Sin 2023 J. Phys. - Conf. Ser. 2523 012023

Journal of Physics: Conference Series
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18th International Engineering Research Conference 2022 (Eureca 2022) IOP Publishing
Journal of Physics: Conference Series 2523 (2023) 012023 doi:10.1088/1742-6596/2523/1/012023
The study of thermal & mechanical properties of EPDM

compounded with TiO2
K X Sin1, H Ahmad 1,2*, Hoon Yap3, Hafizul Azizi Ismail4

1
Taylor’s University Lakeside Campus, No. 1 Jalan Taylor's ,47500 Subang Jaya, Selangor
Darul Ehsan, Malaysia.
2
Digital Innovation & Smart Society Impact Lab, Taylor’s University, Subang Jaya, Selangor,
Malaysia
3
Lee Kong Chian Faculty of Engineering and Science, Universiti Tunku Abdul Rahman,
Bandar Sungai Long, 43000 Kajang, Selangor, Malaysia
4
School of Engineering, Asia Pacific University of Technology & Innovation (APU)
Jalan Teknologi 5, Taman Teknologi Malaysia, 57000 Kuala Lumpur, Wilayah Persekutuan
Kuala Lumpur
*
Corresponding author: hafisoh.ahmad@taylors.edu.my
Abstract. This study attempts to investigate the usage of titanium dioxide as a viable
nanofiller for fabrication of ethylene propylene diene monomer (EPDM)
nanocomposites used as thermal insulators. For this study, three different filler loadings
(1, 3, 5 % wt.) of titanium dioxide nanofiller are incorporated into the polymer matrix
to form the nanocomposites. The thermal and mechanical characteristics of the resulting
nanocomposites were compared to EPDM which has not been compounded with TiO2
nanofiller (neat). The thermal characteristics of the polymers were tested using
thermogravimetric analysis. Mechanical parameters of the polymers were evaluated via
tensile testing with dog-bone specimens according to ASTM D638 standards. Thermal
performance of TiO2-impregnated EPDM nanocomposites showed definite
improvements, with 1% wt. nanofiller loading having 1 °C improvement over neat
EPDM at 5% weight loss and 1 °C improvement at 50% weight loss respectively.
Tensile testing showed lower elongation at break (EB) and higher tensile strength (TS)
characteristics for nanocomposites with 1% wt. & 3% wt. nanofiller loading compared
to neat EPDM. At 5% wt. nanofiller loading, higher EB and lower TS readings were
recorded for the nanocomposite, likely resulting from uneven nanoparticle distribution
during sample fabrication due to nanofiller particle agglomeration.
Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution
of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.
Published under licence by IOP Publishing Ltd 1
1. Introduction
The use of polymeric materials in the industry have been widespread in applications such as
footwear soles, rigid housings, gasket seals etc. Polymeric materials have also attracted many
researchers as a prospective insulator, with regards to their dielectric properties, volume
resistivity, and breakdown voltage alongside its elastic capabilities. Polymeric insulating
materials offer high strength to weight ratio, low mass, and superior weather resistance
compared to conventional insulative materials like glass and ceramic, making it suitable for
replacing conventional insulators used in high-voltage power lines.[1-2]
