous annoncer, monsieur
Fargeot ! fit Claude en souriant.
Mais, maintenant, une inquiétude lui venait sur l’accueil qui
pouvait être fait à ce cousin dont la résurrection lui semblait à elle si
naturelle.
— Il est indispensable, ajouta-t-elle pensivement, que, lorsque je
montrerai à ma tante les objets qui nous ont révélé votre véritable
nom, votre véritable personnalité, je sois en mesure d’affirmer
l’identité de ces objets, en invoquant, à l’appui de mon dire, le
résultat probant d’une expérience décisive… Il faut, en un mot, que
personne ne puisse nier un instant que la clé d’argent apportée par
vous soit celle qui, selon la volonté du duc de Chanteraine, devait
ouvrir le coffre de fer.
— Vous avez raison, répondit Pierre.
A la clarté vacillante de la lanterne qu’on allumait chaque soir
pour monter du logis souterrain aux étages supérieurs, Claude et
Pierre recommencèrent donc, à travers le château obscur, le voyage
qui les avait une fois déjà conduits en face de l’énigme troublante
dont le secret leur était alors demeuré impénétrable.
Avec quelle angoisse, quelle terreur confuse de leurs destinées,
ils avaient parcouru les couloirs déserts !
Et voilà qu’un espoir, un bonheur invraisemblable avait tout
éclairé en eux et autour d’eux ! Voilà que, s’aimant, ils avaient le
droit de s’aimer ! Voilà que Pierre pouvait penser, lorsqu’il soutenait
la jeune fille, lorsqu’il lui prenait la main pour la guider, que cette
course vers un but défini et proche n’était que le prélude et le
symbole d’une autre course plus longue et plus incertaine qui
durerait jusqu’à la mort et qu’il ferait aussi avec Claude, en la
protégeant de sa force, en la réchauffant de son amour, en
s’efforçant d’écarter tout obstacle et tout péril sur les pas de cet être
délicat et doux dont la vie allait lui être donnée.
… Leur marche était lente, un peu hésitante ; ils n’échangeaient
pas beaucoup plus de paroles que la première fois, mais il était doux
à ces fiancés dont les âmes se pénétraient sans le secours des
mots, de se taire ainsi dans l’ombre et le silence qui les
enveloppaient et chacun d’eux croyait entendre penser l’autre, au
fond de son propre cœur…
Soudain, Claude et Pierre tressaillirent, brusquement arrachés à
leur rêve heureux.
Une porte s’était ouverte à quelques pas d’eux et, sur le seuil
d’une chambre éclairée, le vieux Quentin venait d’apparaître, une
lampe à la main… Il était indubitable que, du premier regard, l’ancien
serviteur du duc de Chanteraine avait vu et reconnu l’officier accueilli
plusieurs jours auparavant par mademoiselle Charlotte ; son visage
était très pâle, si pâle que la blancheur s’en confondait presque avec
la neige de sa chevelure vénérable…
Qu’allait penser Quentin ?… Qu’allait-il faire ?… Brusquer une
situation déjà délicate et périlleuse, en ébruitant parmi les habitants
du château la présence de l’étranger, de l’intrus ? Hâter
inopportunément l’heure des explications, des révélations décisives
dont Claude avait désiré être l’intermédiaire ?… Tout perdre peut-
être, en éveillant ainsi contre Pierre la susceptibilité méfiante de
mademoiselle de Chanteraine ?…
Il fallait obtenir de Quentin la promesse de taire jusqu’à nouvel
ordre le secret qu’il avait surpris, il fallait se faire un allié de cet
incorruptible, en lui démontrant la raison d’être et l’importance de ce
sursis…
Claude eut un moment d’angoisse terrible. Toute parole se figeait
sur ses lèvres.
Mais Quentin s’était approché, calme, respectueux :
— Daignez permettre à votre fidèle serviteur d’éclairer vos pas…
fit-il d’une voix grave.
Et, sans attendre de réponse, sans s’informer de la direction à
suivre, il dépassa les jeunes gens et marcha devant eux, toujours
très pâle dans l’orbe lumineux de la lampe que sa main, à peine
tremblante, élevait à la hauteur de ses cheveux blancs…
A la porte de la tourelle il s’arrêta, prit doucement la lanterne des
mains de Pierre et, toujours sans parler, remit au jeune homme le
fanal plus puissant, qu’il avait lui-même porté jusque-là.
— Merci, répondit simplement l’officier, dominé par cette décision
déférente et silencieuse.
Aucune autre parole ne fut dite et déjà Quentin avait disparu
comme une ombre.
— On dirait qu’il a compris, qu’il a deviné… Comme c’est
étrange ! murmura Claude.
Ils descendirent l’escalier de la tourelle et entrèrent bientôt dans
la petite salle boisée de chêne.
— Je vous en prie, agissez pour moi, fit la jeune fille. Vous
connaissez maintenant aussi bien que je le connais, le secret que
mon… que notre grand-père vous a légué comme à moi… Et ce
m’est une grande douceur, mon ami, de m’en remettre à vous de
toutes choses, à cette place même où la vie m’a fait peur… et où je
me sens aujourd’hui si heureuse et si tranquille près de vous.
Tranquille, elle l’était, en effet, non pas seulement parce que son
rêve le plus cher devenait une réalité, mais parce qu’elle avait
inconsciemment retrouvé sa belle foi en une fatalité bienveillante et
