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Co doping effect on structural and optical properties of nickel oxide (NiO) thin
films via spray pyrolysis

Article  in  Optical and Quantum Electronics · September 2019

DOI: 10.1007/s11082-019-2026-2

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Journal of ELECTRONIC MATERIALS, Vol. 48, No. 5, 2019
https://doi.org/10.1007/s11664-019-07074-0
Ó 2019 The Minerals, Metals & Materials Society

Effect of Substrate Temperature on Properties of Nickel Oxide

(NiO) Thin Films by Spray Pyrolysis

RANJIT S. KATE,1 SURAJ C. BULAKHE,1 and RAMESH J. DEOKATE 1,2

1.—Vidya Pratishthan’s, Arts, Science and Commerce College, Baramati, MS 413 133, India.
2.—e-mail: rjdeokate@gmail.com

NiO thin films were deposited on a glass substrate and investigated for the
physical properties optimized through substrate temperature (350–390°C)
using a spray pyrolysis technique. The effect of substrate temperature on
deposited NiO thin film was studied by thermogravimetric analysis and dif-
ferential thermal analysis, X-diffraction (XRD), field electron scanning elec-
tron microscopy, optical absorption and electrical measurement techniques.
XRD analysis indicates that NiO thin films are of a polycrystalline cubic
structure. Optical properties are calculated with help of transmittance and
absorbance data in the wavelength range between 200 nm and 900 nm. The
optical band gap energy values increased from 3.1 eV to 4.0 eV with substrate
temperature. Further, the extinction coefficient, refractive index, and real and
imaginary parts of dielectric constant and optical conductivities of NiO thin
films were calculated. The electrical resistivity measurement shows conduc-
tivity of the NiO thin film increased with increase in substrate temperature.

Key words: NiO, spray, composition, electrical properties, semiconducting

behavior

vacuum evaporation,21 chemical bath deposition22,23

INTRODUCTION
Transition metal oxides can be used as candidate
materials in the supercapacitor, electrochromic dis-
play devices, energy efficient smart windows,
hetero-junction solar cells, gas sensing applications,
p-type transparent conducting films, positive elec-
trode cells and in antiferromagnetic layers.1–10
Nickel oxide is a wide band gap (3–4 eV) semicon-
ductor having high chemical stability, outstanding
durability, low material cost and capable ion storage
material in terms of cyclic stability.11,12 In the
present situation, many researchers are involved in
the synthesis of NiO in thin films form or other
forms, which shows p-type conductivity due to Ni
vacancies and/or O interstitial.13 Thin films of NiO
can be fabricated by various deposition techniques
such as sol–gel,14 dip coating, spin coating, elec-
trodeposition,15 spray pyrolysis,16–19 sputtering,20
(Received October 21, 2018; accepted February 14, 2019;
published online March 1, 2019)
and pulsed laser deposition.24 Amongst all, the
spray pyrolysis is mainly appropriate, a simple
and low-cost method, mostly used for large area
applications.25 This method is broadly used to
prepare oxide thin films in relative to others.26
Other authors have reported the effect of substrate
temperature, precursor molarity, doping and deposi-
tion time on the microstructural and optical proper-
ties of the metal oxide thin films.27,28 The
crystallinity and band gap of very thin NiO films
has been improved with the substrate temperature.
For this reason, this work focuses on the correlation
between the band gap energy and the crystallite size
of NiO thin films with substrate temperature. Hence,
in the present work, the effect of substrate temper-
ature on structural, morphological, optical and elec-
trical properties of NiO thin films is described.
EXPERIMENTAL DETAILS
The nickel nitrate Ni(NO3)2Æ6H2O (0.1 M) (AR
grade, SD fine, 99.5% pure) was dissolved in
aqueous solution and sprayed onto preheated glass

3220
 Effect of Substrate Temperature on Properties of Nickel Oxide (NiO) Thin Films by Spray 3221
Pyrolysis

substrates at different temperatures within 350–

390°C using a simple homemade chemical spray
pyrolysis experimental setup.5 Before, the glass
microslide were cleaned ultrasonically in acetone
solution and then rinsed in distilled water to get a
cleaned surface which is important to start nucle-
ation of deposited films.29 The sprayed droplets
undergo evaporation, solute condensation, and ther-
mal decomposition resulting in a very adherent
blackish thin film of nickel oxide. Formation of
nickel oxide is represented by following chemical
reaction5:
 
2 NiðNO3 Þ2 þ 2H2 O ! 2NiO þ 4ðNO2 Þ " þ 2H2 O
" þ O2 " :
ð1Þ Fig. 1. TG–DTA curve of the precursor.

The decomposition behavior of the precursor was

carried out by thermogravimetric analysis (TGA)
and differential thermal analysis (DTA) (Shimadzu
50). Structural analysis was carried out with an x-
ray diffractometer (XRD Bruker AXS D8 Advance
Model) with the radiation source Cu-Ka (k = 1.5406
Å) in the 2h range 20°–80° with accelerating voltage
40 kV and current scan speed 40 mA. A field
emission-scanning electron microscope (FE-SEM
SU8000 Hitachi) is used to study the surface
morphology and chemical composition of NiO thin
films. The optical characterization was carried out
at room temperature in the wavelength range 400–
900 nm through Uv–visible spectroscopy (Perkin
Elmer Lambda 1050 UV–Vis–NIR spectrophotome-
ter). Surface electrical properties were studied by a
standard two-point probe resistivity unit.

RESULTS AND DISCUSSION

Thermal Decomposition of Nickel Nitrate
The suitable temperature for the decomposition of
Ni(NO3)2 precursor to form NiO, the thermo-gravi-
metric (TGA) and differential thermal analysis (DTA)
has been carried out in the temperature between 0°C
and 900°C in the interval of 10°C/min as shown
Fig. 1. The thermal evolution in air atmosphere takes
place in four consecutive stages corresponding to
weight losses in which the inflection point coincides
with the temperature of the endotherms and
exotherms in a DTA trace. In the temperature range
of 188–350°C, most of the weight loss of nickel nitrate
takes place, resulting in the removal of the acetate
group from the precursor and formation of a NiO
phase. Next to 350°C, the DTA traces are steady with
no more weight loss up to 550°C. The results of TGA/
DTA specified the formation of NiO by decomposition
of nickel nitrate at 350°C.
X-Ray Diffraction Studies
The x-ray diffraction patterns of NiO thin films
are shown in Fig. 2 at different substrate
Fig. 2. X-ray diffraction patterns of NiO films deposited at different
substrate temperatures.
temperatures (350–390°C). All the patterns of the
films are polycrystalline in nature with cubic (bun-
senite, JCPDS 004-0835) phase having a preferred
orientation along (1 1 1) directions and a weak
reflection along the (2 2 0) plane. The peaks (1 1 1),
(2 0 0) and (2 2 0) located around 37.3°, 43.4° and 63°
for all deposition temperatures belonging to the
cubic structure of NiO. The observed unit cell
parameter is in good agreement with standard unit
cell parameters.30 Table I shows the microstruc-
tural properties of NiO thin films deposited at
different substrate temperatures. The average crys-
tallite size of the films is calculated using Scherrer’s
formula31:
kk
D¼ ; ð2Þ
b cos h

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