Nuclear Instruments and Methods in Physics Research B 268 (2010) 36–41

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Nuclear Instruments and Methods in Physics Research B

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

Effect of ion irradiation on the M-Nitroaniline single crystals

T. Kanagasekaran a,*, P. Mythili b, Binay Kumar a, R. Gopalakrishnan b
a
Department of Physics and Astrophysics, University of Delhi, Delhi 110 007, India
b
Department of Physics, Anna University, Chennai 600 025, India

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

Article history: In this report, the modifications in the structural, optical, mechanical, electrical and nonlinear properties
Received 10 March 2009 of 70 MeV Li3+ and 100 MeV Ag7+ ion irradiated M-Nitroaniline single crystals are studied. The irradiation
Received in revised form 20 September induced defect structures at the crystal surface which becomes more prominent at higher irradiation flu-
2009
ences, leading to the enhancement in the optical absorption behaviour and the nonlinear property of the
Available online 27 September 2009
irradiated crystals. The mechanism leading to the enhanced nonlinearity and the blue shift of the irradi-
ated M-NA crystals has been discussed.
PACS:
Ó 2009 Elsevier B.V. All rights reserved.
71.55. i
74.25.Gz
74.62.Dh
76.30.Da
42.65. k

Keywords:
Impurity and defect levels
Optical properties
Effects of crystal defects, doping and
substitution
Ions and impurities
Nonlinear optical properties

1. Introduction
Organic materials offer flexibility to molecular design, virtually
an unlimited number of crystalline structures have a high damage
resistance to optical radiation. Hence, these materials make it
desirable to replace electronic switching circuits in computing
and telecommunication systems. Certain classes of organic mole-
cules possess large second order nonlinear optical (NLO) co-effi-
cient (b). For optimization of second order nonlinearities in
organic molecules two properties are particularly important in
addition to non-centrosymmetry i.e., strong p electron delocaliza-
tion and intramolecular charge transfer stimulated by the presence
of electron donor and acceptor groups. Crystals of nitroaniline
derivatives exhibit the largest second order susceptibilities re-
ported to date for organic solids. Meta-Nitroaniline (M-NA) is a
material with useful electro–optic properties. The effect of SHG
of M-NA is one order higher than that of LiNbO3 [1]. Unlike most
electro–optic crystals, M-NA combines low-permittivity with good
* Corresponding author. Address: Crystal Lab, Department of Physics and
Astrophysics, University of Delhi, Delhi 110 007, India.
E-mail addresses: kanagasekaran@gmail.com, kanagasekaran@yahoo.com (T.
Kanagasekaran).
electro–optic behaviour. This, together with its easy growth into
large single crystals, makes M-NA an attractive material for many
practical applications, such as digital deflectors for fast access large
scale memories.
Ion implantation provides an alternative method of introducing
dopant atoms into the lattice. In this case, a beam of dopant ions
accelerated through a potential of typically 10–100 kV is allowed
to impinge on the surface of the target atom. To achieve deep pen-
etration of ions, the ions must interact and collide, individually or
collectively, with atoms of the solid matrix. During these collisions,
energy will be exchanged between the moving ion and the station-
ary lattice atoms with a concomitant energy loss by the ions and an
energy gain by the atoms. The energy loss serves to slow down the
ions, eventually to rest in the lattice; the atomic energy gain results
in the creation of defects or disorder in the lattice. The thermal
annealing can be used to re-order the lattice. The radiation damage
produced by implantation often produces conductivity changes
that swamp those desired by the addition of the ion. Though
annealing removes the majority of the defect energy states and
trapping centers, some defect sites will persist. There are many re-
ports on the ion irradiation on single crystals [2–4].
Owing to the versatile applications of M-NA in photonic tech-
nologies and NLO applications, the studies on irradiation effect

0168-583X/$ - see front matter Ó 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.nimb.2009.09.027
 T. Kanagasekaran et al. / Nuclear Instruments and Methods in Physics Research B 268 (2010) 36–41 37

