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High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin

Coating Technique: Effect of Annealing Temperature

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DOI: 10.1166/jno.2018.2358

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ARTICLE

High Transparent Titanium Dioxide-Anatase Thin

Films Deposited by Spin Coating Technique:
Effect of Annealing Temperature
M. Dahnoun1 , A. Attaf1, ∗ , H. Saidi 1 , R. Benatia1 , A. Yahia1 , C. Khelifi1 , A. Saadi1 , N. Attaf2 ,
H. Ezzaouia3 , and L. Guerbous4

TiO2 thin films were deposited on microscopic glass (HiLab) substrate by spin coating technique. The influence
of the annealing temperature on the structural, optical and electrical properties was studied. X-ray diffraction
and Fourier transform-infrared absorbance were used to determine the films structural properties, UV-Vis
spectroscopy and photoluminescence to investigate the optical proprieties of thin films and two-point probe
method to study the electrical conductivity. Structural analysis show that the films have tetragonal structure
of anatase with a preferred growth orientation along the (101) plane and the crystallite size increased from
24 nm at 400  C to 81 nm at 600  C where the deformation was changed inversely indicating the films
crystallinity improvement. The films have a high transmittance in the visible region reach to 90% and the
direct and indirect band gaps exhibit a little decrement with annealing temperature. Furthermore, the films
have a low electrical conductivity.
Keywords: Thin Films, Titanium Dioxide, Spin Coating, Annealing Temperature, Structural Properties, Optical Properties.

1. INTRODUCTION
Transparent conductive oxides (TCOs) thin films have
attracted optical and electrical properties which make them
a productive field of many researches. The most attrac-
tive TCOs are ZnO, SnO2 , In2 O3 and TiO2 this last has
been widely investigated for its promised characteristics.
TiO2 thin films are used for a diversity applications: buried
contact solar cells have been fabricated using TiO2 as an
optical coating,1 it has interesting applications in chemistry
due to its behavior as a reaction catalyst,2 photocatalyst,3
gas sensor,4 biocoating material5 pigments,6 transparent
self-cleaning surfaces,7 in microelectronics it has attracted
1
Laboratoire de Physique des Couches Minces et Applications (LPCMA),
University of Biskra, BP 145 RP, 07000 Biskra, Algeria
2
Unité de Recherche “Sciences des Matériaux et Applications,”
Université Mentouri, Constantine, 25000, Algérie
3
Laboratoire des semi-conducteurs, nanostructures et Technologie
Avancée, Research and Technology Centre of Energy, Borj-Cedria
Science and Technology Park, BP 95, 2050 Hammam-Lif, Tunisia
4
Centre de Recherche Nucléaire d’Alger (CRNA), 2 Bd. Frantz Fanon,
BP 399, Alger RP, Alger 16000, Algérie
∗
Author to whom correspondence should be addressed.
Email: ab_attaf@univ-biskra.dz
Received: xx Xxxx xxxx
Accepted: xx Xxxx xxxx
much attention due to its very high dielectric constant (k)
which makes TiO2 an interesting candidate for high-k gate
dielectric. Finally, TiO2 films have been used in the fab-
rication of TiO2 /TiN/TiO2 /glass heat mirrors (structures
with a high transmittance in the visible region and high
reflectance in the infrared).8
TiO2 can exist as an amorphous layer and also in
three crystalline phases: anatase (tetragonal), brookite
(orthorombic) and rutile (tetragonal).9 Anatase is the dom-
inant phase at a low temperature due to its thermodynamic
stability. It has a wide band gap (3.2 eV), high refractive
index at 500 nm which is about 2.5 for bulk titania,10 good
chemical stability, high transmittance in visible range as a
thin film, and high dielectric constant.
Various methods have been reported for the prepa-
ration of TiO2 thin films: spray technique,11–13 sol–
gel method,14 hydrothermal method,15 chemical bath
deposition method,16 DC magnetron sputtering,17 elec-
tron beam,18–20 mist plasma evaporation,21 pulsed laser
deposition,22 and spin coating.23
In the present work spin coating technique was used to
deposit TiO2 thin films on glass substrates. To study the
influence of annealing temperature (Ta ) on structural, opti-
cal and electrical properties we changed Ta from 400  C to
600  C and we fixed the other parameters. The aim of this

