Ceramics International xxx (xxxx) xxx–xxx

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

High energy (150 MeV) Fe11+ ion beam induced modifications of physico-
chemical and photoluminescence properties of high-k dielectric
nanocrystalline zirconium oxide thin films
Vishnu Chauhana, Rashi Guptaa, V. Kumara, J. Rama, F. Singhb, M. Prasadc, S. Kumard, S. Ojhab,
P.A. Alvie, R. Mehraf, Rajesh Kumara,∗
a
University School of Basic and Applied Sciences, Guru Gobind Singh Indraprastha University, New Delhi, 110078, India
b
Materials Sciences Group, Inter University Accelerator Centre, New Delhi, 110067, India
c
Transducers and Actuators Group, CSIR-Central Electronics Engineering Research Institute, Pilani, 333031, Rajasthan, India
d
Department of Applied Physics, Amity School of Applied Sciences, Amity University, Gurgaon, 122413, Haryana, India
e
Department of Physics, Banasthali Vidyapith, Banasthali, 304022, Rajasthan, India
f
Department of Physics, Dr. B. R. Ambedkar National Institute of Technology, Jalandhar, 144001, Punjab, India

A R T I C LE I N FO A B S T R A C T

Keywords: This work presents the influence of dominated electronic energy loss over nuclear energy loss induced by swift
SHI heavy ion (SHI) irradiation on the physico-chemical, optical and other properties of RF grown zirconium oxide
ZrO2 (ZrO2) thin films. For this purpose, thin films of ZrO2 grown on glass substrate were irradiated by 150 MeV Fe11+
XRD ions with a range of fluence from 2E12 to 5E13 ions/cm2 to understand the mechanism of induced modifications
UV–Vis.
and defects generation. The XRD results confirmed that the virgin and irradiated ZrO2 thin films were crystalline
PL
FTIR
in nature with monoclinic and tetragonal structure. The crystallite size varied from 19.93 nm to 46.43 nm with
RBS varying ion fluence. Strain, dislocation density and stacking fault were used to investigate the changes in
structural parameters. Tauc's plot method was employed for the quantitative evaluation of optical energy band
gap (Eg) that exist in the range of 4.45–4.62 eV. The transmittance (%) of the virgin and Fe11+ ions irradiated
samples was determined in the range of 35.69–66.09% using UV–Vis. spectroscopy. Further, the refractive index
was determined using different methods significantly depends on the optical band gap. The broad PL emission
peaks were obtained at 375 nm and 440 nm with the excitation wavelength (λex.) of 300 nm. The variation in PL
intensity with increasing ion fluence was attributed to the creation or annihilation of primary or complex de-
fects. FTIR spectroscopy was employed for the analysis of chemical modifications in vibrational bonds of samples
and the band obtained 660 cm−1was assigned to the asymmetrically coupled Zr–O–Zr stretching which presents
the strong vibration in samples. The band intensity increased up to the fluence 5E12 ions/cm2 and decreased at a
higher fluence of 1E13 ions/cm2. Rutherford backscattering spectroscopy technique was used to determine the
thickness (165 nm) of the samples.

1. Introduction
During last few decades, there has been vigorous development by
researchers as well as industries in the field of ZrO2 thin films due to
their unique and fascinating properties and extensive applications. The
significant role of zirconium oxide in optical and electronic applications
helps to understand its fundamental interest of mechanism that how
high densities of electronic excitation influence the various properties
of ZrO2 thin films. Zirconia is a wide band gap (5–7eV) p-type semi-
conductor with good natural color and exhibit copious oxygen
vacancies on its surface [1,2]. It has been an interesting material due to
its exciting properties such as high mechanical strength, high flexural
strength (> 1000 MPa), stability to high temperatures, high melting
point, high rusting resistance, catalytic behavior in dehydration, high-
dielectric constant (∼25), low electrical conductivity, high hardness
and good chemical stability [3–10]. In addition to these properties,
ZrO2 has interesting optical properties such as low optical loss, large
optical band gap, low absorption, high refractive index and high
transparency in visible and near IR region [11–13]. The existing lit-
erature on the ZrO2 thin films grown by various techniques shows

∗
Corresponding author.
E-mail address: kumarrrpi@gmail.com (R. Kumar).

https://doi.org/10.1016/j.ceramint.2019.06.124
Received 7 May 2019; Received in revised form 22 May 2019; Accepted 11 June 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Vishnu Chauhan, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2019.06.124
V. Chauhan, et al. Ceramics International xxx (xxxx) xxx–xxx