on M-NA is very important from the technical point of view. In this 3. Results and discussion
paper, we report the effect of irradiation with silver and lithium
ions on the structural, optical, mechanical and electrical properties 3.1. X-ray diffraction analysis
of M-NA single crystals.
The XRD pattern of pristine and irradiated M-NA single crystals
is shown in Fig. 2. There is no change in the (orthorhombic) phase
2. Experiment
structure of the irradiated samples; however there are changes in
the lattice parameters (Table 1), which was identified by the struc-
The M-NA single crystals were grown by Vertical Bridgman
tural refinement performed on the pristine and the irradiated crys-
Method (Fig. 1). The sliced wafers of volume (1 cm  1 cm  1 cm)
tals of M-NA. The standard deviation (s.d) values of the lattice
of M-NA crystals were subjected to irradiation. The 100 MeV Ag7+
parameters are given in Table 1. When the lattice undergoes an
and 70 MeV Li3+ ions were irradiated at room temperature with
interaction with the ion on irradiation, it will induce significant
fluences of 1  1011 and 1  1012 ions/cm2. The projected ranges
change in the properties of the lattice atoms. The change in the lat-
of Ag7+ and Li3+ ions in the M-NA crystals were predicted by Monte
tice manifests as line/plane shifting towards the lower or higher
Carlo SRIM-2003, which ascertain the penetration of ions into the
diffraction angle. The change in relative intensity and the shift in
crystal lattice. The nuclear energy loss (Sn) and the electronic en-
the angular position can be explained by change in lattice spacing
ergy loss (Se) values in the M-NA crystals are 2.9 and 6.9 for silver
[5]. In the present case, the peak positions are shifted to the higher
ion and 2.1 and 3.9 keV nm 1 for lithium ion, respectively, as ob-
2h values. This implies that the lattice shrinks. On the other hand
tained from the SRIM-2003 calculations. Since the Se value is larger
we can say that there is a compressive strain field generated in
than the Sn value, the incident Li3+ and Ag7+ ions lose energy pre-
the material. The intensity decreases and width of the peaks in-
dominantly via inelastic collisions with the target electrons.
creases on irradiation, which enumerate that the point/clusters of
Structural analysis of the pristine and the irradiated M-NA crys-
defects are produced along the ion trajectory. It is clear that the lat-
tals was performed by using Bruker XRD (Model D8 Advance) PW
tice strain increases on irradiation. From the above mentioned re-
1600 Powder X-ray diffractometer (Inter University Accelerator
sults it is obvious that Li and Ag ion irradiation has generated
Center (IUAC), New Delhi) with CuKa (k = 1.54606 Å) radiation. Dif-
point/clusters of defects not columnar defects (due to the
fraction were recorded over a range of 20°–70° with the scan rate
Se = 1.2 eV/Å which is less than the Seth = 1.2 keV/Å), in the case
of 2°/min. The UV–vis spectra of both pristine and irradiated M-NA
of Li ion irradiation the defect is less than the Ag ion irradiation.
crystals were recorded in the wavelength range of 200 and
It can be concluded that the strain developed due to the created
1200 nm using a Varian Cary 5E UV–VIS–NIR spectrometer. The
defects is responsible for the modification of different properties
photoluminescence (PL) spectra of the pristine and the irradiated
of the M-NA crystals.
M-NA crystals were recorded using a home assembled PL system
at National Physical Laboratory (NPL), New Delhi, consisting of a
two-stage monochromator, a photomultiplier tube (PMT) with a
3.2. Optical properties
lock-in amplifier for PL detection, and an Ar+ ion laser operating
at 488 nm and 5 mW (corresponding to 0.125 W cm 2) for excita-
The pristine and irradiated M-NA crystals were subjected to
tion in all the measurements. Vickers microhardness tester (mhp-
UV–vis studies and the absorption spectra were recorded at room
100) equipped with a diamond pyramid indenter attached to an
temperature. The absorption of light energy by organic materials in
incident-light microscope (Neophat-2; Carl Zeiss, Germany) was
the ultraviolet and visible region involves promotion of electrons
used for measuring the mechanical hardness of the pristine and
in r, G and n-orbital from the ground state to higher-energy state.
irradiated M-NA crystals. The dielectric measurements were made
The recorded spectra are shown in Fig. 3. From the plot it is ob-
for different temperatures (35–95 °C) using a Hewlett Packard
served that the optical absorption increases with increasing of irra-
4284A LCR meter for pristine and irradiated M-NA crystals for fre-
diation fluence delivered to the M-NA crystals resulting in higher
quencies range from 20 Hz to 5 MHz. Each sample was electroded
concentration of defects [6] and the capture of excited electrons
on either side with air drying silver paste so that it behaved like a
by existing ion vacancies in the irradiated M-NA absorption spec-
parallel plate capacitor. Typical sample thickness was about
trum. Due to the Li3+ ion irradiation, there is a change in the
0.3 cm. A small cylindrical furnace whose temperature was con-
absorption edge and almost uniform increase in absorption. The
trolled by a Eurotherm 818P controller with an accuracy of
pristine spectral structure was not altered much due to irradiation
±0.1 °C was used to house the sample. The SHG efficiency of the
process. Absorption of M-NA crystal increases but no additional
pristine and irradiated M-NA was measured using the Kurtz–Perry
absorption peaks were found. This may be due to the fact that
powder technique.
the energy of the irradiating ion is not enough to move atoms from
lattice to substitution positions. The energy gap values for the pris-
tine sample is 2.30 eV (539 nm) and 2.28 eV (546 nm), 2.25 eV
(550 nm) corresponding to Ag7+ 1  1011 and Ag7+ 1  1012 ion
irradiated samples, respectively. The energy gap values for Li3+
1  1011 and Li3+ 1  1012 ion irradiated samples are respectively
2.29 eV (542 nm) and 2.27 eV (548 nm). It may be mentioned here
that MeV ion irradiation produces point defects such as vacancies,
anti-site defects and interstitials, causing lattice damage. Hence,
the reduction in Eg with increasing ion fluence may arise due to
the effect of band tailing, owing to the defects produced during
irradiation. In fact, the MeV ions excite the electrons from both
the lone pair and bonding states to the higher-energy states.
Vacancies created in these states are immediately filled by the out-
er electrons with Auger processes that, in turn, induce more holes
in the lone pair and bonding orbital, leading to a vacancy cascade
Fig. 1. As grown single crystals of M-NA. process. The vacancies occupied by electrons act as donor centers,
38 T. Kanagasekaran et al. / Nuclear Instruments and Methods in Physics Research B 268 (2010) 36–41

