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TGA of Natural Rubber Composite
TGA of Natural Rubber Composite
TGA of Natural Rubber Composite
Technical Report
a r t i c l e i n f o a b s t r a c t
Article history: As nanosized expanded graphite (EG) reveals a similar layered structure like organoclay and also it has a
Received 13 January 2012 high expansion ratio so rubber chains can easily be intercalated into the gallery space. To improve the
Accepted 3 March 2012 dispersion of EG in the rubber matrices, primarily the surface modification of the expanded graphite have
Available online 15 March 2012
been done and then the modified expanded graphite (MEG)/polar compatibilizer [epoxidized natural rub-
ber (ENR)] master batch have been prepared by solution mixing method in the laboratory. After that the
MEG/ENR master batch have been mixed with bulk natural rubber (NR) in presence and absence of car-
bon black (CB) in a laboratory scale open two roll mixing mill. Wide angle X-ray diffraction (WAXD) and
high resolution transmission electron microscopic (HR-TEM) analysis of the nanocomposites revealed
that MEG was intercalated and as well as delaminated in the NR matrix. Scanning electron microscope
(SEM) images of the nanocomposites showed very rough surface than the pure NR matrix. In presence
of expanded graphite the crack paths are channelized and coincide in one point suggesting the effect
of plate like expanded graphite to acts as a barrier. We have got improved mechanical, thermal and
dynamic mechanical properties for the MEG and MEG/CB loaded NR compounds compared to EG and
EG/CB loaded NR compounds.
Ó 2012 Elsevier Ltd. All rights reserved.
0261-3069/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2012.03.007
A. Malas et al. / Materials and Design 39 (2012) 410–417 411
between polar MEG and nonpolar NR for the fabrication of NR composite was added to the NR matrix in presence (NREGCB and
based nanocomposites. Primarily, ENR/MEG (ENMEG) composite NRENMEGCB) and absence of CB (NREG and NRMEG) in an open
was prepared by solution mixing method in order to get uniform two roll mixing mill. The wt% of the nanofillers was kept constant
dispersion of MEG in the ENR matrix. After that ENMEG composites at 3. Compression molding machine was used for the vulcanization
were mixed with bulk NR in presence and absence of CB with sul- of the rubber compounds at 150 °C and the optimum cure time was
fur as curing agent in a laboratory scale open two roll mixing mill. obtained from the Rheometer.
The changes obtained in the curing characteristics, mechanical, dy-
namic mechanical, morphological and thermal properties had been 4. Characterization techniques
analyzed and compared with the pure one.
4.1. Cure characteristics
2. Materials
Curing study of the nanocomposites was carried out in the
Asbury Carbons (Asbury, NJ) supplied thermally expanded Monsanto Rheometer R-100 testing instrument at 150 °C with 3°
graphite flakes. Natural rubber (RMA-1X) was supplied by the Rub- arc for 60 min.
ber Board, Kottayam, Kerala. Epoxidized natural rubber (ENR) con-
taining 47 mol% epoxidic units was supplied from Agricultural 4.2. Wide angle X-ray diffraction (WAXD)
Product Processing Research Institute, Zhangiang, PR China (spe-
cific gravity, 1.03). MEG with more functional acids (ACOOH) and X-ray diffraction analysis of EG, MEG and hybrid compounds
the hydroxyl groups (AOH) was prepared by oxidation of expanded were done by using a Rigaku Miniflex Diffractometer with Cu Ka
graphite with H2SO4/HNO3 (3:1) at 90 °C for 1 h with vigorous stir- radiation at a generator voltage of 40 kV, a scanning rate 3°/min
ring. CB, type: Intermediate Super Abrasion Furnace (ISAF), Grade: between 7° and 70°, chart speed of 10 mm/2h, current 20 mA and
N234 was bought from Hi-tech carbon. Other compounding addi- wavelength of 0.154 nm at room temperature. The d-spacing of
tives like sulfur, zinc oxide, stearic acid, N-cyclohexyl-2-ben- EG was obtained from the Brag’s equations nk = 2dsin h.