J. Nanoelectron. Optoelectron. 2018, Vol. 13, No. xx 1555-130X/2018/13/001/007 doi:10.1166/jno.2018.2358 1

High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin Coating Technique: Effect of Annealing Temperature Dahnoun et al.

work is to obtain TiO2 thin films with appropriate proper- 12500

ties for photovoltaic applications using a simple and low (101)
coast method. (105)
10000 (211)
(004) (200) (204) 600°C
2. EXPERIMENTAL DETAILS
To prepare the solution we use 0.605 ml of Titanium Tetra 7500

Intensity (a.u)
550°C
Isopropoxide (TTIP) Ti[OCH(CH3 2 ]4 (STREM CHEM-
ICALS) as precursor, 10 ml of ethanol as solvent and
0.210 ml of Acetylacetone, the latter acts as stabilizer 5000 500°C
which its molar ratio to TTIP was fixed at 1. The mixture
was stirred by a magnetic stirrer at 50  C for 3 h until
2500 450°C
obtained a clear, yellowish and a little viscous solution.
The prepared solution was dropped on glass substrate then
it was rotated at 4000 rpm for 30 s using a Holmarc spin 400°C
0
coater. After each coating, the film was dried at 250  C for
10 min on a furnace. This step was repeated for 5 times to 20 25 30 35 40 45 50 55 60 65 70 75 80
obtain a multilayer film. The obtained films were annealed 2θ (degree)
at different temperatures in air furnace for 2 h. The flow
Fig. 2. XRD patterns of annealed TiO2 thin films.
chart of the preparation of TiO2 thin films is shown in
Figure 1.
this direction.24 Also, it is clear that the intensity of (101)
peak slightly increases with the increase of annealing tem-
3. RESULTS AND DISCUSSION perature from 400  C to 600  C, i.e., the increasing anneal-
3.1. Structural Characterization ing temperature improved the crystallinity of TiO2 .9 The
Figure 2 shows the X-ray patterns of annealed TiO2 films. crystallite size was calculated from Scherrer’s formula:25
It has been found that the material observed is TiO2 poly-
crystalline having tetragonal structure of anatase which is D = k/ cos  (1)
agreed with JCPDS (n 21-1272). For a crystalline phase
Where k = 09 is the shape factor,  is the wavelength used
to develop, the depositing atoms should have sufficient
(1,54060 Å),  is the full width at half maximum (FWHM)
energy. This gives the atoms sufficient mobility to place
in radians and  is the Braggs angle. From Figure 3, and
themselves to low energy sites leading to the formation of
Table I, we observe that the FWHM decreases when the
crystalline phases. High substrate temperatures can achieve
annealing temperature increases. Decreasing in the FWHM
the sufficient energy to generate crystalline phases. This
value leads to increase in crystallite size. This may prob-
may be the reason for the growth of crystalline anatase
ably be attributed to the following: when the film atoms
phase in the present study.9 It can be seen that the intensity
obtain enough energy in the annealing process they will
of the (101) direction is higher than the others this may be
migrate and restructure into thin films. The crystallites then
due to the value of the free surface energy is minimal in
grow larger correspondingly.26

Ethanol (10ml) TTIP (0.605ml) Acetylacetone (0.210ml) 0,40 100

FWHM(°)
0,35 D(nm) 90
Stirring at 50°C for 3h 80
0,30
70
FWHM (°)

Clear, yellowish and a

D (nm)

0,25
little viscous solution 60
0,20 50
Spin coating
0,15 40
Drying at 250°C for 10min
30
0,10
Annealed at 400, 450, 500, 550, 600°C 20
400 450 500 550 600
TiO2 thin films T (°C)

Fig. 3. Full width at half maximum (FWHM) and crystallite size D

Fig. 1. TiO2 thin films deposition steps. variations.

2 J. Nanoelectron. Optoelectron., 13, 1–7, 2018

Dahnoun et al. High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin Coating Technique: Effect of Annealing Temperature

Table I. Structural parameters.

