Material Sciences Revista Mexicana de Fı́sica 69 051004 1–8 SEPTEMBER-OCTOBER 2023

Elaboration and characterization of pure ZnO,

Ag:ZnO and Ag-Fe:ZnO thin films: Effect of Ag
and Ag-Fe doping on ZnO physical properties
F. Lekoui
Division Milieux Ionisés & Laser, Centre de Développement des Technologies Avancées,
Cité 20 Août 1956, Baba Hassen, Alger, Algeria.
LPCMME, Département de physique, Université d’Oran 1, Oran, Algeria.
e-mail: flekoui@[Link]
S. Hassani
Division Milieux Ionisés & Laser, Centre de Développement des Technologies Avancées,
Cité 20 Août 1956, Baba Hassen, Alger, Algeria.
E. Garoudja
Plateforme Technologique de Micro-fabrication, Centre de Développement des Technologies Avancées,
Cité 20 Août 1956, Baba Hassen, Alger, Algeria.
R. Amrani
Département des sciences de la matière, Université Alger1 BenyoucefBenkhedda, Alger, Algeria,
LPCMME, Département de physique, Université d’Oran 1, Oran, Algeria.
W. Filali
Plateforme Technologique de Micro-fabrication, Centre de Développement des Technologies Avancées, Cité 20 Août 1956,
Baba Hassen, Alger, Algeria.
O. Sifi
Division Milieux Ionisés & Laser, Centre de Développement des Technologies Avancées,
Cité 20 Août 1956, Baba Hassen, Alger, Algeria.
S. Oussalah
Division Microélectronique & Nanotechnologies, Centre de Développement des Technologies Avancées,
Cité 20 Août 1956, Baba Hassen, Alger, Algeria.
Received 20 December 2022; accepted 13 February 2023

Pure ZnO, Ag doped ZnO and Ag-Fe co-doped ZnO were prepared using thermal evaporation. XRD analysis confirms that all layers present
a hexagonal wurtzite structure; however, there is a small shift in the peaks position due to the distortion of the film’s lattice. Scanning
Electron Microscopy (SEM) analysis reveals the morphological variation of the film’s surfaces due to the doping. Pure ZnO and Ag:ZnO
films have a nanostructured surface, however, Ag-Fe:ZnO films showed a smooth surface without any nanoparticles. Raman analysis showed
the presence of A1 (LO), E2 (high) and local vibrational modes (LVMs) for all layers. Ultraviolet-visible spectroscopy (UV-VIS) analysis
shows that the films have a good transparency and the bandgap decreases with ZnO doping from 3.80 eV to 3.78 eV and 3.70 eV, for pure
ZnO, Ag:ZnO and Ag-Fe:ZnO films, respectively. The electrical properties confirm the semiconductor nature of ZnO films with a resistivity
around 1.4 Ω.cm, and with Ag and Ag-Fe doping, the films behave like conductors with 1.4 × 10−4 Ω.cm and 1.4 × 10−3 Ω.cm, respectively.
These results make the Ag:ZnO and Ag-Fe:ZnO thin films good materials for photovoltaic application.

Keywords: Optoelectronic properties; rapid thermal evaporation; TCO, ZnO films.

DOI: [Link]

1. Introduction advantage makes them ideal candidates for applications in

optoelectronics [1, 2] and photovoltaic’s field [3]. Most op-
tically transparent and electrically conductive oxides (TCO)
Transparent conductive oxides (TCO) are interesting and re- are binary [4] or ternary [5] compounds, containing one or
markable materials in different fields of application. Partic- two metallic elements. Their resistivity could be as low as
ularly, TCO’s possess two important properties that are elec- 10−3 Ω.cm and their extinction coefficient (k) in the visible
trical conductivity and transparency in the visible, hence this
2 F. LEKOUI et al.,