zothiazyl sulphenamide (CBS), Tetramethylthiuram disulfide
(TMTD) were obtained from Bayer (M) Sdn Bhd Malaysia. 4.3. High resolution transmission electron microscopy (HR-TEM)
Composition of the rubber compounds were shown in Table 1. 4.5. Mechanical testing
An open two roll mixing mill was used for the preparation of the
NR/EG (NREG) and NR/MEG (NRMEG) at room temperature; 1:1.4 Mechanical properties of the hybrid nanocomposites were
was the speed ratio of the rotors (front to back). In one batch EG obtained by using Universal tensile testing machine (Hounsfield
was directly added to the NR matrix and in another batch ENMEG H 10KS) under ambient conditions. The tensile stress, modulus
Table 1
Compositions of the rubber compounds.
Ingredients Designation
Pure NR NRCB NREG NRENMEG NREGCB NRENMEGCB
Content (phr)
NR 100 100 100 97 100 97
ENMEG – – – 6 – 6
EG – – 3 – 3 –
Stearic acid 2 2 2 2 2 2
CBSa 0.7 0.7 0.7 0.7 0.7 0.7
Zinc oxide 5 5 5 5 5 5
TMTDb 1 1 1 1 1 1
CB-ISAFc (N234) – 40 – – 30 30
Sulfur 2.5 2.5 2.5 2.5 2.5 2.5
Processing oil – 2 – – 2 2
a
CBS – N-cyclohexyl-2-benzothiazyl sulphenamide.
b
TMTD – Tetramethylthiuram disulfide.
c
ISAF – Intermediate Super Abrasion Furnace.
412 A. Malas et al. / Materials and Design 39 (2012) 410–417
and elongation at break (%) were obtained at room temperature. proves that MEG may be delaminated in the ENR matrix. For NREG
Tensile strength was measured according to ASTM D-412-06 and and NREGCB compounds, the peak at 2h = 26.75° was weaker and
tear strength was determined according to ASTM D-624-00 widened compared to the EG, which indicates the presence of dis-
(2007) [26]. The measured length was 25 mm, and the speed of ordered structure of EG in the nanocomposites. The presence of the
jaw separation was 500 mm/min. main peak of EG at 2h = 26.75° with less intensity for the EG filled
NR vulcanizates indicates that the nanostructure of EG was un-
4.6. Scanning electron microscopy (SEM) changed and hence its crystal morphology was maintained in the
composites [12,28]. For NRENMEG and NRENMEGCB compounds,
SEM analysis of the tensile fractured surface of the nanocom- the peak at 2h = 25.8° was further diminished which proves the
posites was carried out in VEGA TESCAN//LSU instrument after delaminated structure of the nanocomposites.
the fractured surface of the samples were gold coated. XRD presents only a incomplete picture of the dispersion of
nanofiller and absence of peak corresponding to d-spacing does
4.7. Thermo gravimetric analysis (TGA) not always signify the partial exfoliation of the nanofiller in poly-
mer matrix, because XRD is unable to identify regular stacking
Thermo gravimetric analysis of the nanocomposites was done exceeding 8.8 nm [29]. Therefore, to investigate the dispersion
by using a DuPont TGA-2100 thermal analyzer in the temperature morphology of the nanocomposites, microscopic investigation is
range 30–700 °C with a heating rate of 10 °C/min. required [30].
FT-IR analysis of EG and MEG were carried out from 650 cm1 Fig. 2 shows the FT-IR spectrum of EG and MEG. The band at
to 4000 cm1 using Thermonicolet/Nexus 870 FT-IR spectrometer. 3438 cm1 can be attributed to the OAH stretching vibration of
For the powdered sample, firstly powdered were mixed with KBr in phenolic or alcoholic functional groups presents on the EG and
a 1:200 ratio of their weight, and then pressed to form a pellet for MEG flakes [31]. The presence of carboxylic acid groups on the
the measurement. For the polymeric nanocomposites, we have to EG sheets were very less due to that the peak of C@O gr. (ACOOH)
prepare a thin film of thickness in the range 100–250 lm by using was absent for EG. After modification of EG, the C@O peak
compression molding machine. (1735 cm1) was quite evidenced from the MEG curve. The peaks
at 2920 cm1 and 2855 cm1 were due to CAH stretching vibra-
tions. Due to the presence of AOH and ACOOH groups on the EG
5. Results and discussions
and MEG, physical and chemical interactions between polymer
and MEG will be enhanced [15].
