Physica B: Condensed Matter 563 (2019) 30–35

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Physica B: Condensed Matter

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

Physical properties and Rietveld analysis of Fe2O3 thin films prepared by T

spray pyrolysis: Effect of precursor concentration
Rihab Ben Ayed∗, Mejda Ajili, Najoua Kamoun Turki
Université Tunis El Manar, Faculté des Sciences de Tunis, Département de Physique, LR99ES13 Laboratoire de Physique de la Matière Condensée (LPMC), 2092, Tunis
Tunisie, Tunisia

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

Keywords: Iron oxide (Fe2O3) thin films have been prepared starting from iron chloride (FeCl3) precursor by spray pyrolytic
Iron oxide decomposition of FeCl3 on an ordinary glass substrate at 450 °C. The precursor concentration (C) has been varied
Chemical spray pyrolysis from 0.06 to 0.3 mol l−1 keeping the other deposition parameters fixed. The (C) effect on the structural, optical
Precursor concentration and electrical properties has been studied. The XRD analysis shows that Fe2O3 thin film has a rhomboedric
Physical properties
structure with (104) plane as preferential orientation. A degradation of crystallinity followed by a change in plan
MAUD analysis
orientation from (104) to (110) has been observed, when (C) has been raised to 0.2 mol.l−1.The optical trans-
mittance spectrum shows that T(λ) decreases at higher precursor concentration. Optical band gaps w decreased
from 2.21 to 2.08 eV for direct transition and from 2.03 to 1.99 eV for indirect transition when (C) increases from
0.06 to 0.3 mol l−1. The extinction coefficient (k) and refractive index (n) were also has been estimated and
studied. The films deposited with C = 0.14 mol l−1 has shown the maximum mobility of 62 cm2 V−1.s−1 at room
temperature. All physical properties of Fe2O3 thin films investigated in this work were strongly dependent upon
the precursor concentration. The obtained results provide valuable information about structural, optical, pho-
toluminescence and electrical properties of sprayed Fe2O3, which is a very helpful issue for better understanding
and perfection of the semiconductor quality for the optoelectronic application.

1. Introduction
In recent years, interest on oxide thin films semiconductors has
raised due to their attractive physical properties and their usefulness in
a broad range of applications. In iron oxide, three main types, namely,
ferrous oxide (FeO), ferric oxide (Fe2O3) and magnetite (Fe3O4) are well
known. Fe2O3 may crystallize in four phases α, β, ε and δ [1]. Hematite
(α - Fe2O3) is considered to be the greatest material. In fact, it has been
investigated extensively due to its typical properties such as high
electrochemical stability, nontoxicity, low-cost and environmentally
friendly nature [2,3]. It is an n-type semiconductor with rhomboedric
structure. α -Fe2O3 has an optical mid-band gap of about 2.2 eV [4].
This phase is mainly used in the fields of optoelectronics and electronics
such as gas sensor [5,6], solar cell [6,7], a negative electrode in re-
chargeable batteries [8]splitting water [9]and nonlinear optics [10]. On
reviewing other reports, it has been found that various methods used to
prepare iron oxide thin films like sol-gel [11], sputtering [12], chemical
bath deposition [13], chemical vapor deposition [14], successive ionic
layer absorption [15] and chemical spray pyrolysis (CSP) which is the
most widely used method [16]. This method gives numerous
advantages like simplicity, low cost, and the possibility to produce a
large area of thin films. The main advantage of this method is the fa-
cility of optimizing the different growth parameters like volume, tem-
perature, molarity, substrate nature and substrate-nozzle distance
hence saving time and materials. Towards, metal oxide thin films pro-
duction, the CPS method is thoroughly used thanks to the mentioned
advantages. This technique is described by homogenous distributions
and provides thin layers whose grain shape and size are controlled by
the various growth parameters. Some experimental research indicates
that the precursor concentration is a significant factor to affect the
physical properties of thin films [17–19]. In this work, we have ex-
plored the influence of different precursor concentration on the phy-
sical properties of sprayed Fe2O3 thin films on glass substrates.
2. Experimental details
2.1. Sample preparation
The iron oxide (Fe2O3) thin layers were prepared using iron chloride
(FeCl3) as a precursor. Ordinary glass was used as a substrate for the