One of the commonly used polymers as insulators are elastomers. Elastomers are a class of
polymeric synthetic rubbers that has gained popularity in the industry. Common elastomers
used for this application include silicon rubber (SiR) and ethylene propylene diene monomer
(EPDM). SiR has often been the choice material for insulators due to its thermal stability and
weather resistance but is expensive to manufacture.[1–3] EPDM is known to have excellent
weather resistance, good flexibility at sub-zero temperatures, high tensile strength and great
electrical resistance for a lower cost compared to SiR.[2] Thus, interest has been increasing
with regards to the use of EPDM as an alternative to SiR.
Further improvements with regards to the thermal and mechanical properties of the material
can be achieved with the incorporation of inorganic fillers in the material blend such as metal
oxides or metal hydroxides.[4] Elastomeric materials are rarely used alone and are often
combined with additives to improve their base characteristics. Incorporation on inorganic fillers
in the polymeric material improves resistance to tracking, withstand voltage and dielectric
response, and reduce flammability.[5] Other fillers such as plasticizers and stabilizers add
flexibility to the material and protects the mixture from degradation both during the
manufacturing process and in usage. Common fillers include alumina trihydrate, silica, carbon
nanotubes[6], graphene[5–7], organophosphorus compounds and other metal oxides. Titanium
Dioxide (TiO2) represents one of the most common fillers used commercially for a multitude
of applications such as pigments and electrical insulators. Fujishima & Honda reported that
TiO2 can be used as a photocatalyst through their experiments utilizing rutile TiO2 crystals
exposed to UV light to electrolyse water. [10] Titanium dioxide is also used in intumescent
flame retardants to increase char residue, reducing flammability by cutting fuel gases from
combustion of materials. Although some research has been conducted on the thermal and
mechanical properties of TiO2 nanofillers in polymers, not many have been conducted on
EPDM alone without any other composite polymers in its construction.
2
The focal point of this study will be to analyse the effect of different nanofiller loading in terms
of wt.% on EPDM/TiO2 blended nanocomposite material. The blended nanocomposite (TiO2-
filled EPDM) material should offer a marked improvement in thermal and electrically insulative
properties and improved mechanical strength.
The thermal stability of the EPDM/TiO2 nanocomposite material blended in different weight
percentages will be investigated via the use of thermogravimetric analysis (TGA). This method
of testing relies on constant observation of the material’s mass as it is subjected to increasing
temperatures up to 1000°C. This method of testing is widely used for testing thermal stability,
polymer decomposition and degradation, polymer lifespan estimation and effects of additives
on polymer degradation, allowing for the suitability of the material in different operating
temperatures to be tested. [11]
To determine the mechanical strength of the EPDM/TiO2 nanocomposite material blended in

