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JIEC 4051 No. of Pages 11

Journal of Industrial and Engineering Chemistry xxx (2018) xxx–xxx

Contents lists available at ScienceDirect

Journal of Industrial and Engineering Chemistry

journal homepage: www.elsevier.com/locate/jiec

Review

A review on thermomechanical properties of polymers and fibers

reinforced polymer composites
N. Saba* , M. Jawaid*
Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra Malaysia, Selangor, Malaysia

A R T I C L E I N F O A B S T R A C T

Article history:
Received 19 May 2018 Polymer composites offered broad engineered applications, however their diversity get restricted owing
Received in revised form 17 June 2018 to fluctuations in thermomechanical properties during heating or cooling hence great concern required
Accepted 18 June 2018 prior their applications through thermomechanical analysis (TMA). Traditionally, TMA or dilatometry
Available online xxx found to be simple, ideal, reliable, sensitive, excellent and basic thermal analytical technique. TMA
provides valuable information on thermal expansion, glass transitions temperature (Tg), softening
Keywords: points, composition and phase changes on material of having different geometries simply by applying a
Polymer composites constant force as a function of temperature.
Thermal stability
This compilation highlights the basics and experimental of TMA for both research and technical
Thermomechanical analysis
applications and also provide literature on TMA of polymers, hybrid composites, nanocomposites and
Coefficient of thermal expansion
their diverse applications.
© 2018 Published by Elsevier B.V. on behalf of The Korean Society of Industrial and Engineering
Chemistry.

Contents

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Polymers and nanocomposites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Thermal analysis (TA) and thermal stability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Thermomechanical analysis (TMA) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Glass transition temperature (Tg) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Thermal expansion coefficient (CTE) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Basic and principles of TMA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
TMA experimental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
TMA measurements and applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Thermal expansion of thermosetting and thermoplastic polymers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Thermomechanical analysis of polymer composites and nanocomposites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Declarations of interest . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00

Introduction

Polymers and nanocomposites

Polymers possess high specific strength, excellent chemical

stability, electrical insulating properties, better processability and
* Corresponding author at: Biocomposite Technology Laboratory, INTROP,
Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia. low cost [1]. Polymers are widely been applied in the fields of
E-mail addresses: jawaid@upm.edu.my, naheedchem@gmail.com (M. Jawaid). electronics, biomedical, energy and manufacturing industries from

https://doi.org/10.1016/j.jiec.2018.06.018
1226-086X/© 2018 Published by Elsevier B.V. on behalf of The Korean Society of Industrial and Engineering Chemistry.

Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
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past decades. However, the intrinsic low thermally conductive
coefficient and insufficient thermal stability of polymeric matrix
restricted its broader application in the field where good heat
dissipation and low thermal expansion are required [1]. Linear
thermoplastics and thermosets are two major types of polymers
used in advanced polymer composite industries, although they are
quite different from each other. Thermoplastics are ductile, poor
creep resistant, tougher and usually exists in semi-crystalline or in
amorphous phase and on heating beyond the Tm or Tg, they lose
their structure to more deformable and flexible structure [2,3].
Thermoplastics show reshaping and reforming prospects by
simply cooling or heating. While, thermosets are less susceptible
to solvent than thermoplastics, highly flammable, combustible and
crosslinked polymer, hence remain in the solid state such as phenol
formaldehyde, epoxy, polyester or vinyl ester resins [3,4].
Thermosets high crosslinking reactions are usually accompanied
by a sharp change in the material’s mechanical properties such as,
an increase in tensile modulus accompanied by the shrinkage [5].
Polymer composites are the advanced materials alternative
to traditional materials such as metals or ceramics and consist of
at least two constituents of different phase, one of them being
continuous polymeric matrix phase and other is reinforcements
(fibers, filler). Polymer composites possess improved properties
such as tensile/impact strength, stiffness, wear resistance,
thermal conductivity, thermal insulation, corrosion resistance,
weight/temperature dependent behavior and fatigue life.
Polymer composites can be categorized in three sub-classes,
including particles, fibers and structural based composites,
displayed in Fig. 1 [3].
Nanocomposites belong to the groups called nano materials,
where a nanoparticle is dispersed into a polymeric matrix [6]
Nanocomposites structure is usually more complicated and its
properties are determined by the same factors as in traditional
composites [7]. They are defined as a multiphase, high-perfor-
mance dense heterogeneous solid material of 21st century, where
one of the phases has dimensions in the nanometers (10
9 m)
ranges and have extremely large specific surface area and aspect
ratio with respect to microcomposites [8]. Nanocomposites are
characterized by unique characteristic including no fiber rupture,
homogenous structure, optical transparency, better clarity and
unchanged processability [9]. They offer diverse applications in the
cosmetics, medical sciences, food packaging, construction, domes-
tic goods, automotive and many other advanced polymer
composite based industries in contrast to traditional materials.
Thermosetting polymers have several advantages over thermo-
plastic polymers such as higher strength/stiffness, lighter weight
as well as creep and thermal resistance behavior [10]. Though,
thermal expansion is another important physical property for
Fig. 1. Classification of polymer composites [3].
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
polymers that governs their processing and applications, critically
based on the chemical structures [11]. Remarkably, thermome-
chanical behavior and thermal stability of thermosetting polymers
and their composites are quite adequate to be used for varied
applications ranging from coatings, electronics, packaging, adhe-
sives fiber reinforced composites, structural components in aircraft
and aerospace industries [10]. These properties depend on various
factors, including the polymer chemistry, molecular structures,
cross-linking, curing tendency, thermal stability and degree of
polymerization [11].
Thermal analysis (TA) and thermal stability
TA is an important key laboratory technique for industries
based on inorganic and organic chemicals, pharmaceuticals, foods,
petroleum, polymers, polymeric composites and many others. TA
typically used to measure weight loss, heat flow and dimensions
change/mechanical properties as a function of temperature
[9,12,13]. It also characterized the properties including decompo-
sition, crystallization, melting, molecular structure, viscoelastic
behavior, Tg, cross-linking, oxidation, volatilization, coefficient of
thermal expansion (CTE), tensile modulus, composition, process-
ing, stability and mobility (http://www.tainstruments.com/prod-
ucts/thermal-analysis/#ffs-tabbed-11). Currently wide TA
techniques are being known that are widely established including,
thermogravimetric analysis (TGA), differential thermal analysis
(DTA), differential scanning calorimetry (DSC), dynamic mechani-
cal analysis (DMA), thermomechanical analysis (TMA) and
pyrolysis combustion flow calorimetry. Their properties and unit
are tabulated in Table 1.
Furthermore, thermal resistance, durability and heat resistance
often been described by thermal stability. In current scenario
polymer based industries shows a growing interest to obtain
polymers with increased thermal stability [14,15]. Polymers of
higher thermal stability are usually characterized by higher
softening/melting temperatures (Tm), higher thermal decomposi-
tion, high residual mass content and minimal considerable
changes in physical, mechanical and chemical properties besides
higher heat deflection temperature under load, during short or
long exposure to elevated temperature.
Thermomechanical analysis (TMA)
Emergence of modern TMAs brings a renaissance in the last few
years of thermal analytical techniques and is found ideal for
teaching, research and quality control applications, with incom-
parable performance. Commercial application of TMA on polymers
in 1948 grew from hardness to penetration and become a key
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Table 1
Various thermal technique and their properties with unit.
TA measurement technique Abbreviation
Differential thermal analysis DTA
Differential scanning calorimetry DSC
Thermogravimetric analysis TGA, DTG
Thermomechanical analysis TMA
Dynamic mechanical analysis DMA
*
Thermocouple electromotive force.Source: https://www.hitachi-hightech.com/global/products/science/tech/ana/thermal/descriptions/ta.html.
thermal technique in which samples, either polymer or any
polymer composites undergoes distortion/changes under non-
oscillating stress against temperature/time in a specified atmo-
sphere. Interestingly, until now TMA remains as one of the most
elementary tools for material and polymer science as it can
efficiently and accurately detect any possible transitions and
dimensional changes even at the nanometer level [16] for varieties
of liquids, pasty materials or solid as a function of temperature or
time under a applied mechanical force (ASTM D696, ASTM D3386,
ASTM E831, ISO 11359, DIN 51 005) https://www.netzsch-
thermal-analysis.com/en/products-solutions/thermomechanical-
analysis/. It has been further reviewed by researchers that TMA
technique perfectly assembled valuable information on the
dimensional properties such as expansion and contraction of a
thermoset (pure or reinforced) during curing [17]. Research study
elaborated that TMA can effectively be used either alone or in
conjunction with other commercially available TA techniques such
as DSC, TGA, DMA or thermo-conductivity [18], as it is highly
sensitive and more accurate for spotting Tg of polymers and highly
cross-linked materials like, brake linings, polymer composites and
printed circuit boards in comparison to traditional DSC. TMA
believed to be highly sensitive and profound than any other
analytical techniques for characterizing physical and chemical
properties of polymers, composites and nanocomposites materials
that are undetectable [18]. TMA can also be used to measure creep
and creeps recovery of polymeric materials simply by loading and
unloading the samples over periods of time. From few decades,
TMA consequently developed into a strong, reliable, authentic and
powerful technique in analytical laboratory for both research and
applications sectors.