remarkable changes in their optical properties. These properties which dE/dX = (dE/dX)nuc. + (dE/dX)elec. + (dE/dX)rad.
are recommend it as useful support for a large number of applications.
In the radiative process so-called bremsstrahlung and Cerenkov ra-
As compared to the other ceramics, the desirable optical properties of
diation, the energy loss is very small can be neglected. The mechanisms
zirconium oxide such as shading adaptation and drop in the thickness
of nuclear and electronic energy losses are entirely different. The Sn
layer of veneer ceramic are useful to obtain the desired color [3]. As
dominates at low energies in the keV range (∼10keV/amu) and pro-
above mentioned properties of zirconium oxide depend upon the
duce atomic size point defects, cascade of collision with nuclei and
method of synthesis. Due to its favorable optical properties, it has been
cluster of defects. The Se dominates at high energies in the MeV to GeV
used in passivation and protective coatings, protective mirrors, high
range [43–45]. The modifications induced in materials by swift heavy
power lasers, optical filters, beam splitters and industrial application in
ions irradiation are well explained by Coulomb explosion (CE) and
optoelectronics and optical devices [14–17]. Moreover, zirconium
Thermal Spike (TS) models [46–48]. Thermal spike model well explains
oxide has attained great deal of attention towards its exceptionally
that mechanism of irradiation with SHI. SHI produces secondary elec-
important applications in metal–insulator–metal (MIM) capacitors [18],
trons of various energies along the path of incident ion. These higher
solid oxide fuel cells [19], metal-oxide semiconductor (MOS) [20] and
energy travel far away from the track leaving behind a path of posi-
memory devices [21]. Availability of very few literature on the physical
tively charged ions and lower energy electrons transfer their energy to
and chemical study of zirconium oxide thin films and its wide range of
atomic lattice by electron-phonon interaction and comes in equilibrium
significant applications has motivated researchers to synthesize ZrO2
with in very less time i.e. 10−15s. This induces a rise in local tem-
thin films using various synthesis techniques. A. Hojabri has in-
perature along the ion track for a very short duration of time leading to
vestigated the effect of thermal annealing on physical and optical
redistribution of atoms in the material [49–51]. A survey of the avail-
properties of RF sputtered ZrO2 thin films on silicon and quartz sub-
able literature on ion-induced modifications and deposition of several
strate [22].C. M. Lopez et al. deposited the ZrO2 thin films by thermal
oxide thin films reveals that the ZrO2 shows the remarkable changes in
oxidation on Si and SiO2 coated wafers. The optical properties were
optical properties of the material by the effects of ion beam irradiation
determined by using spectroscopic ellipsometry (SE) method and a
[52]. The significant change in UV–visible absorption spectra and op-
theoretical model was used to describe the variation of refractive index
tical density was observed as the YSZ samples irradiated by 2.4 GeV
with incident photon energy [23].U. S. Patel et al. have reported the
Lead (Pb), 1.4 GeV Xenon (Xe) and 2.2 GeV Gold (Au) ion irradiation
effect of different Ar partial pressure used to synthesize ZrO2 thin films
[46]. The decrease in optical energy band gap and transmittance was
and observed variation in optical band gap and refractive index with
observed by 120 MeV Ag9+ ion beam irradiation in ZrO2 thin films as
increasing Ar partial pressure [24]. A large literate is available on
synthesized by sol-gel technique. The evolution of direct bands elec-
structural and optical properties of this material but a very few reports
tronic structure can be ascribed to the existence of oxygen point defects
are available on its photoluminescence (PL) properties. The character-
between valence band and conduction band [53]. M. Rawat et al. in-
ization and enhancement in PL properties of ZrO2 may be used for the
vestigated the modifications induced in electronic and local structure of
future development of information storage devices and other important
Ag (120 MeV) and Ni (130 MeV)ion irradiated ZrO2 thin films by using
applications [25]. The photoluminescence of the oxide materials is
X-ray absorption spectroscopy (XAS) technique and the presence of the
caused by relaxation of electrons and holes on F- centres called oxygen
strain (induced by energetic ion irradiation) in ZrO2 thin films was well
vacancies [9]. R. E. González studied the photoluminescence properties
observed by stiffening of Micro- Raman modes of monoclinic phase
of ZrO2 nanostructures synthesized by the hydrothermal method [26].
[54]. Optical band gap engineering of ZrO2 deals with the shifting of
ZrO2 thin films can be grown by a number of different techniques in-
the emission spectra from Ultraviolet (UV) region to the visible region.
cluding atomic layer deposition technique [27], chemical vapour de-
So, the study based on the variation of optical band gap would be useful
position [7], DC magnetron sputtering [28], physical vapour deposition
for understanding the performance of devices in high radiation en-
[29], chemical bath deposition [30], surface sol-gel method [31], ion
gineering [55]. Several studies of different oxide materials such as
beam sputtering [32] and radio frequency sputtering [33]. Zirconium
Al2O3 [56], CdO [57], LiNbO3 [58], Ga2O3 [59], ZnO [60] and SnO2
oxide has three different structures: (i) monoclinic structure is stable at
[61] are available for the modification induced in optical properties of
1170 °C (ii) tetragonal structure is stable in the temperature range of
thin films under SHI irradiation. However, very less literature is
1170–2370 °C and (iii) cubic structure is estimated above the tem-
available on ion irradiated modification of optical properties of zirconia
perature of 2370 °C. Among all these three structures, a cubic structure
thin films. The high energy ion beam irradiation of 200 MeV Au re-
is considered as the most desirable structure for various potential ap-
sulted into the change in optical density of yttria stabilized zirconia
plications because the ionic conductivity of ZrO2 is important at high
samples [37]. J. Desforges et al. analyzed the optical properties of the
temperature [34–36]. The investigations of radiation-induced an effect
ZrO2 thin films when exposed to ultraviolet irradiation for different
on oxide materials is old phenomenon but synthesis and modifications
hours. They studied that the transmittance increased with the irradia-
of the oxide materials by ion irradiation techniques sustain this old
tion time, also refractive index and extinction coefficient found to be
phenomenon in present time and development of materials research for
lesser in case of UV- exposed ZrO2 thin films [8]. Hence, ZrO2 thin films
the sake of the community is step-by-step process [37,38]. To the best
were characterized by XRD and UV–Visible spectroscopy which was
of our knowledge, very few reports are available on the investigation of
used to examine the crystallographic parameters and optical analysis
SHI irradiation induced modifications on physical and chemical prop-
(transmittance and absorbance etc.) respectively of virgin and irra-
erties of ZrO2thinfilms. The SHI interaction with matter serves as an
diated samples. Further, the optical parameters such as optical band
efficient tool to engineer the physico-chemical and photoluminescence
gap, refractive index and skin depth were also calculated. The PL
properties at the nanoscale [39]. SHI can modify the material properties
emission spectrum was recorded at room temperature by using photo-
in a targeted manner to obtain desired properties [40]. When swift
luminescence (PL) spectroscopy. Fourier transform infrared (FTIR)
heavy ions interact with the electrons of the atoms of material they lose
spectroscopy was used for the analysis of chemical modifications in
their energy without disturbing the nuclei constituted by the lattice.
vibrational bonds of the samples. Rutherford Backscattering spectro-
The deposited energy into the electrons of the atoms causes modifica-
metry was used to calculate the film thickness of the samples.
tion of material via electron-phonon interaction. The swift heavy ions
traversing into solid material lose their energy by types of collision: (i)
elastic collision called nuclear energy loss (ii) inelastic collision called 2. Experimental details
electronic energy loss. The energy loss (dE/dX) has three constituents as
given [41,42]. Zirconium oxide thin films were grown on glass substrate using
Radio Frequency (RF) magnetron sputtering technique. High purity