5.1. WAXD analysis
Fig. 1 shows the X-ray diffraction pattern of EG, MEG, ENMEG 5.3. DMTA analysis
composite, NREG, NRENMEG, NREGCB and NRENMEGCB com-
pounds. Two intense peaks were raised around 2h = 26.75° and Figs. 3a and 3b represents the temperature dependence of dy-
54.4°, which are the characteristic peaks of highly structured namic storage modulus (E0 ) and loss factor (tan d) of the pure NR
graphite carbon (0 0 2) and (0 0 4) for EG [27]. For MEG, the (0 0 2) and the NR based nanocomposites. The EG and MEG loaded NR
peak of EG was shifted towards the lower angle 2h = 25.8° and peak compounds in presence and absence of CB show tremendous
intensity also decreased which indicates the increased interlayer improvement in the dynamic storage modulus compared to the
spacing and decreased in crystallinity of the EG. For ENMEG com- pure one. The MEG loaded NR compounds show highest storage
posite the (0 0 2) peak intensity was more or less diminished which modulus than the EG loaded compounds at room temperature as
well as below room temperature, which may be due to the better
Fig. 1. XRD pattern of EG, MEG and EG/MEG filled NR based nanocomposites in
presence and absence of CB. Fig. 2. FT-IR spectrum for EG and MEG.
A. Malas et al. / Materials and Design 39 (2012) 410–417 413
Fig. 3a. Storage modulus for the pure NR and its nanocomposites.
Fig. 4. TGA curve for pure NR and its nanocomposites.
Fig. 4 shows the thermo gravimetric curves for the pure NR and
the NR based nanocomposites. The onset degradation temperature
was increased for the EG and MEG loaded nanocomposites in pres-
ence of CB compared to the pure one. This may be due to the heat
shielding effect of the added CB–EG and CB–MEG fillers in the NR
matrix and formation of mass transport barrier to the volatile
products produced during the decomposition of the hybrid nano-
composites. The maximum degradation temperature of the nano-
composites was quite same to the pure NR. Rajkumar et al. found
higher thermal stability for nanographite loaded nitrile butadiene
rubber composites with increasing in nanographite loadings [38].
Fig. 3b. Tan d curve for the pure NR and its nanocomposites.
Quan et al. observed a positive effect of graphite nanoplatelets
(GNPs) on the thermal stability of the GNP filled thermoplastic
dispersion of polar MEG in the polar ENR matrix and also may be polyurethane (TPU) nanocomposites [39].
due to the increased interlayer spacing of MEG than the EG flakes. CB/EG and CB/MEG filled NR vulcanizates show better thermal
The polymer chains can easily be entered into the gallery space of stability than EG and MEG filled NR compound this may be due
MEG than EG. Ganguli et al. observed an improved storage modu- to the better heat shielding effect of the dual fillers than the single
lus for the chemically modified graphite/epoxy composites than filler in the NR matrix.
the untreated ones and they found that the rubbery modulus stea-
dily increases with increasing the filler content [32]. Yang et al. 5.5. Curing characteristics
found that after increasing the wt% of EG content in the xNBR ma-
trix, the temperature dependent storage modulus was increased Table 2 shows the curing features of the EG and MEG filled NR
above the glass transition temperature [33]. Wang et al. noticed based nanocomposites in presence and absence of CB. The scorch
that the dynamic storage modulus was significantly improved for time and cure time of the EG and MEG filled rubber compounds
the EG filled NBR nanocomposites than the pure NBR and they ex- in presence and absence of CB are faster than that of the pure
plained it as a result of good reinforcing effect of the nanosized EG NR. The reason for the shorter cure time of the rubber compounds
[34]. Yahaya et al. observed an improved storage modulus for the was may be due to the increased thermal transition of NR in pres-
organoclay filled NR vulcanizates and according to them the inter- ence of EG and MEG which could promote the attainment of vulca-
facial interaction between the intercalated/exfoliated silicate lay- nization reaction. Song et al. reported that the cure time of the acid
ers and the polymer matrix resulting in an improvement in the graphite filled SBR composites in presence of a coupling agent was
storage modulus [35]. faster than the other elastomer composites and a sharp increment
EG and MEG loaded nanocomposites show closeness in glass in the torque value and a similar explanation has been proposed by
transition temperature value and less damping characteristics than them [40]. Maximum torque can be considered as a measure of the
the pure NR. The reduced tan d peak height during dynamic stock modulus of the materials [41] and the torque difference can
mechanical deformation was may be due to the reduced chain be assumed as a measure of the extent of cross linking [42,43].