Fig. 2. XRD pattern of pristine and irradiated M-NA single crystals.

Table 1
The lattice parameters for the pristine and irradiated samples of M-NA.

Sample a (Å) b (Å) c (Å) s.d a (Å) s.d b (Å) s.d c (Å) Crystal structure
Pristine 6.3701 19.24 5.0811 0.0021 0.0011 0.0011 Orthorhombic
Ag 1  1011 6.4252 19.1113 4.8124 0.0031 0.001 0.002 Orthorhombic
Ag 1  1012 6.4491 19.1001 4.211 0.0011 0.0012 0.001 Orthorhombic
Li 1  1011 6.507 19.5291 5.0873 0.0041 0.0031 0.0011 Orthorhombic
Li 1  1012 6.6112 19.7033 5.2371 0.0021 0.0011 0.001 Orthorhombic

Fig. 3. Absorption spectra of pristine and irradiated M-NA single crystals.

which are responsible for broad band absorption. In other words it The units of crystals can be treated as weak charge transfer (CT)
is difficult to form ion vacancies. Ag7+ ion irradiation causes less complexes. When exposed to low energy and low intensity radia-
absorption than the Li3+ ion irradiation in the M-NA crystal. tion, the paramagnetic species are generated in the crystals and
 T. Kanagasekaran et al. / Nuclear Instruments and Methods in Physics Research B 268 (2010) 36–41 39

these defects were detected by EPR [7,8]. The electronic absorption
spectra of M-NA single crystals were thoroughly examined by Ben-
dazoli et al. [9] who measured the polarized spectra and calculated
[by a self-consistent field (SCF) ab initio method] the electronic
singlet–singlet and singlet–triplet transition moments and ener-
gies. Photoluminescence spectra of pristine and irradiated M-NA
crystals are shown in Fig. 4. The photoluminescence intensities de-
crease with increase in the irradiation fluence and finally this emis-
sion disappears or becomes nearly zero, when Ag7+ was irradiated
the emission disappears or becomes nearly zero at a fluence of
1  1012 ions/cm2. The PL intensity is greater for the Li3+ irradiated
than the Ag7+ irradiated samples. The PL band at 2.16 eV for pris-
tine sample exhibiting the yellow luminescence can be attributed
to the donor–acceptor pair (DAP). It has already been reported by
Magdalena Szostak et al. [10] that the doublet–doublet energy
for M-NA radical anion is 2.18 eV. The corresponding M-NA radical
cation amounts to 3.37 eV. The energy values corresponding to Li3+
irradiated at 1  1011 and 1  1012 are 2.28 eV for both the cases.
Whereas for the Ag7+ irradiated at the fluence of 1  1011 and
1  1012 are 2.28 eV and 2.34 eV, respectively. We note from the
above discussion that the blue shift occurs in the M-NA crystals
when subjected to irradiation. GaAsP/GaAs/GaAsSb/GaAs laser
diodes also showed a smaller blue shift indicating that the optical
quality of active layers was improved [11]. The blue shift is the net
result of the effects of charge separation and band filling [12].
When the M-NA crystal is subjected to irradiation, the electron–
hole pairs will be produced in the lattice. The decrease in the inten-
sity of the peak can be attributed to lattice deformation produced
ardness of M-NA crystals follows a linear behaviour with load for
both the pristine and the irradiated samples. The hardness value
of Li3+ ion irradiated sample is less than the pristine samples and
the Ag7+ ion irradiated sample has lesser value than the pristine
and the Li3+ irradiated samples. Decrease in the value of microh-
ardness on irradiation may be attributed to defects on irradiation.
M-NA crystal loses its plasticity and becomes brittle on irradiation,
the effect of Li3+ ion irradiation is less than the Ag7+ ion. This effect
can be explained as the Ag7+ ion irradiation causes much damage
to the lattice than the Li3+ ion. Hence the hardness value of Ag7+
ion irradiation is lesser than that of the Li3+ ion irradiation. The ef-
fect of Ag7+ on the lattice can be evidenced from the XRD studies.
3.4. Electrical properties
The large value of dielectric constant at low frequency is due to
the presence of space charge polarization [15]. The decrease in the
values of dielectric constant with the frequency takes place when
the jumping frequency of electric charge carriers cannot follow
the alternation of the ac electric field applied beyond a certain crit-
ical frequency [16]. The variation of the dielectric constant with
frequency for the pristine and the irradiated M-NA crystals are
50
Pure m-Na
45
silver
40 ionirradiation
Hardness number (Hv)

