IJSTE - International Journal of Science Technology & Engineering | Volume 2 | Issue 11 | May 2016

ISSN (online): 2349-784X

Effect of Annealing Temperature on Optical and

Electrical Properties of Electron Beam
Evaporated NiO Thin Films
A. Madhavi
Research Scholar
Department of Physics
Sri Venkateswara University, Tirupati, 517502, India

G. S. Harish
Research Scholar
Department of Physics
Sri Venkateswara University, Tirupati, 517502, India

P. Sreedhara Reddy
Professor
Department of Physics
Sri Venkateswara University, Tirupati, 517502, India

Abstract
Nickel oxide (NiO) thin films were prepared by electron beam evaporation technique and studied various properties at different
annealing temperatures. The surface morphology of the deposited films was characterized by scanning electron microscopy (SEM)
and the compositional analysis of the deposited films was studied by energy dispersive spectroscopy (EDAX). The effect of the
annealing process on the topography of the prepared NiO thin films was studied by atomic force microscope (AFM) at room
temperature. The optical band gap of the as-deposited film was increased to 3.68 eV with the increase of annealing temperature up
to 400oC, thereafter decreased at higher annealing temperature. Thin film samples annealed at 400oC showed decreased resistivity
compared to other samples.
Keywords: atomic force microscopy, band gap, electron beam evaporation, NiO thin films, SEM, XRD
________________________________________________________________________________________________________
I.

INTRODUCTION

Nickel oxide is a low cost material allowing for good cyclic reversibility, high coloration efficiency and good durability. NiO is a
model for p-type metal oxide material which has very interesting characteristics such as good chemical stability and excellent
electrical properties [1-5]. NiO films are commonly prepared by thermal evaporation, sputtering, spray pyrolysis, electrochemical
deposition, sol- gel and electron beam evaporation techniques [6-10]. NiO thinfilms find very attractive applications on smart
windows or displays to be used in automobiles, buildings or airplanes and are used in gas sensor applications because of the
enhanced electrical properties. The properties of the deposited NiO films by electron beam evaporationtechnique, mainly depend
on the deposition parameters such as substrate temperature, evaporation time, base pressure, working pressure, acceleration voltage
and filament current. In this work, thin films of NiO have been deposited using electron beam evaporation technique and the effect
of annealing temperature on the films has been investigated on structural, morphological, optical and electrical properties.
II. EXPERIMENTAL AND CHARACTERIZATION TECHNIQUES
All the NiO thin films were grown on glass substrates by using electron beam evaporation of high-purity (99.9%) NiO
pellets. A 10 mm diameter NiO pellet was used as a source target for evaporation. The NiO target was placed in copper crucibles
and kept in the water cooled copper hearth of the electron gun for evaporation. The substrates were placed normal to the evaporation
source at a distance of about 50 mm. Before deposition, the material was slowly out gassed with a shutter blocking the vapour
from the sample surface. All the films were deposited at a substrate temperature (Ts) of 473 K. The deposition parameters
maintained during the preparation of NiO films are given in Table 1. The structural properties of the films were analyzed by Seifert
3003TT X-ray diffractometer, using Cu K radiation (k = 0.1546 nm). Microstructure and elemental composition for the prepared
samples were analyzed through EDAX using Oxford Inca Penta FeTX3 EDS instrument attached to Carl Zeiss EVO MA 15
Scanning Electron Microscope. The surface morphology of the deposited films was characterized by atomic force microscope
(Park Systems). The optical band gap of the films was determined using Perkin Elmer Lambda 950 UV-Vis-NIR
spectrophotometer. The electrical properties of the films were analyzed by the Hall Effect measurement system - (HMS-3000VER
3.51.3).

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Effect of Annealing Temperature on Optical and Electrical Properties of Electron Beam Evaporated NiO Thin Films
(IJSTE/ Volume 2 / Issue 11 / 127)

Table 1
The deposition parameters maintained during the preparation of NiO films
Parameters
Values
The target to substrate distance
50 mm
Base pressure
6.6 x 10-5 Pa
Working pressure
2 x 10-4 Pa
Substrate temperature
473 K
Evaporation time
10 min
Accelerating voltage
5 kV
Filament current
120 mA

III. RESULTS AND DISCUSSION

Structural Analysis:
Thermal annealing is one of the most important factors, since annealing temperature can improve the crystal quality and reveal
structural defects in thin films.During the annealing process, the structure and the stoichiometric ratio of the films change due to
the movement of dislocations and defects.Fig.1 shows the X-ray diffraction patterns of NiO films annealed at different
temperatures (30 0C, 200 0C, 300 0C, 400 0C and 500 0C). The crystallite orientation, lattice parameter and crystallite size as a
function of annealing temperature is shown in table 2.

