Chapter 4

Characterization Techniques of Polymer

Composites

Monika Chaparia, Shivali Meena, Neelam Kumari, Sandip P. Choudhury,

Ravi Kant Choubey, and Umesh Kumar Dwivedi

Abstract Polymer composites significantly improve the behavior and capabilities

of materials compared to conventional materials. However, in order to comprehend
the behavior of polymer composites their property profile must be thoroughly under-
stood. This profile comprises aspects such as chemistry, morphology, functionality,
particle size, etc. However, applying a variety of analytical tools is significant to
have a better insight into its characterization. This chapter includes the characteriza-
tion techniques of polymer composites to unravel properties like mechanical perfor-
mance, tribological behavior, microstructural behavior, structural behavior, physical
properties, electrical behavior, rheological properties, thermal behavior, and optical
properties.

Keywords Polymer composites · Characterization · Techniques · Behavior

4.1 Introduction

Polymers are widely used in advanced applications due to their versatility and ease of
molding and adaptable physical and chemical properties. However, a single polymer
cannot satisfy the requirements of advanced application which lead to the idea of
polymer composites. Composites consist of ceramic, metal, fiber, semiconductors,
and other polymers as reinforcement and as matrix. Since, many materials are present
in composition, a variety of factors can influence the characteristics of polymer
composites, such as type, shape, size, and fraction of reinforcing materials [1].
Polymer composites offer remarkable characteristics like good corrosion and wear
resistance, good abrasion resistance, fatigue resistance economic efficiency, light

M. Chaparia · S. Meena · N. Kumari · S. P. Choudhury · U. K. Dwivedi (B)

Amity School of Applied Physics, Amity University Rajasthan, Jaipur 303002, India
e-mail: [email protected]
R. K. Choubey
Department of Applied Physics, Amity Institute of Applied Sciences (AIAS), Amity University,
Noida Campus, Sector-125, Noida, Uttar Pradesh 201313, India

© The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 99
S. Moharana et al. (eds.), Polymer Composites, Engineering Materials,
https://doi.org/10.1007/978-981-97-2075-0_4
100 M. Chaparia et al.

weight, high strength, high stiffness, and faster molding [2–4]. Polymer compos-
ites such as reinforced plastics, fiber-reinforced polymer are of huge importance in
various fields like household, construction, automotive industry, aerospace, marine,
energy, military, sports, communications, electronics, civil, medical, and automobile
[5]. Polymer composites are also used extensively in biomedical applications as hard
(bones) and soft (skin) tissues [6].
Characterization is a comprehensive and universal technique used to investigate
the structure, characteristics, and behavior of a composite, and it plays a vital role
in the process of creating new composites. Through physical, chemical, mechanical,
tribological, rheological, thermal, and optical characterization researchers can better
understand polymer composite materials and its application in industries, automotive,
aerospace, defense, and medical field [7, 8].
For Physical and mechanical testing can be done in accordance with a wide range
of standards, such as ASTM (American society for Testing and Materials), ISO
(International Standard Organization), BS (British Standards), DIN (Deutsches insti-
tute fürNormung - the German Institute of Standatization), or IS (Indian Standard)
utilizing techniques unique to the industry.
• Physical characterization includes density, hardness, and scratch resistance.
• Electrical characterization includes conductivity, dielectric characteristics.
• Mechanical characterization include tensile, shear, flexural and compressive
characteristics.
• Tribological characterization includes wear, friction, lubrication.
• Rheological characterization includes capillary, rotational, Index/Melt Flow Rate.
• Thermal characterization includes DSC (differential scanning calorimetry), DTA
(differential thermal analysis), and TGA (thermogravimetric analysis).
• Optical characterization includes UV/Visible spectrometer.

4.1.1 Characterization Methods of Polymer Composites

4.1.1.1 Mechanical Characterizations

The numerous polymer composites are applicable in various areas like construction;
aerospace, automobile, sporting goods, etc. are greatly influenced by their mechanical
properties. These characteristics determine how the composite material will react to
loads and external forces as well as other contributing elements such as toughness,
resistance to fatigue, and strength.
There are several standard tests to examine the mechanical behavior of composites
like tensile testing, flexural testing, impact testing, and hardness testing according to
various loading circumstances (Fig. 4.1).
4 Characterization Techniques of Polymer Composites 101

Fig. 4.1 Mechanical

characterization testing
techniques

4.1.1.2 Tensile Testing (Tension Testing)

In material science and engineering, tensile testing is a basic technique that is

frequently used in the characterization of materials for a wide range of applications.
It determines how much force is needed to break a composite or plastic specimen as
well as how much the sample expands or contracts before breaking.
Tensile testing is done using flat sandwich or basic tension in compliance with
standards like ASTM C 297, EN 2561, EN 2597 ISO 527-4, ISO 527-5, and ASTM
D 638 [9]. With the help of these tests, stress–strain diagrams can be obtained and
further tensile modulus, tensile strength, and percent elongation can be determined.
Due to composites having a brittle and anisotropic nature, alignment is very critical.
The anisotropic nature means its properties depend on the direction of applied force.
When a composite material is tested in the direction parallel to the orientation of
fibers, the tensile strength is very high and much lower if tested in any different
direction. Basically, high tensile stress-based structures can be utilized in aerospace
industries where maximum tensile strength with excellent axial loading is required.
Generally, ASTMD638 (refer to Fig. 4.2) is used for making composite materials
but ASTMD3039 is required when the polymer has more strength.
Fundamentally, stress is just about a restoring force generated per unit area of
the material. It is represented by the Greek letter σ and is measured in Pascal or N/
m2 (1 N/m2 = 1 Pa). From the given experimental setup, the ratio of the amount
of load applied to the specimen (F) to its original cross-sectional area (A) in the
axial direction yields stress which is measured before the experiment is conducted.
Mathematical expression can be written as
102 M. Chaparia et al.

Fig. 4.2 ASTMD638 test specimen [10]

F
σ = (4.1)
A
In mechanics, strain determines the deformation produced due to stress applied
on a material. It is a unit less quantity and can be expressed as

δL Change in Length
Strain(ε) = = (4.2)
L Original Length

A stress–strain diagram illustrates the connection between the applied load on a

material and the resulting deformation due to that load which is shown in Fig. 4.3
and Table 4.1.

4.1.1.3 Flexural Testing

Flexural testing is done to evaluate the ability of a material to resist or bend. To obtain a
semi-qualitative understanding of the fiber-matrix interfacial strength of a composite,
a flexural test is used. Generally flexural test is employed in brittle materials (both
rigid and semi-rigid materials) like composites, ceramics, and plastic materials. This
test procedure uses a three or four-point bend testing system. The material’s property
to bend before permanently deforming is indicated by its flex modulus. The following
standard explains how to measure flexural properties; ASTM D 790, ASTM D 6272,
ASTM D7264, ISO 178. Numerous specimen shapes are suitable for conducting this
test, but the prevalent specimen size according to ISO standards is 1 cm × 0.4 cm ×
4 Characterization Techniques of Polymer Composites 103

Fig. 4.3 Stress and strain curve showing significant points

Table 4.1 Showing tensile properties with an explanation

Tensile property Justification
Proportional In this region, stress is directly proportional to strain. Within this limit
limit Hooke’s law is obeyed
Elastic limit The highest stress that a substance can endure before permanent deforming
comes under elastic limit
Upper yield The ductile material shows plastic qualities beyond the elastic limit. At this
point point the material needed maximum stress to start plastic deformation
Lower yield At a lower yield point, the minimum load demanded for the material to behave
point as plastic
Ultimate stress The utmost stress a material can endure before breaking is known as the
point ultimate stress point
Breaking or The point at which lastly material breaks. This point is also known as the
fracture point breaking strength of a material

8 cm, rectangular specimens of dimension 16 cm × 2 cm × 0.8 cm × 1 cm × 0.1 cm

for ASTM D790. For ASTM standards, the recommended specimen size is 0.32 cm
× 1.27 cm × 12.5 cm [9] (Fig. 4.4).
For conducting the test on a universal testing machine specimen should be placed
horizontally on the lower supports of the test fixture, then applying a gradually
increasing load on the center of the specimen continuously as long as the specimen
breaks or shows considerable deformation. All parameters like maximum deflection
and speed of loading are defined separately for different standards (ISO, ASTM).
Finally, data can be analyzed by calculating flexural stress and strain (at yield &
104 M. Chaparia et al.

Fig. 4.4 Experimental setup of flexural test a 3-point flexure test, b 4-point flexure test

break), stress–strain curve, and flexural modulus [11]. Akhil et al. conducted exper-
iments to determine an optimum span length for testing the flexural strength of
samples of prepreg materials of glass and carbon and observed the behavior of flex-
ural strength and flexural modulus as per the ASTM standards [12]. Saba et al.
studied the comparative effects of various CNFs reinforced epoxy matrices (0.5%,
0.75%, and 1%) on different mechanical properties (flexural, tensile, and impact).
The study shows a remarkable improvement for 0.75% CNFs/epoxy as compared
to other epoxy nanocomposites due to uniform and homogeneous dispersion in the
epoxy matrix [13] (Fig. 4.5).