2
V. Chauhan, et al. Ceramics International xxx (xxxx) xxx–xxx

Table 1 caused by iron ions were determined using SRIM and TRIM software
Parameters determined from SRIM for 150 MeV Fe11+ ions irradiation [62]. Further, the values of projected range (Rp), longitudinal (LTs) and
Zirconium oxide thin films. lateral (Ls) straggling were also determined using SRIM and TRIM
Ion energy Se (eV/Å) Sn (eV/Å) Rp (Å) LTs(Å) Ls (Å) program as mentioned in Table 1. Ion collision was evaluated by depth
versus Y axis plot and the simulation of 3000 ions anticipated for Fe ion
150.00 MeV 1.212E+03 1.585E+00 14.38 μm 5632 Å 6143 Å trajectories within the targeted ZrO2 material as displayed in Fig. 1. The
TRIM program was used in detailed calculation with full damage cas-
cade mode [63]. Fig. 2. (Left panel) displays generated Zr and O recoil
distribution profile for Fe11+ ions in ZrO2 thin films in irradiation
range. Since the displacement energy for Zr atoms is less than the O
atoms. Fig. 2. (Right panel) displays the profile of target displacement
and target vacancies in the irradiation range due to collision with Fe11+
ions. The target vacancies and target displacement (26/Ions) generated
are similar in irradiation region.

2.1. Characterizations

The prepared virgin and irradiated samples were characterized for

Fig. 1. Ion collision effect of 150 MeV Fe11+ swift heavy ion irradiation.
argon (Ar) gas was used as sputtering gas and deposition was carried
out at room temperature (RT). Before deposition, substrates were che-
mically treated with H2SO4, H2O2 and HF to remove the contaminants
on the surface. The grown thin films were annealed for 24 h at 500 °C
and named as a virgin sample. Further, annealed samples (1 × 1 cm2)
were irradiated with 150 MeV iron ions at the fluence of 2E12, 5E12,
1E13 and 5E13 ions/cm2 in a high vacuum chamber at 1 × 10−6 mbar
with a charge state of 11+ from 15 UD Pelletron tandem accelerator at
IUAC New Delhi, India. The energy (150 MeV) of Fe11+ ions was chosen
such that it could entirely cross the thin films. A constant current of 1
particle nanoampere (pnA) was sustained throughout the irradiation.
The electronic stopping power (Se) and nuclear stopping power (Sn)
its structural, optical, chemical and depth profiling properties using
XRD, UV–Vis. spectroscopy, Fourier transform infrared (FTIR) spec-
troscopy and Rutherford backscattering spectrometry (RBS). XRD pat-
terns were recorded by use of PANalytical system Cu Kα radiation
(λ = 1.54 Å, voltage and current 40 kV and 45 mA respectively) with an
angular range of 20–70°. UV–Vis spectroscopy of samples was done in
the range about 200–600 nm with the help of UV–Visible U-3300
spectrophotometer. Room temperature photoluminescence properties
of virgin and irradiated samples were studied using the instrument
(Horiba Canada PTI QM-8450-11-C) Luminescence Spectrometer in the
spectral range of 325–570 nm with the wavelength of 300 and 310 nm
as the excitation source. FTIR of the samples was performed using
Bruker Alpha-T Attenuated Total Reflection (ATR)-FTIR spectrometer.
Depth profiling of the samples was done using Rutherford back-
scattering spectrometry in channeling condition using 5SDH-1.7 MV
Tandem accelerator at IUAC New Delhi, India. The energy of the He2+
ion beam was 2 MeV.
3. Results and discussion
3.1. Crystallographic structure
Virgin and 150 MeV Fe11+ irradiated ZrO2 thin films were char-
acterized by X-Ray Diffractometer (XRD) technique. The structural

Fig. 2. (Left panel) profile of Zr and O ion recoils in the irradiated range due to collision with Fe11+ ion. (Right panel) generated target displacement and target
vacancies profile for Fe11+ ion beam in ZrO2 thin films in irradiated range.

