Nuclear Engineering and Design 273 (2014) 602–614

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Nuclear Engineering and Design

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Performance evaluation of gamma irradiated SiR-EPDM blends

Deepalaxmi R. ∗ , Rajini V.
SSN College of Engineering, Chennai, Tamil Nadu, India

h i g h l i g h t s

• The effects of gamma irradiation on SiR-EPDM blend are examined.

• Cross-linking reaction is dominant in blends C, D and E, due to higher EPDM content.
• The tensile strength and hardness of blend E is improved by gamma irradiation.
• The blend C and EPDM rich blends (D, E) are found to have superior performance.
• Among C, D and E, suitable blend can be selected for a particular NPP application.

a r t i c l e i n f o a b s t r a c t

Article history: Cable insulation materials (CIM) should perform their safety functions throughout their installed life in
Received 17 September 2013 nuclear power plants (NPP). The CIM will be exposed to gamma irradiation at the installed locations.
Received in revised form 27 March 2014 In order to forecast long-term performance of CIM, the short time accelerated testing was carried out.
Accepted 31 March 2014
Due to its good mechanical strength, ethylene propylene diene monomer (EPDM) is widely used as
CIM. Silicone rubber (SiR) is used in high temperature environments, due to its good di-electric proper-
ties/hydrophobicity. The blending of these two polymers may result in the improvement in their specific
properties. This paper analyses the effects of gamma irradiation on the five different compositions (90-
10; 70-30; 50-50; 30-70; 10-90) of SiR-EPDM blends. The blends were exposed to four different doses
(25 Mrad, 100 Mrad, 200 Mrad and 250 Mrad) of gamma irradiation. The electrical and mechanical param-
eters like volume resistivity (VRY), surface resistivity (SRY), tensile strength (TS), elongation at break (EB),
hardness (H) of the virgin and gamma irradiated blends were determined as per ASTM/IEC standards.
The nature of degradation was investigated using Fourier transform infrared spectroscopy (FTIR). The
simultaneous occurrence of cross-linking and chain scission is found to be the mechanism for ageing in
SiR-EPDM blends. The electrical parameters such as volume resistivity and surface resistivity of all the
blends are found to improve for all doses of gamma irradiation. To validate the influence of cross-linking
reaction of the SiR-EPDM blends under a normal as well as in radiation environment, thermal analysis
has been done using differential scanning calorimetry (DSC) and thermo-gravimetric analysis (TGA). The
morphological changes occurred on the surface of the virgin and gamma irradiated SiR-EPDM blends
were investigated through the scanning electron microscopy (SEM) analysis. The blend C and the EPDM
rich blends (D and E) are found to have the superior performance when compared with SiR rich blends (A
and B). Hence among the three different compositions of EPDM rich blends, suitable blend can be selected
for a particular NPP application.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction materials (CIM) must retain their performance qualities through-

The nuclear power plant (NPP) must be operated with a high
reliability and higher level of safety. The reliability of NPP depends
on control and instrumentation (C&I) systems. Those C&I systems
make use of cables at various power levels. The cable insulation
∗ Corresponding author. Tel.: +91 9884542232.
E-mail addresses: deepalaxmivaithi@gmail.com, deepalaxmir@ssn.edu.in (D. R.).
out their normal operating life and also during abnormal situations
like loss of coolant accident (Banford and Fouracre, 1999; Hosticka
et al., 1980). Due to their superior properties at heavy pollution and
wet conditions, polymeric insulating materials are widely used in
the manufacture of cables, outdoor insulators. Ethylene propylene
diene monomer (EPDM) has a stable and saturated polymer back-
bone structure. Due to this, EPDM is found to have an excellent
resistance to heat, oxidation, ozone and weather ageing. Silicone
rubber (SiR) is widely used for outdoor high voltage application. It