Fig. 4.5 Effect of CNFs filler loadings on flexural strength and modulus of epoxy composites
4 Characterization Techniques of Polymer Composites 105

4.1.1.4 Impact Testing

The purpose of the impact test is to ascertain the reaction of a known material (i.e.
ceramics, polymers, and composites) when subjected to a suddenly imposed stress.
The key objective of this test is to assess the toughness, notch sensitivity, brittle-
ness, impact strength, and as well as notch sensitivity of the engineering materials
depending on the characteristics and test performed. The amount of energy that a
material can withstand before it undergoes breaking or rupturing can be determined
by impact strength or toughness. Most often, it takes a large amount of energy for
tough materials to break while brittle materials exhibit low toughness due to their
limited ability to undergo deformation. The main test configurations for measuring
material characteristics are Charpy and Izod specimen configurations. These tests
differ in the sample orientation which results in the changed direction of stress on
the specimen and their basic procedure involves releasing a known load from a spec-
ified height to collide with the specimen in the test fixture. Usually, various notch
configurations, namely U-notch, V-notch, and keyhole notch are used as the test
specimens for the impact test (as shown in Fig. 4.6) [14, 15].
The dimensions of the conventional Charpy test specimen are 5.5 cm × 1 cm ×
1 cm [9]. ISO 179 is the standard procedure for testing Charpy impact strength [16].
The Charpy V-notch test measures how much energy a material will absorb during
fracture which indicates the material’s notch toughness [17]. The experimental setup
of this test involved a pendulum with a known load released from a specified height to
strike a notched specimen which is placed in a horizontal position. By analyzing the
difference in the hammer’s height before and following the fracture occurrence, we
can precisely determine the amount of energy absorbed by the material. The notch
(with consistent dimensions) and size of the specimen, both factors, play crucial
roles in this test as they greatly influence the conclusions drawn from the test. Izod
test measures materials generally at low temperatures especially plastics. The appa-
ratus consists of a swinging pendulum and strikes the specimen when it is held in a

Fig. 4.6 Shows different notches in the impact test [15]

106 M. Chaparia et al.

Fig. 4.7 Showing the impact strength of adding nano-fillers [18]

vertical position, besides it follows similar criteria as discussed in the Charpy notch
test. This test holds particular significance in circumstances where materials must
withstand sudden stresses including the development of various consumer goods,
and structural gear for safety purposes. ISO 180 and ASTM D256 are the standard
tests used for the Izod impact test [16]. Figure 4.7 displays the impact strength of
epoxy nanocomposites on adding OPEFB nano-fillers (at 0%, 1%, 3%, 5%). In this
investigation, Saba et al. concluded that 3% nano-OPEFB/epoxy nanocomposites
showed improved impact strength in comparison to other nano-fillers [18].
Epoxy composites are greatly explored by the researchers due to their excel-
lent mechanical properties. Mia et al. prepared HrGO hybrids by combining
halloysite nanotubes (HNTs) and reduced graphene oxide (RGO) and incorporated
them into epoxy resin which results in a notable enhancement of mechanical prop-
erties. In comparison to neat epoxy, the results revealed that 0.2 weight % of HrGO
enhanced impact, flexural, and tensile strength by 1048.8%, 29.5%, and 489.9%
respectively [19].

4.1.1.5 Hardness

Hardness is not a fundamental feature but rather hardness is the measurement of

the material’s resistance to localized plastic deformation (a small depression). Also,
the value of hardness can be determined by the interaction of tensile strength, yield
force, and modulus of elasticity. There are various ways to describe the hardness
of a material including (1) resistance to indentation (2) resistance to abrasion or
scratching (3) rebound effectiveness [20]. The most popular technique for quick and
regular hardness measurements is the macro hardness test (Rockwell, Brinell, and
Vickers). The range of indenting forces for the determination of macro hardness
is between 50 and 30,000 N. Generally, the Rockwell hardness test measures the
4 Characterization Techniques of Polymer Composites 107

hardness of plastic. The ASTM D75 standards are commonly followed for examining
the hardness of polymer-based composite materials [21].
Hardness measurement can be measured by the following techniques;
(1) Macro hardness—This is a technique for obtaining mechanical property data
for the bulk material from a small example. The range of indenting forces for the
determination of macro hardness is between 50 and 30,000 N. The procedures
for macro indentation testing are those that include extensive area deformation,
heavy loads, and extremely deep penetrations.

• The Macro Rockwell hardness test

When you apply load to the test object, the macro-Rockwell hardness test measures
(As shown in Fig. 4.8) the indentation’s depth. Hardness is inversely proportional
to the depth of penetration. This test applies to all types of material from plastics to
hardest steels. Therefore, various overlapping scales are used. The R, L, M, E, and
K are frequently used to represent hardness numbers and hardness numbers have no
units. The hardness of a material depends on the hardness number, the higher the
hardness number of scales, the harder will be the material. In this test, indenters that
are either ball-shaped or diamond-shaped are to be used. This test measures how
much deeper an indenter can be pushed by a major load than it can be pushed by a
minor (preliminary) load that was applied earlier.
• The Macro Brinell hardness Test

Simply Brinell hardness test is also an indentation test and it was initially developed
by the Swedish physician Dr. Johan August Brinell. Forging, castings, hot-rolled
and cold-rolled bars, and low- and high- alloy steels can all be tested using the
Brinell method. ASTM E10-15a and ISO 6506-1 are the essential references for

Fig. 4.8 Schematic of indentation process of Rockwell hardness test by using diamond indenter
108 M. Chaparia et al.

Fig. 4.9 Brinell hardness

test

calculating the Brinell hardness of metallic materials and also provide instructions
for consistence and precise measurement of hardness [22, 23]. In this method (As
shown in Fig. 4.9), the surface of the material being examined is penetrated with
a hardened steel ball, commonly composed of tungsten carbide with a specified
diameter (10 mm), under a given load (L).
The Brinell hardness number (HBN) can be determined by the ratio of the test
load (L) (in kilograms) to the spherical surface area of the indentation (in square
millimeters) as shown below [24].

Test Load in Kg
HBN =
Surface Area of Indentation
2L
HBN = √ kg/mm2 (4.3)
π D(D − D2 − d 2 )

where,
L—Test load (in kg).
D—diameter of the steel ball (in mm).
d—diameter of the indentation or impression (in mm).
• The Vicker’s Hardness test (macro and micro)
At Vickers Ltd., Robert L. Smith and George Sandland invented the Vickers hardness
test (Fig. 4.10) in 1921. It determines the size of the impression left by a diamond
4 Characterization Techniques of Polymer Composites 109

indenter to determine the object’s hardness. Compared to the Rockwell hardness test,
the Vickers test uses a lower test load or force. In this test, a square-based diamond
indenter is used [25]. It can measure the hardness of a material at both micro and
macro scales. The diamond pyramid hardness (DPH) or Vickers pyramid number
(HV) is the hardness measurement unit provided by the test. Vickers hardness test
measures the hardness of a wide range of materials including ceramics, metals and
some kinds of polymers. It follows the principle that a square-based diamond indenter
with a facing angle of 136 degrees is impressed on the material surface with a pre-
decided load (between 0.01 kg and 2 kg for micro hardness and 1 kg and 100 kg for
macro hardness test) for a specified dwell time, usually few seconds. During this time,
the indenter created a square-shaped indentation into the material and a calibrated
microscope is used to measure the size of the indentation which is typically no larger
than 0.5 mm. The Vickers hardness test methods are outlined in various standards
like ASTM E384 (covering micro force ranges from 10 to 1 kg), and ASTM E92
(covering macro force ranges from 1 to 100 kg). In addition, ISO 6507 standards
comprise of both micro and macro ranges [26].
kgf )
The ratio, surface area offorce(in
the indentation(in mm2 )
gives the HV as follows [28].

2Fsin θ2
HV =
S2
◦
2Fsin 136
HV = 2
S2
F
HV = 1.854 (4.4)
S2
where,

Fig. 4.10 Schematic of Vicker’s hardness test [27]

110 M. Chaparia et al.

F is the applied force (in kilograms-force).

S is the average length of the diagonals (in millimeters).
θ is the angle between the opposite faces of diamond.
Because HV offers a continuous scale of hardness it is well accepted in research
work.
HV can be represented as xxxVHNyy, for e.g. 340VHN20 or xxxVHNyy/zz if
force duration varies from 10 to 15 s.
Where,
340 represents the hardness number.
HV represents the Vickers hardness scale.
20 represents load in Kgf.
30 represents force duration if it varies from 10 to 15 s [29].

4.1.2 Tribological Characterizations

The Tribology term deals with the study and analysis of friction, wear, and lubrication
between two rotating elements. By understanding what friction, wear, and lubrication
one can understand the term ‘tribology’. There are a lot of examples of friction
and wear like automobile, skating, writing in which friction between two bodies is
necessary for starting and stopping of objects. Whereas, larger amount of friction may
lead to component failure and is also responsible for wear of engine parts and power
loss. For reducing wear due to friction, abrasion, adhesion, and erosion lubrication
techniques are used. No one can stop friction and wear completely but it can be
reduced to a mini level [30]. We will discuss these concepts clearly as follows.

4.1.2.1 Wear

Wear is defined as the damage, sluggish removal of the material or its distortion from
the solid surface due to colliding with the other solid surface (sliding or rolling), even-
tually resulting in the loss of functionality or breakdown of the material. Generally,
gradual material loss caused due to relative motion between two contacting surfaces
is termed as ‘wear’. Tribology is the study of wear and associated processes. Both
mechanical and chemical factors (such as erosion and corrosion) can be a cause of
wear. Wear can be triggered by solids (metallic or non-metallic) or solid particles, by
the action of fluids, and also by liquid droplets entrained in gases that are flowing. A
common example for better understanding wear is worn out of the soles of the shoes
by the action of friction; this reduces the life of the object.
4 Characterization Techniques of Polymer Composites 111

Fig. 4.11 Adhesive wear

There are some broad categories in which wear can be classified depending on
the tribosystem.
(1) Mechanical Wear—When two solid surfaces come into contact due to relative
motion, removal of the material takes place from either of the surfaces that can
result in mechanical wear (mainly in machine parts). It is further divided into
several more parts
(2) Adhesive wear—Adhesive wear happens when the transfer of the material
takes place due to the adhering state acquired by the two bodies when they are
in sliding contact. It is because of the strong atomic bonding forces present at that
particular point (as shown in Fig. 4.11). It creates depressions and indentations
on the surface that can be in the form of pits, voids, or cavities [31]. Two
contact surfaces may experience galling, scuffing and scoring as a result of
intense adhesive wear. This type of wear leads to removal or attachment of the
material from either surfaces and can be reduced by decreasing the roughness
of the surface, by enhancing hardness of the surfaces or by avoiding direct
metal–metal contact [32].
For adhesive wear Archard has given an equation for calculating adhesive wear;

Wd
Vw = K (4.5)
H

where, Vw is the wear volume (mm3 )

K is the sliding constant.
W is the force (in Newton).
D is the sliding distance.
H is the hardness of the soft material (kg/mm2 ).
• Galling—It happens when adhesive wear becomes acute i.e. forming of macro-
scopic protuberance.
• Scuffing—It is a moderate form of adhesive wear i.e. surface roughness or
scratches.
• Abrasive wear—Deformation caused due to the movement of itinerary sharp and
solid asperities across a smooth surface which leads to the removal of some part of
112 M. Chaparia et al.