3
V. Chauhan, et al. Ceramics International xxx (xxxx) xxx–xxx

Table 2
Determination of crystallite size of monoclinic (210) and tetragonal (112) phase
using Scherrer method, Dislocation density (Dd), Strain and Stacking fault (š)
virgin and irradiated ZrO2 thin films.
Fluence Scherrer method Dislocation Strain Stacking
(ions/ density Dd (10−4) fault (š)
cm2) 2θ L (nm) 2θ L (nm) (1014 m−2)

Virgin 39.55 38.55 50.28 19.93 6.97 7.74 0.39979

2E12 39.47 46.43 50.28 24.78 4.63 6.39 0.39982
5E12 39.48 44.11 50.24 21.83 5.13 6.73 0.39993
1E13 39.55 42.00 50.33 21.32 5.66 7.06 0.39920
5E13 39.52 40.09 50.23 20.38 6.22 7.40 0.39972

Fig. 3. XRD patterns of virgin and 150 MeV Fe11+ ion irradiated ZrO2 thin films
at different fluence.

analysis determines the Full width at half maximum (FWHM), crystal-

lite size via Scherrer method, strain, dislocation density and Stacking
fault probability using the XRD patterns. Fig. 3 depicts the XRD patterns
of virgin and 150 MeV Fe11+ ion irradiated ZrO2 thin films at different
doses of 2E12, 5E12, 1E13 and 5E13 ions/cm2. XRD patterns were re-
corded in the range of 2θ from 25° to 70° and depict that the thin films
are crystalline in nature. The XRD patterns show the polycrystalline
nature of the ZrO2 material. The observed XRD patterns affirmed the
monoclinic and tetragonal phase of zirconium oxide thin films. The
experimental XRD data was compared with the JCPDs. The reflections
of the peak oriented the Miller indices as (111), (210), (112), (211) and
(231) at peak positions (2θ) 31.50°, 39.55°, 44.80°, 45.78° and 66.16°
well matches with (JCPDs. 70–2491) which have a monoclinic structure
with space group of P21/c (14). The well pronounced ZrO2 peak was
observed at (2θ) peak position 43.17° and 50.28° oriented at (102) and
(112) planes respectively and corresponds to the tetragonal structure of
ZrO2 (JCPDs No. 81–1544) with the space group P42/nmc (137). It is
revealed that no significant shift in the angular position of diffraction
peaks was determined after Fe11+ ion irradiation. The appreciable
variation in the intensity of the peaks was observed in virgin and ir-
radiated samples. It can be clearly observed that there is no substantial
change in diffraction peak position (2θ) and FWHM of the peaks. The
change in the width of the peak provides the deviation in perfect
crystallinity of the virgin and irradiated thin films. As a result, careful
observations express that there is an appreciable change in peak in-
tensity with increasing the ion dose. The intensity of the peaks at dif-
ferent peak positions is increased with increasing the ion dose up to the
fluence of 5E13 ions/cm2. It is noticed that the increase in peak in-
tensity accounted for the effect of swift heavy ions on scattering factor.
Appreciable enhancement in the peak intensity might be attributed to
change in the electronic density in the crystallographic position and this
enhancement in peak intensity is a clear indication of improvement in
crystallinity of the thin films [64]. The crystallite size of the monoclinic
and tetragonal phase was determined using the plane (210) and (112)
respectively. The peak width is used to determine the crystallite size (L)
and lattice strain (S) of the samples. Debye-Scherrer's method was
employed to calculate the crystallite size using FWHM of the samples
[65–68].
kλ
L=
β cosθ (1)
where, L is the crystallite size, k is shape factor constant (0.94), λ is the
wavelength of X-ray used, θ is the Bragg angle and β is FWHM selected
for the particular peak. The evaluated crystallite size of monoclinic and
Fig. 4. Variation of crystallite size with different irradiation fluence for ZrO2
thin films.
tetragonal structure for virgin and irradiated thin films is tabulated in
Table 2. Fig. 4 shows the variation of crystallite size with ion fluence. R.
Kumaravel et al. have reported a decrease in crystallite size after SHI
irradiation [69]. But in our work, the crystallite size increased for lower
fluence 2E12 ions/cm2 subsequently decreased with increasing the ion
fluence up to 5E13 ions/cm2. The increment in crystallite size for lower
fluence might be attributed to the reduction in the concentration of
oxygen vacancies and release of stress between the grains. For higher
fluence 5E12 ions/cm2, 1E13 ions/cm2 and 5E13 ions/cm2, the incre-
ment in FWHM or reduction in crystallite size may be due to the gen-
eration of lattice defects in the nanostructure by 150 MeV Fe11+ ion
beam [70]. The evolution of lattice strain has been carried out for virgin
and irradiated samples using the following relation [71].
β cosθ
S=
4 (2)
The lattice strain was determined for (210) plane of monoclinic
structure of zirconium oxide thin films. Initially, the determined lattice
strain was found to decrease for lower fluence as compared to virgin
sample and increased up to the higher fluence of 5E13 ions/cm2. The
increase in strain is ascribed to generation of point defects due to swift
heavy ion irradiation which causes the systematic shifting of atoms
from their original position. During the high energy irradiation process,
the energy lost by the highly energetic ions generates some defects
(point or extended defects) which cause the degradation of crystalline
quality with increasing the ion fluence [70,72]. A dislocation is con-
sidered as irregularity or crystallographic defect in the crystal structure.
The movement of dislocations is hindered by other dislocations exist in
the material. Statistically, dislocations are a sort of topological defects.
Hence, the dislocation density (Dd) signifies the magnitude of defects