toute providentielle. Il lui semblait maintenant n’avoir plus qu’à se
laisser conduire par cette volonté supérieure et toute-puissante dont
Pierre devenait, à ses yeux, l’incarnation terrestre, l’infaillible
représentant.
Cependant quand, à l’appel des deux devises, la boiserie se fut
écartée, quand la première serrure eut joué, laissant tomber de
quelques pouces la lourde porte de métal, Claude se prit à trembler.
Si Pierre s’était trompé, avait été trompé plutôt ; si la clé
d’argent…
Un grand frisson la parcourut toute ; instinctivement, elle ferma
les yeux pour ne pas voir ce qui allait advenir…
Mais, presque aussitôt, elle entendit un léger grincement
métallique, puis un bruit sourd… elle regarda…
L’armoire avait achevé de s’ouvrir.
Alors la pensée ne vint pas à Claude plus qu’à Pierre,
d’interroger les grands coffres d’or et d’argent qui apparaissaient
dans la profondeur du mur et dont les reflets se réveillaient
superbement au contact de la lumière. La jeune fille tendit ses mains
à Pierre qui les prit dans les siennes et tous deux se sourirent, les
doigts entrelacés, des larmes plein les yeux…
La porte de fer et la boiserie furent refermées sans que Claude et
Gérard de Chanteraine eussent pu soupçonner la valeur ou même la
nature de cette fortune que le vieux duc avait jalousement recueillie
et cachée pour eux.
Que leur importait ? Si leurs cœurs, en un élan de
reconnaissance, donnèrent, à cette minute même, un souvenir à
l’aïeul, ce fut seulement parce que ce grand prévoyant, dont on avait
tant souri, les avait fiancés dans le passé ; ce fut parce que ce
vieillard chimérique, qui croyait aux légendes, s’était révolté contre la
triste évidence des choses positives, pour garder Claude à Gérard,
pour nier que la mort eût pu séparer ceux que l’amour devait unir…
… Puis, Pierre se retrouva seul dans le boudoir de la Belle au
bois.
Claude lui avait dit :
— Ayez patience, je viendrai vous chercher bientôt.
A son tour, il se sentit bouleversé de crainte, d’inquiétude.
Il attachait fort peu de prix à la fortune et le nom de Fargeot, tel
qu’il l’avait porté, et qu’il le portait, lui semblait, à vrai dire, valoir le
nom de Chanteraine. Il croyait fermement qu’il y a plus d’honneur
pour un homme à mériter l’estime et la considération de ses
semblables par ses actes personnels et son caractère propre qu’à
les tenir d’un nom et d’un titre illustrés par les œuvres plus ou moins
lointaines d’aïeux plus ou moins légendaires… Mais seul, le nom de
Chanteraine permettrait à l’officier républicain d’épouser Claude.
… Ce qui se décidait dans le salon de l’épinette ou sous les yeux
des vieux portraits, c’était l’avenir de cet amour passionné qui avait
pris la vie de Pierre.
Et le jeune homme se disait douloureusement qu’il ne lui était
guère permis d’attendre de mademoiselle Charlotte de Chanteraine
et des cousins de Plouvarais, l’adorable confiance que Claude lui
avait témoignée.
Dans cette famille, hostile par naissance et par conviction, aux
idées qu’il avait lui-même respectées et défendues, dans ce milieu
étroit où, loin d’être considérés comme de sérieuses garanties
d’honneur et de loyauté, le caractère de sa personnalité, son grade,
l’histoire de sa vie ne pouvaient que le desservir, peut-être allait-il
passer pour un imposteur ?
Les bijoux qu’il avait remis à mademoiselle de Chanteraine
étaient indéniablement ceux que le vieux duc avait jadis confiés à sa
belle-fille, mais comment prouver qu’Antonin Fargeot avait bien
réellement sauvé l’héritier des Chanteraine ou comment prouver que
Pierre, l’enfant élevé par le maître d’école, était bien l’orphelin
qu’Antonin Fargeot avait sauvé ?
A force de songer à l’incrédulité qui accueillerait certainement la
communication de Claude, Pierre en arrivait à trouver cette
incrédulité légitime et à discuter lui-même son droit de revendiquer
un nom dont rien n’affirmait irréfutablement qu’il fût l’héritier.
Devenu possesseur avant la Révolution, et par un concours de
circonstances quelconque, des objets qui avaient appartenu au petit
Gérard, Antonin Fargeot n’avait-il pas pu, dans le but d’assurer une
destinée brillante à Pierre, son véritable fils, broder sur des faits
réels l’histoire racontée à tante Manon ?
A ces suppositions, des remords se mêlaient, car Pierre se
reprochait bien vite de salir ainsi la mémoire d’un homme dont le
caractère ne lui paraissait pas avoir justifié jamais une accusation de
cette nature…
… Et l’absence de mademoiselle de Chanteraine semblait ne
plus devoir finir, et l’anxiété du jeune homme s’exaspérait dans cette
attente impuissante…
Enfin, Claude entra, et, prenant par la main celui qu’en dépit de
toute opinion étrangère elle était décidée à considérer comme son
cousin, elle l’entraîna dans la salle des portraits où mademoiselle
Charlotte de Chanteraine, M. de Plouvarais, mademoiselle Marie-
Rose et le fidèle Fridolin étaient réunis.
IV
LE DUC DE CHANTERAINE
Il était visible qu’un événement important venait de troubler les