http://dx.doi.org/10.1016/j.nucengdes.2014.03.037
0029-5493/© 2014 Elsevier B.V. All rights reserved.
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
has excellent dielectric properties coupled with high temperature
stability. However, SiR has poor mechanical strength. EPDM when
added to SiR imparts good mechanical strength and outstanding
resistance to attack by oxygen, ozone and weather (Brown, 1994).
Hence, the base polymer materials chosen were SiR and EPDM. The
two most widely used diene ter monomers are primarily ethyli-
dene nor bornene (ENB) followed by Di-Cyclo-Penta-Diene (DCPD).
The type of diene monomer used is ENB. Because it has fastest and
highest state of cure, good tensile, good compression set resistance.
Blending of these two polymers (SiR-EPDM) is an effective way
to develop new material with improved characteristics. The newly
formed blend may have good di-electric characteristics, thermal
stability, improved mechanical strength and resistance towards
polluted environment. Compounded alloys can have excellent elec-
trical and mechanical properties due to the presence of EPDM and
may be hydrophobic because of silicone content (Simmons et al.,
1997; Raja Prabu et al., 2007; Ehsani et al., 2004; Kole and Tripathy,
1994). The five different compositions of SiR-EPDM blends (90:10;
70:30; 50:50; 30:70; 10:90) were prepared. The optimal blend ratio
has been identified using particle swarm optimization technique by
the authors (Deepalaxmi et al., 2013). Many researchers have inves-
tigated the performance of gamma irradiated LDPE/EVA blend and
polyethylene (Rajini and Udayakumar, 2009; Du and Gao, 2009;
Chung Lee et al., 2006; Rajini and Udayakumar, 2006). Also the
effect of gamma irradiation on ethylene-octene polymers (Chipara
et al., 1999) and the radiation induced degradation of NBR-EPDM
rubbers have been reported (Roberto Benson et al., 1999). The effect
of gamma irradiation on NR/CSM (choloro sulphonated polyethyl-
ene) and NBR/CSM rubber blends have been investigated (Gordana
Markovic Milena et al., 2009). Several studies have been done on
the effects of gamma ray/proton irradiation on the properties of
polypropylene and methyl silicone rubber (Emilie Gautriaud et al.,
2007). The effect of gamma irradiation on SiR-EPDM blend has
never been reported.
So the five different compositions of SiR-EPDM blends were
exposed to four different doses of (25 Mrad, 100 Mrad, 200 Mrad,
250 Mrad) gamma irradiation. The electrical properties like volume
resistivity (VRY), surface resistivity (SRY) and mechanical proper-
ties like tensile strength (TS), elongation at break (EB) and hardness
(H) of the virgin and gamma irradiated blends were measured as per
ASTM/IEC standards. The comparison of electro-mechanical prop-
erties of the blends with their base polymers was discussed in detail
(Deepalaxmi et al., 2013).
The gamma irradiation can cause macroscopic changes in the
electrical/mechanical properties of this newly formed SiR-EPDM
blend. The changes in electrical/mechanical properties may be due
to some alterations in the chemical structure of SiR-EPDM blends.
The nature of alteration may vary with respect to the irradiation
dose. Hence it is essential to investigate the effect of gamma irra-
diation upon the electro-mechanical properties of the SiR-EPDM
blends. The functional groups responsible for the above changes
may be investigated through one of the physico-chemical investi-
gation techniques like FTIR.
To estimate cross-linking densities of virgin and gamma irradi-
ated SiR-EPDM blends, a calorimetric analysis has been done using
differential scanning calorimetry (DSC) and thermo-gravimetric
analysis (TGA). DSC is used to characterize the thermo-physical
properties of polymers such as melting temperature (Tm ), heat
of melting, Percent crystallinity, crystallization temperature (Tc ),
glass transition temperature (Tg ), presence of re-cyclates/regrinds,
plasticizers and polymer blends. TGA helps to predict their ther-
mal stability under a practical situation (Rajesh Babu et al.,
2010).
The morphological changes of the virgin and gamma irradiated
samples of SiR-EPDM blends have been analyzed through the scan-
ning electron microscopy (SEM) analysis.
603
2. Experimental
2.1. Materials
Commercially available SiR, EPDM were used for this research.
SiR, EPDM and other additives were supplied by M/S Joy Rubbers,
India.
2.2. Sample preparation
Five different compositions of SiR-EPDM blend were prepared
using two roll mixing mill (Shoail make). The detailed sample
preparation procedure was explained in Deepalaxmi et al. (2013).
Blend A – SiR 90%/EPDM 10%.
Blend B – SiR70%/EPDM 30%.
Blend C – SiR 50%/EPDM 50%.
Blend D – SiR 30%/EPDM 70%.
Blend E – SiR 10%/EPDM 90%.
2.3. Gamma irradiation
The gamma irradiation of SiR-EPDM blends was carried out
using 60 CO Gamma chamber facility available at Radiological
Safety Division, Indira Gandhi Centre for Atomic Research (IGCAR),
Kalpakkam, Tamil Nadu, India. The gamma chamber has an irradia-
tion volume of 1 l with a dose rate of 3 KGy/h. The doses applied
were 25 Mrad, 100 Mrad, 200 Mrad and 250 Mrad. The duration
(time) of gamma Irradiation was 83 h, 333 h, 649 h and 817 h
respectively.
IEEE 383 suggests the dose rate of 150 Mrad for an acceler-
ated ageing of polymeric materials. Hence two doses above and
below the suggested one (150 Mrad) were selected for the present
research. This is to forecast the long term survivability of the
newly formed blend during their operating life. Three samples were
exposed to the same dosage and investigations were carried out.
All the results presented in this paper, are the average of the three
investigations made at the same conditions.
3. Characterization of SiR-EPDM blends
The virgin and gamma irradiated samples of SiR-EPDM blend
have been characterized for their electrical and mechanical prop-
erties as per ASTM/IEC standards.
3.1. Electro-mechanical characterization
3.1.1. Mechanical characterization
The virgin and gamma irradiated samples of SiR-EPDM were
tested for their mechanical characteristics. The tensile strength
and percentage elongation at break were assessed by ASTM D-412,
using universal testing machine (Make-Hounsfield). The test was
carried out on dumb bell specimens at room temperature. Hardness
was measured using Shore A Duo (Make-Durotech) as per ASTM
2240. The sample dimensions were 5 cm × 5 cm × 0.3 cm square
shaped specimen.
3.1.2. Electrical characterization
The volume and surface resistivity of the virgin and gamma irra-
diated samples of SiR-EPDM were measured (as per ASTM D257)
using a test cell along with mega ohm meter (Make Prestige Elec-
tronics). The sample size of 10 cm × 10 cm × 0.3 cm square shaped
specimen was used for the measurement. The surface resistivity
was measured by applying 500 V DC between main and guard elec-
trode. The similar procedure was adopted for the volume resistivity
also.
604 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614

3.2. Physico-chemical characterization

3.2.1. Fourier transform infrared spectroscopy (FTIR)

FTIR produces an infrared spectral scan of samples that absorb
light. It provides the information about the chemical bonding or
molecular structure of the materials. FTIR spectra of all the virgin
and gamma irradiated samples were obtained using IR spectropho-
tometer (Make Perkin Elmer) in the wave number ranging from
500 cm−1 to 4000 cm−1 .

3.2.2. Scanning electron microscopy (SEM) analysis

To study the micro surface changes of the gamma irradiated SiR-
EPDM blends and the morphology of the surface, Scanning Electron
Microscope (Make HITACHI) is used. SEM analysis was done on a
square shaped sample of size 1 cm × 1 cm with a magnification of
5–300,000.

