Journal of Non-Crystalline Solids 356 (2010) 856–863

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Journal of Non-Crystalline Solids

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

Radiation induced modification of dielectric and structural properties

of Cu/PMMA polymer composites
Dolly Singh a, N.L. Singh a,*, Anjum Qureshi a,b, P. Kulriya c, Ambuj Tripathi c, D.K. Avasthi c, Arif N. Gulluoglu b
a
Department of Physics, M.S. University of Baroda, Vadodara 390002, India
b
Department of Metallurgical and Materials Engineering, Marmara University, 81040 Istanbul, Turkey
c
Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110067, India

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

Article history: In this study, composite films consisting of an insulating polymethyl methacrylate (PMMA) polymer
Received 11 October 2009 matrix and metal powder (Cu) additive were prepared by solution costing method. These films were irra-
Received in revised form 23 December 2009 diated with 140 MeV silver ions at the fluences of 1  1011 ions/cm2 and 1  1012 ions/cm2. The radiation
Available online 3 February 2010
induced changes in dielectric, structural and surface properties of PMMA/Cu composites were studied
using impedance/gain phase-analyzer, X-ray diffraction (XRD), scanning electron microscopy (SEM),
Keywords: and atomic force microscopy (AFM). It was observed that the dielectric properties and ac electrical con-
Measurement techniques
ductivity increased significantly with the concentration of dispersed metal powder (Cu) and also with the
Polymers and organics
Radiation
fluence. This reveals that ion beam irradiation creates free radicals, unsaturation etc. due to emission of
Thermal properties hydrogen and/or other volatile gases, which makes the polymer more conductive. XRD analysis of the
pristine and irradiated samples shows that the crystallinity improved upon irradiation at low fluence
and deteriorated on further increase of the fluence, which could be attributed to cross linking of polymer
chains at low fluence and degradation at higher fluence. High energy ion beam irradiation of semicrys-
talline polymer composite films changes its Tg behavior as observed from DSC analysis. This result is also
corroborated with the results of XRD. The average surface roughness and topography of surfaces changed
with the concentration of filler and also with the ion fluence as revealed from AFM/SEM analysis.
Ó 2010 Elsevier B.V. All rights reserved.

1. Introduction tivity. The abrupt increase in electrical conductivity is called the

Conductive metal polymer composites are becoming important
owing to their potential applications such as antistatic materials,
self regulating heater, electromagnetic absorbing material and pre-
vention of static electricity accumulation [1,2]. It is found that the
electrical performance of the material is highly dependent on com-
posites microstructure in addition to the nature of filler [3]. On the
basis of this consideration, electrical percolation threshold can be
adjusted either by segregated distribution or by selective distribu-
tion of filler during manufacturing [4]. At low filler loadings, the
particles are almost homogenously distributed in polymer matrix
without any contact between adjacent filler particles. The conduc-
tivity of these composites is comparable to that of polymer matrix.
With increasing filler concentration, however, the filler particles
begin to form cluster in which the particles are contact with each
other. At a certain filler concentration, the growing clusters reach
a size which enables contacts between them and a continuous
network structure of the conducting filler is formed. The network
formation can be detected as a drastic increase in electrical conduc-
percolation threshold of the filler material [5].
Swift heavy ion (SHI) is the technique that provides a general
method for the modification of physical, chemical, and mechanical
properties of the polymer/polymer composites [6,7]. By controlling
the experimental conditions (monomer concentrations, radiation
dose rates, and irradiation environments) one can tailor the final
properties of the materials in order to produce new materials for
specific application. Interaction of high energy ion beam with poly-
mer results in the formation of gaseous products accompanied by
polymer crosslinking (i.e. formation of intermolecular bonds), deg-
radation (i.e. scission of bonds in the main polymer chain and in
side chains) and some other secondary processes [8].
The present work reports the development of polymethylmeth-
acrylate (PMMA)/Cu composites and to study the electrical and
structural behaviors as a function of filler concentration and irradi-
ation fluence. A systematic study of SHI induced effect on the elec-
trical and structural properties of polymer composites is not much
reported.
2. Experimental details