different weight percentages, tensile tests will be conducted on the material. Three types of
forces: tensile, compressive and shear forces lead to the deformation of polymeric material,
with the types of deformation being stress and strain. In a tensile test, this stress-strain
relationship will be utilized to determine the strength of the material. Tensile tests are conducted
by constructing a material in a dumbbell or ‘dog bone’ shape and applying stress to the material
until maximum strain is achieved resulting in the material rupturing or breaking apart.[12]
The measurement of the electrically insulative qualities of the nanocomposite material will be
conducted using simulations. Data from both tests will be compiled and analysed to determine
the unique characteristics of each material.
1.1. Ethylene Propylene Diene Monomer (EPDM)
EPDM (ethylene propylene diene monomer) is a type of saturated elastomeric polymer derived
from the polyethylene family, consisting of ethylene, propylene, and diene. Through the
variation of the ethylene content in the polymer, the crystalline structure of the polymer can be
modified, with a high level of crystallinity contributing positively to the mechanical strength of
the material. [13] The lack of double bonds in the polymer chain also contributes to the
durability of the material towards degradation in contact with heat, water, UV, and ozone
compared to other rubbers. A high ethylene content also lends high filler acceptance to the
EPDM material, allowing for a higher filler loading for improved strength characteristics.[14]
This has led to it being used in conjunction with a wide variety of materials for different
applications. A common usage form of EPDM is in the use of cable insulation due to its weather
3
resistance capabilities and relative dielectric strength[15,16] Another usage of EPDM is also in
the creation of thermoplastic elastomers (TPE), which are composite materials comprising of
polymers and elastomers, lending the polymer enhanced elasticity and moldability.[15,16]
1.2. Titanium dioxide
Titanium dioxide (TiO2) is an oxide of titanium commonly found in three different polymorphic
forms: anatase, brookite, and rutile. The most common polymorphic form of TiO2 is rutile,
representing the thermodynamically stable state of titanium dioxide. The largest use of the
material is as a pigment for paints, replacing poisonous lead white, food additives and even in
manufacturing of photovoltaic cells. [8,17,18] Titanium dioxide is also shown to have
electrically insulative properties, with dielectric constants reaching 100.[20] N. Hidayah et al.
found that TiO2 also imparts beneficial thermal properties to polymer nanocomposites due to
increased molecular weight of the polymer matrix[21]. Thermogravimetric analysis performed
by M. T. Ramesan et al. on different wt.% of samarium-doped TiO2 polyaniline nanocomposite
at temperature ranges from 180-500 C show much reduced material decomposition compared
to pure polyaniline.[22] Char residue of the decomposed material remaining after 500 °C for
pure polyaniline (PANI) is only 52.04% compared with the 56.76, 58.64 and 60.95% char left
for 5, 10 and 15 wt.% nanoparticles containing PANI, which indicate increased heat resistance
of TiO2-doped PANI compared with unmodified PANI.[22]
Figure 1.1 : TGA graph of polyaniline with samarium-doped TiO2 nanofiller showing weight
loss of material at different temperature scales
4
Figure 1.2: Thermogravimetric curves (graph a) and Arrhenius plots for thermogravimetric
analysis of PTFE (graph b)
1.3 Nanocomposites
Nanocomposite materials have made a big headway into the production of next-generation
materials. Using a multitude of different materials compounded together with the addition of
nanofillers, the properties of the base material can be enhanced and improved upon, allowing
for lighter weight, higher strength, better weather resistance etc. Strong interest has been shown
in the usage of nanofillers such as graphene[6,7] and carbon nanotubes[4,21] in a variety of
applications such as bioengineering and aeronautics.
The filler loading of the nanomaterial and the nanocomposite blending process must be
optimized to prevent particle agglomeration or uneven nanoparticle distribution which may
negatively influence nanocomposite performance. At low densities and blend ratios, dispersion
of titanium dioxide fillers was not uniform with particle agglomerations on the surface of the
blended SiR/EPDM nanocomposite material according to S. Vijayalakshmi et al.[2] Higher
particle densities and blend ratios of TiO2 were found to have better coverage of the material
surface, with best coverage being at 5 % wt. which provides the best tensile strength readings,
decreasing at 10 % wt. For elongation at break (EB) tests, lower density nanoparticle size leads
to better elasticity of the material due to the brittle structure of high density TiO2 grain sizes.
5
M. T. Ramesan et al. [22] also noted the coarser surface finish of 15% wt. samarium doped
TiO2 polyaniline nanocomposite material due to nanoparticle agglomeration, suggesting
improper blending being one of the causes. Thus, it can be considered that blending ratios are
an important factor in the performance of the nanocomposite.
Figure 1.3: Scanning Electron Microscope (SEM) images of TiO2 nanoparticles embedded on
SiR-EPDM blend in low density (left) and high density (right) particle sizes with wt% from 1,
5, and 10 (top to bottom). Note the large nanoparticle clusters circled in red.
1.4 Mechanical strength
Mechanical strength of a material is the ability of the material to resist force. The mechanical
forces that are typically inflicted on a material include stress and strain.
Stress is represented as the force per unit area applied to the material under test (expressed as
N/m2 or psi units and with the Greek symbol σ), show in this equation:
𝐹𝑜𝑟𝑐𝑒 (𝑁)
𝜎= 𝑁/𝑚2 (1)
𝐶𝑟𝑜𝑠𝑠 − 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 (𝑚2 )
Strain represents the change in length of the material due to stress, measured as the ratio of the
material’s deformation length to its original length. [Sekhar Bag, Dibyendu]. Strain also leads
to the contraction of the material as it stretches, with the ratio of contraction to elongation being
referred to as Poisson’s ratio (γ).
𝑆𝑡𝑟𝑒𝑡𝑐ℎ𝑒𝑑 𝑙𝑒𝑛𝑔𝑡ℎ − 𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ

𝛾= (𝑢𝑛𝑖𝑡𝑙𝑒𝑠𝑠) (2)
𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ
6
From these two equations, another metric known as Young’s modulus can be derived, which
is the ratio of stress developed relative to strain developed in the material, measured in Pascals
(Pa). The characteristic equation being:
𝜎 𝑁2
𝑌= ; 𝜎 𝑏𝑒𝑖𝑛𝑔 𝑠𝑡𝑟𝑒𝑠𝑠 & 𝛾 𝑏𝑒𝑖𝑛𝑔 𝑠𝑡𝑟𝑎𝑖𝑛 (3)
𝛾 𝑚
This equation can be used to determine the relative rigidity of the material and evaluate its
suitability for different applications.
1.5 Thermal properties
Evaluation of the thermal properties of materials can be done using thermogravimetric analysis
and linear rate of burning. In thermogravimetric analysis, the kinetics of each stage of
decomposition can be derived via the weight loss over time of the material using the Arrhenius
equation, which describes the rate of reaction relative to temperature and energy required for
the reaction[24] :
𝑑𝑤 𝐸
= 𝐴𝑒 −𝑅𝑇 (4)
𝑑𝑡
Where RT is the average kinetic energy (T being temperature in kelvin and R being gas
constant), E is the activation energy and A is the pre-exponential factor which represents the
molecules that begin reaction regardless of activation energy being present.
The linear rate of burning evaluates the flammability of the material, providing information on
flame path on a horizontal surface, flame spread rate, sample burning behaviour and ease of
extinguishing combustion with the burning rate, V derived from the equation:
𝐿
𝑉 = 60 𝑚𝑚/𝑠 (5)
𝑡
where L is the length of burned material in millimetres (mm) and t is the time in second(s). N.
Hidayah et al. used linear rate of burning to test the thermal properties of nanoparticle infused
EPDM/PP thermoplastic elastomer (TPE) blend. [1] A clear decrease of the burning rate in the
7
presence of TiO2 nanofillers can be observed but was outperformed by zinc oxide (ZnO) which
exhibited a longer burning rate.[1]
Figure 1.4 : Graph of burning rate of composite PP/EPDM TPEs with/without nanofillers
2. Research Methodology
The objective of this study is to investigate the thermal and mechanical properties of titanium
dioxide (TiO2) filled EPDM. Analysis on the characteristics of the material will be conducted
via the usage of thermogravimetric analysis and tensile strength tests.
2.1. Sample preparation