3.3. Thermal analysis

Differential scanning calorimetry (DSC) is a thermal analy-

sis tool for measuring the thermal properties like heat capacity,
crystallinity, curing and oxidation/decomposition. DSC measures
the amount of heat generated/absorbed by a material which is
undergoing a chemical reaction due to thermal effect. The melting
behaviour of the specimens was observed using (sold by TA instru-
ments) DSC-Q10 apparatus. The experiments were performed in
nitrogen atmosphere, at a heating rate of 5 ◦ C/min along with a
temperature range of (0–800) C◦ . Indium was used as a standard.
Thermo gravimetric analysis (TGA) is a testing method that
measures changes in weight of a material in relation to changes in
temperature. It is primarily used to measure the composition and
thermal stability of materials. The experiments were performed in Fig. 1. (a) Variations in volume resistivity of the blends A and B for various doses of
nitrogen atmosphere, operated in the range 0–400 ◦ C at a heating gamma irradiation. (b) Variations in volume resistivity of the blends C, D and E for
rate of 20 ◦ C/min using SDT Q 600 (sold by TA instruments). various doses of gamma irradiation.

4. Results
4.1. Effect of gamma irradiation on SiR-EPDM blends
Gamma irradiation of polymeric materials may result in (a)
cross-linking, (b) chain scission and (c) oxidation reaction. The
cross-linking and chain scission reactions may modify the macro-
molecular chains of the material. The cross-linking corresponds
to the formation of a covalent link between two adjacent macro-
molecules. This results in the formation of a three dimensional
network. The chain scission leads to the scissoning of macro molec-
ular chains. Oxidation leads to both chain scission and cross-linking
which may result in the embrittlement of the CIM. The loss of
mechanical integrity may result in the loss of electrical integrity
(IAEA-TECDOC-932).
4.1.1. Effects on electrical parameters
Figs. 1(a) and 2(a) depict the variations in volume resistivity
and surface resistivity of SiR rich blends A and B for various doses
of gamma irradiation. Figs. 1(b) and 2(b) depict the variations in
volume resistivity and surface resistivity of EPDM rich blends D and
E and blend C (having 50:50 composition of SiR-EPDM) for various
doses of gamma irradiation.
From Fig. 1(a) and 1(b), the volume resistivity (VRY) of all the
blends is found to increase for all doses of gamma irradiation. The
SiR rich blends A and B have higher VRY compared to the blend
C and EPDM rich blends D and E as expected. Though VRY seem
to decrease for dose levels of 100 Mrad and above, their values are
higher than their respective virgin ones. From Fig. 2(a) and (b), it is
noted that the surface resistivity (SRY) of both the SiR and EPDM
rich blends tend to improve for 25 Mrad. The SRY of SiR rich blends
A and B is found to decrease for higher doses of gamma. But they are
higher than their respective virgin values. The decrease in VRY and
SRY for above 25 Mrad may be due to the simultaneous occurrence
of cross-linking and chain scission reaction in them. The SRY of the
blend C (50:50 composition of SiR-EPDM) and EPDM rich blends D
and E are found to increase for all doses of gamma. This may be due
to the occurrence of the dominant cross-linking reaction in them
(due to higher EPDM content). The dominant reactions responsible
for electrical changes need to be ascertained through FTIR.
4.1.2. Effects on mechanical parameters
Fig. 3(a), (b) and (c) depicts the variations in tensile strength,
elongation at break and hardness of five different compositions of
SiR-EPDM blends for various doses of gamma irradiation.
From Fig. 3(a), the tensile strength (TS) of SiR rich blends A
and B is found to reduce for all the doses of gamma irradiation
(25 Mrad, 100 Mrad, 200 Mrad and 250 Mrad). This may be due to
higher cross-linking density and reduced segmental mobility. In
blends A and B, maximum cross-linking occurred during the blend-
ing process itself. Hence when blends A and B are exposed to gamma
irradiation, there is a lesser probability of having a cross-link forma-
tion. Hence chain scission reaction predominates in it. Hence when
a small mechanical force is applied on a highly cross-linked CIM
(due to the lesser cross-linking probability), CIM may become brit-
tle very quickly. Hence the tensile strength of the SiR rich blends (A
and B) was reduced at 25 Mrad and 100 Mrad dose of gamma irra-
diation. But at higher doses of gamma (200 Mrad and 250 Mrad),
tensile strength of the SiR rich blends (A and B) was reduced to
zero. In SiR rich blends A and B, severe discolorations were also
observed at 200 Mrad and 250 Mrad. Also they became very brittle.
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614 605

Fig. 2. (a) Variations in surface resistivity of the blends A and B for various doses of
gamma irradiation. (b) Variations in surface resistivity of the blends C, D and E for
various doses of gamma irradiation.

In EPDM rich blends D and E and in blend C, dominant cross-

linking mechanism has been noticed for all doses of gamma
irradiation. This may be due to the higher EPDM content in them.
Due to the formation of cross-link, a large amount of mechanical
force can be withstood by a CIM. Because during the conduc-
tion of mechanical performance parameter measurement using
universal testing machine (UTM), dumb bell shaped specimen of
CIM has been extended between the fixed and moving head. In
Fig. 3. (a) Variation in tensile strength of the blends A, B, C, D and E for various doses
a cross-linked CIM, it is very difficult to release/detach the side of gamma irradiation. (b) Variation in elongation at break of the blends A, B, C, D and
chains which were attached to the main back bone of the poly- E for various doses of gamma irradiation. (c) Variation in hardness of the blends A,
mer during the cross-link formation. Hence tensile strength of the B, C, D and E for various doses of gamma irradiation.
blends C, D and E was increased for all doses of gamma irradi-
ation. Especially, the blend E is found to have the improved TS
for all doses of irradiation. The blends C and E have their maxi-
mum TS value at 100 Mrad. The blend D has its maximum TS at and blend C are found to have a better mechanical strength com-
250 Mrad. pared to the SiR rich blends. The blend C has a lower reduction in
The elongation at break (EB) of a CIM is an indicator of the state EB at 25 Mrad. The blend D has a slight reduction in EB value at
of degradation. The reduction in elongation to 50% of its absolute is 100 Mrad and 250 Mrad. At 200 Mrad, blend E is found to have a
considered as the failure criterion for CIM. It is generally accepted lower reduction in EB.
that 50% elongation after a design basis event (DBE) test represents
a material that is still in a functional state electrically with a satis-
factory degree of margin before failure (IAEA-TECDOC-932). From 4.1.3. Effects on surface hardness
Fig. 3 (b), EB of all the blends is found to reduce for all doses of From Fig. 3(c), it is inferred that the hardness (H) of the SiR rich
gamma irradiation. The reduction in EB is less than 50% absolute blends (A and B) is maximum at 100 Mrad and 250 Mrad. But the
elongation for SiR rich blends (A and B). This may be due to the hardness of the blends C and D increased only at 250 Mrad, whereas
predominant gamma induced cross-linking. The EPDM rich blends the hardness of the blend E is found to improve for all the doses of
(D and E) and blend C are found to have EB greater than 50% abso- gamma irradiation. This may be due to the predominating effect of
lute at 25 Mrad and 100 Mrad. So the EPDM rich blends (D and E) cross-linking reaction (due to higher EPDM content).
606 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614