* Corresponding author. Tel.: +91 265 2795339; fax: +91 265 2795569. Polymethylmethacrylate (PMMA) (molecular weight 36,000)
E-mail address: singhnl_msu@yahoo.com (N.L. Singh). was purchased from Vesbo Company, Turkey and Cu metal powder

0022-3093/$ - see front matter Ó 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jnoncrysol.2010.01.006
 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863
with average particle size of the order of 50 lm was purchased
from Alfa Aesar (USA). The filler concentration was varied from
10–40% (w/w) in the composites. Filled PMMA composites were
prepared by mixing of Cu-filler with PMMA matrix by means of
solution casting method. Tetrahydrofuran (THF) was used as a sol-
vent to dissolve the polymer. The mixture of polymer and filler was
stirred at ambient temperature using magnetic stirrer at a high
speed of around 700 rpm until all polymer grains were dissolved.
After obtaining a homogeneous mixture, the mixture was poured
on clean glass trough. The solvent was evaporated at ambient tem-
perature (25 °C, 1 °C) to get films (thickness120 lm) of polymer
composites which were then dried in vacuum oven at 30 °C [9].
The prepared polymer composite films were irradiated with
140 MeV Ag11+ ions in the material science facility of the 15 UD
Pelletron at Inter University Accelerator Centre (IUAC), New Delhi,
India. The projected range (Rp) and energy loss were calculated
using code SRIM-2003 [10]. The projected range, electronic energy
loss (Se) and nuclear energy loss (Sn) of 140 MeV Ag11+ ions in
PMMA was found to be 24 lm, 9.6  102 eV/Å and 2.9 eV/Å,
respectively. The ion beam was scanned in X–Y plane in order to
expose the target of an area of 1  1 cm2. The beam current was
kept of the order of 0.5 pnA and irradiated at the fluences of
1  1011 and 1  1012 ions/cm2.
The alternating current (ac) and dielectric properties of the
composite films were measured by means of impedance/gain
phase-analyzer (Solartron 1260) in the frequency range 100 Hz to
10 MHz at ambient temperature. The XRD analysis was carried
Fig. 1. Frequency dependence of the dielectric constant of PMMA/Cu composites at different filler concentration for (a) pristine samples, (b) irradiated at a fluence of
1  1011 ions/cm2, and (c) irradiated at a fluence of 1  1012 ions/cm2.
Fig. 2. Frequency dependence of the dielectric loss of PMMA/Cu composites at different filler concentration for (a) pristine samples, (b) irradiated at a fluence of 1  1011 ions/
cm2, and (c) irradiated at a fluence of 1  1012 ions/cm2.
857
out using powder X-ray diffractometer (Bruker D8 advance) with
Cu–Ka radiation (k = 1.5418 Å). The angle of incidence between
the beam and sample surface was kept at 0.1°, and the diffraction
patterns were recorded in the range of 5–60°. The surface topogra-
phy of pristine and irradiated surfaces was studied using an atomic
force microscopy (AFM) in the tapping mode (Digital Nanoscope
IIIa Instrument Inc.) and also with scanning electron microscopy
(SEM) (F Model: JEOL JSM 5600). Differential scanning calorimetry
(DSC) measurement was carried out in the temperature range 30–
150 °C with a heating rate of 5 °C/min for all measurements. More-
over, our DSC results are correlated to X-ray diffraction results.
3. Results
3.1. Electrical properties of composites
The capacitance and dielectric loss were measured in the fre-
quency range 100 Hz–10 MHz using an impedance gain phase-ana-
lyzer. Fig. 1(a)–(c) shows the variation of dielectric constant of
PMMA/Cu composites as a function of frequency at different con-
centration of Cu-filler and at a different fluence of Ag11+ ions
(140 MeV). For a pure PMMA film, the dielectric constant is 2.5
at a frequency of 1 MHz. After inserting 10% Cu-particles in poly-
mer matrix, the dielectric constant increased to 8.8. It was ob-
served that the dielectric constant increases with increasing the
concentration of the copper. Similar results were also observed
858 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863