∗
Corresponding author.
E-mail address: rihabbenayed149@gmail.com (R. Ben Ayed).

https://doi.org/10.1016/j.physb.2019.03.029
Received 17 February 2019; Received in revised form 20 March 2019; Accepted 21 March 2019
Available online 23 March 2019
0921-4526/ © 2019 Elsevier B.V. All rights reserved.
R. Ben Ayed, et al.
deposition of Fe2O3 thin films by chemical spray pyrolysis technique,
the precursor solution was prepared by dissolved FeCl3 in bi-distilled
water. The precursor concentration in the spraying solution has been
varied from 0.06 to 0.3 mol. l−1. The starting solution (100 ml) with the
previously mentioned concentration sprayed through a nozzle using
compressed air as carrier gas at a constant spray rate of 5 ml/min onto
both ultrasonically cleaned preheated glass substrate at 450 °C. The
Fe2O3 have been formed on preheated substrates by the following re-
action [20]:
2FeCl3 + 3H2 O→ Fe2 O3 + 3H2 ↑ + 3Cl2↑
After deposition the film thickness (e) has been evaluated using the
weight difference method with the following relation [21]:
m
e=
Aρ
where m is the weight of the deposited Fe2O3 layer, A is the area of the
substrate and ρ is the volume density of grown material constant in the
bulk form equal to 5.24 g cm−3.
2.2. Characterization technique
The crystal structure of the elaborated Fe2O3 thin layers has been
investigated by X-Ray diffractometer “XPERT-PRO” with CuKα radia-
tion (λCu = 1.5406 Å) over diffraction angles (θ) ranging from 20 to
70°.
In crystallography, the lattice constants a and c are related to the
interplanar spacing (dhkl) and Miller indices (h, k, and l) by the fol-
lowing relation of the rhomboedric system [22]:
1 4 l2
2
= 2 (h2 + k 2 + hk ) + 2
dhkl 3a c (3)
where dhkl values of Fe2O3 thin films are calculated using Bragg equa-
tion [22]:
2dhkl sinθ = nλ
where n, θ, and λ are respectively, the diffraction order (n = 1), the
Bragg angle and the X-Ray wavelength.
Moreover, from the XRD patterns the crystallite size by using the
well Known Scherrer formula [23]:
0.9λ
D=
β. cosθ
where λ is the wavelength of the incident X-ray (1.54A) and β is the
full-width at half maximum of the preferential peak.
In addition, the dislocation density was calculated from the grain
size by using Williamson and Smallman's formula [23]:
1 large number of defect was appeared and developed through the
δ=
D2
The micro-strain presented as the change in the size of a body
preferred to its original size, and measured from the change of the
lattice spacing using the relation below [24]:
dhkl − d 0hkl
ε=
d 0hkl
where d 0hkl is the strain-free lattice spacing of the (hkl) lattice plane and
dhkl is the lattice spacing.
The transmission T (λ) and reflection R (λ) spectra were recorded
by using a UV–Vis–NIR spectro-photometer (Perkin-Elmer Lambda 950
spectrophotometer) in the wavelength range of [250–2500] nm at room
temperature taking ambient air as reference. Photoluminescence