range (VIS) could be less than 0.0001, due to their wide band in acetone and ethanol for five minutes prior to each deposi-
gap (Eg = 3 eV). This remarkable combination of conduc- tion experiment. After that, they were inserted into a vacuum
tivity and transparency is usually impossible in intrinsic ox- chamber to be heated to the proper temperature. High cur-
ides; however, it is obtained by manufacturing them with the rent power is used to heat the crucible to ∼ 1600◦ C, when
introduction of appropriate dopants [6] or by making mul- ZnO is sublimated. The particles of the evaporated materials
tilayers [7, 8] with metallic intermediate layer. The most complete their journey by being deposited on the substrate
known and used oxides are zinc oxide (ZnO) [9,10], tin oxide surface. Ag:ZnO and Ag-Fe:ZnO films were elaborated us-
(SnO2 ) [11] and indium tin oxide (In2 O3 ) [12]. ing a mixture of powder with mass concentration (90,10)%
ZnO doped with metallic elements (ZnO:M) is a promis- and (90,10,10)%, respectively.
ing TCO material Current research works focus on the re- The structural and morphological properties of films were
placement of ITO thin films, which are currently the most identified by XRD technique. We used Philips X’Pert ma-
widely used TCO in many applications, because of concerns terials powder diffractometer (MPD) with a Cu-kα cathode
related to sustainability (indium is a rare material) and cost source and 1.54 Å of wavelength, EA 125 Omicron, Lab
[13]. ZnO has attracted attention as TCO material, given that Ram H-Resolution from Horiba JobinYvon and Helios Nano
it is abundant and nontoxic [14], has a wide band gap (3.3 eV) Lab TM 650 andscanning electron microscopy (SEM, JEOL
and a low resistivity (Ω.cm). Optoelectric properties of ZnO JSM-6360LV) with an acceleration voltage between 5 and
depend on deposition technique, annealing and the element 15 kV, respectively.
nature used. Depending on where the Silver (Ag) is posi- The optical transmittance of the deposited thin films was
tioned within ZnO crystal lattice, Ag-doped ZnO (ZnO:Ag) investigated by OPTI ZEN 3220UV spectrophotometer in
can exhibit either n- or p- type conduction [15]. The type of UV-Visible-NIR range. The optical parameters were ex-
ZnO conduction depends on the rivalry between Ag+ Zn and tracted by using artificial bee colony (ABC) algorithm based
Agi since these defects coexist peacefully in the ZnO lat- method, which is detailed in our previous work [18]. To de-
tice. In addition, iron (Fe) is known to bethe most chemically termine the generated thin films’ thickness and optical con-
stable of these transition metal dopants, and it exists in two stants, only transmittance spectra are used. The utilised the-
different oxidation states that have ionic radii that are sim- oretical model of transmittance spectra [19]:
ilar to Zn2+ (0.74 Å), (0.78 Å and 0.64 Å). Fe could thus Ax
be suitable since the crystal structure of ZnO is not altered, T = , (1)
B − Cx cos ϕ + Dx2
making it possible for it to penetrate the Zn lattice either sub-
stitutively or interstitially and contribute more charge carriers where
¡ ¢
to increase conductivity [16]. In this direction, experiments A = 16ns n2 + k 2 , (2)
have been conducted to dope Ag into ZnO before co-doping h i£ ¡ ¢ ¤
2
Fe to reduce the native defect states. This strategy enabled B = (n + 1) + k 2 (n + 1) n + n2s + k 2 , (3)
researchers to get beyond current challenges such alloy and £ 2 ¤
cluster formation. B. Sankara Reddy et al. [17] demonstrated C = (n − 1 + k 2 )(n2 − n2s + k 2 ) − 2k 2 (n2s + 1)
the enhancement of optoelectronic properties of ZnO using ·
Ag-Fe co-doping. × 2 cos ϕ − 2k sin ϕ ? 2(n2 − n2s + k 2 )
In this work, pure ZnO, Ag doped ZnO and Ag-Fe co- ¸
doped ZnO thin films were elaborated. The objective is to
+ (n2s + 1)(n2 − 1 + k 2 ) , (4)
make a comparative study between the three layers in terms
of variation of their structural, morphological and mainly op- h i£ ¡ ¢ ¤
2
toelectronic properties depending on the doping nature. The D = (n − 1) + k 2 (n − 1) n − n2s + k 2 , (5)
elaboration technique was chosen to their simplicity and low
4πnd
cost. This kind of study has not been sufficiently investi- ϕ= , (6)
gated in the research literature. In this innovative approach, λ
noteworthy effects were found through a comparison of ZnO, x = exp (−αd) . (7)
Ag:ZnO, and Ag-Fe:ZnO thin films.
In Eqs. (1)-(7), ns and n are the refractive indexes of the
substrate and thin film, respectively; d is the thickness of the
2. Experimental procedures film that has been deposited; α is the absorption coefficients;
λ is the wavelength and k is the extinction coefficient. The
On a glass substrate, zinc oxide, silver and iron powder from Cauchy dispersion model was used to determine the refrac-
Sigma Aldrich with 99.99% of purity, were evaporated to ob- tive index values and is denoted by the following [19]:
tain Pure ZnO, Ag:ZnO and Ag-Fe:ZnO thin films. A pump-
β1
ing device, a vacuum chamber with a substrate holder and an n (λ) = α1 + , (8)
electrical component that supplies a high current to a crucible λ2
containing material for evaporation make up the experimen- β2
k (λ) = α2 + 2 , (9)
tal setup. All substrate samples were ultrasonically cleaned λ