by the number of researchers [11,12–15]. The dielectric constant

was found to increase further upon SHI irradiation.
Frequency dependence of the dielectric loss of the composites
as a function of filler and fluence are shown in Fig. 2(a)–(c). It is ob-
served that the dielectric loss decreases exponentially and became
less dependent on frequency. Dielectric loss is also observed to in-
crease as fluence increased.
Fig. 3(a)–(c) shows the conductivity of PMMA/Cu composites
with frequency of applied electric field, filler concentration, and
fluence. It is observed that the conductivity increases gradually
with frequency for pure PMMA and 10% Cu composite, while for
higher filler concentration conductivity is observed to be frequency
independent up to 1 MHz and then shows strong dependence on it.
Our results are supported with measurement of McLachlan et al.
[16]. Conductivity is also observed to increase with increasing
the fluence of ion beam.

3.2. X-ray diffraction (XRD)

Fig. 5(a) shows the spectra of pure PMMA and showing the Fig. 4. Variation of conductivity with filler concentration at a frequency of 1 MHz
amorphous nature. Fig. 5(b) and (c) represents the PMMA/Cu com- for pristine and irradiated samples.

posites (for 10% and 40% Cu) before and after SHI irradiation at dif-
ferent fluences. The peaks are obtained at 2h = 38.92, 43.28, 45.26,
3.4. Surface morphology
and 50.43 in all the cases. The nature of peaks indicates the semi
crystalline nature of the samples.
Surface morphology of pristine and irradiated composites was
The most prominent peaks are observed around 2h = 43.28 and
studied using atomic force microscopy in contact mode. The 3-
50.43 in all cases. These peaks are due to pure Cu metal (JCPDS: 85-
dimensional morphology of pristine and irradiated (at a fluence
1326) and another peaks are due to copper oxide (CuO) at around
of 1  1012 ions/cm2) samples are shown in Fig. 7(a)–(d) on
38.92 and 45.26 (JCPDS: 80-0076). It means the composite materi-
5  5 lm2 area. The average surface roughness values are 0.54
als are accompanied by an inter phase of CuO between polymer
and 23.0 nm for pristine composites with filler concentration of
matrix and Cu-filler.
10% and 40%, respectively and those of irradiated samples, the
roughness values are 1.53 and 31.52 nm, respectively. SEM images
3.3. Differential scanning calorimeter (DSC) were taken for pristine and irradiated samples of 10% and 40% Cu
dispersed PMMA composites at 15 kX magnification. There are sig-
Polymethylmethacrylate (PMMA) is a well-known thermoplas- nificant changes in surface topography after irradiation. Fig. 8(a)–
tic polymer exhibiting the glass transition temperature Tg (charac- (d) shows SEM images of pristine and irradiated composites.
teristic of amorphous phase). Fig. 6 shows DSC thermograms of
pristine PMMA, pristine and irradiated PMMA + 40% Cu composite
samples. Tg of the pure PMMA is observed at 72.9 °C and 4. Discussions
PMMA + 40% Cu composite pristine and irradiated at fluences of
1  1011 and 1  1012 ions/cm2 at 95.9, 98.5, and 93.5 °C, Conductivity of the material was calculated using following
respectively. equation

Fig. 3. Frequency dependence of the conductivity of PMMA/Cu composites at different concentration of Cu-filler (10% to 40%) for (a) pristine samples, (b) irradiated at a
fluence of 1  1011 ions/cm2, and (c) irradiated at a fluence of 1  1012 ions/cm2.
 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863 859