spectra of the samples were performed using Perkin-Elmer LS 55
Fluorescence spectrometer with an excitation wavelength of 350 nm.
Hall Effect measurements were carried out to determine the electrical
properties in the Van Der Paw configuration.
Physica B: Condensed Matter 563 (2019) 30–35
-1
(110) C=0.3 mol.l
(104)
(012)
-1
C=0.2 mol.l
Intensity (a.u.)
-1
(1) C=0.14 mol.l
C=0.1 mol.l
-1
(2)
-1
C=0.06 mol.l
20 30 40 50 60 70
2 (°)
Fig. 1. XRD patterns of α-Fe2O3 thin films deposited with different precursor
concentrations.
3. Results and discussion
3.1. Structural properties
In order to study the effect of precursor concentration on the
structural properties of Fe2O3 thin layers deposited on preheated glass
(4) substrate at 450 °C from a purely aqueous solution of FeCl3 with various
molar concentration (C = 0.06, 0.1, 0.14, 0.2 and 0.3 mol. l−1). The X-
Ray diffraction patterns of the five samples for different (C) values
(Fig. 1) were proved that high purity hematite films were produced, this
is well consistent with the JCPDS card no. #720469 (space group R-3c),
free from other iron oxide phases and impurities. The layers exhibit
preferred orientation with the (104) plan of the rhomboedric structure.
We observed that (104) peak intensity rises gradually when (C) has
(5)
been increased from 0.06 to 0.14 mol. l−1, this indicates an improve-
ment of the crystallinity of the grown layers. Furthermore, the increase
of precursor concentration to 0.2 mol. l−1 leads to a degradation of
crystallinity with a change of preferential peak to (110). This may be
due to the big amount of precursor. Indeed, at higher concentration a
growing structure causing damaged crystal [25].
(6)
From the positions of the diffraction peaks, the lattice parameters
and the volume cell of the α phase were calculated. As observed in
Table 1 a = b and c were in the range of 5.025–5.073 Å and 13.727 to
13.865 Å, respectively. No observable variation with C was noticed.
Such a small difference may be due to the uncertainty of calculation.
The obtained results at C = 0.14 mol l−1 are the closest to the corre-
(7)
sponding values of bulk hematite (a = b = 5.038 Å, c = 13.771 Å, and
V = 302.72 Å3) with the higher major peak intensity showing the
highest crystallinity among all samples [26].
Additionally, the average crystallite size has been estimated by
applying the Debye Scherrer equation to the preferred orientations, the
obtained values fell in the 42.37–71.25 nm range (Table 2). Other
parameters such as dislocation density (δ) and micro-strain (ε) were
calculated. Table 2 shows maximum values of δ and ε for thin films with
(C) equals to 0.2 and 0.3 mol. l−1. Thin films thickness measurements
of the present iron oxide were carried out for all the layers at different
precursor concentrations. The estimated values of the thickness have
31
R. Ben Ayed, et al. Physica B: Condensed Matter 563 (2019) 30–35