Rev. Mex. Fis. 69 051004

 ELABORATION AND CHARACTERIZATION OF PURE ZNO, AG:ZNO AND AG-FE:ZNO THIN FILMS:. . . 3

where α1 , β1 , α2 and β2 are four fitting parameters.

Finally, the electrical resistance was quantified by Keith-
ley’s 2400C four point probe.

3. Results and discussion

3.1. XRD analysis

During the evaporation process the ZnO powder changes

state from solid to vapor, it is subdivided giving Zn atoms
and oxygen O [9, 20]. The Zn condenses on the substrate,
while a large amount of oxygen pumped by the pumping
group and the amount adsorbed by the layer formed will not
be able to give an oxide phases. This is the reason why the
samples deposited must go through the annealing step. After
annealing the samples will be oxidized and the ZnO phase F IGURE 1. XRD patterns of pure ZnO, Ag:ZnO and Ag-Fe:ZnO
appears. In Fig. 1 pure ZnO presents peaks at 2θ = 31.89◦ , thin films.
34.53◦ and 36.47◦ corresponding to (100), (002) and (101)
planes respectively, which can be attributed to the hexagonal
wurtzite structure of ZnO (ICDD 00-036- 1451 2). In addi- λ
a= √ , (12)
tion to these peaks, there are other planes at diffraction angles sin θhkl 3
2θ = 47.71◦ , 56.80◦ , 63.10◦ and 68.19◦ correspond to ZnO
0.9λ
(102), (110), (103) and (112), respectively. With silver dop- D= . (13)
ing, it can be observed the appearance of the peaks which FWHM · cos α
correspond to the Ag phases: (210), (111), (200), (220) and
FWHM, θ and λ are respectively the full width at half
AgO phase (220) at 2θ = 27.69◦ , 38.7◦ , 41.54◦ , 65.45◦ and
maximum, the Bragg diffraction angle, the wavelength of the
54.26◦ , respectively. It can be noticed too, that the peaks cor-
used X-rays source and D is the crystallites size. To deter-
respond to the ZnO wurtzite (100), (002) and (101) shifted to
mine these parameters, (002) and (101) ZnO’s peaks were
the lower angles with a difference of approximately ∼ 13◦ .
selected. The strain toward the c-axis εc and a-axis εa were
XRD analysis of Ag-Fe co-doped ZnO films shows the ap-
estimated by [23]:
pearance of the majority of ZnO and Ag peaks and there are
no peaks that correspond to the Fe phases. The disappear- c − c0
ance of Ag(210), ZnO(102), Ag(220) and ZnO(103) peaks is εc = × 100, (14)
c0
probably due to the distortion of Ag:ZnO mesh by the Fe ad-
dition. It can also be noticed that ZnO peaks shifted to higher a − a0
εa = × 100, (15)
angles with a difference of approximately ∼ 2◦ . a0
It is preferable to detect the variation of these structural
features while computing the lattice parameters “c” and “a” where a0 = 0.3249 nm and c0 = 0.5205 nm.
based on the Bragg relationship in first order, to comprehend According to the results in Table I, the strain towards
the change of physical properties our layers. In ZnO’s hexag- c axis is tensile (positive) and towards a axis is compres-
onal wurtzite structure [21, 22]: sive (negative). It is noticed that the strain along both axis
µ ¶ increases with silver doping and decreases with Ag-Fe co-
1 4 h2 + k 2 + hk l2
2 = + , (10) doping. Especially, a very small variation of the strains is
dhkl 3 a2 c2
observed along a axis. These results are in good agreement
λ with the other reports, where the films were grown on quartz
c= , (11)
sin θhkl substrate using sputtering technique [24].