contact surfaces or loss of the material place due to the presence of macroscopic
protuberances which are forced against solid surface resulting in abrasive wear.
For example because of the interaction of the surface of the car tyre (smooth
surface) and road (hard surface), the tyre sole is worn out with the time. Chand
et al. examined the abrasive wear behavior of polymer composites reinforced with
sisal fibers and published the results they discovered [33]. Abrasive wear can be
understood by two modes i.e. two-body abrasive wear or three-body abrasive wear
[34]. Sandpapers and grinding wheels, glass papers are commonly used as coated
abrasives (paper or cloth sheets on which abrasive material like grit is attached to
one face). Nowadays these abrasive materials are replaced by the materials like
silicon carbide paper or aluminum oxide paper for removing the material from
surfaces (for painting, removing old paint, furnishing of wood) while sandpapers
are manufactured in a variety of grit sizes. According to ISO 9352 and ASTM
D 4060, the Taber Abrasion Test can be used for evaluating abrasive wear as
reduction of mass.
For the single abrasive wear, the volume of the wear Vw can be explained by;

Wd Wd
Vw = αβ K (4.6)
H H
where, α is the asperity shape factor (typically 0.1)
β gives the degrees of wear by an asperity (typically 0.1 to 1.0).
W is the force (in Newton).
K is the sliding constant.
d is the sliding distance.
H is the hardness of the softer material (kg/mm2 ).
Vw gives the wear volume (mm3 ).
(1) Erosive Wear
Erosive wear is a form of mechanical wear, sometimes known as Erosion Wear is a
degradation of the surface material due to direct impingement of the liquid or solid
particles on the material’s surface with a very high velocity. A noble illustration of
erosive wear occurs when raindrops of different velocities impact the Earth surface,
leading to erosion [34]. So erosion can be (1) solid erosion (2) liquid erosion (3)
liquid impact erosion (4) slurry erosion and (5) cavitation.
• Solid erosion
In this type of erosion (Fig. 4.12), the solid materials’ surface is deformed due to the
repeated impact of high-speed solid particles (carried by air) which gradually erodes
the materials’ surface. A number of factors affect the rate of erosive wear mainly the
material properties of the particle (shape, impingement angle, and collision velocity).
4 Characterization Techniques of Polymer Composites 113

Fig. 4.12 Solid erosion

The maximum wear rate for ductile materials occurs at approx. 30◦ angle of
impingement (α) in which the material is separated out by cutting action due to
the impact of abrasive particles, while for non-ductile materials it is determined by
the angle of impingement (α) being normal to the surface (90◦ ) and due to splin-
tering action, the surface material is removed [35]. The sharp bend or curves tend to
erode more than mild bends. An Air jet of oxide particles bombarded on the surface
(Abrasive particles behave like little secateurs) and amount of damage depends on
the abrasive particle mass (m), impingement angle (α), impingement velocity and
sharpness factor of the particle (F) [25].

Erosion(degree of damage) = Kmv2 Af (4.7)

where, k is the constant.

• Liquid erosion
In material and mechanical engineering, liquid erosion refers to mechanical damage
of the solid materials’ surface due to the repeated impact of high-speed liquid particles
which gradually erode the materials’ surface. This type of erosion mainly occurs in
pipes of metals (copper, steel) in various industries including wind energy, aerospace,
mainly in gas and steam turbines, nuclear power plants, power generation plants
where liquid flow is involved having passive oxide films for resistance to corrosion.
114 M. Chaparia et al.

The protective layer of oxide is removed by the impact of liquid. Perforation of

elbows of pipe occurred due to repeated impingement of the liquid. However, this
type of mechanical damage or erosion occurs above some threshold velocity [36].
• Liquid Impact Erosion
In this type of erosion, high velocity liquid droplet impinges on the surface of the
solid. Aircraft rain erosion is the standard example, as the speed of raindrops is very
high in comparison to the speed of aircraft (which is approximately 400 m/s), all
the forward-facing surfaces like nose, windshields, leading edges of the spar, engine
inlets are eroded or damaged.
• Slurry Erosion
For slurry handling equipment (i.e. valves, pumps, and pipelines) used in usually
mineral processing, mining industries, systems related to oil and gas production,
and in hydraulic machineries, slurry erosion is an issue of major concern due to its
considerable adverse effects such as loss or removal of material [37–39]. Due to the
transmission of slurries carrying abrasive particles in hundreds of kilometers long
pipes (i.e. in coal pipelines), slurry erosion occurs [40].
The subsequent factors responsible are;
Particle characteristics (mass, shape factor, hardness, density).
Flowing slurry characteristics (temperature, viscosity, concentration, turbulence,
corrosivity).
Impingement condition (impact angle, impact level, impact velocity or energy).
Time and Temperature.
Target surface properties (toughness, hardness, corrosion resistance, microstruc-
tures).
• Cavitation
Cavitation is a specialized form of liquid impact erosion in which tiny gas bubbles (or
voids) are formed as a result of external influences in a liquid. These vapor cavities
or bubbles (i.e. where the pressure is low) collapse when pressure increases subse-
quently, produce intense shockwaves and water jets that can degrade the material. In
hydraulic pumps, propellers, control valves, submerged planes, pump impellers and
also in spillway in dams, cavitation erosion is often experienced.

4.1.2.2 Friction

When the two surfaces are in contact then a tangential force resists the relative motion
of two bodies. If the surfaces are smooth than there will be no resistive force hence,
the rough surface will have more friction. Temperature, nature of the material and
roughness are the major factors that affect friction. Friction can be static (rest), kinetic
(dynamic), or rolling. Frictional forces can have both aspects good or bad as we are
unable to walk without friction. According to Amontons equation the frictional force
is directly proportional to the nominal load
4 Characterization Techniques of Polymer Composites 115

F = μW (4.8)

μ is the proportionality constant which is known as coefficient of friction.

4.1.2.3 Lubrication

Lubrication is a process in which we separate two contacting surfaces by a layer of

lubrication at the interface to make them smooth and to minimize the effect of wear
due to friction, abrasion, adhesion and erosion, so that metal–metal contact can be
avoided. In the process of lubrication, lubricants (oil and grease) are applied to the
surface for making a separation between two layers so that the substance ready to
shear while adhering to the surface. Lubrication is mainly used to increase effec-
tiveness, lifespan, and efficiency of machineries. Lubricants also serve as sealants
and coolants. Therefore, the important factor is the viscosity of lubricants for the
formation of film. Lubricants (Fig. 4.13) can be classified as:
Liquid lubricants—The majority of lubricants are liquid and are generally based on
one type of base oil but to meet the special performance requirements mixture of
base oil is also used like natural oil, water, lanolin, vegetable oil, mineral oil etc.
According to their origin into two groups lubricants may be classified as:

Fig. 4.13 Various kinds of lubricants

116 M. Chaparia et al.

• Mineral oils: Those lubricating oils which are refined for reduction of some
molecular reactions from naturally occurring crude oil are termed as mineral
oils.
• Synthetic oils: Synthetics oils are man-made lubricants which are typically created
by artificial chemical compounds. Mainly polyalphaolefins (PAOs) is commonly
used as synthetic oil. Synthetic oils produce lower friction, less evaporation, heat
resistance which led to better lifespan, nonetheless these oils are expensive.
Oil is the main ingredient for formation of grease, as greases contains 75–80% of
oils.
• Solid lubricants
Liquid lubricants or say greases cannot be useful for lubricating bearings operated
at extremely high temperatures, in vacuum, or under extremely powerful radiation.
So dry lubricants or solid lubricants are used for better advantages and applied in
the form of powders or thin films for reducing friction between two moving surfaces
such as boron nitride, Teflon, molybdenum disulfide, graphite, tungsten disulfide.
Due to their lamellar structure, oxidation prevention, thin film formation these mate-
rials possess excellent additive properties. Even some materials stay lubricious at
extremely high temperature. Solid lubricants are extensively employed in various
industries including aviation, marine and coastal applications, automotive etc.
• Semi-solid lubricants
Greases: oil is the main component in grease which is responsible for lubrication.
Grease is preferred because of multitude reasons including ease of confinement, low
friction and substantial better service life at reasonable cost. Three key ingredients
are combined to create greases: thickener, additives, base oil (refer to Fig. 4.14).
Thickeners can be simple soap base, complex soap base or non-soap base such as
calcium soaps, lithium, clay, sodium, polyurea, lithium complex, aluminium complex
that are mixed with some minerals or synthetic oils (as shown in Table 4.2). Generally,
grease does not perform the application of cleaning and cooling like other fluid
lubricants because of its semisolid nature [41]. Other than these, greases carry out all
the responsibilities of a fluid lubricant. Grease is the most expedient and cost effective
lubricant for preventing block out contaminants and leakage due to its water resistive
nature.
• Gaseous lubricants

In comparison to liquid lubricants, gaseous lubricants exhibited considerably supe-

rior compressibility and lower viscosity (also viscosity increases with the increase of
temperature). Molecular composition of the gaseous lubricant remains unchanged at
extreme temperature range (low or high) whereas liquid lubricants are unstabble over
a wide range of temperature. The liquid lubricant changes its molecular composition
at high temperature and is converted into a gaseous form. Because of their chemical
stability there is no chance that the lubricant would contaminate the ball bearings,
which is crucial for the tools used in many industrial sectors particularly in food,
4 Characterization Techniques of Polymer Composites 117

Fig. 4.14 Lubricating grease composition

Table 4.2 Different types of thickners

Simple soap Complex soap
Lithium Calcium Aluminium Lithium Calcium
Barium Sodium Strrontium Aluminium Barium
Mixed soap Titanium
Non-Soap
Clay, Alumina, Polyurea, PTFE, Silica gel

electronic and medical industries, and in many aerospace applications (such as aero-
static and aerodynamic bearings). Gases such as argon nitrogen, oxygen, hydrogen,
carbon dioxide, and acetylene are most widely preferred gaseous lubricants [42].
However, air is the most viably employed gas lubricant which is preferably utilized
in fluid bearing.

4.1.3 Microstructural Characterizations

A vital aspect of material science is microstructural characterization, which entails

the microscopic interpretation and as well as analysis of the interior structure of
a material. Understanding the mysteries concealed in the microscopic realm of
materials are the goal of this area of research, known as microstructural charac-
terization. The morphological features can be revealed by appropriate preparation
118 M. Chaparia et al.

of samples. The dimensions of the particles or grains, shape, and phase boundaries
all are defined by the microstructural morphologies. The interaction of incident radi-
ation with specimen is resulting in variation of image contrast which reveals the
information about morphological properties. Microscopy such as scanning electron
microscopy and transmission electron microscopy is one of the several methods used
in microstructural characterization [43].