chères habitudes de tout ce petit monde paisible et routinier du
château.
Comme lors de la première et mémorable rencontre,
mademoiselle Charlotte avait daigné faire deux pas au-devant de
Pierre et elle poussa l’amabilité jusqu’à lui tendre une main qu’il se
permit de baiser… ce qui ne déplut pas.
— Bonjour, monsieur Fargeot, commença-t-elle, ma nièce Claude
qui a toujours des papillons plein la tête, me dit que vous êtes mon
neveu et tout est possible, je le sais, au temps où nous vivons…
Mais vous ne serez point étonné de me trouver encore un peu
étourdie du récit que je viens d’entendre… La vérité est que je n’en
ai jamais ouï de plus extravagant !
— Je ne puis m’étonner, madame, répondit le jeune homme en
souriant tristement, ni de votre surprise ni de votre incertitude… Et je
ne saurais que supposer moi-même, si les faits qui m’ont été révélés
tout récemment par la digne femme que j’appelais et appellerai
toujours tante Manon n’avaient confirmé, avec une précision bien
étrange, ceux dont je tenais le récit, soit de mademoiselle de
Chanteraine, soit de vous…
— J’avoue, monsieur, reprit complaisamment mademoiselle
Charlotte, qu’il y a des présomptions assez sérieuses pour que vous
soyez, en effet, Gérard de Chanteraine ; mais vous m’accorderez
qu’il y en a de non moins frappantes pour que vous ne le soyez
pas… Ainsi, comment croire qu’un vrai Chanteraine aurait pu
combattre contre le roi, sans que tout son être se révoltât ?
— Je n’ai pas combattu contre le roi, madame, répliqua
doucement Pierre, j’ai combattu pour la France que j’ai servie
fidèlement, dès que j’ai eu l’âge de le faire, imitant en cela, je crois,
tous les Chanteraine du passé…
— Vous l’avez servie dans les armées de la République !… N’y
avait-il pas, monsieur, une autre armée où vous eussiez pu la
servir ? fit mademoiselle Charlotte avec une sévérité solennelle qui
lui seyait si drôlement qu’il eût été difficile de n’en pas sourire en tout
autre moment.
Mais Pierre n’était point d’humeur à sourire.
Aux paroles de la vieille demoiselle, un flot de sang lui monta au
visage.
— L’armée des princes ! s’écria-t-il, eh bien ! non, madame, non.
Indépendamment de toute question politique, j’adore ma patrie !
Aurais-je été royaliste, aurais-je émigré… me serais-je même
engagé dans l’armée de là-bas que… ah ! je le sais, je le sens !…
Quand j’aurais vu le premier soldat étranger passer la frontière, un
instinct puissant, irrésistible aurait crié en moi et m’aurait jeté parmi
les adversaires de mon parti à qui j’aurais demandé une place, pour
défendre avec eux le sol du pays.
En parlant ainsi, sans brutalité, mais avec une conviction
profonde, toute son âme ardente vibrant dans les notes graves de sa
voix, l’officier s’était transfiguré. Un moment il avait oublié le nom
souhaité, il avait oublié Claude elle-même. On eût dit que le souffle
héroïque des jours de 92 venait de passer encore une fois sur le
jeune et mâle visage de ce colonel de vingt-quatre ans.
Mademoiselle Charlotte fut touchée de cette sincérité.
— Je crois, monsieur, avoua-t-elle, que votre cœur eût été digne
d’une meilleure cause… cependant si séduisante et courageuse
qu’elle soit, votre profession de foi n’en correspond pas moins au
raisonnement le plus spécieux, et je persiste à croire qu’un
Chanteraine…
A ce moment, on vit une chose si étonnante que les murs de
Chanteraine eux-mêmes crurent en reculer de surprise et d’effroi…
Le vieux Quentin qui s’était faufilé, on ne sait comment dans la salle
des portraits et dont la présence était trop familière à tous les
habitants du château pour que personne s’en fût aperçu ou, tout au
moins troublé, le vieux, le fidèle Quentin venait de couper la parole à