Table 1
Structural parameters of α-Fe2O3 films with various precursor concentrations.
C (mol.l−1) Pic préférentiel 2θ(°) dhkl (Å) I (u.a) a (Å) c (Å) V (Å3)

0.06 (104) 33.024 2.7124 309.49 5.058 13.816 306.19

0.1 (104) 33.247 2.6948 571.66 5.025 13.727 300.20
0.14 (104) 33.233 2.6958 643.18 5.030 13.727 300.79
0.2 (110) 35.384 2.5367 289.97 5.073 13.855 308.84
0.3 (110) 35.401 2.5356 486.85 5.071 13.865 308.88
Fiche PDF (104) 33.117 2.7028 999 5.038 13.771 302.72
(110) 35.611 2.5190 699 5.038 13.771 302.72

Table 2 analysis [28]. The Rietveld refinement of Fe2O3 thin films with a pre-
The variation of thickness (e), grain size(D), dislocation density(δ), and mi- cursor concentration of 0.14 mol. l−1 is shown in Fig. 3. The red solid
crostrain (ε) versus precursor concentrations. fitting curve represents the calculated pattern and the black dots re-
Concentration FWHM (°) e (nm) D (nm) δ(1014 m−2) ɛ(x 10−2 present the experimental XRD pattern and the bottom line shows the
(mol.l−1) (%)) fitting between of them. Depending on the literature [29] the quality of
data from structural fitting is generally checked by Goodness fit (GoF)
0.06 0.1163 376.59 71.25 1.96 0.35
and R- values (Expected error (Rexp) and Bragg factor (Rb)). Results
0.1 0.1338 539.44 61.96 2.60 −0.29
0.14 0.1171 564.31 70.80 1.99 −0.25 obtained have revealed that the two phases, namely hematite belonging
0.2 0.1476 885.49 56.49 3.13 0.70 to iron oxide formation [30] and low-cristobalite, belonging to the
0.3 0.1968 1862.59 42.37 5.56 0.65 substrate [31] are coexisting. This Confirms that Fe2O3 crystalize in the
rhomboedric structure. In a perfect way, GoF close to 1 is performed.
Thence, according to this value, we can conclude that the experimental
been reported in Table 2 and presented in Fig. 2 versus precursor and refinement data match very well.
concentration. As previously shown, the calculated film has thickness
increased from 376.59 nm to 1862.59 nm as (C) has been increased 3.3. Optical properties
from 0.06 mol. l−1 to 0.3 mol. l−1, respectively. In addition, the α-
Fe2O3 thin films have ranged in color from orange to deep red, more- The transmittance T (λ) and reflectance R (λ) spectra of iron oxide
over less adherent layers were formed and this can decolled easily thin films derived from the five different concentrations are shown in
which in turn reduces the crystallinity. It is worth noting that, the Fig. 4. Almost all the films are practically transparent in the long wa-
thickness of the layer is nearly proportional to the precursor con- velength of the visible region and high absorbent, in the UV and the
centration as depicted in Fig. 2. These results are coherent with other short wavelength of the visible region, It can be noticed that the
compounds prepared by chemical spray pyrolysis technique [27]. transmittance of the as-deposited films of precursor concentration is
equal to 0.06 mol. l−1 is virtually similar to that of the films of C = 0.1
3.2. Rietveld analysis and 0.14 mol l−1 [70–85] %. While, when the precursor concentration
reaches 0.2 mol l−1, T(λ) shows a significant change that was decreased
In order to verify and confirm the rhomboedric structure of the to 65% and 35% for C = 0.3 mol l−1 which may be due to the increase
Fe2O3 thin films. An analysis using MAUD (Materials Analysis Using in the thickness of the layers and consequently less transparent samples
Diffraction) software was performed, which is based on Rietveld ana- [32]. Moreover, R(λ) spectra shows the presence of interference fringes
lysis and Warren–Averbach methods in combination with Fourier which indicate the homogeneity of our layers.

2000
Experimental data
Linear Fitting

1600

1200
e(nm)

800

400

0,05 0,10 0,15 0,20 0,25 0,30

-1
C(mol.l )
Fig. 2. The variation of layers thickness versus precursor concentration.

32
R. Ben Ayed, et al. Physica B: Condensed Matter 563 (2019) 30–35

Fig. 3. Rietveld refinement patterns of α-Fe2O3 films deposited with C = 0.14 mol l−1 (dots for experimental and solid line for simulated curves).

The optical analysis by means of transmittance T (λ) and reflectance C=0.06 mol.l-1
R (λ) measurements allows us to determinate the absorption coefficient C=0.1 mol.l-1
at varying precursor concentration, respectively. Using the following C=0.14 mol.l-1
30
formula [6]: C=0.2 mol.l-1
C=0.3 mol.l-1
1 1
α= Ln ( )
(8)
(x10 cm )
e T
-1
20
Fig. 5 gives the absorption plots against wavelengths in the range
4