4.1.3.1 SEM

Scanning Electron Microscope, often referred as SEM. Instead of light microscope,

SEM is more preferred as it uses high energetic focused beam of electrons scanned
across the specimen for generating various signals that contains all information about
the specimen’s surface topology depending on the depth of the specimen resulting
in the images at a much greater resolution.
The interaction of atoms and electrons in the specimen generates a number
of signals that encompasses information regarding composition of the specimen,
bonding, shape and size of the particles, various defects, texture, and surface topog-
raphy. An external monitor is used to detect the image by correlating the electron
intensity and beam position of the incident ray. Higher resolution (better than 1 nm)
can be achieved by using SEM.
SEM can directly analyze a variety of solid materials, however when dealing with
biological materials and insulating samples, specialized image techniques (i.e. low
vacuum or low KV imaging) are often employed to mitigate surface charging and
beam induced damage. For reducing the charging on insulating samples, a fine layer
of conducting material like platinum or gold is sputtered.
Principle
Due to the interaction of atoms and electrons in the sample, various signals including
Secondary electrons (for topographical image), Backscattered and Diffracted back
scattered electrons (determines surface composition or crystal structure) and char-
acteristic X-rays (photons), and also certain materials emit visible light via a
phenomenon called cathodoluminescence (CL) are ejected from the sample which
are collected by the detectors to convert them into signals for creating the final image,
which is shown in Fig. 4.15.
Sample Preparation
There is a requirement of special sample preparation due to the use of electron beam
and low vacuum conditions. One of the most critical precaution is to dehydrate the
samples because water vaporizes in a vacuum. For obtaining a well suited sample
suitable for SEM analysis firstly, ensure that it is appropriately shaped and sized
according to your specimen stage. To facilitate standard SEM imaging, specimen
should possess, electrical conductivity particularly on the surface, and should be
grounded to prevent the buildup of electrostatic charge. All conductive specimens
like metals need little preparation.
4 Characterization Techniques of Polymer Composites 119

Fig. 4.15 Various levels of electron penetration [44]

Non-conductive materials are needed to be made conductive for minimize

charging and to improve conductivity by generally coating with a thin layer of elec-
trically conductive materials like platinum, gold, graphite, tungsten and chromium
by the process of low vacuum sputtering. For this process a device called ‘sputter
coater’ is used in which argon gas is ionized when exposed to an electric field in
a vacuum chamber. Negatively charged gold foil is attracted by positively charged
argon ions, as after collision releasing gold atoms and hence these gold atoms adhere
to the surface resulting in a fine conductive layer of gold.
Instrumentation and Working
Basically SEM contains several key components including electron source (filament)
for generating focused electron beam, electron lenses (objective lenses, condenser
lenses), detectors for all type of signals (i.e. electron detectors, X-ray detectors),
specimen chamber and a data display monitor or software.
Generally, SEM analysis process can be accomplished using the procedure
outlined by Goldstein et al. [46]. Some additional clarity for SEM analysis is provided
by referring to Fig. 4.16 for further understanding. At the top of the microscope a
beam of electrons is produced by thermionic emission from an electron gun (tung-
sten filament is used due to its highest melting point and lowest vapor pressure) and
subsequently accelerated through the column at a designated acceleration voltage
ranging from 1 to 30 keV. To produce a fine beam of electrons (for reducing diam-
eter) or for converging the beam it is pass through the condenser lenses and apertures
and finally through an objective lens which is used to focus the beam of electrons
onto the sample. A vacuum environment must be maintained throughout the entire
120 M. Chaparia et al.

column. Depending upon the electron source used, voltage with which the beam is
accelerated and the lens system decides the diameter of the beam which ranges from
less than 1–20 nm. Scan coils which are positioned above the objective lens control
the position of the electron beam on the specimen and enable the electron beam to
scan in a raster- like pattern across the specimen’s surface in the X–Y plane.
Thus, this scanned beam interacts with the specimen producing a variety of signals
such as secondary electrons, reflected and back scattered electrons, and characteristic
X-rays.
• Secondary electrons resulting from the inelastic scattering are the low energy
electrons (approx. 10–50 eV) by which we can obtain topographical information
nearby the surface and SEs are detected by Everhart Thornley detector.

Fig. 4.16 SEM (Scanning Electron Microscope) [45]

4 Characterization Techniques of Polymer Composites 121

• Backscattered electrons results from the elastic scattering at high angles (greater
than 90 ◦ ) from the deeper surface and are redirected backward towards the source.
Higher atomic number elements generate more backscattered electrons, hence a
brighter image is created, where it provides information regarding compositional
difference of a specimen.
In a study conducted by Hajsman et al. different kinds of SEM imagining were
tested at pressure 30 Pa (refer to Fig. 4.17) and reported that the utilization of
backscattered electrons (as shown in Fig. 4.17 is the most appropriate method for
both identifying the difference in the chemical composition and also for observing
morphology [47].
These signals can be detected by suitable detectors and can be seen as an image on
a computer monitor. As the scanned area becomes progressively smaller, the corre-
sponding magnification will be higher in SEM often reaching up to a million times
(approximately 1,000,000 × in some modern models) [48]. Chand et al. investigated
the influence of a coupling agent on abrasive wear performance of polypropylene
composites reinforced with chopped jute fibers and also showed their results with
SEM analysis. Fractography showed in Fig. 4.18a illustrates two notable aspects:
first, the presence of twist in the fibers resulting from the melt mixing process and
second, the generation of internal defects. The Fig. 4.18b provides a closeup view of
a MA-g-PP treated jute fiber within a PP composite and it distinctly illustrates the
improved compatibility between the surface of the coated fiber and matrix. Definitely,
this treatment led to an increased elongation in the CT composite. They discovered
that the utilization of the coupling agent enhances wear resistances in contrasting to
not employing a coupling agent [33].

Fig. 4.17 Image of SEM, a high vacuum, b low vacuum secondary electrons, c low vacuum
backscattered electrons [47]
122 M. Chaparia et al.

Fig. 4.18 a SEM showing magnified view of smooth surface of MA-g-PP solution-treated jute
fiber-PP composite (CT) [33] and b SEM showing magnified view of fractured surface of MA-g-PP
melt-mixed jute fiber-reinforced PP composites (MT) [33]

As discussed before about resolution of SEM, in contrast, TEM provides signif-

icantly greater spatial resolution (∼ 0.1 nm), because of its distinctive imaging
mechanism.

4.1.3.2 TEM

By zooming into the atomic scale, scientists can examine the basic components of
the materials. In transmission electron microscopy, a high energetic focused beam
of electron (accelerated voltage range from 60 to 300 kV) is transmitted through the
ultra-thin specimen by whom we can analyze matter at the nanoscale at an extremely
high resolution. Typically, the sample consists of, usually less than 100 nm in thick-
ness; or it can be a suspension on a grid. The sample is placed in the middle of the
column. After the interaction of the sample with electrons, the resulting image can
be magnified on a device like as fluorescent screen or by a CCD camera (charged
coupled device) on a computer screen. TEM gives us a 2D image while SEM provides
a 3D image (as shown in Fig. 4.19).
Magnification of TEM can reach a maximum of 50 million and a resolution of up
to 0.5 angstroms.
The basic difference between SEM and TEM is that SEM uses scattered or
reflected electrons whereas TEM uses transmitted electrons. TEM provides invalu-
able information about its inner structure (crystal structure) and morphology at a
higher resolution. TEM, due to its ability to give microstructure of the materials
(polymers, metals etc.) at nanoscale, is employed in research field (such as nanotech-
nology, semiconductor) and many other applications like cancer research, geology,
virology, biology as well as in environmental science.
4 Characterization Techniques of Polymer Composites 123

Fig. 4.19 a SEM image provides details on the surface’s morphology, b TEM image illustrates the
internal structure of the specimen [49]

4.1.4 Structural Characterizations

4.1.4.1 XRD

In material science, X-ray diffraction is an analytical technique of crystallography

which is used to understand about arrangement of atoms in solids (i.e. atomic and
molecular structure) in which constructive interference occurs between X-rays and
the crystalline structure results in X-ray diffraction. The intensities and scattering
angles of these diffracted beams can be determined by which we can identify the
crystal structure. In 1912, Laue claimed that the x-ray wavelength used is comparable
with the distances between atoms of solids, so x-rays are chosen for the technique. The
diffraction pattern can be examined by using Bragg’s law. When we are mentioning
that x-rays are scattered by atoms, we actually mean scattered by the electrons within
atoms. The intensity of x-rays is graphed against the scattered angle; by analyzing
the position, angle and intensities of peaks of the diffraction patterns we can identify
the structure of the material [50]. We interpreted that the crystal size is inversely
proportional to the width of the x-ray diffraction meaning narrow peaks indicate
larger crystals, whereas broad peaks suggest smaller crystals.
Joseph John Thomson discovered that when unpolarized x-rays impinges on
itinerary electrons, then the scattered intensity at a distance d from the origin for
one particle of mass m and charge e is given by

nIo e4
I= (1 + cos2 α) (4.9)
2(mc)2 c2 d 2

where,
I—intensity of x-rays at some point M,
124 M. Chaparia et al.

e—Charge on electrons,
n—Number of electrons.
d—Distance between origin and point M.
Io —Intensity if x-rays incident on a free electron at origin.
m—Electron mass.
α—Angle between incident and scattered beam.
Generally, among different types of X-ray diffractometers (Fig. 4.20) that are
available for crystal structure analysis, the most preferable diffractometer used
for nanomaterial analysis is the Debye- Scherrer Diffractometer (Powder Diffrac-
tometer). It has the ability to provide adequate information regarding the crystal
structure of the nanoparticles, polycrystalline materials and thin films. Basically,
a monochromatic source of X-rays, powdered sample and detector are used for the
whole setup of the diffractometer. The sample undergoes rotation within a monochro-
matic x-ray beam and the detector scans across the complete 2θ range. Usually a
Scintillation counter, proportional counter, semiconductor counter, and gas propor-
tional counters the signals are detected depending on the type of the sample required
to be analyzed [50, 51].

Fig. 4.20 Schematic of X-ray Diffractometer [51]

4 Characterization Techniques of Polymer Composites 125

4.1.5 Physical Characterization

Physical characterization of the polymer composite entails the quantitative or quali-

tative measurements such as density, surface roughness, and hardness. Using this
conclusive technique, size, weight, roughness, porousness, toughness, softness,
strength and other characteristics can be determined. Physical characterization is
typically done after fabrication of the polymer composite or material.