mademoiselle Charlotte de Chanteraine !
— Rien n’est plus facile, déclarait-il, que de s’assurer de l’identité
de Gérard de Chanteraine…
— Oh ! parle, parle, Quentin ! supplia Claude malgré elle.
— Pendant le temps que M. le marquis et madame la marquise
passèrent à Chanteraine, continua le vieillard, notre enfant, qui
commençait à peine à marcher, fit une chute dont chacun s’effraya…
Une coupe de cristal que le pauvre petit avait prise sur la table, sans
que la nourrice s’en aperçût, s’était brisée dans le choc et l’avait
blessé à la main…
— A la main et au front, acheva M. Fridolin.
— C’est vrai, je n’ai point oublié ce détail, confirma mademoiselle
Charlotte pensive. L’enfant perdit beaucoup de sang jusqu’au
moment où les deux plaies purent être recousues… et le médecin
qui soignait Gérard annonça que la cicatrice de ces coupures ne
s’effacerait probablement jamais…
— Je m’en souviens, s’écria M. de Plouvarais.
— Je m’en souviens aussi, acquiesça mademoiselle Marie-Rose.
— Moi, je ne me souviens de rien, murmura Pierre avec une
sorte de lassitude découragée, car ce débat lui était affreusement
pénible… Cependant, j’ai à la main une marque assez profonde… et
que je me suis toujours connue…
Mais, tandis que le colonel Fargeot parlait, Quentin s’était encore
rapproché. Tout à coup, avec une familiarité affectueuse de vieux
serviteur, il posa sa main sur le front du jeune homme et écarta
brusquement la masse ondée des cheveux bruns. Alors, apparut à la
tempe gauche, très nette sur la peau hâlée, une petite cicatrice
blanche.
— Voyez ! s’écria-t-il. Puis il y a la ressemblance qui m’a ébloui,
moi, tout de suite !…
Et saisissant la main que Pierre avait instinctivement ouverte
pour y chercher la trace de la bienheureuse blessure, le vieil homme
la baisa, le front courbé :
— C’est un beau jour pour moi, monsieur le duc, murmura-t-il.
— Embrassez-moi donc, mon neveu, fit mademoiselle Charlotte
passant sans transition du doute à l’enthousiasme. Je ne
m’attendais certes pas à me découvrir un neveu dans l’armée de ce
monsieur Bonaparte… mais, par ma vertu, il fait bon revoir un
Chanteraine !
Et se tournant vers Fridolin, elle conclut :
— Je vous disais bien, magister, qu’il était impossible qu’un
simple petit officier républicain ressemblât à ma nièce de
Chanteraine !… Mais vous êtes de ces gens qui en remontreraient à
leur curé !
La fidèle sujette du roi sans couronne et le soldat du Premier
Consul s’embrassèrent des plus cordialement. Il y eut un moment de
joie et d’effusions un peu folles.
Puis, tandis que le jeune duc cherchait les yeux de Claude,
n’osant, à cette minute, dire des lèvres ce que son cœur sentait, le
chevalier de Plouvarais, qui, malgré ses airs évaporés ne laissait
pas de voir souvent les côtés pratiques de la vie, remarqua qu’on
avait oublié de dîner…
— C’est vrai, mon Dieu ! exclama mademoiselle Marie-Rose.
— Et voici le jour ! ajouta Fridolin, désignant les rideaux baissés
au travers desquels passaient les lueurs du matin.
— L’aurore ! s’écria Pierre. La belle aurore d’un des plus beaux
jours de ma vie !
Il regarda encore Claude dont les yeux s’illuminaient, comme le
ciel, de clartés ardentes et douces. Puis, d’un mouvement spontané,
il rejeta les rideaux, il ouvrit la fenêtre, les persiennes, faisant éclater
aux prunelles éblouies des emmurés la lumineuse vision des ruines
en fleurs…
Sur les choses du passé, les ors atténués, les étoffes pâlies,
longtemps dérobés au jour, glissa la chaude caresse du soleil
levant… Alors, il parut à Claude que, d’une extrémité de la pièce à
l’autre, le portrait du vieux duc souriait à celui de la jeune marquise.