Annealing Deformation Dislocation density Stress Lattice Lattice

temperature ( C) D (nm)  · 103  · 1014 (ligne/m2  (GPa) constant a (nm) constant c (nm)

400 24,355 1.424 16859 −0,201 3,768 9,302

450 30,448 1.139 10787 −0,161 3,771 9,472
500 34,790 0.996 8262 −0,141 3,780 9,326
550 30,448 1.139 10787 −0,161 3,775 9,410
600 81,130 0.427 1519 0,0604 3,791 9,569

The residual strain ( and dislocation density ( were
determined as follows:27
 =  cos /4
Where  is FWHM in radians and  is the Braggs angle.
h2 + k2 /a2 + l2 /c 2 (5)
The dislocation density is defined as the length of dislo-
cation lines per unit volume of the crystal, and it is esti-
mated from the subsequent relation using simple approach
of Williamson and Smallman:28
 = 1/D2
The strain values for the TiO2 films deposited at the
annealing temperature of 400, 450, 500, 550 and 600
are 1.424, 1.139, 0.996, 1.139, 0.427 (10−3  respectively.
Our results revealed a decrease of strain in the films
with annealing temperature. This is due to the increase
of crystallite size with temperature that led to reduction
in inter-crystalline barriers as grain boundary area in the
layers. Moreover at higher growth temperature, the sur-
face mobility increases, allowing the film to decrease its
total energy by growing large grains thereby decreasing its
grain boundary area.29
The micro stress was calculated using the following
formula:30
stress =
/2 · E (4)
Where E is the Young’s modulus of the material
(282.76 GPa),  is the strain of the film. As show in
1.6
Table I, the negative (positive) sign indicates that the film
is in compressive (depressive) stress.
The lattice constants ‘a’ and ‘c’ for the films are calcu-
(2) lated from:30
1/d 2 =
From Table I, and Figure 5 we observed that the ‘a’
and ‘c’ values are less than the standard values of TiO2
(a = 3.785 nm and c = 9514 nm) JCPDS (no. 21-1272)
(3) which indicate that the stress is compressive for
Ta < 550  C, whilst when Ta = 600  C the lattice constants
become greater than the standard values and the stress was
converted into depressive correspondingly which leaves
some suggests to that the appropriate annealing tempera-
ture to prepare a stress-free TiO2 films is between 550  C
and 600  C.
3.2. Fourier Transform-Infrared (FTIR)
Figure 6 shows the Fourier transform-infrared absorbance
spectra of TiO2 films. The peak around 445 cm−1 is
assigned to the stretching vibration mode of Ti–O–Ti bond
and the peak located around 540 cm−1 is assigned to the
Ti–O stretching vibration mode. Larbot et al.1 and Chhor
et al.32 have divided the range of the low frequencies of
TiO2 [400–800] cm−1 to two parts. The first is between
[436–495] cm−1 which related to the vibration of Ti–O–Ti
and Ti–O bonds, the second part is from 550 to 653 cm−1
which associated to Ti–O bond. Moreover, we observe that
18 the intensity of the two peaks increases with increasing
dislocation density δ x 1014 (ligne/cm2)

deformation
1.4 dislocation density 16
0,15
14
deformation (ε x 10–3)

1.2 stress
0,10
12
1.0 0,05
10
0.8 0,00
8
stress (GPa)

400 450 500 550 600

0.6 –0,05
6 Annealing temperature (°C)
0.4 4 –0,10

0.2 2 –0,15

0.0 0 –0,20
400 450 500 550 600
–0,25
T (°C)
–0,30
Fig. 4. Deformation ( and dislocation density ( as a function of
annealing temperature. Fig. 5. The variations of stress with annealing temperature.

J. Nanoelectron. Optoelectron., 13, 1–7, 2018 3

High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin Coating Technique: Effect of Annealing Temperature Dahnoun et al.

5,5 Ti-O 5.0

400 °C n(400 °C)
5,0 450 °C 4.5 n(450 °C)
500 °C
4,5 n(500 °C)
550 °C 4.0
4,0 600 °C Ti-O-Ti n(550 °C)

Refractive index
n(600 °C)
Intensity (a,u)