5. Discussion Table 1d
Functional groups formed at 200 Mrad.

5.1. Electro-mechanical performance of SiR-EPDM Wave number (cm−1 ) Functional group

3751–3901 Alcohol ( OH) free

For the SiR-EPDM blend, it has been observed that cross-linking 2500–3300 Acid ( COOH) stretch, strong
and chain scission may modify the macromolecular chains of the 1550–1650 Amide (N H) bending, medium
material. The consequence is the change in the mechanical proper- 1400–1600 C C aromatic stretch
1345–1385 Nitro (N O) stretch, strong
ties of the material. It should also be noted that the oxidation due
600–800 C Cl stretch, strong
to the gamma irradiation cannot be eliminated totally. 500–600 C Br stretch, strong
The effect of dominant mechanism can be noted from the
changes in mechanical properties. From Fig. 3(a) and (b), it can be
Table 1e
inferred that there is a simultaneous occurrence of chain scission
Functional groups formed at 250 Mrad.
and cross-linking in SiR-EPDM blends. This phenomenon depends
on the applied gamma doses. Wave number (cm−1 ) Functional group
The decrease in TS of the SiR rich blends (A and B) is due to dom- 3621–3904 Alcohol ( OH) free
inant chain scission reaction of SiR. An increase in VRY and SRY of 2500–3300 Acid ( COOH) stretch, strong
1670–1820, 1640–1690 (1687) Carbonyl (C O) stretch, strong
all the blends is due to dominant cross-linking reaction of EPDM.
1550–1650 Amide (N H) bending, medium
An increase in SRY, VRY with simultaneous decrease in EB (<50% 1400–1600, 1515–1560, 1345–1385 C C aromatic stretch Nitro (N O)
absolute) is noted for SiR rich blends (A and B) for lower levels of stretch, strong
irradiation (<100 Mrad). For higher doses of gamma irradiation, the 1000–1300 Ether (C O) stretch, strong
density of the cross-linked network increases. Hence the free move- 1210–1320 Acid (C O) stretch, strong
600–800 C Cl stretch, strong
ment of the free radicals is prohibited. This results in the decrease
500–600 C Br stretch, strong
in the probability of cross-linking (Zhang et al., 2003). This is clear
from the decrease in SRY, VRY with the corresponding increase in
hardness at 100 Mrad and 250 Mrad in A and B. cross-linking. These connections have hindered the carrier as well
The cross-linking have been identified as a dominant ageing as the chain mobility.
mechanism in blends C, D and E (due to the higher EPDM con-
tent), for all doses of gamma irradiation. The cross-linking leads 5.2. Fourier transform infrared spectroscopy (FTIR) analysis
to decrease in elongation at break, increase in hardness and a slight
increase in tensile strength. The sufficient enhancement in elec- The FTIR spectra have been obtained to identify the mechanism
trical properties has been noticed for the (C, D and E) blends for for the change in electrical and mechanical parameters of all the
all doses of gamma irradiation. The factor behind this situation five blends after the gamma irradiation. FTIR was employed to iden-
is formation of new connections between molecular chains after tify the chemical integrity of all the blends as a function of gamma
irradiation doses. FTIR confirmed the formation of various new
functional groups/chemical bonds after the gamma irradiation.
Table 1a FTIR spectra for all samples were obtained for all doses of gamma
Functional groups formed at 0 Mrad.
irradiation. Here FTIR spectra of the blend C are only presented
Wave number (cm−1 ) Functional group as a sample. The effect of gamma irradiation on the material is
3200–3600 Alcohol ( OH) free identified by comparing the various functional groups formed after
2850–3000 CH3 , CH2 , C H alkane ageing with that of the virgin ones. The FTIR spectra of the virgin and
2100–2360 Si H gamma irradiated samples of blend C are depicted in Fig. 4(a)–(e).
1620–1680 C C alkene, stretch, variable The dominant functional groups present in various blends for var-
1000–1160/1020–1000 Si O Si/Si CHi CHs
ious doses of gamma irradiation are given in Tables 1a–1e.

Table 1b 5.3. Discussion on FTIR spectra

Functional groups formed at 25 Mrad.
The newly formed functional group alcohol ( OH) free in the
Wave number (cm−1 ) Functional group
range of 3500–3700 cm−1 has been observed in blends A and B for
3836–3930 Alcohol ( OH) Free all levels of gamma irradiation. Also the occurrence of new group
3010–3100 Alkene C H stretch, strong
acid ( COOH) group in the band range of 2500–3300 cm−1 was
2500–3300 Acid ( COOH) stretch, strong
2000–2150 Si H (amorphous silicon) noticed in blends B, C and D and E for some of the doses of irradia-
1600 Amide (N H) bending, medium tion. The OH group may be taken as an index for the resistivity of
1515–1560, 1345–1385 Nitro (N O) stretch, strong the CIM. The highly electro-negative oxygen atom in ( OH) group
600–800 C Cl stretch, strong
may attract and trap free electrons thus increasing the resistivity
of the materials. It can be observed from Tables 1a–1e that the
absorbance of alcohol ( OH) free group in all blends is increased
Table 1c
Functional groups formed at 100 Mrad. upto 100 Mrad. This has resulted in increase in VRY and SRY of all
blends. This trend is maintained for all doses for the blends C, D and
Wave number (cm−1 ) Functional group
E.
3674–3917 Alcohol ( OH) Free The higher VRY and SRY values for SiR rich blends A and B at
3010–3100 Alkene C H, stretch, strong 25 Mrad is justified by the presence of alcohol ( OH), stretch, free
2500–3300 Acid ( COOH) stretch, strong
1700–1725 Acid (C O) stretch, strong
group at 3909 and 3930 cm−1 with absorbance values of 25% and
1550–1650 Amide (N H) bending, medium 11% respectively. Also the blend D has the maximum VRY. This
1210–1320 Acid (C O) stretch, strong is due to the availability of the acid ( COOH), stretch, free group
1345–1385 Nitro (N O) stretch, strong at wave numbers 2651 cm−1 with absorbance values of 1.5%. It
600–800 C Cl stretch, strong
is inferred that the blend A is found to have maximum VRY at
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614 607