350–800 nm. As previously shown, these layers have height absorbance

in the UV and most of the visible region (λ ≤ 700 nm) than decrease
gradually in the rest of spectra. From the analysis of this figure, we can
10
notice that the absorption coefficient has high values
(6 × 104 ≤ α ≤ 35 × 104 cm−1) for all films. In addition, its values
have increased as the precursor concentration was increased. These
high values of α suggest that Fe2O3 thin film is a suitable candidate for a
large variety of optoelectronic applications. 0
400 500 600 700 800
It is well known that the relation between the absorption coefficient
(nm)
(α) and the incident photon energy (hυ) given by Tauc formula which
allows us to estimate the band gaps energies values (Eg) [24]: Fig. 5. The absorption coefficient (α) spectra of α-Fe2O3 deposited with dif-
ferent precursor concentrations.
(αhυ)1/n = A(hυ-Eg) (9)

Where A is a constant, α is the absorption coefficient, hυ is the reflectance spectra (dR/dλ) of all the layers (Fig. 7) [33]. It is clear that
absorbed photon energy, Eg is the optical band gap energy relating to the absorption edge shifted toward the longer wavelength side. This
the direct transition (n = 1/2) or indirect photon assisted transitions result has proved the decrease of the band gap. In fact, it was found that
(n = 2) (Fig. 6). Optical band gap was ranged from 2.08 to 2.21 eV for there is a good agreement for Edir
g values and a slight difference for Eg .
ind

direct transition and from 1.99 to 2.03 eV for indirect transition, which
are typical values for Fe2O3 [6]. The band gaps energies were found to
decrease as the precursor concentration increase (Table .3). J. Raj
Mohamed et al. [27] have found the same effect of precursor con-
centration on band gap energy of In2S3 thin films. In addition, It has
been confirmed the band gaps energies values using the differential
It should also be mentioned that there is a matching between the
shifting of the absorption edge of optical transmittance spectra
(Fig. 4(a)) and the values of the optical band gaps energies (Table 3).
This confirms the rightness of the calculated values of Eg as well as the
quality and reliability of the realized optical measurements.
For further investigation, the refractive index n(λ) and the

-1
C= 0.06 mol.l
80
(a) -1
(b) C= 0.1 mol.l
-1
C= 0.14 mol.l
60 -1
C= 0.2 mol.l
-1
C= 0.3 mol.l
Transmission T (%)

60
Reflexion R (%)

40
40

-1
C= 0.06 mol.l
-1
C= 0.1 mol.l
20 -1 20
C= 0.14 mol.l
-1
C= 0.2 mol.l
-1
C= 0.3 mol.l
0
500 1000 1500 2000 500 1000 1500 2000 2500
nm) (nm)

Fig. 4. The optical transmission (a) and reflection (b) spectra of α-Fe2O3 deposited with different precursor concentrations.

33
R. Ben Ayed, et al. Physica B: Condensed Matter 563 (2019) 30–35

5 5
C= 0,14 M C = 0,14 M

4
4
eV. cm )
-1

3
2
( h

Eg= 2,16 eV 2
1
Eg = 2,02 eV

0 1
1,5 2,0 2,5 1,8 2,0 2,2
h (eV)
h eV)

Fig. 6. (αhυ)1/n versus hυ plots for α-Fe2O3 thin layers deposited with C = 0.14 mol l−1 (a) n = 2 and (b) n = 1/2.

Table 3 C=0.06 mol.l-1

Energies band gaps values of α-Fe2O3 sprayed thin films. C=0.1 mol.l-1
1,2 C=0.14 mol.l-1
Function Tauc dR/dλ
C=0.2 mol.l-1
Egdir (eV) Egind (eV) Egdir (eV) Egind (eV) C=0.3 mol.l-1

C (mol.l−1) 0.06 2.21 2.03 2.15 1.80

0.1 2.17 2.02 2.14 1.80 0,8
0.14 2.16 2.02 2.12 1.79
k( )
0.2 2.15 2.00 2.11 1.78
0.3 2.08 1.99 2.02 1.77

0,4
-1
C=0.06 mol.l
-1
C=0.1mol.l
-1
C=0.14mol.l
dir
Eg C=0.2mol.l
-1 0,0
-1 400 500 600 700 800
C=0.3mol.l nm)
indir
Eg Fig. 8. The variation of extinction coefficient (k) versus wavelength for thin
dR/d

films deposited with different precursor concentrations.