2pfC p Dt C 0 ¼ eo A=t ðivÞ

r¼ ðS=mÞ ðiÞ
A
where, A and t are the area of electrode and thickness of the sample,
where Cp is the capacitance measured, f is the frequency, D is dielec- respectively. eo permittivity of vacuum = 8.85  1012 F/m.
tric loss, A and t are the cross sectional area of the electrode and Fig. 1(a)–(c) represents the enhancement in dielectric constant.
thickness of the sample, respectively. The enhancement in dielectric constant is attributed to interfacial
The general expression for the complex dielectric permittivity polarization of heterogeneous system consisting of phases with
(e*) of a material is considered as different dielectric permittivities and conductivities. The system
e ¼ e0  ie00 ðiiÞ under investigation is a heterogeneous system, i.e. PMMA/Cu com-
posites with different concentrations of copper metal dispersed in
The real part of the permittivity is defined as the polymer matrix. It became more heterogeneous as filler con-
0
e ¼ Cp=C 0 ðiiiÞ centration is increased in the system due to the formation of inter-
faces between the dispersed phase and polymer matrix. At low
where, C0 is defined as content of Cu metal, the metal particles are isolated, i.e., placed

Fig. 5. XRD spectra of (a) Pure PMMA sample, (b) PMMA + 10% Cu of pristine and irradiated samples, (c) PMMA + 40% Cu of pristine and irradiated samples.
860 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863
so far apart that there is no interaction between them. As the Cop-
per content is increased, clusters of particles are formed. A cluster
may be considered as a region in the polymer matrix where metal
contents are in physical contact or very close to each other. The
average polarization associated with a cluster is larger than that
of an individual particle because of an increase in the dimensions
of the metallic inclusion and, hence, greater interfacial area [17–
20]. From this point of view, the dielectric constant of the compos-
ites will be higher than that of the pure polymer. The experimental
results in Fig. 1 are in agreement with this explanation. The in-
crease in dielectric constant of irradiated samples may be attrib-
uted to the disordering of the material by means of chain
scission in polymer composites. Radicals or dangling bonds are
created by the release of pendant atoms such as hydrogen. Cross-
linking occurs when two dangling bonds on neighbouring chains
unite [8,21]. The increase in dielectric loss with increasing filler
contents may be attributed to the interfacial polarization mecha-
nism of the heterogeneous system. Further, moderate increase in
tan d occurs due to the irradiation [22].
The conductivity of the composite is related directly to the con-
ductivity of filler, the matrix and quality of the electrical network
form. The increase in conductivity with increasing frequency and
filler concentration/ion fluence is a common respond for polymer
composites (Fig. 3(a)–(c) and Fig. 4). It is assumed that an electrical
conducting path and network of connections could be formed in
composites with increasing the filler. It is known that electrical
conductivity of such composite depends on the type and concen-
tration of the dispersed filler. As shown in figure, there are two
trends, the first one (from 100 Hz to 1 MHz) is frequency indepen-
dent conductivity and another (from 1 MHz to 10 MHz) is fre-
quency dependent conductivity for 20–40% composites as shown
in Fig. 3(a)–(c). The first trend is contributed by free charges avail-
able in the composite system whereas the second, which is fre-
quency dependent conductivity, is due to trapped charges which
are only active at higher frequency [23,24]. As shown in figure,
0% and 10% composites behave as a insulating phase and after fur-
ther doping at higher concentration, samples show conductive
Fig. 6. DSC patterns for pure PMMA (pristine); pristine and irradiated PMMA + 40% Cu composites at two different fluences.
behavior [16]. It is also observed that the conductivity increases
with increasing irradiation fluence. Irradiation is expected to pro-
mote the metal to polymer bonding and convert the polymeric
structure into a hydrogen depleted carbon network due to emis-
sion of hydrogen and/or other volatile gases. It is this carbon net-
work that is believed to make the polymers more conductive [25].
The X-ray diffraction patterns indicate that the intensity of dif-
fraction peaks of PMMA/Cu composites increases gradually at low
fluence (1  1011 ions/cm2) but decreases on further increase of the
fluence (1  1012 ions/cm2) for both composite samples, Fig. 5(b)
and (c). The increase in intensity at low fluence means that the
sample became crystalline at low fluence but on further increase
of the fluence, the intensity of the diffraction peaks decreased
and broadened and tends towards the amorphisation at higher flu-
ences due to increase of unsaturation, free radicals etc. The crystal-
lite size has been calculated before and after the irradiation using
Scherrer’s equation [26].
b ¼ Kk=L cos h ðvÞ
where b is FWHM in radians, k is the wavelength of X-ray beam
(1.5418 Å), L is the crystallite size in Å, K is a constant which varies
from 0.89 to 1.39, but for most cases it is close to 1. The percentage
crystallinity of the composites was determined by area ratio meth-
od. In this method the areas of amorphous and crystalline parts of
the pattern were calculated. The average crystallite size and crystal-
linity (%) are listed in Table 1. The appearance of sharp peak in com-
posite indicates some degree of crystallinity and the degree of
crystallinity increases upon irradiation of PMMA/Cu composites at
a fluence of 1  1011 ions/cm2 (Table 1) for both composites (i.e.
10%, 40%). Interaction of ion beam with composite resulted in the
formation of gaseous products accompanied by cross-linking i.e.
formation of intermolecular bonds at the fluence of 1  1011 ions/
cm2. On further increase of the fluence, irradiation induced large
amount of energy deposition in the composite and leads to decrease
in crystallite size, which may be attributed to splitting of crystalline
grains [27].
 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863 861