Fig. 2. Glass transition of polymeric mateiral.
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
3
Property Unit
Difference temperature 
C or mV*
Enthalpy W = J/sec
Mass Gram
Deformation Meter
Elasticity Pa = N/m2
Glass transition temperature (Tg)
Glass transition temperature (Tg) is an important physical
properties of material (thermoset polymer) which marks a change
in mechanical behavior or the initiation of phase changes. It is
usually defined as the temperature region where the polymer
shows transitions from a glassy, hard material to a soft, pliable and
rubbery material [19,20], shown in Fig. 2.
Thus Tg describes the temperature beyond which the sample or
polymer is in the rubbery stage and below that the polymer is in
the glassy or in brittle stage. The glassy region is marked by high
stiffness and interlocking bonds along with restricted molecular
chains movement while rubbery region marked polymeric chains
mobility on exposure to higher temperature [21]. Remarkably
depending on the requirements, some polymers have applications
below or some have above the specific Tg. Research study declared
that Tg is however notably different from Tm, as at melting point
the sample under investigation starts to melts while at Tg sample
get softer [20]. Besides the dimensional change of a material, Tg
can also be monitored and measured by using a TMA instead of
DMA and DSC. Comparative determination of Tg from DSC, DMA
and TMA techniques are displayed in Fig. 3. Excitingly, Tg of a
material can be obtained from a CTE curve (TMA graph) by
observing the intercept of the two curves of a plot between
temperature versus displacement [20], described in Fig. 4.
Thermosets polymer above the Tg behave as a highly viscous
liquid or ductile solid but below the Tg material behave as a hard
and brittle solid. Among many thermosets, like epoxies, polyesters
and vinyl, epoxies are one of the most important thermoset
polymers and are highly cross-linked in the cured state. Cured
thermoset (epoxies) are highly crosslinked hence on heating at
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Fig. 3. Comparative Tg from TMA, DSC and DMA thermal techniques.
Fig. 4. Plotting Tg from TMA.
higher temperatures they does not melt or reflow (unlike
thermoplastic), instead shows small softening. Literature reported
that epoxies can be used explicitly depending on the required
applications either at above or below their Tg [20].
Thermal expansion coefficient (CTE)
When a material is subjected to higher temperature thermal
expansion is an important phenomenon in many applications.
They usually undergo thermal expansion, however rarely certain
materials undergoes contraction upon heating, this phenomena is
called negative thermal expansion (NTE). A large positive thermal
expansion (PTE) is useful in thermal actuators and medical vessel
dilators that operate based on human body temperature [22]. NTE
is useful for canceling the thermal expansion of ordinary materials
in high-temperature or high-precision devices [22]. Such NTE is
isotropic and shows no hysteresis [23]. These materials perceived
great industrial demands as they has tendency to control or reduce
the thermal expansion of other materials, usually achieved by
doping Ge or Sn metals [23]. The development of high performance
fuel cells and thermoelectric converters immensely required the
technology of regulating thermal expansion [23]. Currently a wide
variety of NTE materials as filler are known that can lower or
reduced the higher thermal expansion of polymer to zero CTEs or
some time negative, leading to opens a new milestone in
composite science and technology [24,25]. The well known NTE
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
are antiperovskite manganese nitrides, antiperovskites, beta-
eucryptite (LiAlSiO4), ZrW2O8 [25], iron perovskite (SrCu3Fe4O12)
[26], Bi1
xLnxNiO3 (Ln: lanthanoid) [27,28], β-eucryptite/silicon/
carbide [29] and La(Fe, Si, Co)13 [30].
Thermal expansion is an important thermal property to define
the promising end use application and to model residual stresses in
a polymer composites [31]. TMA is a highly sensitive technique for
the determination of both thermal expansion and contraction of
cured/filled polymer composites [17]. Researchers revealed that
thermal expansion coefficient is the fundamental and critical
physical property of solid materials generally used to define the
change in dimension of material with temperature, thus affects the
processing and applications of polymer composites [23,32].
Thermal expansion would be linear or non-linear, remarkably it
would be linear if the material does not shows phase transition
with the temperature and this linear expansion is called coefficient
of thermal expansion or the CTE, perceived by TMA http://www.
andersonmaterials.com/tma.html. CTE is a thermal property
calculated above and below the Tg and regarded as the
temperature dependent normalized number that describes the
material mechanical expansion or contraction at different temper-
atures. It is usually expressed as a coefficient per unit temperature
interval at a given temperature or in units of per degree Kelvin
(K
1) [32,10] and are usually defined as α, calculated by using the
Eq. (1) [23,33].
DL
a¼ ð1Þ
L DT
Where, L = initial length of sample.
Researchers also illustrated that based on the volume and
temperature data from computer simulations such as Quantum
mechanical, Monte Carlo (MC), Molecular dynamics (MD), Meso-
scopic and Continuum, or macroscopic scale simulation, CTE can
also be determined from Eq. (2) [34].
u = 1/V0 (@V/@T) P (2)
Where P is the pressure, V is the volume, T is the temperature of
system and V0 is the volume at a specific temperature.
Notably, until now several mathematical model expression
based on finite element and analytical micromechanical approach
for effective CTE determination was postulated [35]. Among
analytical micromechanical approaches, concentric cylinder model
(CCM) applied to investigate the thermal expansion response of
the long fiber reinforced composites [36], Voigt model which
assumed the existence of a uniform strain in the composites after
the imposition of a uniform temperature change. While, Reuss
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model which assumes the prevalence of a uniform stress in the
composites after a uniform temperature change and the well-
known Turner’s model, used for effective composites CTE
investigation which usually account inter-particle interactions
with moderate inclusion volume fractions [37,38].
CTE governs the effects such as crystallization, solid–solid
transitions and softening besides the promising applications of a
polymer matrix and provides valuable insight in their composi-
tion. Research study reported that CTEs varies inversely with a
Young’s modulus [39]. It is also inversely proportional to the
bond strength of the material and hence governs their melting
point. In the case of polymers the thermal expansion depends
mostly on intermolecular forces. Moreover, as the bond length
between atoms is almost independent of temperature a polymer
possess lower thermal expansion than the respective low-
molecular liquid (monomer). Below Tg the polymer thermal
expansion is much lower since the polymer chains are closely
packed with strong intermolecular forces, empirically, αrubber
 2.5αglass. Polymers with weak, secondary and intermolecular
bonds (low Tm) possess high CTE while materials like metals,
(high Tm) and ceramics are strongly bonded have low CTE, also
low Tm metals have high CTE values. Additionally, isotropic
materials have same CTE in all directions and anisotropic materials
have different CTE for each direction such as, graphite fibers
reinforced epoxy composites shows three distinct thermal
expansions corresponding to the x, y, and z directions. In isotropic
material such as an amorphous polymer, the volumetric expansion
coefficient is in average three times the linear expansion
coefficient αv  3αL http://www.intertek.com/analytical-laborato-
ries/thermal-analysis/. Research study also reviewed that lower