4
V. Chauhan, et al.
Fig. 5. Variation of strain and dislocation density with different irradiation
fluence for virgin and irradiated ZrO2 thin films.
present in the film. Dislocation density provides the information about
the deformation of the lattice sight in the well-arranged crystal lattice
of the material. It can be generated in material unlike point defects,
vacancies etc. [73]. Moreover, a larger amount of dislocation density
indicates the greater hardness.
The number of dislocations in a unit volume is known as dislocation
density which was evaluated by crystallite size using the following re-
lation [74].
1 and it is found to be decreased from 4.62 to 4.53 eV at higher fluence.
Dd =
L2 (3)
where, L is the crystallite size of the thin films. The determined values
of dislocation density (d) for virgin and irradiated ZrO2 thin films are
tabulated in Table 2. Fig. 5 depicts the variation of strain and disloca-
tion density with ion fluence.
In crystallography, stacking fault is considered as planer defect and
it is a kind of defect describes the disordering of crystallographic planes
[75,76]. Stacking fault probability (š) was determined from the fol-
lowing relation [77,78].
Δ(2θ) ⎤
Š= 0.2529⋅⎡
⎣ tanθ ⎦ (4)
Fig. 6 depicts the stacking fault of the virgin and irradiated samples
as evaluated by the inverse of the slope of the linear fitting determined
from the plotting between 2θ and tanθ.
3.2. Absorbance, transmittance and band gap
The optical properties were analyzed for virgin and Fe11+ ions ir-
radiated zirconia samples with a range of ion fluence of 2E12, 5E12,
1E13 and 5E13 ions/cm2 by UV–Vis spectrophotometer. UV–Visible
absorption of ZrO2 thin films, deposited on glass substrate was per-
formed in a spectral range of 250 nm–600 nm at room temperature
(RT). However, it is noted that the swift heavy ion irradiation of iron
ions on ZrO2 samples initially causes a blue-shift in absorption edge for
the lower dose as compared to the virgin sample. But for the higher
dose, Fe ions irradiation causes a red-shift in absorption edge. Careful
observation reveals that iron ions irradiation cause slight variation in
shifting of absorption edge with increasing the ion fluence as displayed
in Fig. 7. Increase in optical band gap is governed by the blue shift and
alternately for the decrease in optical band gap [79]. The optical
transmittance of ZrO2 films were also studied at RT with the wave-
length taken in the range of 250 nm–800 nm. Fig. 7 inset displays the
virgin and irradiated zirconia thin films are optically transparent. The
transmittance of samples lies in the range of 35.69–66.09% and poly-
crystalline ZrO2 thin films depict an optical fringe [80]. For all the
5
Ceramics International xxx (xxxx) xxx–xxx
samples, it is observed that the transmittance is low in the Ultraviolet
region. But invisible region of the spectra, the curves shows the high
transmittance of energy. An easy look at spectra shows a progressive
increase in value of transmittance (%) as the fluence increased up to
5E12 ions/cm2. Further, the transmittance (%) decreased for the ZrO2
thin films irradiated at higher fluence 1E13 and 5E13 ions/cm2. This
continuous increment in transmittance (35.69–66.09%) up to the flu-
ence of 5E12 ions/cm2 is ascribed to improvement crystallinity of the
sample after irradiation [81]. For the higher fluence, the reduction in
transmittance might be due to the generation of localized energy levels
between valence and conduction band [82]. Further, an absorption
edge is used to determine the optical energy band gap of materials. The
optical band gap (Eg) of ZrO2 thin films have been evaluated by using
the Tauc relation [83,84].
(αhν)n = Z (hν- Eg) (5)
Where, Z is proportionality constant, α is known as absorption
coefficient, ν is the frequency, h represents plank's constant, Eg is op-
tical band gap energy and the value of n determine the type of transi-
tion. It is 2 and ½ for direct and indirect band transition respectively.
The absorption coefficient (α) is evaluated using the relation α = 2.303
(A/t), where A is absorbance and t is the thickness of the sample. The
value of photon energy (hν) extrapolated to α = 0 provides an ab-
sorption edge which corresponds to optical band gap energy. Fig. 8
displays the plot of (αhν)2 vs. hν for virgin and irradiated zirconium
oxide thin films. Fig. 9. shows the variation in the value of band gap
energy of virgin and irradiated samples. At lower fluence, the value of
band gap increased from 4.45 to 4.62 eV as compared to virgin sample
The optical band gap of ZrO2 thin films increased at lower fluence
(2E12 – 5E12 ions/cm2) due to Burstein – Moss (B-M) shift [85]. The
reduction in optical band gap can be described on the basis of the
thermal spike model. This model explains that the interaction of swift
heavy ions with the material leads to transfer of their energy to the
target electrons which results into the electronic excitation from lower
energy states to higher energy states. In this process, the vacancies are
created in these states. By the process of Auger effect, these generated
vacancies are immediately filled by the outer electrons which causes
vacancy cascade process which leads to breaking of bonds and ioniza-
tion of the atoms responsible for changing the local structural order
results into decrease in the band gap of the material [62,86]. Further,
the decrease in band gap may be due to the radiation induced defects
like antisite oxygen and oxygen vacancies. The high energy irradiation
induced lattice damage defects levels of oxygen below the conduction
band that results into decrease in band gap [60,69]. The band gap also
decreases due to formation of band tail states that effect the properties
of most of the semiconductor optoelectronic devices [59]. Costantini
et al. [37] focused on point defects formation in yttria stabilized zir-
conia by 200 MeV Iodine and 2.6 GeV Uranium high energy ion irra-
diation samples. They showed the generation of color centres: oxygen
mono-divacancy as determined by electron paramagnetic resonance
spectroscopy. The change in the value of optical band gap concludes
that the SHI irradiation can tailor the properties by creating controlled
defects [87]. The determined values of optical band gap and transmit-
tance (%) are mentioned in Table 3. Several studies have reported the
band gap of zirconium oxide thin films. In contrast, S. Venkataraj et al.
have reported that the optical energy band gap lies in the range of
(4.52–4.67 eV) of zirconia thin films prepared by DC magnetron sput-
tering as a function of oxygen flow rate (2.9–4.0 sccm) [88].V. Sunke
et al. determined the increased in band gap (3.49–5.48 eV) of DC
magnetron sputtered ZrO2 thin films when thermally oxidized at a
temperature of 300 °C–500 °C [89]. H. Rath et al. reported the change in
the band gap by the influence of 297 MeV and 511 MeV Ni ion irra-
diation on TiO2 material [90]. Moreover, the change in band gap in-
dicates that swift heavy ions create lattice disorder by the effect of
V. Chauhan, et al.
Fig. 6. Plot between tanθ and 2θ for (a) virgin and Fe11+ ion irradiated ZrO2 thin films at fluence (b) 2E12 (c) 5E12 (d) 1E13 and (e) 5E13 ions/cm2. The slope of the
liner fitting was used to determine the stacking fault.
dense electronic excitation in the material. This can be the formation of
defects level i.e., shallow energy levels near conduction band. This can
be responsible for the transition from valence band to those levels in-
stead to band-to-band transition (BBT) which results in a change in the
band gap. The decrease in the optical band gap provides an indication
of increase in oxygen vacancies of the ZrO2 lattice due to the ion irra-
diation. Although the change in the value of band gap might be due to
modification of density of surface defects induced in the lattice of zir-
conium oxide [91].
3.2.1. Refractive index and skin depth
The refractive index (RI) of a material is the fundamental and
technological importance due to application in various optical devices
[92]. The band structure of the material relies on band gap and re-
fractive index. The transparency of incident spectral radiation is also
determined by RI of the material. Among several optical parameters,
6
Ceramics International xxx (xxxx) xxx–xxx
the controlling of refractive index (n) and band gap (Eg) plays a sig-
nificant role. The correlation between these parameters is necessary for
the determination of the refractive index of newly developed materials
[93,94]. The RI of virgin and Fe ions irradiated ZrO2 samples was
calculated by using different models given by different research group.
The first equation was provided by Moss who suggested that all
energy levels are scaled down by a factor of n4 in the dielectric medium
[95].
n4 = K/Eg (6)
where K is constant which is equal to 95. This equation does not hold
good for low and high energy band gap materials.
N. M. Ravindra et al. proposed the equation that suggests the direct
relation between band gap and refractive index [96].
n = 4.84–0.62 Eg (7)
V. Chauhan, et al. Ceramics International xxx (xxxx) xxx–xxx