Fig. 8. SEM images of (a) PMMA + 10% Cu (pristine), (b) PMMA + 10% Cu (fluence
Fig. 7. AFM images of (a) PMMA + 10% Cu (pristine), (b) PMMA + 10% Cu (fluence 1  1012 ions/cm2), (c) PMMA + 40% Cu (pristine), and (d) PMMA + 40% Cu (fluence
1  1011 ions/cm2), (c) PMMA + 40% Cu (pristine), and (d) PMMA + 40% Cu (fluence 1  1012 ions/cm2).
1  1012 ions/cm2).
862 D. Singh et al. / Journal of Non-Crystalline Solids 356 (2010) 856–863

Table 1
FWHM, crystallite size and % crystallinity of pristine and irradiated Cu/PMMA composites for 10% and 40% concentration of filler.

Two theta FWHM Crystallite Size Crystallinity Two theta FWHM Crystallite size Crystallinity
(deg.) (B rad.) (nm) (%) (deg.) (B rad.) (nm) (%)
Pristine (PMMA + 10% Cu) Pristine (PMMA + 40% Cu)
38.928 0.2032 46.08 1.24 38.914 0.1670 57.03 1.67
43.282 0.2029 46.82 6.35 43.262 0.1854 51.33 16.26
45.261 0.2195 43.57 0.88 45.239 0.1859 45.29 2.71
50.437 0.2861 34.10 4.71 50.396 0.2612 37.56 7.19
Average crystallite size = 42. 64 ± 5.86 nm Average crystallite size = 47.80 ± 8.34 nm
Average crystallinity = 3.29 ± 2.67% Average crystallinity = 7.0 ± 6.64%
1  1011 ions/cm2 (PMMA + 10% Cu) 1  1011 ions/cm2 (PMMA + 40% Cu)
38.90 0.1728 54.18 7.7 38.820 0.1733 55.0 1.94
43.259 0.1899 50.00 5.6 43.165 0.1890 50.32 8.86
45.231 0.2019 47.3 2.5 45.157 0.1893 50.65 1.07
50.38 0.2743 35.5 1.13 50.306 0.2595 37.65 6.22
Average crystallite size = 46.78 ± 8.01 nm Average crystallite size = 48.40 ± 7.48 nm
Average crystallinity = 4.32 ± 2.91% Average crystallinity = 9.82 ± 3.73%
l  1012 ions/cm2 (PMMA + 10% Cu) l  1012 ions/cm2 (PMMA + 40% Cu)
38.89 0.1968 47.57 4.63 38.877 0.1745 53.65 1.57
43.28 0.2365 24.09 3.26 43.227 0.2072 46.66 7.87
45.23 0.2176 43.9 0.77 45.210 0.1943 49.67 0.82
50.40 0.278 35.10 0.58 50.378 0.2738 35.81 5.22
Average crystallite size = 37.66 ± 10.45 nm Average crystallite size = 46.32 ± 7.64 nm
Average crystallinity = 2.31 ± 1.97% Average crystallinity = 3.87 ± 3.28%