dimensional stability signifies higher CTE values while higher
dimensional stability with temperature governs lower CTE [40].
Lower CTE values materials such as quartz and glass take the
advantages for use in solder joints failing, optical instruments,
motors binding and composites splitting on bond lines. Thus CTE is
an important material property, particularly when the composites
are subjected to a temperature-changing environment, thus a
major comprehensive and elaborate study on the thermal stability
and CTE of fiber reinforced polymer composites are essential
requirements [36].
Fig. 5. (a–c). (a) TMA instrument (b) block diagram of TMA and (c) Mounted sample [41].
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
5
Basic and principles of TMA
TMA is a very sensitive micrometer, closely related to
dilatometry (vertical dilatometer) and its basis involves the
accurate investigation of material dimensional (length) change
as a function of temperature under a defined mechanical force or
negligible load (e.g. DIN 51 045). The basis of TMA instrument
involves a heat sink, furnace with temperature control system,
thermocouple to measure the temperature of sample and flush of
nitrogen gas in environmental chamber [41]. TMA instrument,
block diagram and mounted sample on TMA stage are shown
respectively in Fig. 5(a–c) [41]. TMA instruments precisely apply
forces and measure dimensional changes even at a nanometer
scale, under controlled temperature, time, force and atmosphere.
Moreover, changes in the free volume (vf) of a material are
measured with TMA instrument very accurately by the absorption
or release of heat associated with that change.
TMA experimental
TMA instrument consists of an analytical route that accurately
and precisely determine the position calibrated against known
standards [42]. Experimentally, sample is inserted into the furnace
touched by the probe, provided with thermocouple to measure the
temperature and also connected with the force generator and
linear variable differential transformer (LVDT) for length detector.
Changed in the furnace temperature having sample by applying the
force from generator via probe are recorded. Deformation in
sample with changing temperature such as thermal expansion and
softening is measured as the probe displacement through the
length detector. Several types of the TMA instrument probes
(illustrated in Fig. 6.) such as tension, penetration, expansion,
bending, shrinkage, creep and swelling are currently available.
These probes are critically depends on the variety of sample
geometries used such as fibers, rods, films or cylinders and the
requirements on the measurement purpose. Table 2 listed the
different types of probes and their measuring properties.
Notably, most TMA is a TA technique having the ability to ramp
stresses at variable rates and used to run flexure tests on rubbers
and plastics to determine the Young’s modulus [41]. However, a
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Fig. 6. TMA geometries for testing.
Source: https://www.linseis.com/en/our-products/thermomechanical-analysis/tma-pt1000/.
Table 2
Different types of TMA probes for different materials geometry.
Probes Measuring properties
Expansion/ Deformation by the thermal expansion, CTE, Tg, and
compression compression modulus
Penetration Softening temperature, melting behavior and Tg
Tension Thermal expansion, thermal shrinkage, intrinsic material
properties and viscoelastic parameters
3-Point Bending properties and distortion temperature
bending
TMA cannot be used to test the mechanical strength of metallic
samples because the applied forces are extremely small. Presently,
all TMA instruments are manufactured with the multiple models
along with latest technology and processes for highly sensitive
research and development (R&D) to provide high quality assur-
ance, reliable and reproducible results data.
TMA measurements and applications
TMA applications are the simplest, reliable and sensitive among
the other existing TA techniques. TMA have wide applicability and
can precisely measure multiple material properties through
standard operating modes either by Q400 or the Q400EM.
Moreover, the Q400EM also deals with creep, stress relaxation,
stress/strain, dynamic TMA and modulate TMA modes http://
www.tainstruments.com/wp-content/uploads/BROCH-TMA-
2014-EN.pdf. Thermal expansion curve or TMA plot can effectively
be used to investigate Tg of a polymer or polymer composite
materials as the polymer shifts from glassy to rubbery state with a
dramatic change in free molecular volume in terms CTE change as a
function of temperature at constant pressure or as a function of
pressure at constant temperature [17].
Interchangeable probes at varied loads are being used by TMA
dilatometer to analyze or measure different properties including
the compression modulus, softening temperature, shrinkage, Tg,
crystallization, CTE, tensile modulus, thermal expansion, Tm,
crystalline phase transition temperature, crystalline to amor-
phous transition temperatures, warping, creep and stress relaxa-
tion under load by measuring the material dimensional change by
keeping temperature, time and applied force as variable functions
(http://polymerdatabase.com/polymer%20physics/tma.html).
TMA instrument easily, explicitly and rapidly measures heat flow,
weight loss and mechanical properties besides evaluating varied
intrinsic material properties like sample displacement (growth,
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
Nature of materials Probe adjustments
Solids and soft or irregular samples, Probe rests on a sample on a stage with minimal
powders and films downward pressure
Extremely for characterizing thin –
coatings
Film, plugs, powders and fiber (quartz Movement of the probe is measured electrically
glass, alumina, and metals) by a LVDT attached to the probe
Stiff materials and composites –
shrinkage, movement etc.). It also found to be highly profound in
providing required data dealing processing, production condi-
tions, product performance parameters, composition, stability,
molecular structure, application possibilities and mobility for
various materials as a function of time or temperature under
applied force. TMA also measures several intrinsic viscoelastic
properties like polymers blend tensile modulus, polymer mor-
phology, viscosity and copolymers along with some processing
properties like phase behavior, flow modeling, foaming, polymer-
ization, cure and crosslinking. TMA provides valuable insight on
swelling behavior, polymer blends, polymer morphology, volu-
metric change during sinter process evaluation and phase
transformation on array of samples of different sizes and shapes.
Moreover, the application diversity of TMA instruments prolongs
from quality control to R&D that required designing motors and
food products processing items like chips and bread. The most
typical domains of TMA applications include many industries
based on plastics, laminates, elastomers, pharmaceuticals, dental
waxes, food processing, inorganic and organic chemicals analysis,
agriculture, electronics, elastomers, textiles, ceramics, carbona-
ceous materials, adhesives, paints, dyes, fibers, organics, cos-
metics, films, glass, metals, automotive, construction materials,
aviation, aerospace, polymers and polymer composite materials.
Besides this, TMA acquires its remarkable position in textile,
mining and heavy duty industries. Researchers reported that
thermoset polymer composites having low CTE, high temperature
stability and flexural strength in combination with cost effective-
ness are gaining huge attention as a potential metal substitutes for
many structural applications [43]. Recently research study
clarified that thermal stability effectively be exploited to
contemplate the structural insight of polymer nanocomposites
and hybrid composites that offer numerous applications in the
aerospace, automobile, architecture, constructional, electrical,
electronic and heavy appliances [44].
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Thermal expansion of thermosetting and thermoplastic Table 3