3,2

2,8

500 600 700 800 2,4

(nm)
n( )

Fig. 7. The differential of reflexion spectra of α-Fe2O3 deposited with different

precursor concentrations. 2,0
C=0.06 mol.l-1
extinction coefficient k(λ) of Fe2O3 films for the different precursor C=0.1 mol.l-1
1,6 C=0.14 mol.l-1
concentrations have been calculated using the following formula [6]:
C=0.2 mol.l-1
λ (1 − R)2 C=0.3 mol.l-1
k= Ln 1,2
4πe T (10)
400 500 600 700 800
1−R nm)
1 + [1 − ( 1 + R )2 (1 + k 2 )]1/2
n= 1−R Fig. 9. The variation of refractive index (n) versus wavelength for thin films
(1 + R ) (11) deposited with different precursor concentrations.

Fig. 8. Shows that the refractive index variation of Fe2O3 thin films
against wavelength (λ) for C = 0.06, 0.1, 0.14, 02 and 0.3 mol l−1. The indicating the transparency of the films. As well as some other semi-
curves show a proportional increase of n with λ (nm). Otherwise, the conducting thin films have shown the same behavior [34].
refractive index was found in the range [1.6–4.6]. The Extinction
coefficient (Fig. 9) values are in the range [0.12–0.65]. k(λ) has 3.4. Photoluminescence
reached the maximum in the strong absorption region (λ≤ 700 nm)
then decreases to reach zero as increasing the incident wavelength It is well known that PL is one of the important studies that can

34
R. Ben Ayed, et al. Physica B: Condensed Matter 563 (2019) 30–35

C=0.06mol.l-1 Fe2O3 thin films with different molar concentration (0.06, 0.1, 0.14, 0.2
50 C=0.1mol.l-1 and 0.3 mol l−1). The influence of precursor molarity was discussed
C=0.14mol.l-1 upon the structural, optical and electrical properties. All the grown
C=0.2mol.l-1 films have exhibited good crystalline structure in rhomboedric crystal
40 C=0.3mol.l-1 form (α- Fe2O3) with (104) as preferential orientation up to the con-
centration of 0.14 mol l−1 and than change to (110). The layers have
Intensity (a.u.)

30
showed an average optical transmittance of [70–85]% in the visible
region at a lower concentration. The index refraction and extinction
coefficient has been estimated from the transmission and reflexion data,
20 recorded spectra over the wavelength [400–800] nm were found to be
dependant on the precursor concentration. Analysis of the optical ab-
sorption revealed a direct and indirect optical transition associated to
10 α- Fe2O3. It is also worth noting that, the band gaps values were nar-
rowed from 2.21 to 2.08 eV for the direct transition and from 2.03 to
1.99 eV for the indirect transition with the increment in precursor
0 concentration. In addition, a minimum of electrical resistivity in the
400 500 600 700
order of 0.39 105 Ω cm was obtained for C = 0.14 mol. l−1. Besides, an
(nm) increase of resistivity, accompanied by a decrease of transmission and
Fig. 10. PL spectra of thin films deposited with different precursor concentra- degradation of crystallinity was observed at higher concentration.
tions. Results indicate that the precursor concentration could control the
physical properties of Fe2O3 thin films elaborated by chemical spray
pyrolysis. However, further investigations are of interest in order to
Table 4
understand the influence of the other growth parameters on the en-
The variation of ρ, μ and N of α-Fe2O3 films deposited with different precursor
concentrations.
hancement of the electrical properties of Fe2O3 thin films before their
applications in optoelectronics devices.
C (mol.l−1) ρ (x105 Ω cm) μ (cm−2.V−1.s−1) N (x1012cm−3)

0.06 3.87 4.7 3.40 References

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In this work, chemical spray pyrolysis technique was used to deposit

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