Table 3
Transmittance (%), direct optical band gap (Eg) and refracted index determined
from Reddy (R), Moss (M), Ravindra (RI) and V. Kumar (VK) of virgin and
irradiated ZrO2 thin films.
Fluence (ions/cm2) T (%) Eg (eV) (Refractive index)

R M RI VK

Virgin 35.69 4.45 1.743 1.479 1.321 2.077

2E12 65.25 4.59 1.714 1.457 1.234 2.056
5E12 66.09 4.62 1.708 1.452 1.215 2.052
1E13 58.75 4.56 1.720 1.462 1.252 2.061
5E13 52.81 4.53 1.726 1.466 1.271 2.065

Fig. 7. Optical absorption and inset transmittance (%) spectra of ZrO2 virgin
and irradiated thin films with 150 MeV Fe11+ beam at different fluence.

Fig. 10. Plot of variation of refractive index with ion fluence determined using
the method proposed by Reddy et al.

Further, Reddy et al. have given the modified form of Moss relation
which provide the empirical relation between RI and energy band gap
[97].

12.417
n=
2
Eg − 0.316 (8)
Fig. 8. Tauc plots of (αhν) vs. photon energy by linear extrapolations to de-
termine the direct band gap values of virgin and irradiated samples.
The values of the refractive index determined using this relation are
plotted in Fig. 10. The equation proposed by Reddy et al. provide a
better agreement with the experiment value as compared to Moss
model. All the above-proposed equations have some limitations for low
or high band gap materials. Consequently, V. Kumar et al. approached
to a relation to determine the refractive index of mixed materials in-
cluding group IV,III-IV and II-IV, semiconductor, halides, insulators and
oxide materials [97].

n= Z Ekg (9)

where, Z and k are constant 3.6668 and −0.32234 respectively. The

Fig. 9. Plot of variation in value of direct band gap vs. ion fluence of ZrO2
virgin and irradiated thin films.
estimated values of the refractive index using all the above relations are
listed in Table 3. It is observed that the value of refractive index slightly
decreased up to the dose of 5E12 ions. cm−2 and slightly increased for
the dose of 1E13 and 5E13 ions. cm−2. Many researchers observed the
decreased value of the refractive index in the range of 2.18–2.04 as the
ZrO2 thin films were grown by DC magnetron sputtering [22] .P. S.
Chaudhari et al. reported the increase in the value of the refractive
index indicates the phase transition due to swift heavy ion beam irra-
diation in silicon oxide thin films [98].
The classical skin depth or penetration depth (χ) is defined as the
distance at which the amplitude of electromagnetic wave decreased by
a factor ‘e’ after traversing a thickness [99]. It can be determined using
the following relation [100,101].

7
V. Chauhan, et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 11. Skin depth vs. photon energy of virgin and Fe11+ ions irradiated zir-
Fig. 12. PL emission spectra of virgin and irradiated ZrO2 thin films with an
conia thin films at different ion fluence of 2E12, 5E12, 1E13 and 5E13 ions/
excitation wavelength of 300 nm.
cm2.

1
χ=
α (10)

The skin depth is related to the factor of the absorption coefficient.