Fig. 4. (a) FTIR Spectra for the blend C for 0 Mrad dose of gamma irradiation. (b) FTIR spectra for the blend C for 25 Mrad dose of gamma irradiation. (c) FTIR spectra for the
blend C for 100 Mrad dose of gamma irradiation. (d) FTIR spectra for the blend C for 200 Mrad dose of gamma irradiation. (e) FTIR spectra for the blend C for 250 Mrad dose
of gamma irradiation.

100 Mrad. This is due to the presence of alcohol ( COOH), stretch;
free at wave number 3917 cm−1 and 3785 cm−1 with absorbance
values of 18% and 74% respectively (as from Tables 1a–1c). From
Tables 1d and 1e, it can be observed that at 200 Mrad and above,
there is a decrease in alcohol ( OH) free group in blends A and
B. Except blend E, VRY of all the blends are slightly reduced at
200 Mrad. This may be due to the reduction in alcohol ( OH),
stretch, free group content. The drop in VRY of the blends A and
B are evident from Fig. 1(a) and (b). The resistivity decreases (those
values are greater than their virgin) at higher doses. This may be
due to the reduction in the carrier mobility. This is also because
of the higher cross-linking density (Roberto Benson et al., 1999).
The blend C has its highest VRY and SRY values at 250 Mrad. This
may due to the presence of acid ( COOH) at 2554 cm−1 with the
3% absorbance.
The blend C and EPDM rich blends (D and E) have an increased
SRY for all doses. This is due to the presence of acid ( COOH) group
at 2500–3300 along with alcohol ( OH) free group. The blend E has
the maximum SRY at 100 Mrad. This is due to the occurrence of alco-
hol ( OH), stretch, free group at wave numbers 3752 cm −1 with
the maximum absorbance 87%. The blend C has the minimum SRY.
This may be due to the reduced acid ( COOH) stretch, strong group
content at 2642–2434 cm−1 . The blend E has the maximum SRY at
200 Mrad. This is due to the occurrence of alcohol ( OH), stretch,
608 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
free group at wave numbers 3772 cm−1 with the absorbance 60%.
The blend C has the minimum SRY. This may be due to the reduc-
tion in acid ( COOH) stretch, strong group at 2750–2554 cm−1 . The
blends C and D have their maximum SRY values at 250 Mrad. The
blend C has the acid ( COOH) group at wave number 2554 cm−1
with the absorbance 3.
The tensile strength of the EPDM rich blend E is improved for
all doses of gamma radiation due to the cross-linking (dominant
ageing mechanism) (Gordana Markovic Milena et al., 2009; Emilie
Gautriaud et al., 2007; Zhang et al., 2003; Manisara Phiriyawirut
et al., 2008; Chin-Chiuan Kuo et al., 2012). New groups such as C H
(alkane, bending, strong), Si O Si at 1455 cm−1 have been noticed.
The complete disappearance of Si O Si at 1000–1160 cm−1 for
blend A at 25 Mrad, 100 Mrad, 200 Mrad indicate that chain scis-
sion has the dominating effect which results in the decrease in TS
of it. The reappearance of the same group at 250 Mrad indicates
that cross-linking has also occurred in blend A. The increased cross-
linking density results in reduced segmental mobility leading to
brittleness of the blend A. It is inferred that TS of the blends C and E
are improved at 25 Mrad. This is due to the availability of the new
groups such as C H (alkane, bending, strong) and Si O Si group
at wave numbers 1458 cm−1 and 1018 cm−1 with absorbance val-
ues of 22% and 19% respectively in blend C. Also the blend C has
larger C C (alkene, stretch, variable) content at 1629 cm−1 with
32% absorbance. The blend E is found to have the new groups such
as C H (alkane, bending, strong) and Si O Si group at wave num-
bers 1458 cm−1 and 1083 cm−1 with absorbance values of 9% and
17% respectively. It is inferred that blend E is found to have its max-
imum TS at 100 Mrad. This is due to the availability of the new
group C C (alkene, asymmetric stretch, strong) at 1949 cm−1 with
the absorbance values of 4%. TS of the blend C has been improved,
due to the increase in C C (alkene, stretch, variable) content at
1627 cm−1 with 32% absorbance. The TS of the blends C and D is
also improved due to the availability of new C C (aromatic stretch)
group at 1459 cm−1 and 1406 cm−1 with absorbance values of 19%
and 8% respectively.
For the higher doses, the appearance of C C (aromatic stretch)
has resulted in increase in TS of the blends C, D and E. It is inferred
that TS of the blends C and E are slightly reduced (even then
those values are greater their virgin values) at 200 Mrad. It may
be due to the absence of C C (alkene, stretch, variable), Si O Si
group in them. But the blend D has been found to have lesser drop
in TS value. This is due to the presence of C C (alkene, stretch,
variable) and Si O Si groups at 1638 cm−1 1018 cm−1 with 34%
and 24% absorbance. The blend C has the maximum TS at 250 Mrad.
This is due to the appearance of the new functional group C C
(aromatic stretch) at 1440 cm−1 with the absorbance 21%. The
EPDM rich blends (D and E) also have the increased TS. This is due
to the appearance of the C C (aromatic stretch) at wave numbers
1508 cm−1 , 1599 cm and 1600 cm−1 with the absorbance 50%, 60%
and 45% respectively. It is also inferred that TS of SiR rich blends
(A and B) are reduced. This is due to the absence of these groups in
them.
The elongation at break (EB) of all the blends is reduced for all
doses of gamma irradiation. This is due to the dominant cross-
linking reaction. This condition is validated by the formation of
new groups such as C H alkane (bending, strong), C C aromatic
stretch, C C alkene (asymmetric stretch, strong) in the band ranges
of (1350–1480) cm−1 , (1400–1600) cm−1 and (1900–2000) cm−1
respectively. The elongation values of the SiR rich blends (A and B)
are found to be lesser than 50% of their absolute elongation value
for all doses of gamma irradiation. But the EPDM rich blends (D and
E) and blend C are found to have better EB (greater than 50% of their
absolute elongation) values at 25 Mrad and 100 Mrad. This may be
due to the increase in C C alkene (stretch, variable) and Si O Si
content in them.
Table 2
Melting and curing/cross-linking temperature of virgin SiR-EPDM blends.
Blend Tm (◦ C) Tcure (◦ C)
A 227–292 –
B 217–279 379
C 149–167 273
D 180–208 263
E 166–195 260
The hardness of the blends (A, B, C and D) are decreased at
25 Mrad. This is due to the absence of C C (aromatic stretch) group
in them. The hardness of the blends (A, B, D and E) is increased with
respect to their virgin counterparts at 100 Mrad. But the hardness
of the blend C has been slightly reduced at 100 Mrad. The hard-
ness of all the blends is increased at 250 Mrad. The presence of C O
(carbonyl, stretch, strong) in blend B and the presence of C C (aro-
matic, stretch, strong) in blends C, D and E are responsible for the
increased hardness. The increase in C H alkane (bending, strong)
and Si O Si content has been noticed in blends A, C and D. The
increase in CH3 group content for all doses of gamma irradiation has
resulted in the improvement of hydrophobicity of the all blends.