Considering the thermal properties of the composites, we must
point out the important property of the glass transition tempera-
ture (Tg) of polymer. This is defined as the temperature where
the plastic becomes hard and brittle when cooled rapidly after
heating. At the glass transition temperature, the weak secondary
bonds that stick the polymer chains are broken, and the macromol-
ecule starts to move. As shown in Fig. 6, the increase in Tg of com-
posite may be due to the interaction of Cu metal particles with
PMMA in more ordered state [28,29]. It is also observed that Tg
of composite shifted towards higher temperature at a fluence of
1  1011 ions/cm2, which reveals that the composite became more
crystalline. On further increase of the fluence (i.e. 1  1012 ions/
cm2) , Tg shifted to lower temperature, which reveals that the irra-
diation leads to chain scission and subsequently reduction in
molecular weight. As a result, the system is changing towards
more disordered state. It is also confirmed with XRD results.
The Change in surface morphology of PMMA/Cu composites be-
fore and after ion beam irradiation can be seen from the series of
AFM images as shown in Fig. 7(a)–(d) and SEM images as shown
in Fig. 8(a)–(d). SEM images show the agglomerated metal particles
in the composites. The increase in surface roughness (Ra) with
increasing concentration of metal particles may be due to the in-
crease of density and size of metal particles on the surfaces of
the polymeric films [30]. The increase in surface roughness due
to irradiation may be attributed to large sputtering effect [29].
SEM images are used to examine the texture of the fractured
surface of the composites. It can be seen that the metal particles
are isolated at 10% Cu-filler i.e. there is no interaction between
them (Fig. 8(a)). As the Cu content is increased (i.e. 40% Cu-filler),
clusters of metal particles are formed (Fig. 8(c)). A cluster may be
considered as a region in the polymer matrix, where particles are
in physical contact or very close to each other. Aggregates of micro
cluster are clearly visible on the surface and metal/polymer phases
increase due to ion beam irradiation as shown in Fig. 8(b) and (d).
5. Conclusions
The ac conductivity of the composites increases with increasing
the frequency, concentration of filler and also with ion fluence. The
dielectric constant and dielectric loss are observed to change sig-
nificantly with filler concentration and ion fluence. The increase
in conductivity and dielectric properties of the composites due to
ion beam irradiation may be attributed to (1) metal to polymer
bonding and (2) conversion of the polymeric structure into a
hydrogen depleted carbon network due to the emission of hydro-
gen and/or other volatile gases. Thus irradiation makes the poly-
mer more conductive. The X-ray diffraction patterns of the
composites show an increase in crystallinity at a fluence of
1  1011 ions/cm2 and decreases on further increase of the fluence.
It means polymer composite improved the crystallinity at low flu-
ence and tends to change into the amorphous phase on further in-
crease of the fluence. Thermal property of the composite was
studied by DSC analysis and it reveals that the Tg shifted towards
higher temperature at low fluence and shifted towards lower tem-
perature on further increase of fluence. It means that the compos-
ite system is moving towards the crystalline state at low fluence
and tends to change towards disordered state (amorphous) at
higher ion fluence. XRD analysis also supports these results. The
surface roughness increases as filler concentration increases and
also with the ion fluence as revealed from AFM studies. SEM micro-
graphs reveal a texture consisting of agglomerates of Cu-particles
with path contacts in matrix.
Acknowledgements
Authors are thankful to the operating staff of Pelletron, Inter
University Accelerator Centre, New Delhi for providing irradiation
facilities. Financial support given by IUAC, New Delhi is gratefully
acknowledged. UGC-DRS Lab is also gratefully acknowledged.
One of the author (A.Q.) is thankful to the TUBITAK fellowship of
Turkey.
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