Fig. 11 depicts the variation of penetration depth as a function of in-
cident photon energy for virgin and Fe11+ ions irradiated zirconium
oxide thin films with different fluence. For lower photo incident energy,
skin depth increases up to the certain photo energy of 2.24 eV, due to
reduction in the probability of absorption [99]. Further, skin depth
decreases beyond the incident photon energy and then it becomes zero
at a certain value of photon energy. The wavelength and energy at
which skin depth becomes zero is called cut off wavelength (λ cut − off )
and cut-off energy (Ecut − off ) respectively [102]. The value of Ecut − off was
determined 5.34 eV. As a function of fluence, the skin depth increased
up to the fluence of 5E12 ions/cm2 and decreased at higher fluence.

3.3. Photoluminescence study

Photoluminescence is a very sensitive technique for determining the

sample quality, structural defects i.e. oxygen vacancy, interstitials and
optical properties of the materials. Photoluminescence (PL) emission
spectra of virgin and irradiated samples were determined from (Horiba
Canada PTI QM-8450-11-C) Luminescence Spectrometer in the wave-
length range 325–570 nm. The photoluminescence spectra of virgin and
irradiated ZrO2 thin films using iron ions (Fe11+) with a different flu-
ence of 2E12, 5E12, 1E13 and 5E13 ions/cm2 are presented in Fig. 12 at
an excitation wavelength of 300 nm. Fig. 13 presents the PL spectra of
the virgin sample at an excitation wavelength of 300 nm and 310 nm. In
Fig. 12, it is observed that the PL peaks of the broad emission bands of
the virgin and irradiated sample are almost the same in same wave-
length position but having variation in intensities for different ion
fluence. PL results indicate that ion fluence does not alter the lumi-
nescence mechanism of zirconium oxide thin films. The broad PL
emission spectra is due to the formation of defects (oxygen vacancies
and oxygen interstitials) [43]. The virgin and irradiated samples have
two photoluminescence bands peaked at 375 nm and 440 nm. A broad
emission band at 375 nm is UV emission. Another, broad emission band
peaked at 440 nm is ascribed to the blue emission [103]. The intensity
of PL emission bands of virgin sample is weak as compared to the ir-
radiated samples. For lower fluence, 2E12 and 5E12 ions/cm2 the in-
tensity of both the bands is maximum and then reduced for the higher
fluence. It is attractive that swift heavy irradiation of 150 MeV Fe ion
enhances the quantum efficiency and emission range of ZrO2
Fig. 13. PL spectra of virgin ZrO2 sample with an excitation wavelength of
300 nm and 310 nm in the wavelength range 325–570 nm.
nanocrystaline thin films at lower fluence [104]. Moreover, the incre-
ment in PL intensity at lower fluence is attributed to the increase in the
concentration of defects. The generation of point defects in the lattice
might be due to the atomic displacement which is caused by the ions,
neutrons and fast electrons. Moreover, the radiation dose of the ions
must be very high for the formation of complex defects from the
random association of point defects. Hence, swift heavy ions irradiation
is considered as very high density excitation for the formation of high
defects density along the ion track [105]. At fluence of 1E13 and 5E13
ions/cm2, the generation of exciton takes place which might be trapped
by the defects. Hence, when ZrO2 thin films were irradiated at higher
fluence, PL intensity reduced as compared with the lower fluence
samples [106]. The decrease in photoluminescence intensity of emis-
sion spectra might be due to the annihilation of primary defects and
generation of complex defects. H.S. Lokesha et al. reported the incre-
ment in photoluminescence properties of ZrO2:Dy3+ under SHI irra-
diation of 100 MeV Ni7+ ions beam [107]. The trend of the peak in-
tensity of PL spectra as a function a ion fluence is well agreement with
the optical study. Similar PL spectra was observed by L. Chen et al. [15]
for yttria-stabilized zirconia thin films irradiated by 500 keV Xe6+ ion