CTE of epoxy and nano materials.
polymers
Polymer/materials CTE in  C
Thermal expansion property is the major physical property Epoxy 45–75 ppm/ C
when a polymeric materials structure are exposed in a tempera- Silica 0.5 ppm/ C,
ture changing environment based on conformation, chemical Boron nitride 0.5 ppm/ C
Alumina 6.6 ppm/ C
structures and bond strength within polymers [32]. Generally
Diamond 0.8 ppm/ C
polymers have minimum CTE value in the range of 30–40 ppm K
1
and highest over 100 ppm K
1 which is quite more than those of Source: https://polymerinnovationblog.com/fillers-action-reducing-coefficient-
metals and ceramics, which has CTE in the range of several to thermal-expansion-thermosets/.
20 ppm K
1 [24]. Thus large thermal expansion of polymer
represents the most primary factors that suppressed their nearly to 1. On the other hand, boron nitride (BN) filler results fast
industrial value [24,38]. Research studies reported that polymers CTE reduction at relatively lower contents, on account of high
having flexible linkages and bent bonds display large values of CTE aspect ratios. Incorporating high contents of silicon nitride or fused
compared to rod like polymers consisting of rigid segment and silica fillers in the polymer can also results low CTEs [43].
extended bond. Thermosets like epoxies, on curing form three Remarkably, effective CTE reduction also been observed by
dimensional networks and high crosslinking dense material at adding diamond and alumina fillers which shows transitional
sufficiently low temperatures. They possess lower CTE in glassy or value between the silica and BN, however in many polymer
solid state below Tg, while CTE increases in rubbery state beyond composite applications, diamond is generally not been used as it is
Tg. This change can be ascribed on the basis that the crosslinking relatively expensive. Table 3 evidently revealed that cured filled
restrain the Brownian motion of the polymeric chains in the glassy epoxies possess three dimensional network and highly branched
state, leaving only small vibrations to happen, while in rubbery structures with relatively small thermal contraction and expansion
state an increase of free volume, Brownian polymeric chain in response to different temperature ranges. Incorporated fillers in
movements and decrease in density are observed resulting thermosets possess different thermal expansions with respect to
increase in CTE values [8,45]. Thus cured thermosets polymers the matrix and generally shows no volumetric shrinkage during
beyond Tg get converted to more flexible and pliable state due curing, while thermosetting polymer undergoes volumetric
enormous increase in polymeric chain mobility which thereby shrinkage due to the formation of solid network having covalent
alter several changes in physical properties like reduced stiffness in bonding, all this leads to internal stresses in the material, altering
rubbery state, that can be measured through dynamic force based its conductivity, thermomechanical response and rheology [55].
TMA [5]. Research studies explored that the thermal expansion and All this broadens the industrial applications of cured filled epoxy in
Tg of thermoset polymer frequently changed by incorporating or the advanced structural composites, microelectronics, space
adding small quantity (in low contents) of nano fillers, such as vehicles, marine vessels and optical devices [5]. CTE of some of
carbon black, calcium carbonate, nano metal oxide, nano-graphite the most common thermoplastics applicable in polymer compo-
[46], talc, nanoclay [47], carbon nanotubes (CNTs) [48], organically sites are listed in Table 4.
modified clays (OMMT), montmorillonite (MMT), magnesia,
mesoporous silica [49], alumina or other filler materials [50]. Thermomechanical analysis of polymer composites and
The noticeable change in thermal stability, Tg and thermal nanocomposites
expansion reveal the effectiveness of using these nano fillers to
reduce the residual stress in the polymer composites [40,48]. It can Natural fibers reinforcement substituted the use of conven-
be explained by the fact that the CTE for nano materials are tional or synthetic fibers in polymer composites to developed eco-
relatively lower with compared to unfilled/unmodified polymer composites and bio-composites in order to meet the alarming
[51–53,17]. Potential reduction in linear and axial CTE also been demand of green products among consumers [14,56]. Fibers
observed by incorporating graphite nano-platelet (GNP) in the reinforced polymer composites are the inexpensive, advanced
composites [50]. With the same 2D geometry, the GNP effectively engineered and commercially available materials that are required
lowered the CTE of composites as relative to nanoclay reinforced in hi-tech applications due to their contrapuntal properties [57].
polymer composites, besides improving other functionalities such
as optoelectronics and electrical conductivity to the composites Table 4
[50]. CNTs also regarded as promising candidate to minimize or to CTE of most common thermoplastics polymer used in polymer composite
lowered the CTE to zero of variety of polymer and metal materials industries.
to fabricate composites since CNTs have small (even negative) CTEs Thermoplastic polymers CTE value in  K
[39]. It has also been explored that experimental CTEs of CNTs
PE (Polyethylene) 180–200
greatly depend on the axial and radial alignment because the CNTs PP (Polypropylene) 200
were dispersed randomly in the matrix [54]. CTE reduction in PTFE (Polytetrafluoroethylene) 135
polymer nanocomposites accounts for reduction of polymer chain PVDF (Polyviylidenefluoride) 130
segmental motion due to the hindrance offered by the incorpo- PTFE (Polytetrafluoroethylene) 112–125
Acetal 110
ration of nano filler like OMMT [40] and CNTs. Moreover, research Nylon 50–90
study marked that CTE of MWNTs is negative; hence the well PVC (Polyvinylchloride) 70
dispersed and functionalized MWNTs incorporation reduces the PC (Polycarbonate) 65
CTE of composites. While extent of CTE reduction for nanoclay PETP Polyester 60–65
PSU (Polysulphone) 60
based composites greatly depends on the particle rigidity, efficient
PPSU (Polyphenylenesulphone) 55
stress transfer to nanoclay layers, high aspect ratio and degree of PEEK (Polyetheretherketone) 25–50
nanoclay platelets dispersion in the matrix [17]. CTE of some of the PPS (Polyphenylene Sulphide) 50
most common nano filler reinforcement in epoxy is tabulated in PEI (Polyetherimide) 45
Table 3. From Table 3 it is evident that they play an important role PAI (Polyamide-imide) 25–30
PBI (Polybenzimidazole) 25
in minimizing CTE reduction. Spherical silica nanoparticles are the
most common, least expensive filler and possess lower aspect ratio Source: http://www.engineershandbook.com/Tables/plasticthermalexp.htm.

Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
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Recently, addition of nano materials even in a lower content to the
polymer composites system showed a considerable improvements
in mechanical, thermal and thermomechanical properties without
altering the composition, processing and weight of the composites
[58,59]. Several research findings has been reported showing the
effect of incorporated natural/synthetic fibers in polymer compo-
sites on physical, mechanical, thermal and dynamic properties.
Although thermal expansion is one of the most sensitive issues
which must be explored or studied in order to extend the outdoor
and high-end applications through thermal techniques besides
physical, mechanical and dynamic properties. Notably, the
polymer, hybrid or nanocomposites materials normally undergo
changes in dimension and thermomechanical properties during
heating or cooling, thus it is quite important to analyze their CTE.
Moreover in laminated composites, CTE exclusively rely on the
orientation of fibers, fiber volume fraction, nature of polymer
matrix and other filler reinforcement [31]. Thus accurate
determination of CTE or thermal expansion is essential, as a low
CTE and good thermal stability are necessary to expand the use of
composites where temperature changes dramatically and vigor-
ously, such as composite coatings on the surfaces of aircraft,
aerospace craft, microelectronics submarines and buildings [60].
However until now a very minimal report or studies has been
conducted, to explore the effect of fibers or nano materials
reinforcement in polymer/hybrid composites on thermal expan-
sion and CTE. Some of the most remarkable work is reviewed here
which deals the thermal expansion analysis through TMA
techniques, which generate accurate, reliable and reproducible
data on CTE, Tg and Tm. Recently, CTE of epoxy and nano epoxy
composites were investigated by TMA where oil palm nano filler
were incorporated in epoxy at different weight (1%, 3%, 5%) by hand
lay-up to fabricate epoxy nanocomposites in both rubber and
glassy regions [61], shown in Fig. 7 [61]. Researchers observed that
on increasing oil palm nano filler content upto 3% CTE of the epoxy
composites decreases but beyond 3% it slightly get increased.
The increased CTE value for the 5% loading can be ascribed to
poor dispersion and agglomeration of the added filler particles,
creating free space for polymer segmental motion. Interestingly
TMA graph also shows that all oil palm nano/epoxy composites
present lower thermal dilatations than the epoxy composites in
both regions, revealing the existence of synergy between the oil
Fig. 7. TMA graph of epoxy and epoxy nanocomposites [61].
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
palm nano filler and epoxy polymer, indicating improved
dimensional stability and CTE compared to pure epoxy composites
[61]. Researchers in other study investigate and compared the
thermal expansion behavior by TMA of fumed silica nanoparticles
having particle diameters of 12 and 40 nm reinforced in bisphenol
E-cyanate ester [62]. They observed that addition of silica lowered
the CTE value of all nanocomposites compared to pure cyanate
ester, which is in agreement with Schapery’s upper limit and Shi’s
model. Further TMA indicates that 12 nm silica nanocomposites
displayed lower CTEs than the 40 nm for equal volume fractions. In
other study oxidized multi-walled carbon nanotubes (MWCNTs)
functionalized with Fe3O4 (Fe3O4/O-MWCNTs) with good magnetic
properties are used to modify epoxy for cryogenic applications
[63]. They observed that ordered Fe3O4/O-MWCNTs effectively
reduce CTE of epoxy composites along with it also improved the
mechanical properties. Recently, thermomechanical properties of
cellulose nanofibers of having diameter of 70–90 nm derived from
dry softwood (Pinus sp.) and hardwood (Eucalyptus sp.) cellulose
waste reinforced unsaturated polyester resin (UPR) are investigat-
ed [64]. Furthermore, poly-urea elastomer nanocomposites based
on inorganic MoS2 nanotubes and Mo6S2I8 nanowires were
fabricated and their Tg were analyzed through TMA [65]. TMA
results depicts that the incorporation of nanoparticles in extremely
lesser amount leads to increase in Tg as compared to the pure
elastomeric matrix. In other study raspberry-SiO2 (R-SiO2) nano-
particles were prepared and reinforced in epoxy to fabricate R-
SiO2/epoxy composites by a solvent free curing process and their
CTE were investigated through TMA [66]. TMA result shows that
addition of R-SiO2 particles is effective filler to increase both Tg and
to decrease CTE of the epoxy composites. Remarkably, in another
study polyethylene (PE) composites are reinforced with different
low fractions (0.5–4 mass %) of vinyltrimethoxysilane (VTMS)
functionalized Al2Mo3O12 by micro-compounding and their CTE
were calculated and compared by TMA, described by Turner’s
model and ultrasonic method [67]. TMA tests indicate a consider-
able reduction in CTE of polymeric materials without altering any
notable physical properties. Result analysis declared 46 %
reduction in CTE by loading only 4% nano filler compared to PE
revealing the existence of strong filler matrix interaction, better
Young’s modulus and thermal stability [67]. Moreover, researchers
also evaluated the effects of thermal expansion on shape memory
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performance of polyurethanes and their organoclay, carbon
nanofiber, carbon black and silicon carbide reinforced nano-
composites through Kerner and Halpin phenomenological models
[68]. They claimed that thermal expansion exerts negative effect
on recovered strain and it depends on the magnitude of
temperature gradient, CTE and the level of tensile strain. Recently
in other study attempt were made to incorporate axially aligned
MWCNTs in epoxy composites to determine axial CTE over the
temperature range
10 to 90  C, using Turner’s model at lower
volume fractions, for the production of zero CTE composite