5.4. Scanning electron microscopy (SEM) analysis
Fig. 5A1, B1, C1, D1 and E1 are the SEM micrographs of all the
samples of virgin blends for a magnification of 500. Fig. 5A2, B2,
C2, D2 and E2 are the SEM micrographs of all the five blends for a
4000 magnification. Fig. 6A1, B1, C1, D1, E1 and A2, B2, C2, D2, E2
are the SEM micrographs of all the blends exposed to 25 Mrad dose
of gamma irradiation for a magnification of 500 and 4000 respec-
tively. Fig. 7A1, B1, C1, D1, E1 and A2, B2, C2, D2, E2 are the SEM
micrographs of all the blends exposed to 250 Mrad dose of gamma
irradiation for a magnification of 500 and 4000 respectively.
It is inferred from Fig. 5, that the surface of the SiR rich blends
(A and B) had some rough corrugations and they have some ball
like micro structures. This may be due to the less miscibility of the
blends. Whereas the surface roughness of the EPDM rich blends (D
and E) are found to be less. The good miscibility of the EPDM rich
blends is indicating.
It is inferred from Fig. 6, the surface of SiR rich blends (A and
B) is un-even and has rough portions. The surface of blend A and
B has cracks. But the surface of blend C (50% SiR and 50% EPDM) is
smooth. The surface smoothness of EPDM rich blends (D and E) is
moderate and some voids are noticed in surface of blend D.
The surface of SiR rich blends (A and B) has highly deeper cracks.
Also the erosion of the material is noticed for 4000 magnification.
The surface of blend C (50% SiR and 50% EPDM) has a little amount
of erosion. The surface smoothness of EPDM rich blends (D and E)
is reduced due to the formation of some rough portions for 500
magnifications. At 4000 magnification, erosion has been observed
in blend D. The compatibility of the blend E is high.
5.5. Thermal analysis
5.5.1. Differential scanning calorimetry (DSC)
Fig. 8(a)–(c) shows the DSC thermograph of three different com-
positions of virgin SiR-EPDM blends (A, C and E). The melting and
curing/cross-linking temperatures of the virgin SiR-EPDM blends
are given in Table 2.
It is inferred from Table 2, the melting temperature range of
un-irradiated (virgin) SiR rich blends (A and B) is (227–292) ◦ C and
(217–279) ◦ C respectively. The blends C, D and E are found to have
Tm range at (149–167) ◦ C, (180–208) ◦ C and (166–195) ◦ C respec-
tively. The low melting point of blends C, D and E is due to the
higher EPDM content.
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
Fig. 5. SEM micrographs of all the samples of virgin blends – A1, B1, C1, D1 and E1
– 500 magnification; A2, B2, C2, D2 and E2 – 4000 magnification.
The cross-links may play some role in enhancing the melting
temperature of the blends. The higher melting point range of the
blends A and B suggest that the melting process is being controlled
by the occurrence of self cross-linking reaction during the blending
process. Hence the tensile strength of the virgin blends A and B are
higher than the remaining blends (C, D and E).
609
Fig. 6. SEM micrographs of all the samples of Gamma irradiated (25 Mrad) SiR-EPDM
blends – A1, B1, C1, D1 and E1 – 500 magnification; A2, B2, C2, D2 and E2 – 4000
magnification.
The cross-linking occurs in curing process is an exothermic
which results in a positive peak in DSC. The curing point of blend B
is 379 ◦ C, whereas the curing point of the other blends C, D and E lie
at 273 ◦ C, 263 ◦ C and 260 ◦ C. It is noticed that the Tcure of the blends
C, D and E are higher than that of the virgin EPDM whose curing
point lie between 130–175 ◦ C. The Tcure is totally absent in blend A.
This is due to the higher bonding energy of Si O bond (452 KJ/mol)
in SiR. Hence the cross-linking density of blend A is higher. Also this
may be due to the occurrence of larger amount of self cross-linking
reaction in it during the blending process itself. This is reflected in
610 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
Fig. 7. SEM micrographs of all the samples of gamma irradiated (250 Mrad) SiR-
EPDM blends – A1, B1, C1, D1 and E1 – 500 magnification; A2, B2, C2, D2 and E2 –
4000 magnification.
the tensile strength of virgin blend A (which is the highest among
the five blends).
Fig. 9(a)–(c) shows the DSC thermographs of gamma irradiated
(25 Mrad) blends A, C and E. Fig. 10 (a)–(c) shows the DSC thermo-
graphs of gamma irradiated (250 Mrad) blends A, C and E.
It is inferred from Fig. 9, the melting temperature (Tm ) of blend A
is reduced to 234 ◦ C. The blend A has the lesser probability of cross-
linking. The Tm of the remaining blends (B, C, D and E) are increased
to 290 ◦ C, 368 ◦ C, 229 ◦ C and 229 ◦ C, respectively. This may be due to
the higher probability of cross-linking reaction in them. The curing
temperature (Tcure ) of SiR rich blends (A and B) is decreased due to
lesser probability of cross-linking reaction in them. But the EPDM
rich blends (D and E) are found to have increased Tcure values of
Fig. 8. DSC thermographs of different compositions of Virgin SiR/EPDM Blends (a)
– Blend A, (b) – Blend C, (c) – Blend E.
375 ◦ C and 359 ◦ C. The blend C is also found to have higher Tcure of
380 ◦ C. Among the five blends blend C is found to have a highest
tensile strength value at 25 Mrad. The tensile strength of the EPDM
rich blends (D and E) is higher than SiR rich blends (A and B). This
may be due to the higher probability of cross-linking.
It is inferred from Fig. 10, Tm of blend A is increased to 309 ◦ C
(which is greater than 25 Mrad case). The Tm values of EPDM rich
blends (D and E) are increased to 261 ◦ C and 280 ◦ C, respectively.
Tcure of the SiR rich blends (A and B) are reduced slightly which
are less than their un-irradiated case. Hence reduction in tensile
strength is noticed at 250 Mrad. This may be due to the lesser
probability of cross-linking. The blend C is found to have highest
Tcure value. Hence tensile strength of the blend C is highest among
the remaining blends. The Tcure of the EPDM rich blends (D and E)
are reduced slightly when compared with 25 Mrad case. Even then
those are greater than virgin ones.
5.5.2. Thermo gravimetric analysis (TGA)
Fig. 11(a)–(c) shows the TGA curves of three different compo-
sitions of SiR/EPDM blends (blend A, C and E) along with their
derivative weight (DW) curves.
The high peak of melting temperatures suggest the melting
process is being kinetically arrested by cross-linking, thereby
resulting in higher melting temperatures. Fig. 12(a)–(c) shows the
TGA curves of three different compositions of gamma irradiated
(25 Mrad) SiR/EPDM blends (blend A, C and E) along with their
derivative weight (DW) curves
Fig. 13(a)–(c) shows the TGA curves of three different composi-
tions of gamma irradiated (250 Mrad) SiR/EPDM blends (blend A, C
and E) along with their derivative weight (DW) curves.
The pyrolysis of elastomers characteristics of the virgin and
gamma irradiated SiR-EPDM blends (25 Mrad and 250 Mrad) are
given in Tables 3a–3c, respectively.
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614 611