3,5 3.5

3,0 3.0
2,5 2.5
2,0
2.0
1,5
1,0 1.5
0,5 1.0
0,0 300 400 500 600 700 800 900 1000 1100
1000 900 800 700 600 500 400 Wavelength (nm)
Wavenumber (cm–1)
Fig. 8. Refractive index variations.
Fig. 6. Fourier transform-infrared absorbance spectra of the annealed
TiO2 thin films. their RF-sputtered TiO2 films with anatase phase. In this
work, a slight decrease in transmittance is observed with
annealing temperature due the improvement of the crystal- the increase of annealing temperature as can be seen in
lization degree which confirms the results obtained from Figure 7. Saini et al.34 and Yang et al.35 also reported
the DRX. the decrease of transmittance with increasing anneal-
ing temperature. Also we note that the reflectance was
changed inversely with the transmittance i.e., the top of
3.3. Optical Characterization
the transmittance were corresponding to the bottom of the
Figure 7 represents the transmission and reflection spec-
reflectance and vice versa.
tra of TiO2 thin films in the wavelength range of
The refractive index n was calculated at different wave-
300–1100 nm. We note that the films have a high trans-
lengths using the following relation:36
mittance in the visible region reach to 90% and they have
a very weak transmittance in the UV region close to 0% n =
1 + R/
1 − R + 4R/
R − 12 − k2 
1/2
(6)
this last is due to the excitation and the migration of the
electrons from the valence band to the conduction band. Where k = /4 is the extinction coefficient, is the
It is observed that the deposition temperature does not absorption coefficient and  is the incident wavelength.
significantly affect the transmittance. It may be attributed Figure 8 manifests the refractive index curves for the films
to the slight variation of crystallinity and the absence of annealed at different temperatures. From Figure 8 and
phase transformation in the grown anatase TiO2 films. Table II, we can see that the value of refractive index of the
Wang et al.33 reported higher visible transmittance in films at  = 550 nm close to the value of bulk TiO2 . Also,
we note that the refractive index increases with annealing
temperatures for T > 500  C which found to be 2.10, 2.41
100
T(%) and 2.79 at 500, 550 and 600  C respectively. The increase
may be attributed to higher packing density within the film
80 and a slight increase in crystallization. Hasan et al.9 also
observed an increase in refractive index with annealing
(400 °C) temperature in their RF-sputtered annealed films.
T(%) , R(%)

60 (450 °C) The optical band gap was estimated using Tauc’s
(500 °C)
(550 °C)
model37 in the high absorbance regions of the transmit-
R(%) tance spectra:
40 (600 °C)
h = A
h − Eg n (7)

20 Where is the absorption coefficient, h is the photon

energy, Eg is the optical band gap, A is an h independent
constant and n has four numeric values
1/2 for allowed
0 direct, 2 for allowed indirect, 3 for forbidden direct and
400 600 800 1000 3/2 for forbidden indirect optical transitions). The direct
Wavelength (nm) and indirect band gaps were determined by the extrapola-
Fig. 7. Transmittance and reflectance spectra of annealed TiO2 thin tion of the linear region of
h2 versus h and
h1/2
films. versus h curves respectively. As can be seen from

4 J. Nanoelectron. Optoelectron., 13, 1–7, 2018

Dahnoun et al. High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin Coating Technique: Effect of Annealing Temperature

(a) 4,00E+011 (b) 800

400 °C 400 °C
450 °C 700 450 °C

(αhν)1/2 (cm–1.eV)1/2
(αhv)2 (cm–1.eV)2
3,00E+011 500 °C 600 500 °C
550 °C 550 °C
600 °C 500 600 °C
2,00E+011 400
300
1,00E+011 200
100
0,00E+000 0
3,0 3,2 3,4 3,6 3,8 4,0 3,1 3,2 3,3 3,4 3,5 3,6 3,7 3,8 3,9 4,0
hν (ev) hν (ev)

Fig. 9. Extrapolation of linear region: (a) for

h2 versus h, (b) for
h1/2 versus h.

Figure 11 and Table II, the direct and indirect band gaps grains are not preferentially oriented, the emitted light may
for the annealed films were insignificantly larger than the not be effectively detected, or the grain boundary may
bulk anatase band gap (3.2 eV). In the other hand, the val- produce different kinds of defects such as non-radiative
ues deduced in this work are in good agreement with the defects.41 42
findings of Hasan et al.9 and Wang et al.33 Also, we note
that the optical gap decreases with the increase of anneal- 3,80
ing temperature due to the improved crystalline structure Eg(direct)
of the TiO2 thin films with annealing temperature.38 Analo- Eg(indirect)
3,76
gous trend for the direct and indirect optical band gap was
reported by Ting et al.39 Yoo et al.40 reported an increase
of indirect band gap in their RF-sputtered TiO2 films with 3,72
Eg (eV)