EPDM (ethylene propylene diene monomer) rubber was supplied by Petronas, with nominal
density of 949 kg/m3 and melting temperature range of 170-210 °C. TiO2 (Titanium dioxide)
nanofiller with average diameter of 100 nm (nanometer) supplied by Sigma Aldrich. The
compounding process of EPDM/TiO2 nanocomposite is done by melt blending at 50 rpm in a
Haake internal mixer, with temperature at 3 zones set at 180 °C to obtain even heating during
the melting process. Four ratios of filler loading in the polymer matrix: 0 wt. %, 1 wt. %, 3 wt.
% and 5 wt. % TiO2 was utilized.
The resulting blends were then compressed into sample sheets using a scientific hot press
machine under 80 bar pressure for 3 minutes. Samples were moulded into 150mm x 150mm
dimensions with thickness of 5mm.
8
2.2. Thermogravimetric analysis

Thermogravimetric analysis was performed with a PerkinElmer TGA 8000 thermogravimetric
analyser with temperature range of 30-600°C at 10 °C min-1 heating rate, under nitrogen
atmosphere with purge rate 20 ml min-1.
2.3. Tensile tests

Tensile test specimens were injection moulded into dog-bone shaped specimens (ASTM D638).
At least five injection-molded specimens of each sample were submitted to impact resistance
and tensile tests in an EMIC AIC 1 apparatus and in an EMIC DL 200 apparatus (5000 N load
cell, 10mm min-1 speed).
3. RESULTS AND DISCUSSION
3.1 Mechanical Properties
The experimental data from tensile testing such as tensile stress, Young’s modulus and
elongation at break are presented in Graphs 1.5, 1.6, and 1.7 respectively. It can be observed
that the stiffness of test samples is improved by addition of TiO2. This is evidenced by the
higher Young’s modulus (YM) readings (1.052 MPa at 3% wt. TiO2 compared to 0.746 MPa
for neat EPDM) and lower elongation at break (EB) readings (69.4% elongation at 3% wt. TiO2
compared to 170.17% elongation for neat EPDM) in comparison with neat EPDM. Tensile
stress readings were shown to be inconsistent with an increase from 4.41 MPa to 4.7 MPA
going from neat EPDM to 1% wt. TiO2, decreasing to 2.57 MPa at 3% wt. TiO2 and increasing
to 3.21 MPa at 5% wt. TiO2.
9
6.00
1.200
4.70 1.052
5.00
1.047
1.000
4.00 4.41
0.811
Young's Modulus (MPa)

0.800
Stress 3.21
3.00 2.57
(MPa) 0.746
0.600
2.00
0.400
1.00
0.200
0.00
0 2 4 6
Percentage TiO2 nanofiller(%) 0.000
0 Percentage
2 TiO2 nanofiller(%)
4 6
Figure 1.5: Tensile stress relative to Figure 1.6: Young’s modulus relative to
nanofiller content nanofiller content
180.000
170.174
160.000
157.559
140.000
120.000
Elongation at 100.000 86.938

break
(%
80.000 69.419
elongation)
60.000
40.000
20.000
0.000
0 1 2 3 4 5 6
Percentage TiO2 nanofiller(%)
Figure 1.7. Elongation at break relative to nanofiller content
10
The reduction in YM and EB characteristics of the nanocomposite at 5% wt. nanofiller loading