Fig. 10. DSC thermographs of different compositions of gamma irradiated

(250 Mrad) SiR/EPDM Blends (a) – Blend A, (b) – Blend C, (c) – Blend E.

Table 3c
Fig. 9. DSC thermographs of different compositions of gamma irradiated (25 Mrad) Pyrolysis of elastomers (POE) of gamma irradiated SiR-EPDM blends at 250 Mrad.
SiR/EPDM Blends (a) – Blend A, (b) – Blend C, (c) – Blend E.
Blend Ti (◦ C) Tf (◦ C) POE (%)

A 217 219 3.04

Table 3a 351 402 73.48
Pyrolysis of elastomers (POE) of virgin SiR-EPDM blends. 448 474 19.39
B 351 399 64.2
Blend Ti (◦ C) Tf (◦ C) POE (%) 446 472 20.39
A 360 399 61.42 C 227 306 18.27
447 466 11.43 451 491 48.71
B 359 100 62.56 D 316 362 35.98
445 470 13.24 445 485 44.92
C 207 318 31.64 E 217 296 18.72
462 492 36 85 461 490 38.83
D 218 328 44.9
458 490 44.71
E 204 316 33.07
459 489 40.13
The pyrolysis of elastomers is a thermo-chemical decomposition
of organic material at elevated temperatures without the partici-
Table 3b
pation of oxygen. The pyrolysis involves the simultaneous change
Pyrolysis of elastomers (POE) of gamma irradiated SiR-EPDM blends at 25 Mrad. of chemical composition and physical phase, and is irreversible. All
the virgin blends are found to experience two step decomposition.
Blend Ti (◦ C) Tf (◦ C) POE (%)
It is inferred from Table 3a, the temperature at which loss of volatile
A 344 401 81.02 components (Ti ) is initiated at 360 ◦ C and 359 ◦ C in the virgin SiR
446 470 13.11
rich blends (A and B). The blend C and EPDM rich blends (D and E)
B 343 39S 79.28
C 221 293 15.33 are found to have Ti values of 207 ◦ C, 218 ◦ C and 204 ◦ C, respectively.
382 40S 7.978 The final decomposition temperature (Tf ) of SiR rich blends (A and
463 492 42.55 B) is 466 ◦ C and 470 ◦ C respectively. The Tf of blend C and EPDM
D 213 296 22.38 rich blends (D and E) are 492 ◦ C, 490 ◦ C and 489 ◦ C, respectively.
391 413 8.845
The difference between the Ti and Tf is smaller in SiR rich blend
463 491 42.24
E 22S 328 13.07 (A and B). This may be due to the occurrence of higher level of self
461 492 43.49 cross-linking during the blending process itself. The blends C, D and
E are found to have larger difference between the Ti and Tf . This is
612 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
Fig. 11. TGA thermographs of different compositions of virgin SiR/EPDM Blends (a)
– Blend A, (b) – Blend C, (c) – Blend E.
may be due to the occurrence of lower level of self cross-linking
reaction in them during the blending process.
The drop in initial temperature (Ti ) and rise in final decomposi-
tion temperature (Tf ) is noticed in blend A at 25 Mrad and 250 Mrad.
The reason for this effect is the higher cross-linking density (HCLD)
of blend A. At 25 Mrad both Ti and Tf decreases in blend B. This
results in moderate cross-linking density (MCLD) in blend B. But
at 250 Mrad, drop in Ti and rise in Tf is noticed in blend B. This
contributes the HCLD.
The rise in initial temperature (Ti ) is noticed in blend C at
25 Mrad and 250 Mrad. The final decomposition temperature (Tf )
remains constant at 25 Mrad and undergoes a slight reduction at
250 Mrad. Also the blend E is found to have a drop in Ti and rise in
Tf at 25 Mrad and 250 Mrad. This may be due to the dominant cross-
Fig. 12. TGA thermographs of different compositions of gamma irradiated (25 Mrad)
SiR/EPDM Blends (a) – Blend A, (b) – Blend C, (c) – Blend E.
linking reaction in them. The probability of cross-link formation in
blend C and E are increased. This results in moderate cross-link den-
sity (MCLD) values for blend C and E. The blend D has drop in Ti and
rise in Tf at 25 Mrad. At 250 Mrad, rise in Ti and fall in Tf is noticed
in blend D. Hence blend D is found to have LCLD. Table 4 gives the
maximum degradation temperature virgin and gamma irradiated
SiR-EPDM blends (25 Mrad and 250 Mrad).
The maximum degradation temperature (Tmax ) of the un-
irradiated SiR rich blends (A and B) is lesser than un-irradiated
blend C and EPDM rich blends (D and E). With the gamma
irradiation exposure, Tmax of blend B is decreased at 25 Mrad