4.1.5.1 Density

Density is seen as a crucial factor because polymer composites are thought to be

lightweight and attain higher strength to weight ratio than metals and ceramics. The
density of the polymer composite is especially dependent on specific densities of
reinforcement and matrix, the void content and their respective volume fractions.
The measure of bulk density is weight to volume ratio that can be written as:

Density(ρ) = m/v (4.10)

where “m” is the mass and “v” is the volume, and both of them can be measured
through the weighing scale and measurement equipment. Another way to find out
the density of the material is the Archimedes principle. According to Archimedes’
principle, when an object is submerged in a liquid, its apparent weight reduces by
a quantity equivalent to the weight of the liquid that is being displaced. As a result,
density can be calculated using Eq. (4.11), where the mass of the substance/material
in immersion liquid and air.
mA
ρA = ρL (4.11)
[mA − mL ]

where “mA ” is the mass of substance in air, “mL ” is the mass of substance in immersion
liquid, and “ρL ” is the density of the immersion liquid. Although it can be used to
determine the bulk density of the polymer composite, it is not preferred for the
exact density because the polymer composite is a two or more phase material that
contains different constituents with differing densities and volume fractions. Thus,
the equation for the two phase polymer composite can be expressed as following
Eqs. (4.12) and (4.13) of each of the parts:

ρc = ρf vf + ρm vm (4.12)

1
ρc = mf (4.13)
ρf
− mm
ρm
126 M. Chaparia et al.

4.1.5.2 Particle Size

• Particle size is very important in processing, handling, and performance of

polymer raw materials and final products. The size and shape of the raw compo-
nents indicate the flow behavior in the feeding system in a manufacturing operation
as an element of raw material handling. The kind of feeder needed to effectively
transport raw materials from preservation to the processing machinery and the
produced material again to the station is determined by the size and shape of
the particles. For proper handling, various feeder types are needed for materials
including liquid colorants, powders, cylindrical or spherical resin pellets, and
glass fibres. The processing features of polymers are influenced by the particle
size, so that bigger pellets might need more energy or melting time, whereas
very small pellets can melt swiftly. The overall performance of parts is also
affected by particle size. For instance, smaller particle sizes are desirable for faster
absorption of drug in healthcare while bigger ones take more time to completely
dissolve in the solvent. Numerous studies have shown that nano-fillers can be used
in much smaller ratios than micro-fillers to achieve similar reinforcing effects.
However, nanoparticles need special handling, processing, and safety procedures
as well as precise apparatus for appropriate dispersion in the polymer matrix. The
standard test technique for determining the particle size of plastic substances
by employing a mechanical sieving apparatus is described in ASTM D1921.
According to the standard, using an antistatic agent is necessary for substances
that are likely to produce static charge in order to minimize coarse bias. Schlappa
et al. [52] used emulsion polymerization to develop high-solid-content (12–55%
w/w) polystyrene and polyvinyl acetate diffusion of polymeric particles with
an average particle diameter of 50–500 nm. Both approaches were investigated
using common methods for determining particle size, such as static light scattering
(SLS) and dynamic light scattering (DLS), and their results were then compared
with inline PSD (particle size distribution) observations made using PDW (photon
density wave) spectroscopy on undiluted samples. The study demonstrated that
there is a good agreement between analysis techniques when comparing particle
size observations of undiluted polystyrene dispersions. Vinayagamoorthy et al.
[53]investigated the influence of particle size on the physical and mechanical
characterizations of limestone (0.2, 0.4, 0.6, 0.8, 1 mm size particles) and jute-
reinforced polypropylene composite, and found best behavior for composites with
particle size of 0.6 mm and 0.8 mm.
4 Characterization Techniques of Polymer Composites 127

4.1.6 Electrical Characterization

One of the significant areas of interest for polymer composites is electrical appli-
cations. For monitoring large scale composite structures electrical inspection tech-
niques (such as electrical impedance or electrical resistance methods) are most suit-
able techniques as they are fast, low-cost real-time techniques. Electrical characteri-
zation of a composite material refers to the material’s behavior in an electric condi-
tion. Whenever a field is applied, free electron/charge carrier movement takes part and
due to this there is material response in terms of electrical behavior. Different mate-
rials exhibit different electrical behavior i.e. some composite material exhibits better
electrical characteristics than the others. Polymer composites with different electrical
behaviors are very important in selecting materials for various defer motives.

4.1.6.1 Electrical Conductivity

Conductivity of any material exhibits the ability of that material to pass an electric
current or signals through itself. It is basically the movement of free ions/charges/
electrons that move freely. In case of metals and semiconductors, electrons play the
crucial role as charge carriers, while for ionic compounds ions acts as charge carriers.
Conductivity is affected by temperature as it is directly proportional to temperature.
The reason behind this dependency is that when temperature is increased then the
kinetic energy of free charges also increases resulting in fast movement of free charges
which enhances the conductivity and acts inverse in decreasing temperature. There
exist very few conductivity measurement techniques that are basically categorized
into two techniques, one is contact method which contains two types of techniques i.e.
2-point probe and 4-point probe, and the other is the non-contact method i.e. inductive
conductivity method. Mironov et al. [54] prepared the graphite/polypropylene and
graphite/polyvinylidenefluride (PVDF) composite, and studied the electrical conduc-
tivity. The comparative electrical conductivity is measured by the four-electrode
(FE) and four-point probe (FPP) method for PVDF composite bar samples with
varying graphite/carbon filler concentration. Here, the FE method provides better
conductivity for the composite compared to the FPP method because of surface
roughness and structural non-uniformity of the conductive polymer composite. Prior
researcher has stated that FPP approach is not advised for any polycrystalline mate-
rial because “localized impurity segregation at grain boundaries in polycrystalline
material may result in large resistivity variations”. Gong et al. [55] fabricated carbon
nanotube (CNT)- epoxy based polymer composites and characterized the effect of
CNT agglomeration on electrical conductivity by using the four-point probe method.
Here, CNT was chemically treated with a strong acid to improve the dispersibility
and then mixed with epoxy to make a CNT-polymer mixture which was degassed in
a vacuum oven before being injected in molds. The electrical conductivity measure-
ment was taken by four-point probe technique (ASTM F1529-97) for CNT-epoxy
based polymer composite samples where conductivity exhibited rapid increased
128 M. Chaparia et al.

values from 10–14 S/m to 10–5 S/m with increasing CNT concentration. Cheng et al.
[56] reviewed the studies on ECT (eddy current testing) of CFRP (carbon fiber-
reinforced plastic) composites which comprises several unidirectional carbon fiber/
epoxy plies that have been piled together. Mook et al. [57] employed a HF (high
frequency) eddy-current sensor to identify small faults such as delamination, impact
damage, matrix rich layers, and fiber orientation. The ECT system for CFRP detec-
tion typically consists of a function generator, lock-in amplifier, power amplifier, a
2D stage, and PC to collect data and control stage. In order to successfully extract
the minor signal change caused by the weak conductivity of CFRP, the sensitivity
and gain of the lock-in amplifier should be strong enough.
(1) Contact Method
2-point probe and 4-point probe are two well-known and mostly used contact tech-
niques. In the 2-point probe system, a known current or voltage is applied to the
material while two electrodes are attached to the opposite side of a material, typi-
cally a rectangular prism or rod. In the 4-probe technique, the two inner probes assess
the voltage drop those resulting from applying a current between the two outer probes
(As shown in Fig. 4.21). This method has benefit over the 2-point probe that it can
get rid of the contact resistance present in the 2-point probe technique. It should
be emphasized that, in contrast to four electrodes, the four-point probe approach is
created for materials with excellent uniformity, such as homogenous silicon wafers
or thin films that are deposited [58].
(2) Inductive Conductivity Method
In inductive conductivity measurement (Fig. 4.22), an electrode less conductivity
meter or toroidal conductivity meter is used. Inductive conductivity meters have

Fig. 4.21 Schematic diagram of a 2-point probe and b 4-point probe system
4 Characterization Techniques of Polymer Composites 129

Fig. 4.22 Schematic diagram of inductive conductivity meter [60]

a corrosion-resistant casing in which 2 metal coils are present. One coil known
as the drive coil generates the alternating voltage and the remaining coil acts as
the receiver, and the material which will be measured acts as the core. Drive coil
generated voltage induces a voltage in the receiving coil which results in the flow of
current in proportion to the material’s conductivity. The induced current and voltage
in the receiving coil is correlated to conductivity. The material with conductivity
greater than 15 micro siemen/cm works best with inductive conductivity in meters.
One of the most popular non-destructive investigation methods that doesn’t require
any physical contact between the test sample and sensor is eddy current testing (ECT),
which may be used to inspect electrically conductive materials at very high speed
[59, 60].

4.1.6.2 Dielectric Measurement

Polymer composite dielectric systems are developed in response to the demand for
high energy density pulse power energy storage devices [61]. These systems combine
the processability and breakdown field strength of polymers with their high dielectric
constants to create a composite material. Dielectric characteristics comprise complex
permittivity (εr ) and complex permeability (μr ). And, a complex permittivity and
complex permeability contain a two constituents’ part. Here, we will discuss about
the complex permittivity that possesses the imaginary part known as the dissipation
factor and the real part known as the dielectric constant. Dielectric constant is a
measure of amount of energy stored in material when an external field is applied.
There are many methods to measure complex dielectric characteristics and each
method attains its own constraints such as materials, specific frequency, applications
etc. However, many measurement instruments are being used to measure dielectric
parameters based on the application. The instrument that offers accurate calculation
of the electrical parameters for the unknown material in the required frequency
130 M. Chaparia et al.

range might be taken into consideration. Designing of the sample holder plays a very
crucial part in measuring accurate dielectric characteristics. Dielectric properties in
low, medium and high frequency ranges are reviewed by Field et al. [62]. For the very
low frequency range, electrode polarization phenomena will be in consideration. For
higher frequency ranges, coaxial sample holders are modeled. For the microwave
frequency range, transmission line, free space, and resonant cavity techniques are
being used. Suresh et al. [63] investigated the electrical permittivity of P(VDF-
TrFE)-CuO nanocomposites using an coaxial probe technique in the microwave
frequency range which provides non-destructive and broadband observations. Where,
the increase in the nanofiller concentration up to 10 wt% in the composite results
in a reduced value of permittivity. Willert-Porada et al. [64] tested three different
composites in the laminate structure glass-polyurethane, polypropylene-glass and
woven carbon-fiber with the polymer using three different methods which are coaxial
probe, SPDR and cavity perturbation. By investigating permittivity, they found that
cavity perturbation provided the less value of permittivity as compared with SPDR
and coaxial probe. For frequency in MHz range, Meena et al. [65, 66] prepared
CoFe2 O4 /MWCNTs/epoxy and BaFe2 O4 /MWCNTs/epoxy composites with varying
ferrite concentration and investigated dielectric properties using the LCR meter in
the frequency range from 40 Hz to 4 MHz. The dielectric measurement techniques
(Fig. 4.23) are as follows:

Fig. 4.23 Types of dielectric

measurement techniques
4 Characterization Techniques of Polymer Composites 131

(1) Coaxial Probe Method: This is a non-destructive testing approach also known
as “open ended coaxial probe method”. A conventional coaxial probe measure-
ment set-up comprises of an impedance or network analyzer, coaxial probe
and specific software. Reflection coefficient is measured through the vector
network analyzer (VNA), where, the electromagnetic field (EM field) encoun-
ters an impedance mismatch between the polymer composite sample and probe
resulting in reflection along coaxial line where the EM field is propagating. And,
these reflected signals (reflection coefficient) are measured and converted into
permittivity values at different frequencies. This method is most commonly used
due to its minimal sample handling, broad frequency range, and both in vivo and
ex vivo measurements. Temperature controlled environment can be accessible
while measuring the parameter. This method is limited to provide reflection
measurement only.
(2) Transmission Line Method: In this method, a specimen is placed in a coaxial
line or waveguide section, and the transmission line is attached to VNA through
two ports that provide the scattering parameters which are S11 (reflected signals)
and S21 (transmitted signals). To determine the variation of the scattering
parameter this method uses the electromagnetic wave reflected and transmitted
through the samples [67]. The complex permittivity (dielectric characteristics)
is then evaluated by converting these scattering parameters. There are mostly
two conversion methods—Nicolson-Ross-Weir (NRW) and NIST interactive
conversion methods. To obtain the direct calculation of complex permittivity
from S-parameters, the NRW method is used. The transmission line method
covers the large frequency range at low temperature.
(3) Free Space Method: This method covers the measurements on flat and large
materials under high temperature in a wide band frequency range. In this set-up,
two antennas are connected to VNA while facing each other and a sample holder
is placed between both the antennas. The measurement of S-parameters will be
taken once without the testing material on the sample holder and once with the
testing material on the sample holder. The impact of the sample holder can be
eliminated with the use of the de-embedding function of the network analyzer,
leaving only scattering parameters for transmission and reflection coefficient of
the mounted test material to be computed. Ample sample thickness is able to
avoid multiple reflections between the sample and antenna. Time domain gating
can be used to eliminate the energy diffraction caused by the edge of the antenna
and also the multiple reflections. To ascertain the dielectric characteristics, a
program can be used to post-process the measured transmission and reflection
coefficient.
(4) Resonant Method: This method obtains permittivity with more accuracy than
the others while having the limitation on frequency and loss properties of the
materials. Resonant methods have so many types such as reentrant cavity, cavity
resonant, split cylinder resonator etc. This section contains a general technique
used in the cavity resonator. There are two resonant methods that are mostly used.
All permittivity measurements and measurements of medium to high loss mate-
rials can be done using perturbation methods, and a measurement on low VNA
132 M. Chaparia et al.

MUT is a low loss measuring technique. However, the perturbation method is

well suited when employing TM cavity design. To ascertain the dielectric prop-
erties, it is possible to monitor the quality factor and resonance frequency of
resonance characteristics dependent on MUT in a cavity. For dielectric charac-
teristics, the first measurement can be done by measuring the quality factor and
resonant frequency of an empty cavity. And, the second measurement is taken
when MUT is inserted into the cavity. The frequency, Q-factor and volume can
then be used to compute the material’s permittivity. This kind of measurement
does not require calibration of the network analyzer. Any field modifications
while the sample is inside the cavity will cause the observed resonant frequency
or Q-factor to shift. This measurement needs to be done using a network analyzer
that has a high frequency resolution. With the use of the resonator technique,
the device being studied either becomes the resonator itself or a component of
a resonant structure. Resonator techniques are typically employed to measure
capacitance and the dielectric constant in the high frequency range that involves
injection of current or voltage into an L-C resonant circuit. A conventional
capacitor-containing oscillatory circuit tuned to resonance, and the appropriate
capacitance value is then calculated. The circuit then tuned to resonance once
more by adding a capacitor with the dielectric in parallel with the conventional
capacitor.
(5) Parallel Plate Method: In this method, dielectric properties of the measured
dielectric material depend on electrical and physical parameters, frequency of
interest and the level of accuracy. In the parallel plate method, the substance
being measured is placed between the conducting parallel plates of a capac-
itor, which also serves as a sample holder. This approach needs an impedance
analyzer or LCR meter to measure capacitor impedance. The real and imaginary
components of the dielectric constant are then calculated using the measured
capacitance and dissipation factor (dielectric loss). With a frequency range of up
to 1.8 GHz, this approach has high accuracy with minimal sample preparation
and set-up requirements. For thin flat samples this techniques works best. The
knowledge of length, width, and thickness of the material and plates as well as
the capacitance and dissipation factor of the measured material are helpful in
calculating the dielectric constant of a material. The dielectric constant for the
measured material can be calculated using the following Eq. (4.14):

tCp
εr = (4.14)
Aε0

where, t is thickness of the sample (m), Cp stands for parallel capacitance of the
sample (F), A stands for the area of the electrode’s surface (m2 ) and ε0 stands for
permittivity in vacuum or free space (8.854 ×10−12 F/m).
4 Characterization Techniques of Polymer Composites 133

4.1.6.3 Dielectric Strength and Breakdown

The electrical strength of an insulating material is referred as its dielectric strength.

An applied field (maximum voltage) strong enough to break down the insulating
properties of an insulator that allows charge flow through the material (breakdown)
is measurement of dielectric strength expressed as Volts per unit thickness [68].
Material with high dielectric strength is proven to be better electrical insulator. To
measure the dielectric strength, there exist three basic standard testing methods: the
short-time methods, the slow rate-of-rise method, and the step-by-step method. All
the methods use the same set-up to testing, where the test specimen is placed between
two well aligned electrodes in a sample holder. After placing the sample carefully,
the sample holder is mounted in an air/insulating oil bath. Some researchers inves-
tigated the dielectric breakdown strength of the polymer composite [69, 70]. Song
et al. [69] prepared BaTiO3 incorporated PVDF (polar) or epoxy (non-polar) compos-
ites modified by Dopamine where BaTiO3 was used as nanofibers and nanoparticles
correspondingly with the polymer matrix and Dong et al. [70] prepared the poly-
imide composite with inclusion of polydopamine coated graphitic carbon nitride.
They investigated the dielectric breakdown strength of the polymer composite by
using Dielectric Wihstand Voltage Test. Stoyanov et al. [71] investigated the break-
down strength of carbon black/rubber composite using a (Trek-model) high voltage
amplifier.
(1) Short-time Method: It is a conventionally used test method for quality control
tests. In this method, the voltage across the two electrodes is gradually increased
at a constant rate (500 V/sec) until a breakdown occurs. It is a longer time taking
test.
(2) Slow rate-of-rise method: In this method, the electrodes of test are subjected
to a voltage that starts at 50% of breakdown voltage and lasts until breakdown
happens.
(3) Step-by-step: In this method, the test electrodes are exposed to the appropriate
initial voltage over the specified time until breakdown takes place.
The dielectric breakdown test (Fig. 4.24) is standardized by JIS C2110, ASTM
D149, EC 60243-1, etc.

4.1.6.4 Impedance Measurement

Impedance spectroscopy is used to measure impedance of any composite that consists

of applied alternating voltage and wide frequency range. The voltage response of the
material is recorded and after that the resultant impedance can be used to define the
electrical characteristics of the polymer and its composites.
Impedance spectroscopy is a versatile and effective method for analyzing the
relationship between grain boundaries, gain, and electrode–electrolyte interface. This
approach explains the electrical conduction phenomena in the presence of an external
applied field (AC input signals). All impedance response exhibits a low frequency
134 M. Chaparia et al.

Fig. 4.24 Schematic diagram of dielectric breakdown test

spike with a high frequency semicircle where the low frequency spike represents the
generation of a double layer capacitance at interface as a result of low frequency
ion migration, and the high frequency semicircle represents the parallel arrangement
of a resistor and a capacitor. The intercepts on the x-axis of the impedance plot are
used to calculate resistance. The impedance has the same SI unit (ohm) as resistance
but differs from resistance in a way that it has both phase and magnitude whereas
resistance possesses only magnitude.
There are various impedance measurement techniques based on different factors
such as measurement range and accuracy, operating frequency and ease in measure-
ment. Bridge method is one of methods used in standard laboratory that covers
DC to 300 MHz frequency range. This method is of low cost with high accuracy
in the wide frequency range based on different types of bridge but it needs to be
manually balanced. Resonant method is used in high Q device that covers 10–
70 MHz frequency range but it needs to be tuned to resonance that provides low
impedance measurement accuracy. I-V method is suitable for probe type tests for
grounded device measurement in the 10–100 MHz frequency range that limits its
operating voltage based on the transformer used in the probe. RF I-V method is
used for RF component measurements, which cover 1–3 GHz with high accuracy
and provide wide impedance range at high frequency. Network analysis method
is used in RF component measurements at any frequency above 300 kHz with high
frequency range, and provides good accuracy when characteristic impedance is close
to unknown impedance. Auto balancing bridge method is applicable for generic
component and grounded measurement, and provides high accuracy over a wide
impedance range for 20 Hz to 110 MHz frequency, as shown in Fig. 4.25.
The study of impedance allows us to distinguish the real and imaginary part of the
complex impedance which gives the structure property relationship of [72, 73]. By
changing the applied frequency in an EIS measurement, a significant number of infor-
mation is attained. The Nyquits and Bode plots are two graphs that are mostly used
4 Characterization Techniques of Polymer Composites 135

Fig. 4.25 Various impedance measurement techniques

to adequately depict this complex dataset [74]. Markevich et al. [75] presented the
electric impedance spectra of CNTs-reinforced polyethylene polymer composite in
the frequency range from 0.1 kHz to 0.12 GHz using the concept of a double electrical
layer between the electrolyte and electrically conducting composite by EIS measure-
ment technique. Helseth et al. [76] investigated the impedance spectra of MWCNTs-
PDMS (polydimethylsiloxane) composites and found that experimental results are
well fit by an electrical RC-circuit with a single relaxation time, and force-dependent
capacitances and resistances. Ilgaz et al. [77] presented the impedance properties
of SWCNT/VE (single walled carbon nanotube/vinylester) glass fiber-reinforced
polymer composites in the frequency range from 10–2 to 107 Hz at temperature from
300 to 420 K. They obtained Nyquist and Bode plots of impedance and interpreted
the performance by Cole–Cole technique.
Complex Impedance:

Z ∗ (ω) = (Z ' − jZ '' ) (4.15)

Here, Z' = |Z|Cosθ and Z'' = |Z|Sinθ, where θ is phase.