414 A. Malas et al. / Materials and Design 39 (2012) 410–417
Table 2
Cure characteristics of the rubber compounds.
Sample code Min. torque (dN m) Max. torque (dN m) Torque difference (dN m) Scorch time (min) Cure time (min) Cure rate index
Pure NR 3.1 53.1 50.0 2.2 3.1 83.4
NRCB 4.0 85.3 81.3 1.7 2.7 92.3
NREG 2.3 56.1 53.8 2.1 2.7 130.6
NRENMEG 1.8 58.2 56.4 2.0 2.6 140.7
NREGCB 2.4 88.5 86.1 1.6 2.5 115.3
NRENMEGCB 2.5 90.4 87.9 1.6 2.4 130.4
Table 3
Mechanical properties of the rubber compounds.
25%, 39%, 103% and 147% increase in tear strength, 242%, 321%,
450% and 484% increase in modulus value at 300% elongation
respectively compared to the pure NR. One of the main targets for Fig. 6b. HR-TEM image of NREG compound.
rubber reinforcements is to improve resistance against tearing.
The flake or sheet like structure of EG obstructs the propagation
of fracture lines and thus improves the tear resistance as well as
the strong reinforcing effect of the EG and MEG in presence and ab- as well as in the NR matrix. This may be due to its higher polarity
sence of CB resulting in a huge improvement in the tensile strength than the EG because MEG contains considerable number of both
and tear strength of The NR vulcanizates. Many researchers investi- the ACOOH and the AOH groups on its surface which enhanced
gated the effect of nanoclay, which exhibits sheet like structure like the interaction between it and polar compatibilizer (ENR) and the
EG, on the mechanical properties of different rubber. They observed rubber-filler interaction as confirmed from WAXD results and high
that a good dispersion of silicate layers and high interfacial resolution transmission electron microscopic (HR-TEM) images.
adhesion between rubber and nanoclay are generally associated
with increased tensile strength and tear resistance [44–46]. Ismail 5.7. SEM analysis
et al. found that after increasing the incorporated graphite content
in SBR matrix, the tensile strength of the composites was increased The tensile fractured surface of pure NR compound and EG/MEG
[47]. Song et al. observed an improvement in overall mechanical filled NR vulcanizates in presence and absence of CB were shown in
properties of the exfoliated graphite and acid graphite filled SBR Figs. 5a–5f. SEM images of the nanocomposites show complex
based nanocomposites [48,40]. Yang et al. observed a drastic uneven torn surface, whereas the unfilled NR shows simple torn
improvement in the mechanical properties of the EG filled xNBR surface without complexity. This may be demonstrated by the
composites [33]. The modulus of all the nanofiller (EG and MEG) better interactions between the MEG and the NR matrix. It was
loaded NR compounds was increased drastically in presence and evident from the SEM images that after incorporation of EG and
absence of CB, which may be due to the restrictions of polymer MEG in the NR matrix in presence and absence of CB, the number
chain mobility or increase in the cross link density [49]. MEG loaded of tear path was increased and also the tear paths were broadened
NR compound shows better mechanical properties than the EG which proves the better interactions between the nanofiller and the
loaded compounds because of its finer dispersion in ENR matrix rubber matrix and resulting in a huge improvement in the overall
416 A. Malas et al. / Materials and Design 39 (2012) 410–417
Fig. 6c. HR-TEM image of NRENMEG compound. Fig. 6e. HR-TEM image of NRENMEGCB compound.
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