materials for use in electronic devices [39]. CTE investigation
revealed that nanotube CTEs tended to become less negative with
increasing temperature. Since MWCNTs possess high Young’s
modulus, aspect ratios and large negative CTE, which is relatively
less with compared to conventional negative CTE materials [39]. In
other findings polymer composites filled with NTE antiperovskite
manganese nitrides materials were fabricated by injection
molding, and their thermomechanical properties were investigat-
ed [24]. In another work researchers reported the processing of
polymer derived ceramic tapes (polysiloxane) filled with
ß-eucryptite and/or SiC [29]. They claimed that developed material
possess sufficient mechanical stability (flexural strength and
young’s modulus) and their CTE can be adjusted from positive
to moderate negative values simply by altering filler composition.
Furthermore, in other exciting study, a predictive micromechanical
model for the evaluation of CTE based on the analytical solution
and differential scheme of particulate composites which is a
building materials, with ceramic including both solid or hollow
inclusions are gaining attention [38]. Researchers in other work
incorporated the NTE antiperovskite GaNMn3 as the conductive
materials with small particle size (0.7 mm or 2.3 mm) into the
epoxy composites based on percolation theory [69]. They revealed
that it can be a promising candidate for embedded-capacitor,
organic printed-circuit-boards and in decoupling applications
having linear CTE less than 10 ppm/K [69]. Moreover, in other study
CTE of graphene nano-platelets reinforced polyetherimide ther-
moplastic composites fabricated by injection molding are evaluat-
ed [50]. Results revealed that incorporation of graphene nano-
platelets effectively reduce the CTE of the polyetherimide
composites. In other reported study, thermomechanical properties
of epoxy filled with two silica spherical nanoparticles and
nanofibers were investigated as a function of aspect ratio of silica
filler and concentration [70]. They found that silica nanofiber/
epoxy have 1.4 times greater CTE compared to spherical silica
nanoparticle/epoxy and regarded it as potential material in
advanced electronic packaging industry and under-fill material.
In other findings, researchers fabricated the mesoporous silica KIT-
6/epoxy polymer composites as excellent low thermal expansion
material [71]. Most recently polylactic acid (PLA) reinforced with
bleached kraft soft wood (BKSW) biocomposites with fibers
content up to 35% were fabricated by injection molding and their
thermomechanical properties are investigated [72]. Result analysis
revealed a considerable reduction in thermal expansion with the
addition of cellulosic BKSW to the PLA composites both in the
glassy and rubber region most probably due to the lower CTE of the
BKSW compared with pure PLA. Recently graphene foam and
graphene sheets as filler are incorporated in pliable polydime-
thylsiloxane (PDMS) and their thermal expansion behaviors were
analyzed [73]. They observed that graphene foam/PDMS compo-
sites show much lower CTE than those of graphene sheet/PDMS
composites and pure PDMS. Researchers regarded it as attractive
and promising materials to be used in electronic and photonic
devices for thermal management. In other work, theoretical
calculations were conducted to develop a general standard or
parameter to determine the CTE using Green’s function method
and the effect of microstructural properties such as, volume
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
9
fraction, aspect ratio and the orientation of graphene fillers in
epoxy composites were evaluated [60]. They predicted that CTE of
the graphene/epoxy composites effectively get reduced by the
orientation dispersion of graphene additive. Interestingly, an
attempt were also made to fabricate high performance insulating
materials having high thermal conductivity, low CTE and low
dielectric loss from hexagonal boron nitride (hBN) and 2, 20 -
diallylbisphenol A (DBA)-modified 4,40 -bismaleimidodiphenylme-
thane (BDM) resin [74]. Result analysis revealed that with increase
in hBN content, dielectric loss and CTE gradually decreases while
thermal conductivity increases linearly, due to better interfacial
interaction between hBN and BDM/DBA resin. They further
claimed that developed hBN/BDM/DBA composites would conveys
striking probable applications in aerospace and electronics
industries as high-performance insulating materials.
Earlier researchers developed a model by using simplified
version of Lee and Westmann’s theory to envisage CTE of hybrid
composites, dealing the effect of isotropic or anisotropic fiber
materials, fiber orientation, fiber aspect ratio, hollow or solid
nature of spherical reinforcements and voids content [75].
Literature reported that based on calculation they perceived that
elastic modulus and thermal properties of short fiber/hollow
sphere composites are satisfactory enough to designed a very high
speed integrated circuit (VHSIC) board applications [75]. Remark-
ably, in other study thermal expansion of a composite materials
embedded on polarimetric fiber sensors having an acrylate coating
are fabricated and characterized for measuring strain and
temperature [76]. Furthermore, in other reported work, commer-
cial thermoset bismaleimide, bisnadimide and cyanate ester were
used to incorporate with high loading of fused silica or silicon
nitride fillers [43]. Their flexural strength, filler distribution along
with CTE, thermal stability and Tg were investigated. TMA result
declared that fused silica or silicon nitride reduced the CTEs of all
composites, however a commercial two-component bismaleimide
resin found to be attractive material having the CTE around
15 ppm K
1and Tg around 340  C. In another finding, DMA,
electrical conductivity, morphological properties along with CTE
of epoxy composites filled with spherical nano and micro flakes
sized silver (Ag) particulate filler are investigated [77]. Both