due to displacement of cations which is confirmed by the XRD

35 lithium ion
studies. The energy gap values in the photoluminescence study irradiation
are compatible with the UV–vis study, which ascertains the forma- 30
tion of the defects on irradiation. Hence with Li3+ ion irradiation
25
(rather than Ag7+ ion) on M-NA crystals, it is possible to create
electrically transparent windows along with the optical activity 20
of laser structure without any damage to the active region.
15

3.3. Mechanical properties 10

5
The apparent microhardness of solids depends on the applied
indentation test load. This phenomenon, known as the indentation 0
size effect (ISE), usually involves a decrease in the apparent 0 20 40 60
microhardness with increasing applied test load, i.e., with increas- “load in g”
ing indentation size [13,14]. M-NA crystals exhibit the ISE in both
Fig. 5. Variation of microhardness values with load for pristine and irradiated M-
the pristine and the irradiated samples. Fig. 5 is a graph showing NA single crystals.
the variation of the microhardness values with load for the irradi-
ated and pristine samples of M-NA. It is observed that the microh-

1.2 6 12
m-NA pure Ag 1 x10 ions/cm 2
11 11
1.0 Ag 1 x 10 5 Ag 1 x10 ions/cm 2
Dielectric constant (ε')

12
Ag 1 x 10
12
Li 1 x10 ions/cm2
Li 1 x 1011 Pure m-NA
0.8 4 11
Li 1 x10 ions/cm 2
Li 1 x 1012
Intensity

0.6 3

0.4 2

1
0.2

0
0.0
2 3 4 5 6 7
500 550 600 650 700 750 800 Log frequency (H z)
Wavelength (nm)
Fig. 6. Variation of dielectric constant for pristine and irradiated M-NA single
Fig. 4. Photoluminescence spectra of pristine and irradiated M-NA single crystals. crystals.
40 T. Kanagasekaran et al. / Nuclear Instruments and Methods in Physics Research B 268 (2010) 36–41
shown in Fig. 6. The dielectric constant was found to increase by a
factor of nearly 3, after Li3+ ion irradiation of fluence of
1  1011 ions/cm2. The drastic increase in dielectric constant due
to ion irradiation may be correlated to the defects created along
the ion tracks. Incident heavy ions get embedded in the crystal;
lose energy by both the inelastic collisions that dominate near
the end of the irradiated ions and elastic collisions. The increase
in dielectric constants for Li3+ ion irradiated samples may be attrib-
uted to the disordering of the crystal lattice by the ion beam [17].
When the fluence is 1  1011 ions/cm2 the damaged regions are
isolated from each other as the ion produces a region of amorphous
material surrounded by regions containing defects [18]. As we in-
crease the fluence to 1  1012 ions/cm2, more ions are activated
with the lattice disorderness and causing more activation of inter-
action between the ions thus increases the capacitance hence the
dielectric constant increases.
In the case of Ag7+ ion irradiation on the M-NA crystals, there is
a notable decrease in the dielectric constant value. The decrease in
dielectric constant is attributed to the decrease in the degree of
electronic polarization and to the increase in the free volume due
to the diffused Ag7+ ion. The flow of space charge carriers is ob-
structed and thus the build up of space charge polarization is im-
peded [19]. We know that the dielectric constant is directly
proportional to the electro–optic co-efficient (reff). The increase of
the dielectric constant of M-NA crystals on Li3+ ion irradiation im-
plies that the irradiation with the Li3+ ion can be used to construct
the more efficient electro–optic modulators.
3.5. Nonlinear properties
Kurtz–Perry powder method [20] is an important and popular
tool to evaluate efficiency of nonlinear optical materials. The sec-
ond harmonic conversion efficiency of the title M-NA crystal was
studied using a 1064 nm Nd:YAG laser. The input laser beam was
directed on the M-NA pure and irradiated powder packed on the
optically plane glass plate to get maximum second harmonic gen-