the increase of annealing temperatures. 3,55

3,50
3.4. Photoluminescence
Figure 11 presents the photoluminescence spectrum of 3,45
anatase TiO2 films annealed at different temperatures, from
3,40
this figure we can see that there are five interesting emis-
sion peaks at 385 (ultraviolet luminescence), 414, 438, 477 3,35
and 524 nm (visible emission). The PL spectra of anatase 400 450 500 550 600
TiO2 materials is because of three kinds of physical ori- Annealing temperature (°C)
gins namely self-trapped excitons, oxygen vacancies and Fig. 10. Direct and indirect optical gap (Eg ) as a function of annealing
surface defects.17 temperature.
The visible emission can be attributed to the radiative
defects related to the interface traps existing at the grain
boundaries and which are emitted from the radiative tran- 120 385 400 °C
450 °C
sition between these levels and valence band. This last can
100 500 °C
be confirmed by the decrease of the peaks intensities with 414 438
550 °C
the decrease of the grain boundary area. However, if the
PL Intensity (a,u)

80 600 °C

60
Table II. Refractive index (n), direct and indirect optical gap (Eg ) as a
477
function of Ta . 40

Annealing Refractive index Direct Indirect

20 524
temperature ( C) n at 550 (nm) Eg (eV) Eg (eV)

400 2,47 3,778 3,512 0

450 2,25 3,769 3,410
500 2,10 3,751 3,406 350 400 450 500 550 600 650 700 750
550 2,41 3,745 3,389 Wavelength (nm)
600 2,79 3,727 3,362
Fig. 11. Photoluminescence patterns of TiO2 thin films.

J. Nanoelectron. Optoelectron., 13, 1–7, 2018 5

High Transparent Titanium Dioxide-Anatase Thin Films Deposited by Spin Coating Technique: Effect of Annealing Temperature
100
Conductivity σ (Ω .cm)–1
80
60
40
20
0 in annealing temperature higher than 450  C due to the
400 450
Annealing temperature (°C)
Fig. 12. Electrical conductivity variations.
Table III. Electrical conductivity values.
Annealing temperature ( C)
 · cm)−1
400
450
500
550
600
3.5. Electrical Conductivity
The electrical conductivity was extracted by two-point
probe method by a pico ampere meter (Keithley 617).
Using the following formula:43
=
1/R ·
L/W · d (8)
Where: R is the resistance, L is the distance between
the two metal contacts, W is the channel width and d
is the thickness of the film. Figure 12 reveals the varia-
tion of the conductivity of TiO2 films which have a neg-
ligible variation with annealing temperature except a high
observed value (96.42 ( · cm)−1  at 400  C. The low con-
ductivity for Ta ≥ 450  C may be due to the adsorption
of air oxygen atoms. The oxygen atoms are first physi-
cally adsorbed at the grain boundaries and on the surface
of the thin films and acts as traps. After that, they become
chemisorbed by capturing the conduction electrons, which
binds them to the surface leading to decrease in free carrier
concentration.44
4. CONCLUSIONS
Spin coating technique was used successfully to prepare
high transparent and (101) oriented TiO2 -anatase thin films
on glass substrates. The deposited films have a poly-
crystalline structure with a preferential growth orientation
according to the (101) plane of the anatase phase as can be
seen from XRD patterns, the crystallite size increases from
24 nm to 81 nm when annealing temperature increases
from 400  C to 600  C causing a decrease in strain and
dislocation density. From FTIR study we inferred that the
6 J. Nanoelectron. Optoelectron., 13, 1–7, 2018
Dahnoun et al.
annealing temperature improves the crystallization degree.
The UV-Vis characterization showed that TiO2 films are
high transparent with a value between 70% and 90% in
visible range. Also, we observed that the fall of transmit-
tance between 300 nm and 400 nm indicates that the films
absorb the light ultra violet which makes them appropri-
ate for optical window applications. Moreover, the direct
and indirect optical gaps reveal a decrease with annealing
temperature. TiO2 films exhibit low electrical conductivity
adsorption of air oxygen atoms and the effect of factors
500 550 600 like defect association and chemical changes especially for
spin-coated films which cannot be ruled out.
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