Fig. 1: X-ray diffraction patterns of NiO films deposited at different annealing temperatures
Table 2
Crystallite size, Orientation and lattice parameter values of NiO thin films deposited at different annealing temperatures by Electron beam
evaporation method
Sample (oC) Orientation Crystallite size (nm) Lattice parameter (nm)
30
(220)
8.12
0.4213
200
(220)
10.43
0.4208
300
(220)
12.26
0.4204
400
(220)
13.04
0.4188
500

(220)

14.82

0.4196

Table 2 shows Crystallite size, Orientation and lattice parameter values of NiO thin films deposited at different annealing
temperatures by Electron beam evaporation method.
The intensity of the (220) preferred orientation increased with increasing the annealing temperature up to 400 oC and decreased
further increasing the annealing temperature. The intensity of (220) orientation decreased and another peak with orientation (111)
was observed when the films annealed at 500 oC. The films annealed at 400 oC exhibited better crystallinity when compared to
other films.
Morphological Studies:
The effect of annealing temperature on the surface morphology of the films was assessed by SEM. SEM micrographs of NiO
thin films annealed at different temperatures are shown in Fig. 2. It was observed that the as-deposited NiO thin films

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Effect of Annealing Temperature on Optical and Electrical Properties of Electron Beam Evaporated NiO Thin Films
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exhibited dense surface and fine grains were observed at 300 oC annealed films and the grain size was increased with increasing
annealing temperature. It was obvious that the accelerated inter-diffusion between the deposited atoms and the glass substrates
might played an important role in increasing the grain size.

Fig. 2: SEM image of of NiO thin films at annealing temperatures (a) 30 0C, (b) 200 0C, (c) 300 oC, (d) 400 oC and (e) 500 oC

Surface Morphology Studies:

To examine the effect of the annealing process on the topography of the films, room temperature AFMstudies were performed and
the AFM images of the prepared sample were shown in Fig.3.

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Effect of Annealing Temperature on Optical and Electrical Properties of Electron Beam Evaporated NiO Thin Films
(IJSTE/ Volume 2 / Issue 11 / 127)

Fig. 3: AFM images of NiO thin films Annealed at temperatures 30 oC, 300 oC and 500 oC

The as-deposited films exhibited a very smooth surface, with a mean roughness of 8.81 nm. When the films annealed at 200 oC,
columnar structures grew independently, building up high mountains and deep valleys on the surface. On further increasing the
annealing temperature to 300oC, the density and height of columnar structures increased as well. The formation of columnar
structures was ascribed to the grain nucleation and growth during the crystallization process. At higher annealing temperature
(500oC), surface roughness of all the films increased due to increasing the columnar structures.
Compositional analysis:
Fig.4 confirmed the presence of Ni and O elements in the NiO thin films. The films annealed at 300oC were nearly stoichiometric.
However, no significant change was observed in elemental composition upon further annealing. Elemental Si arises due to the
glass substrate. At high temperatures, due to increase in surface roughness, Si peak intensity was decreased.

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Effect of Annealing Temperature on Optical and Electrical Properties of Electron Beam Evaporated NiO Thin Films
(IJSTE/ Volume 2 / Issue 11 / 127)

Fig. 4: EDS spectra of NiO thin films at annealing temperatures 30oC, 300oC and 500oC

Optical Properties:
The optical transmittance spectra of the as-deposited and annealed NiO films are shown in Fig. 5 (a). The optical transmittance of
the as-deposited film was about 31%. The optical transmittance of the films increased from 39% to 48% with increasing
of annealing temperature from 200 to 300 oC. On further increasing the annealing temperature to 500 oC, the transmittance of
the films decreased to 34%.The absorption edge was shifted towards lower wavelength with the increase of annealing temperature.

Fig. 5: (a) Optical transmittance spectra and (b) Plot of (hv)2 and (hv) of NiO films as a function of annealing temperature

The absorption edge was shifted towards lower wavelength with the increase of annealing temperature. The increase in
transmittance of the films was related to an increase in grain size of the films.
The reduction in the number of unsaturated bonds decreased the density of localized states in the band structure, consequently
increased the optical band gap. The variation of optical band gap with the annealing temperature of NiO thin films at different
annealing temperatures was shown in Fig. 5 (b). The optical band gap of the as-deposited film was 3.43 eV and increased to
3.68 eV with the increase of annealing temperature up to 400 oC, thereafter decreased to 3.48 eV at higher annealing temperature
of 500oC. H. Wang et al. reported the similar behavior of decreasing optical band gap from m 3.93 eV to 3.55 eV [11].

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Effect of Annealing Temperature on Optical and Electrical Properties of Electron Beam Evaporated NiO Thin Films
(IJSTE/ Volume 2 / Issue 11 / 127)

Electrical Properties:
Fig.6 shows the effect of annealing temperature on resistivity, mobility and carrier concentration of NiO thin films. The electrical
resistivity of NiO thin films has a strong dependence on the microstructural defects existing in NiO crystallites, such as nickel
vacancies and interstitial defects. The increase of carrier concentration, carrier mobility and decrease of resistivity may be due to
the improvement of the crystallinity during thermal annealing, which was also evident from XRD studies. Thin film samples
annealed at 400oC showed decreased resistivty compared to other samples.

Fig. 6: Behaviour of resistivity, mobility and carrier concentration of NiO thin films as a function of annealing temperature

IV. CONCLUSION
A systematic procedure was adopted in the preparation of NiO thin films using electron beam evaporation technique and the
properties of these films were systematically studied at various annealing temperatures. The films annealed at a temperature of
400 oC exhibited single phase columnar growth with better optical and electrical properties which are suitable for sensor
applications.
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