spherical nano and micro flakes Ag reinforced epoxy composites
display marked improvement in flexural modulus with increasing
filler loads, however the results are more pronounced for spherical
Ag/epoxy nanocomposites TMA analysis also revealed consider-
able reduction in CTE value for all filled epoxy composites
compared to pure epoxy composites [77]. Recently, in other study
the Tg and CTE of polymer composites were evaluated through
static force thermomechanometry and modulated temperature
thermomechanometry (mT-TM) [78]. They found that reversing
dimension change curves undergoes continuous expansion even
after Tg but sensitivity get decreased with crosslinking and fiber
content. However, non-reversing curves showed marked contrac-
tions with increasing temperature. In other study, CTEs of
unidirectional glass fibers reinforced polyimide composites con-
taining silica nanoparticles are investigated [36]. The effects of
fiber and silica nanoparticle volume fraction/properties, diameter
and aspect ratio on the CTE of polyimide hybrid composites were
explored to provide a guideline to design composites with optimal
CTEs [36]. In other findings effect of fiber content (40 wt%–60 wt%)
on the CTE of microfibrillated cellulose reinforced phenolic resin
biocomposites are investigated [79]. Thermal expansion results
shows lower CTE of 10 ppm/K at 60 wt% suggesting a strong
thermal expansion restriction rate below 60 wt% of fiber content,
signifying efficient reinforcement effect of cellulose microfibrils in
phenolic resin. Latterly, kenaf/epoxy hybrid nanocomposites were
fabricated by adding 3% oil palm nano filler, MMT and OMMT,
through hand lay-up technique and their CTE were analyzed and
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JIEC 4051 No. of Pages 11
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Fig. 8. TMA graph of kenaf composites and kenaf hybrid nanocomposites [40].
compared by using TMA (Fig. 8) [40]. Researchers evidently
observed a sharp reduction in CTE values with the incorporation of
filler to the kenaf/epoxy composites indicating minimal expansion
of kenaf fibers within epoxy matrix.
They also declared that a comparable dimensional stability or
CTE value is observed for oil palm nano filler/kenaf/epoxy with
MMT/kenaf/epoxy, although the CTE values are relatively lesser
with respect to OMMT/kenaf/epoxy hybrid nanocomposites.
Furthermore, thermomechanical properties of basalt fiber (BF)
filled high density polyethylene (HDPE) and co-extruded wood
plastic composites (WPCs) with BF/HDPE composite shell were
analyzed [80]. They reported that CTE of pure HDPE get reduced by
incorporating BF into HDPE. In other reported work researchers
fabricated composites by crosslinking UPR with methyl ethyl
ketone peroxide reinforced with the granite scrap powder at 20%,
30%, 40% and 50% by wt. and their CTE along with Tg are examined
by TMA [81]. They revealed that increasing the filler content to
granite/polyester resin blends composites reduces the CTE in all
cases. However 50% filled composites shows lower CTE value and
better thermal stability at all temperature attributed on account of
better dispersion of added filler within UPR polymer.
Conclusion
TMA is the extremely versatile and simplest TA techniques
compared to available TA technique. TMA instrument provides
valuable reproducible data with great precision on the thermal
expansion, small deformation and CTE of material placed on
platform attached with the probe, relatively more accurately and
rapidly. TMA system can perform either static or dynamic
measurements due to a built in force/frequency generator having
different probes for different purposes. TMA provides valuable
information on softening temperature, Tg, viscoelastic behavior,
crystallization and solid-solid transitions besides this it also
conveys material structure, surface integrity, roughness, molecular
composition, cure and crosslinking polymerization. TMA tech-
nique can be effectively applied to typical ceramics, carbonaceous
materials, glass, coatings and even metals over a wide range of
temperature, besides varied materials geometry in the form of rod,
fiber or film. It is also been applicable for a variety of thermosets,
thermoplastic polymers and elastomers and their polymer
composites to expand their outdoor applications as the polymers
undergoes expansion and contraction on exposure to higher
temperature, especially thermosets like epoxies. Currently TMA
offers convincing application in the different sectors ranging from
aviation/aerospace, quasi-static loading, electroplating technolo-
gy, microelectronics, constructional, cosmetics, food packaging
and in divertor industries.
Please cite this article in press as: N. Saba, M. Jawaid, A review on thermomechanical properties of polymers and fibers reinforced polymer
composites, J. Ind. Eng. Chem. (2018), https://doi.org/10.1016/j.jiec.2018.06.018
Present article highlights the immense importance of thermo-
mechanical characterization besides other TA characterizations in
the fields of advance polymer, polymer composites and material
science. This article also provides valuable information for TMA
instrument, technique and its basis of working. It also offers
valuable data regarding the elaborative TMA applications in
several industries besides polymer composites. The further study
and research work would involve the utilization of agro-industrial
wastes deposition in the fabrication of green polymer composites,
having extremely lower value of thermal expansion along with
improved physical, mechanical and thermal stability at relatively
higher temperature to compete the traditional materials like steel,
cement and metals in constructional and other structural
applications.
Declarations of interest
None.
Acknowledgements
The authors are grateful to Malaysian Industry-Government
Group for High Technology (MIGHT) for Financial support of this
work Under Newton-Ungku Omar Fund Grant No: 6300873 and
6300896.
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