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Polymer Nanocomposite Materials:

Applications in Integrated Electronic

Polymer Nanocomposite-Based Smart Materials: From

3D and 4D Printing of Polymer Nanocomposite Materials:

Principles of Electronic Materials and Devices 4th

Quantum Materials, Devices, and Applications Mohamed

Polymer science and innovative applications materials,

Lectures on Digital Design Principles (River Publishers

Applications of Polymer Nanofibers Anthony L. Andrady

Electronic Devices and Circuits S. Salivahanan

Applications in Integrated Electronic Devices

Bibliographic information published by

© 2021 WILEY-VCH GmbH, Boschstr.

All rights reserved (including those of

Print ISBN: 978-3-527-34744-5

Typesetting SPi Global, Chennai, India

Printed on acid-free paper

1 Introduction of Polymer Nanocomposites 1

2 Fabrication of Conductive Polymer Composites and Their

2.3.2.2 Surface Coating 31

3 Biodegradable Polymer Nanocomposites for Electronics 53

4 Polymer Nanocomposites for Photodetectors 77

List of Abbreviations 123

5 Polymer Nanocomposites for Pressure Sensors 131

6 The Application of Polymer Nanocomposites in Energy

6.4 Separator 174

7 Functional Polymer Nanocomposite for Triboelectric

8 Polymer Nanocomposites for Resistive Switching

9 Polymer Nanocomposites for Temperature Sensing and

10 Polymer Nanocomposites for EMI Shielding Application 267

Polymer nanocomposites combining the merits of polymers (e.g. light weight,

01 June 2020 Ye Zhou

Introduction of Polymer Nanocomposites

0.1 nm 5 nm 100 nm 10 000 nm 1 000 000 nm

0.5 nm 10 nm 1000 nm 100 000 nm 10 000 000 nm

Figure 1.1 Nanomaterials peculiarities of size scale.

Figure 1.2 Number of publications per year on “nanomaterials,” “nanocomposites,” and

1.2 The Advantage of Nanocomposites

Since the fillers of nanocomposites are nanoscale, the performances of nanocom-

Plates Spheres Rods

1.3 Classiﬁcation of Nanoscale Fillers

1.3.1 One-Dimensional Nanoﬁllers

Table 1.1 Overview of nanomaterials classiﬁed by their nanoscale dimensions.

Plate Rod Sphere

• Montmorillonite clays • Carbon nanofibers (CNFs) • Nano-silica (n-silica)

characteristics, such as nanoplate [15], nano-disk [16], nano-wall [17–23], etc.,

1.3.2 Two-Dimensional Nanoﬁllers

1.3.3 Three-Dimensional Nanoﬁllers

1.4 The Properties of Polymer Nanocomposites

Figure 1.4 Signiﬁcant properties of polymer nanocomposites.

1.5 Synthesis of Polymer Nanocomposites

Table 1.2 Summary of common methods for synthesis of polymer nanocomposites.

Technique Suitable ﬁller Suitable matrix Solvent Controlling factors

Ultrasonication- All types Liquid or viscous Required Sonication

1.5.1 Ultrasonication-assisted Solution Mixing

1.5.2 Shear Mixing

1.5.3 Three Roll Milling

1.5.4 Ball Milling

1.5.5 Double-screw Extrusion