8
V. Chauhan, et al.
Fig. 14. FTIR spectra of virgin and 150 MeV Fe11+ ions irradiated ZrO2 samples
with different ion fluence of 2E12 ions/cm2, 5E12 ions/cm2 and 1E13 ions/cm2.
beam. They detected two strong broad emission centered at 420 nm and
530 nm (green emission) ascribed to band-edge transition and existence
of oxygen vacancies (FAA) respectively in the surface of YSZ samples. In
Fig. 13, it is observed that there is not much difference in PL emission
band spectra of ZrO2 virgin sample by taking the different excitation
wavelength except the variation in intensity of bands. For the excitation
wavelength (λexc.) of 300 nm, the intensity of the band peaked at
440 nm is greater than the intensity of the band centered at 375 nm.
While for the excitation wavelength of 310 nm, the intensity of the
bands at 440 nm was more as compared to the intensity of the band
appeared at 375 nm.
3.4. FTIR results
Fourier transform infrared (FTIR) spectroscopy was used for the
analysis of chemical modifications in vibrational bonds of RF grown
ZrO2 thin films irradiated with 150 MeV Fe11+ ions beam with a range
of different fluence as depicted in Fig. 14. The influence of Fe ion ir-
radiation on zirconium oxide thin films can be clearly observed in FTIR
spectra under similar conditions. FTIR spectra of virgin and irradiated
thin films show peaks at 660 cm−1, 715 cm−1, 1240 cm−1, 1337 cm−1
and 1557 cm−1 as depicted in Fig. 14. It is expected an IR active mode
at a lower wave number of 660 cm−1 and assigned to the asymme-
trically coupled asymmetric Zr–O–Zr stretching. The intensity of the
peak at this position is increased up to the intermediate fluence of 5E12
ions/cm2 and decreased at higher fluence 1E13 ions/cm2. The peak at
this region of lower wave-number presents the strong vibration of all
the samples. The variation in intensity and area under this peak sig-
nifying the change in chemical composition or chemical modification
induced by Fe ion beam irradiation [108]. Further, there is no sig-
nificant change in intensity of the peaks of irradiated samples as com-
pared with virgin sample for the bands 715 cm−1, 1240 cm−1,
1337 cm−1 and 1557 cm−1. This signifies the high resistance of zirco-
nium oxide to ionic radiation [109,110]. The IR spectrum of virgin and
Fe irradiated thin films shows a peak at 715 cm−1. This peak can be
essentially assigned to the asymmetric motion of oxygen (O) atoms w.
r.t the center of symmetry. Consequently, this mode is due to asym-
metric O–Zr–O stretching and formed by the movements of zirconium
(Zr) and oxygen (O) atoms [111]. The FTIR transmittance band at
1240 cm−1 and illustrates the evident of Zr–O stretches [112]. The peak
at 1337 cm−1 is ascribed to the absorption of non-bridging OH groups
[113]. The peak towards the high wave-number at 1565 cm−1 is at-
tributed to the Zr–OH vibration [114]. According to H. Liu et al., the
band appeared at 1340 cm−1 and 1590 cm−1 ascribed to O–H bending
9
Ceramics International xxx (xxxx) xxx–xxx
Fig. 15. RBS spectra of virgin ZrO2 thin film.
vibration [115]. Careful observation of the peaks reveals that there is
little shifting in the band position of the peaks 1240 cm−1 and
1337 cm−1 towards the lower wave-number for the fluence of 5E12
ions/cm2 and 1E13 ions/cm2. This important feature of continuous
shifting of the peak towards lower wave-number can be elucidated as a
relief of high compressive stress of zirconium oxide thin films by ion
beam irradiation [116,117].
3.5. Rutherford Backscattering Spectrometry
The characteristics of Rutherford Backscattering Spectrometry make
it mainly useful for investigation of thin/multi-layer films. RBS is par-
ticularly used for determination of depth profile of heavier elements in
light element matrices. RBS spectra are recorded in RBS yield or in-
tensity counts versus energy channel number. The energy, intensity
counts and FWHM of the peak give the information of elemental
composition and thickness of the layer [117]. The RBS measurements
were carried out with a beam of 2 MeV He2+ ions, stable beam current
20 nA incident on the sample and with charge of 10 μC. The spectra of
virgin ZrO2 sample is presented in Fig. 15. The XRUMP code was used
to simulate the experimental data to provide the information of the
thickness profile of the sample [118]. The FWHM of the Zr peak ob-
tained at channel no. 1586.83 provide the thickness of the sample. It
can be inferred from the simulation (not shown here) that the thickness
of the thin films is 165 nm.
4. Conclusions
Physico-chemical and Optical modifications of RF grown ZrO2 thin
films were studied with reference to 150 MeV Fe11+ swift heavy ion
beam irradiation. After irradiation, the structural, optical and chemical
properties were found to be tailored owing to the modifications induced
by the dense electronic excitation of SHI in ZrO2 samples. XRD patterns
revealed that the virgin as well as irradiated thin films were highly
crystalline in nature. Appreciable enhancement in the peak intensity
might be due to change in the electronic density in the crystallographic
position. The change in strain is due to a change in defects density that
varies with increasing ion fluence. The study has shown the influence
on optical band gap and transmittance (%) varied from 4.45 eV to
4.62 eV and from 35.69 to 66.09% respectively after ion beam irra-
diation of zirconium oxide samples. The variation in the value of optical
band gap may be due to modification of the density of surface defects
induced in the lattice of zirconium oxide. The refractive index of virgin
and irradiated samples was found to be decreased up to a particular
fluence 5E12 ions/cm2 and increased at higher fluence as determined
by different methods. The reduction on PL emission intensity at 440 nm
V. Chauhan, et al.
was observed with increase in ion fluence due to formation of defects
during SHI irradiation. The excitation wavelength varied form
300 nm–310 nm does not change the PL emission spectra except the
change in the intensity of the emission band. The FTIR spectra depicted
the chemical modifications in vibrational bonds of virgin and irradiated
samples. The peaks towards the lower wave number display the strong
vibration and little shifting of the band 1240 cm−1 and 1337 cm−1at
higher fluence may be due to the relief of high compressive stress of
thin films by swift heavy ion beam irradiation. The integration of fra-
mework on the detailed optical study of ions irradiated ZrO2 thin films
grown by RF sputtering is currently emerging and promising approach
for the suitable applications in high reflectivity mirrors, optical sensors
and wear resistant protective coatings.
Acknowledgments
One of the authors Dr. Rajesh Kumar is thankful to Inter University
Accelerator Center (IUAC), New Delhi, India, research project (Ref:
IUAC/XIII.3A/59319) and the FRGS Project No. GGSIPU/DRC/FRGS/
2019/1553/15 for provide financial assistance in the concerned for the
smooth completion of this research work. Mr. V. Chauhan would like to
acknowledge for Senior Research Fellowship (UGC-SRF) provided by
the University Grants Commission (UGC), Govt. of India, New Delhi,
India. One of the authors Dr. R. Kumar is sincere thanks to Prof. N.
Koratkar for providing the RF sputtering facility at Rensselaer
Polytechnic Institute (RPI), New York, USA. The authors (R. Kumar and
V. Chauhan) acknowledge to University Science Instrument Centre
(USIC), Department of Physics & Astrophysics, and University of Delhi,
India for providing PL measurements. We would also like to thank
editor and reviewers for their effort and expertise in reviewing this
research paper that helped in further improving the quality and stan-
dard of the manuscript.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.ceramint.2019.06.124.
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