√
|Z(ω)| = Re(Z(ω))2 + Im(Z(ω))2 (4.16)
136 M. Chaparia et al.

(1) Nyquist Plot-Equivalent Circuit Method

The presented equivalent electrical circuit here is Randles circuit (Fig. 4.26), which
involves Ru , charge transfer resistance (Rct ) and impedance Zw called the Warburg
impedance.The plot between the real component Z' (resistive terms) and the imag-
inary component Z'' (inductive and capacitive terms) serves as the foundation for
depiction of impedance data which is evaluated by Nyquist plot (Cole–Cole plot),
which uses the formalism given in Eqs. (4.17) and (4.18) [78, 79].

Rct + σ ω− 2
1

Z' = Ru + 2 2
(4.17)
(σ ω 2 Cdl + 1) + ω2 Cdl 2 (Rct + σ ω− 2 )
1 1

2
ωCdl (Rct + σ ω− 2 ) + σ 2 Cdl + σ ω− 2
1 1
''
−Z = 2 2
(4.18)
(σ ω 2 Cdl + 1) + ω2 Cdl 2 (Rct + σ ω− 2 )
1 1

Fig. 4.26 Nyquist plot of equivalent Randles circuit

4 Characterization Techniques of Polymer Composites 137

Each point in the Cole–Cole plot represents impedance corresponding to the

magnitude and direction of the vector at a specific frequency. Nyquits plot exhibits a
semicircular arc with an offset from the point of origin that corresponds to resistance,
Ru [80]. Where, Ru is the resistance of the solution, Cdl is the capacitance of the
electrical double layer, Rct is the charge transfer resistance, and Z w is the Warburg
impedance which expresses mass transfer.
The reactance is very high (Xcdl >> Rct + Z w ) at low frequency (ω → 0), Z'' =
−1
ωCdl
is very high therefore the whole current will flow through Ru , Rct and Z w . In
this frequency region mass transfer phenomena is dominated in the electrochemical
process.
Thus the Eqs. (4.19) and (4.20) will be

Z' = Ru + Rct + σ ω− 2
1
(4.19)

Z'' = −σ ω− 2 − 2σ 2 Cdl
1
(4.20)

By solving both equations,

Z'' = Z' − Ru − Rct + 2σ 2 Cdl (4.21)

For −Z'' = 0, a straight line can be seen in low frequency range with slope 1
(θ = 45◦ ), which intercepts the real axis (x-axis) at

Z' = Ru + Rct − 2σ 2 Cdl (4.22)

−1
When Rct >> Z w is taken into account at high frequency (ω → ∞), Z'' = ωC dl
is
very low and thus Ru , Rct and Cdl all act to impede current flow. In this frequency
region charge transfer phenomena is dominated in the electrochemical process.
By solving the equations under considerable condition, we obtain:
( ) ( )2
' Rct 2 ( '' )2 Rct
Z − Ru − + Z = (4.23)
2 2

Therefore, varying Z' with respect to Z'' results in a semicircle plot with radius of
Rct
2
and its centre at Z' = Ru + R2ct and −Z'' = 0.
Thus, the Randles circuit exhibits resistive behavior at both low and high frequen-
cies, and the values of Ru and Ru + Rct can be discovered as the semicircle’s real axis
intercepts.
(2) Broad Band Dielectric Response Method
Broad band dielectric response method known as “bode plot” is another method used
to measure impedance, here, impedance is plotted between magnitude to impedance
and frequency. Normally, Impedance magnitude and frequency are plotted on log
138 M. Chaparia et al.

Fig. 4.27 Bode plot for Randles circuit

scale (log |Z| vs log ω), while phase angle is plotted linearly. Bode plot for equivalent
Randles circuit is shown in Fig. 4.27.

4.1.7 Rheological Characterization

The term “Rheology” is derived from the greek word “Rheologia” i.e. “Rheo” means
flow and “logia” means study of. Under the effect of stress, a material’s body experi-
ences flow and deformation that is known as rheology and the type of deformation is
influenced by the conditions of material’s body [78, 81]. Elastic deformation occurs
in an ideal solid (known as Hooke solid), which means that if the force is removed the
solid will revert to its initial state. In this instance, the required energy for deformation
will be recovered once the stress is ended. Rheology has evolved to cover a wide range
of topics, with substantial advancements achieved in fields like suspensions, coating
and polymer rheology. According to particular needs, rheological additives can vary
the viscosity, flow and deformation characteristics. Rheology also contributes in
providing information of polymer extrusion and how the process of deformation in
impacted by temperature. Viscometers and rheometers have advanced in simulating
industrial and handling situations to assess the performance of materials as a func-
tion of stress level and temperature. The polymers are usually melted or softened
into rubbery or liquid form to get in appropriate shape and then cured (solidified)
4 Characterization Techniques of Polymer Composites 139

to sustain those shapes. The flow behavior of polymer melts is able to process the
polymeric material into any form therefore melt flow behavior of polymeric materials
plays a crucial role in understanding polymer processability. Several works [81–86]
have been reported on rheological characterization of polymer composites. Lim et al.
[87] investigated the nonlinear behavior of polymer composites in the presence of
high magnitude oscillating shear flux. In order to investigate the polycaprolactone/
MWCNTs nanocomposites in (COGA) flux, they employed a variety of analytical
techniques. According to zero deformation nonlinearity and deformation magnitude,
they estimated the nonlinear component through the rheology of the Fourier transfor-
mation. By increasing MWCNTs content, they were able to compare nonlinear and
linear viscoelastic characteristics. Lewandowski et al. [88] studied the rheological
behavior of wood-polymer composite (WPC) with polypropylene using capillary
rheometer with shear rate of 10 s−1 to 912 s−1 . They found that with increasing
wood flour amount, the viscosity and the flow rate of the substance comprising of
the WPC matrix, and the loss of pressure of composites corresponding to entrance
effects are reduced by a significant amount.

4.1.7.1 Viscosity

The term viscosity reflects the resistance to flow which is considered a critical flow
characteristic of the polymeric material. Various viscosities of different polymer
composites or materials are advantageous in many applications such as putty and
sealants are higher in viscosity and paints are lower in viscosity (As shown in
Fig. 4.28). In polymeric composites processing, a different viscosity of the mate-
rial is required as low and high viscosity have their own need while working with
different polymers’ processing requirement. Low viscosity is required in injection
molding for filling the thin walls and voids, while high viscosity is needed in blow
molding and extrusion. The methods to measure viscosity are as follows.

(1) Capillary Viscometer

This method measures the viscosity of Newtonian fluids with more accuracy. Through
this capillary, time taken for a fluid to flow can be measured. The measurement of
viscosity using an appropriate capillary viscosity is done at a temperature of 20 ±
0.1 ◦ C, unless otherwise specified. In this technique, bulb (A) is filled with enough
of liquid being tested to fill the viscometer through tube (L), bringing the liquid to
20 ◦ C beforehand unless otherwise specified but made sure that the liquid level in
bulb (B) is below the exit to the ventilation tube (M). Unless otherwise specified,
viscometer is placed in the water bath of temperature 20 ± 0.1 ◦ C, kept upright, and
allowed to stand for at least 30 min to allow the temperature to stabilize. The liquid
level in the tube (N) should be raised to a level that is about 8 mm over the mark (E)
before tube (M) is closed. By closed tube (N) and open tube (M) the liquid level can
be maintained. To the nearest one-fifth of a second, time required is measured for
the liquid level to fall from mark (E) to (F), with the open tube (N).
140 M. Chaparia et al.

Fig. 4.28 Various methods to measure viscosity

(2) Rotational Viscometer

The idea behind the technique is to measure the torque or force experiences while it
rotates in a liquid at a constant angular speed. Shear-independent viscosity is used
to measure the viscosity of Newtonian liquids, while shear-dependent or apparent
viscosity is used to measure the viscosity of non-Newtonian liquids. There are two
categories of rotating viscosities that are absolute and relative viscometer. The flow
within the measuring geometry is clearly defined by absolute viscometers while the
flow in the measuring geometry is not defined in relative viscometers.
(3) Falling Sphere Viscometer
This viscometer works on “Höppler” principle and uses falling sphere to measure
the dynamic viscosity of transparent Newtonian fluids. The fluid to be examined
is contained inside a cylindrical tube that is inclined and contains sphere rolls and
slides. The time it takes for the sphere to fall a certain distance throughout the fluid
by the measurement tube directly determines the viscosity which is expressed in mPa
s. In order to assess how long the sphere requires to drop back, the tube with it can
then be inverted upside-down.
(4) Vibrational Viscometer
Vibrational viscometer generates waves inside the liquid in order to function. The
Hydramotion technique uses shear waves since viscosity is a shear measure that
may only be accurately in shear conditions. In vibrational viscometer, a constant
displacement magnitude is applied to the vibration of an oscillator that is placed in
4 Characterization Techniques of Polymer Composites 141

a liquid. The power required for the vibration can be observed, and this can be used
to determine the viscosity of the liquid.

4.1.7.2 Melt Flow Index

In this technique, a thermoplastic polymer’s ease of melting is measured. It is

described, when the polymer (in gms) flows in ten minutes across a die with a
particular length and diameter under pressure from a specific weight at a specific
temperature, both ISO 1133 and ASTM D1238 describe the procedure. Low molec-
ular weight is correlated with a high melt flow rate, which is an indirect measurement
of molecular weight. Melt flow rate also serves as a measure for how well melt of
material flows under pressure. To measure melt flow rate, Melt Flow Index test
(Fig. 4.29) is conducted in which the material is loaded in the melt flow index tester
at a temperature higher than its melting point. This tester contains of an inner die
and outer zone, and both are electrically heated. After loading the sample within the
inner die it takes some time to melt entirely. The screw punch then begins to descend
at a consistent speed while the melt flow indexer is turned on, pushing the melting
polymer out of the opening at the bottom of the die. The time it takes to flow out the
10 gm of polymer across the die is used to compute the melt rate. Several material
features, including processing behavior, stability, long term viscoelastic behavior
throughout end usage, etc., can be predicted using the melt flow rate. As a result, it
is a crucial quality control factor for many plastic and polymer products. Therefore,
the melt flow index test is carried out to determine whether the polymer material is
suitable to utilize.