is likely due to agglomeration of nanofiller particles. Poor distribution of nanoparticles typically
occur during incorporation of nanoparticles into the polymer matrix, resulting also in a coarser
surface texture. The uneven particle size in the nanocomposite material also acts as nucleation
sits for micro-voids and crazes when stress is applied to the nanocomposite, reducing strength
of the nanocomposite. [25] Stress-whitening was also seen in the 3% wt. and 5% wt. samples,
indicating uneven particle size distribution in the nanocomposite matrix causing crazing and
cavitation [17].
3.2 Thermal properties
The experimental results from TGA testing are presented in Graphs 1.8, 1.9 and 1.10 for weight
loss against temperature, 5% weight loss temperature against nanofiller percentage and 50%
weight loss temperature against nanofiller percentage respectively. From Graph 1.1, weight loss
occurs past the 400°C threshold mark for the EPDM-TiO2 nanocomposites, with neat EPDM
showing weight loss approximately during the 280°C mark. Residual mass of the samples after
pyrolysis was 2% for neat EPDM, 5% for 1% wt. TiO2 nanocomposite, 5% for 1% wt. TiO2
nanocomposite, 10% for 3% wt. TiO2 nanocomposite and 13% for 5% wt. TiO2 nanocomposite.
At 5% sample weight loss, EPDM samples containing TiO2 nanofiller display higher
temperature readings compared to neat EPDM (4.8% for 1% TiO2 , 6.3% for 3% TiO2 and 6.7%
for 5% TiO2 respectively) as shown in Figure 1.6. Similarly, marginally higher temperature
readings were recorded at 50% sample weight loss (0.8% for 1% TiO2, 1.3% for 3% TiO2 and
1.4% for 5% TiO2 respectively) as shown in Figure 1.7. The addition of TiO2 nanofiller to
EPDM is visibly shown to display higher thermal stability compared to that of neat EPDM,
likely due to the dispersion of TiO2 nanoparticles in the polymer matrix resulting in a protective
layer preventing against decomposition [22].
11
120
100
Sample Weight (%)
80
60
40
20
0
0 100 200 300 400 500 600 700
Temperature (°C)
EPDM 0% Ti EPDM 1% Ti EPDM 3% Ti EPDM 5% Ti
Figure 1.8: EPDM TGA percentage weight loss as a function of temperature
440 471
470.32
470 469.65
435 430.21 438.36
436.84
469
430
Temperature (°C)
Temperature (°C)
467.51
468
425
467
420
466
415
465
410 464
410.47 463.6
405 463
0 2 4 6 0 2 4 6
Percentage TiO2 nanofiller(%) Percentage TiO2 nanofiller(%)
Figure 1.9: Sample nanofiller content Figure 1.10: Sample nanofiller content
relative to temperature at 5% weight loss relative to temperature at 50% weight loss
Increased char residue was also found in samples with higher nano filler concentrations, namely
EPDM loaded with 3% wt. TiO2 and 5% wt. TiO2 nanofiller. Char formation is often promoted
in composite materials as a method to increase flame retardant properties of the material. Char
formation effectively creates a barrier between the residual material preventing further
combustion, while also representing a reduction in theoretical heat generation from combustion
12
of the char [26]. Therefore, it can be said that the increase in char residue from addition of TiO2
nanofiller positively impacts the thermal stability of EPDM.
Figure 1.11 Increased char residue on high TiO2 nanofiller samples (numbered 3 and 4)
4. Conclusion
In this paper the effects of TiO2 nanofiller on mechanical and thermal properties of EPDM
nanocomposites were studied. The mechanical results of EPDM-TiO2 nanocomposites
displayed improved mechanical strength compared to neat EPDM, with increased stiffness of
the material evidenced from lower elongation at break and higher Young’s modulus. At 5%
wt% TiO2 nanofiller content, a reduction in Young’s modulus and an increase in sample EB
readings was recorded due to uneven nanofiller distribution resulting from nanoparticle
agglomeration. Thermal properties of EPDM-TiO2 nanocomposite had noticeably superior
characteristics compared to neat EPDM, displaying increased char formation and higher
breakdown temperatures across all nanofiller loading percentages.
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This content was downloaded from IP address 39.40.34.82 on 27/11/2023 at 13:32

The study of thermal & mechanical properties of EPDM

K X Sin1, H Ahmad 1,2*, Hoon Yap3, Hafizul Azizi Ismail4

To determine the mechanical strength of the EPDM/TiO2 nanocomposite material blended in

1.1. Ethylene Propylene Diene Monomer (EPDM)

1.2. Titanium dioxide

1.4 Mechanical strength

𝑆𝑡𝑟𝑒𝑡𝑐ℎ𝑒𝑑 𝑙𝑒𝑛𝑔𝑡ℎ − 𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ

1.5 Thermal properties

2.1. Sample preparation

2.2. Thermogravimetric analysis

2.3. Tensile tests

3. RESULTS AND DISCUSSION

3.1 Mechanical Properties

Young's Modulus (MPa)

Elongation at 100.000 86.938

Figure 1.7. Elongation at break relative to nanofiller content

The reduction in YM and EB characteristics of the nanocomposite at 5% wt. nanofiller loading

3.2 Thermal properties

EPDM 0% Ti EPDM 1% Ti EPDM 3% Ti EPDM 5% Ti

Figure 1.8: EPDM TGA percentage weight loss as a function of temperature

[1] Hidayah I N, Mariatti M, Ismail H and Kamarol M 2015 Evaluation of PP/EPDM

[8] Azizi S, Momen G, Ouellet-Plamondon C and David E 2020 Performance improvement of

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