and 250 Mrad. This is due to the lesser probability of cross-link
formation in it. At 25 Mrad, Tmax of blend C and E is increased.
 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614 613

The Tmax of blend E is increased at 250 Mrad. This may be due

to the dominant cross-linking reaction in them. The probability of
cross-link formation in blend C and E are increased. This results in
moderate cross-link density (MCLD) values for blend C and E. At
250 Mrad, drop in Tmax is noticed in blends C and D. Hence blend D
is found to have LCLD.

6. Conclusions

The electrical parameters such as volume resistivity and surface

resistivity of all the blends are found to improve for all doses of
gamma irradiation The un-irradiated SiR rich blends A and B are
found to have the maximum VRY, SRY, TS and EB due to the occur-
rence of dominant self cross-linking reaction during the blending
process itself. The un-irradiated EPDM rich blends D, E and also
the blend C are found to have the moderate VRY, SRY, TS and EB
values. Because they have the lesser probability of cross-linking
reaction.
After the gamma exposure of 25 Mrad, VRY, SRY of the SiR rich
blends A and B are improved due to the HCLD with a simultaneous
decrease in TS and EB. The SiR rich blends A and B are found to have
the highest VRY at 100 Mrad and highest SRY at 25 Mrad. This is
due to the dominant cross-linking reaction with HCLD. But for the
higher doses of gamma irradiation, VRY and SRY decreased along
with the decrease in TS and EB. This is due to the occurrence of dom-
inant chain scission reaction in them along with lesser probability
of cross-linking.
The VRY, SRY of the EPDM rich blends D, E and blend C are
improved for all doses of gamma irradiation. The TS of blend E is
improved for all doses of gamma irradiation. This is due to occur-
rence of gamma induced dominant cross-linking reaction in them.
This is due to MCLD.
The elongation at break of all the five blends has been reduced,
for all doses of gamma irradiation. But the blends C, D and E are
found to have EB (greater than 50% their absolute elongation) values
at 25 Mrad and 100 Mrad. Among the five blends, blend C is found
to have the least deterioration in elongation value.
On the whole, the blend C and the EPDM rich blends (D and
E) are found to have improved electrical properties (volume resis-
tivity and surface resistivity) along with the reduced elongation,
improved tensile strength and hardness.
The factor behind all these effects may be due to the formation
of new functional groups and dominant cross-linking mechanism
during the gamma exposure.
The blend C has a significant improvement in SRY, VRY along
with an insignificant decrease in EB for all doses. The TS of the
blend C is improved for all doses. It is concluded that the blend
C and the EPDM rich blends (D and E) are found to have the supe-
Fig. 13. TGA thermographs of different compositions of gamma irradiated
rior performance when compared with SiR rich blends (A and B).
(250 Mrad) SiR/EPDM Blends (a) – Blend A, (b) – Blend C, (c) – Blend E.
Hence among the three different compositions of EPDM rich blends,
suitable blend can be selected for a particular NPP application.
The selection may be based on the predicted performance of these
blends under accumulated doses.
Table 4
Maximum degradation temperature virgin and gamma irradiated SiR-EPDM blends
(25 Mrad and 250 Mrad).

Blend Tmax -degree (◦ C)

Acknowledgements
0 Mrad 25 Mrad 250 Mrad

A 383.74 383.74 383.94 The authors gratefully acknowledge the financial support
B 386.15 381.33 384.94 extended by SSN College of Engineering for carrying out this
C 478.89 482 51 476.49 research work. The authors are also conveying their sincere grat-
D 478.89 478.89 471.67
itude to the Radiological Safety Division, Indira Gandhi Centre for
E 478.89 481.3 480.1
Atomic Research (IGCAR), Kalpakkam, Tamil Nadu, India for pro-
viding the gamma irradiation facility.
614 D. R., R. V. / Nuclear Engineering and Design 273 (2014) 602–614
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