4.1.7.3 Shear Stress

In order to evaluate the shear stress, the rheometer works on “shear mode”. This
rheological system consists of a coaxial clamp and a cylindrical heating furnace that
can be sealed. The coaxial clamp (parallel plates clamp) is connected to a mechan-
ical testing arrangement to manage the shear rate throughout the test. To take the
measurements, the furnace is preheated to 180 ◦ C (experimental temperature) and
then the furnace is turned on to fix the parallel iron plates with the sample to the
fixture; and finally, the furnace was turned off and the temperature is maintained for
15 min so that the sample melts completely.

4.1.8 Thermal Characterization

Thermal analysis evaluates the kinetic and thermophysical characteristics of the

material with respect to temperature i.e. it investigates the reaction of a substance
when being cooled or heated. The properties of a material can be estimated with time
142 M. Chaparia et al.

Fig. 4.29 Schematic

diagram of melt flow index
testing

or temperature. The most frequently used temperature dependent analysis techniques

(Fig. 4.30) are differential scanning calorimetry (DSC), thermogravimetric analysis
(TGA), and differential thermal analysis (DTA) [89–91].
TGA measures the sample mass in a controlled environment furnace as a function
of temperature or time. DSC observes that when temperature varies chemical reac-
tions and phase transitions produce heat effect. Finally, by observing the sample’s
behavior towards temperature, DTA can detect and investigate the composition of
a material. Dweck et al. [92] developed and investigated the thermal characteris-
tics of polymeric composites. The TG/DTA characterization were performed under
temperature from room temperature at 800 ◦ C. In this technique, samples from
the composite’s top, bottom, centre, and lateral side were obtained to examine the
uniformity of polymer distribution. The polymer concentration of the composite can
often be easily calculated from the overall area that comprises the corresponding
DTG peaks because of its burning in oxidized environment analysis. Thamer et al.
[93] reported thermal characterization techniques for epoxy/hexagonal boron nitride
composites such as TGA, DTA and DSC, and the results exhibited enhanced thermal
stability of nanocomposites. They used Coast-Redfern technique to analyze the
deformation at 10 ◦ C/min constant heating rate in air by obtaining TGA and DTG
curves.
4 Characterization Techniques of Polymer Composites 143

Fig. 4.30 Various thermal characterization techniques

4.1.8.1 DSC

It measures the heat flow rate (mW = mJ/sec) difference between the inert reference
and material sample (between reference pan and sample pan) with varying tempera-
ture and time. Absorbed heat by the sample is a response of the endothermic process
while released heat by the sample is the response of the exothermic process. Heat
flows through the sample material can be the response of heat capacity (heating),
Glass Transition (Tg ), melting, evaporation or other endothermic processes. And,
released heat out of the sample can be the response of heat capacity (cooling),
crystallization, curing, oxidation, or other exothermic processes. In this technique,
temperature for the sample material and reference both are kept same throughout the
experiment. According to DSC analysis designed temperature program, the temper-
ature of the sample holder should rise linearly with time. As for the reference sample,
it should have a precise heat capacity over the temperature range that will be scanned.
The reference sample material must also maintain its stability, high purity and lack
of significant change during the temperature scan. Indium, bismuth, lead, and tin
are typically in use as reference standards, although additional standards such as
polyethylene and fatty acid are suggested for the study of polymers and organic
molecules, respectively. There are two mostly used DSCs that are Heat-flux DSC
144 M. Chaparia et al.

involving heat flux difference between the reference and sample material and power
differential DSC that involves the difference of power supplied to the reference and
sample material.

4.1.8.2 DTA

Differential thermal analysis (DTA) is an alternate of DSC that is quite similar to

DSC. Herein, the difference in temperature is the result of phase change and other
processes as reference and the sample material is heated equally. In this technique,
the reference and sample material are arranged uniformly in a furnace. Here, the
sample and reference temperatures are varied in the furnace which is controlled
by a temperature programme. In order to measure the difference in temperature
between the reference and sample, a differential thermocouple is arranged as shown
in Fig. 4.30(1). Additionally, the thermocouple on the sample side is used to measure
the temperature of the sample material. Reference materials are substance that does
not change in the measuring temperature range (often-alumina). As the furnace starts
heating up, a slight delay is found in starting of heating of the reference and sample
material due to their individual thermal (heat) capacity and finally they both heat
up gradually in accordance with the temperature of the furnace. After the heating
starts, ΔT varies until a static condition is attained, and then it changes until it
achieves stability that is consistent with the difference in thermal capacity between
the reference and sample material. The baseline is the signal that is in a stationary
state. For instance, as the temperature increases and melting takes place in the sample
material, then rise in temperature stops and ΔT rises as shown in Fig. 4.30(2a). When
melting stops, ΔT reaches the peak and the temperature curve quickly returns to the
baseline. This allows us to determine the reaction temperature and sample transition
temperature from DTA signal (ΔT signal) as shown in Fig. 4.30(2b).

4.1.8.3 TGA

TGA evaluates weight change of a sample material as a function of temperature.

It is a potent and reliable method for investigating stability and variation in the
weight of a material. This change in weight of a sample though heating (at constant
rate) can be attributed to a particular reaction of a material towards a thermal stress.
This technique is ideal for in-depth investigation of breakdown temperatures and
confirming that a material functions properly within a specific temperature range.
In this process, sample and the weighing mechanism are exposed to a carrier gas.
Through gas–liquid or gas–solid reactions, carrier gas can interact with sample mate-
rial while also protecting the internals from oxidation or corrosion above 500 ◦ C.
Reducing environment can be helpful in preventing the oxidation of a specific mate-
rial or can discover the gas–solid phase reduction processes. Exploring metal organic
framework or porous materials that are catalytic is made easier with this method.
4 Characterization Techniques of Polymer Composites 145

4.2 Optical Characterization

According to Shirakawa et al. [94], Macdiarmid [95], and Heeger [96], conducting
polymer polyacetylene can be employed as a dopant to the material that influences
conductivity of the doped material. Since then polymers are the widely investigated
materials for optoelectronic applications. The electronic and optoelectronic mate-
rials are in great attention due to their implementation of different optical func-
tions, including modulation, switching, generation, and optical waveguide struc-
ture detection generated on the substrate. Polymers are appropriate material for
optoelectronics and photonic applications. Optical characteristics are one of the
most crucial characteristics for investigating the electronic properties of polymer
composites [97–99] that are shown in Fig. 4.31. These methods depend on either the
nonlinear optical characteristics of the polymer composite or the movement of elec-
trons from HOMO (highest occupied molecular orbital) to the LOMO (lowest unoc-
cupied molecular orbital). Ananda et al. [100] performed UV–visible spectroscopy
on PVA/Gly:Na2 SO4 composite film to validate the characteristics absorption with
regard to sodium sulphate content for 300 to 800 nm wavelength. From the UV/
Vis absorption spectra, they observed higher transmission percentage for PVA/Gly
which reduced with sodium sulphate content. The decrease in transmission value
indicated variation in optical band gap attributed to structural change in the polymer.
Larosa et al. [101] prepared polycarbonate (PC)/MWCNTs composite and performed
UV–Vis spectroscopy by double beam configuration in the 300–700 nm wavelength
range. They observed that the prepared composite exhibits absorption band at around
289 nm. In this section, optical measurement techniques to characterize the polymer
composites are discussed.

4.2.1 UV–VIS Absorption

A method for measuring electromagnetic wave absorption as a function of wavelength

and frequency is called absorption spectroscopy. The variations in the absorption
spectra can be used to analyze the interaction between radiation and electrons that is
caused by the absorption process. There are several literatures [102–104] on appa-
ratus and technical elements of absorption spectroscopy that conclude that the sample
holder, monochromator, light source, and optical detector are four fundamental parts.
In general, a single or double beam is used by absorption spectrophotometer from
which a single beam is compatible and easy to use, and the double beam comprises
two beams that split into two optical pathways. In the double beam system, the first
splited beam travels through the reference, while the second splited beam travels
though the sample. The double beam provides more precise, stable and accurate data
over the single beam system.
146 M. Chaparia et al.

Fig. 4.31 Schematic diagrams of optical spectroscopy

In the UV–VIS absorption process, the intensity of incident light reduces when
passing through the medium. The absorbed intensity by the sample can be evaluated
by Lambert–Beer laws as shown in Eq. (4.24).

I = I0 e−αt (4.24)

where I0 represents intensity of the incident light, I is the transmitted light, α is the
absorbance coefficient that is the measurement of how strongly the light is absorbed
by the sample at some particular wavelength, and t is the sample thickness. This
equation represents the exponential decay of light intensity with respect to thickness
of the sample.

4.2.2 Optical Reflectometry and Ellipsometry

Optical reflectometry is contactless and non-destructive and that involves interac-

tion between sample and reflected light. Reflectometry is inexpensive and simple
because the system employs non-polarized light to serve as light source i.e. tungsten
4 Characterization Techniques of Polymer Composites 147

bulb. While, ellipsometry involves the impact of polarization of light to investigate

the optical characteristics therefore the instrument must handle delicately to observe
the polarization state variation. Ellipsometer consists of some essential parts that
are optical source, analyzer, polarizer, detector and phase inducer, where UV-based
deuterium light serves as the light source. There are numerous different types of
polarizers, including calcite, wave plate, linear, and wire grid polarizers that change
the particular polarization state into an elliptical, plane, right, or left circular polariza-
tion. Phase inducers such as wave plate, phase modulators, and compensator serve to
attain specified elliptic polarization. A polarized-type analyzer investigates the light
which reflects from the sample. Optical reflectometer and ellipsometer measurements
are used to attain thickness of the film sample and optical constant.

4.3 Conclusion

Characterization of composite materials is an essential step in the formation of

new products. The characterization of polymer composite materials confirms that
advanced composite materials fulfill the application performance standards through
the industrial perspective. By physical and chemical characterization, quality control
can be ensured to expand the understanding of materials and products. In conclusion,
various techniques can be utilized for characterizations of polymer-based compos-
ites which includes mechanical, tribological, microstructural, structural, physical,
electrical, rheological, thermal and optical properties.

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