eration. A photomultiplier tube was used to detect the emitted
green light. Urea was used as a reference material in the present
study. It is found that the frequency doubling efficiency of pristine
M-NA crystal is comparable to that of urea. Thus the SHG relative
efficiency increases slightly with increasing fluence in the case of
Li3+ irradiated M-NA crystals. The details of relative efficiency are
given in Table 2.
The influence of radical anions on NLO properties bvec for a neu-
tral molecule of M-NA and for the negatively charged ion was stud-
ied earlier [10]. In light of which we find that the charged species
may constitute intermediates in the molecular mechanism of NLO
phenomena leading to a four fold increase [10] of bvec in charged
species as compared with neutral ones suggests that radical ions
once photogenerated mechanically can contribute to the molecular
mechanism of NLO generation. Hence we can conclude that the ion
irradiated M-NA crystals had the radical ions generated, leading to
the charge separation, hence the irradiated samples resulted with
higher SHG efficiency compared to that of the pristine sample.
Table 2
Comparison of second harmonic generation efficiency of the pristine and the
irradiated M-NA crystals.
Sample Input energy SHG conversion
mJ/pulse efficiency
Pristine 5 2.5 V (Urea
Li3+ irradiated at a 1011 ions/cm2 5 3.0 V (Urea
Li3+ irradiated at a 1012 ions/cm2 5 3.3 V (Urea
Ag7+ irradiated at a 1011 ions/cm2 5 2.6 V (Urea
Ag7+ irradiated at a 1012 ions/cm2 5 2.6 V (Urea
The defects induced due to low dose ion irradiation has not created
any drastic change in noncentrosymmetric crystal structure of M-
NA and hence its nonlinear properties. However, when the irradi-
ation dose was increased the SHG efficiency increases. The reason
to this may be the defect structure of the lattice [21].
4. Summary and conclusions
In summary, we have studied the 70 MeV Li3+ and 100 MeV Ag7+
ion irradiation induced modifications in the structural, optical,
electrical, mechanical and nonlinear properties of M-NA single
crystals. We find that there is no structural phase change in the
M-NA crystals due to irradiation. However lattice strain increases,
as a result the peak positions are shifted to higher 2h values (in
both Li3+ and Ag7+ ions). The optical absorption increases with
increasing fluence of ion irradiation and with the reduction in Eg
by increasing ion fluence may arise due to the effect of band tailing,
owing to the defects produced during irradiation. The blue shift oc-
curs in the M-NA crystals when subjected to irradiation. The blue
shift is the net result of the effects of charge separation and band
filling occurring due to the auger effect. The energy gap values in
the photoluminescence study are compatible with the UV–vis
study, which ascertains the formation of the defects on irradiation.
Hence with Li3+ ion irradiation (rather than Ag7+ ion) on M-NA
crystals, it is possible to create electrically transparent windows
along with the optical activity of laser structure without any dam-
age to the active region. The mechanical strength of pristine and
irradiated M-NA crystals was studied. The increase of the dielectric
constant of M-NA crystals on Li3+ ion irradiation implies that the
irradiation with the Li3+ ion can be used to construct more efficient
electro–optic modulators. The ion irradiated M-NA crystals had the
radical ions generated, leading to the charge separation, hence the
irradiated samples resulted in higher SHG efficiency compared to
that of the pristine sample.
Acknowledgements
One of the authors Dr. T. Kanagasekaran acknowledges Univer-
sity Grants Commission for awarding Dr. D.S. Kothari Postdoctoral
Fellowship. We are grateful to Dr. G. Bhagavannarayana and Dr.
Shailesh N. Sharma for helping in the Photoluminescence studies.
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