TABLE I. Lattice constants ‘a’ and ‘c’, FWHM, crystallites size D, micro strains ²a and ²c of different films.
Parameters c a FWHM D ²c ²a
Films (nm) (nm) (radian) (nm)
ZnO 0.5251 0.2878 0.12217 26.54 0.0088 -0.1141
Ag:ZnO 0.5267 0.2877 0.01745 8.53 0.012 -0.1145
Ag-Fe:ZnO 0.5252 0.2878 0.10472 30.96 0.009 -0.1142

Rev. Mex. Fis. 69 051004

4 F. LEKOUI et al.,

F IGURE 2. Variation of () FWHM and crystallite size, b) a and c lattice parameters, with doping nature variation of ZnO thin films.

TABLE II. The rest of the identified Raman peaks of ZnO layers.
Pure ZnO layers Ag:ZnO layers Ag-Fe:ZnO layers Identification References
A1 ( TO ) A1 ( TO ) - A1 ( TO ) modes [30]
E1 (LO) - E1 (LO) E1 (LO) modes [28]
625 - - Disorder caused by Zn+ and oxygen vacancies [29, 30]
A1 (LO)+E2 (Low) A1 (LO)+E2 (Low) - Multi phonon modes of ZnO [28]
- 730 720 Molecule with Ag+ and Fe+ [30]
781 804 795 Multi phonon modes of ZnO [28]

Figure 2a), b) shows the variation of crystallites size for shifts in frequency depending on whether the film is doped
pure ZnO, Ag:ZnO and Ag-Fe:ZnO thin films. It has been with Ag and co-doped with Ag-Fe elements [28].
found that crystallite size decrease with silver doping; this The E2 (high) bond is present in all samples, indicating
last caused the augmentation of the compressive strains to- that the ZnO structure has been maintained even after the ad-
wards c-axis and the tensile strains towards a-axis. This dition of Zn, Ag, and Fe. This supports the findings of the
change can be related to high mobility of silver atoms which XRD investigation. E2 (high) phonons’ frequency location is
form other phases with annealing temperature and block the altered from pure ZnO to a lower frequency ∼ (431 cm−1 ).
growth of ZnO crystallites [25, 26]. In the other hand the This indicates that tensile strain, which is exactly perpendic-
addition of Fe atoms leads to the increase of surface energy, ular to the a axis, occurs in the lattice. Local vibration modes
which reduces the stresses and allows the crystallites to grow (LVM) in the Raman spectra may increase as pollutants are
again [27]. added to the mesh. The disruption of the crystal’s transla-
tional symmetry by impurity-induced defects is one proposed
physical basis for understanding LVM. With wave vectors far
3.2. Raman analysis from the Brillouin zone, phonon scattering occurs as a result
of the wave vector no longer being preserved [29]. Due to
In order to investigate crystallization and structural disorder, the substantial Ag and Fe atoms in the ZnO crystal, LVM
the Raman spectrum is a vital and adaptable diagnostic tool. modes are present in all samples. The rest of phonon modes
Raman spectra are used to look at the ZnO vibrational char- are summarized in Table II.
acteristics. The hexagonal wurtzite-structured ZnO nanopar-
ticles fit within the P63mc space group. Only the optical 3.3. SEM and EDS analysis
phonons near the Brillouin zone’s point participate in first-
order Raman scattering for the ideal ZnO crystal. Figures 3a), Figures 4a), c), e) depicts the SEM anaylsis of the morpho-
b) and c) show the Raman spectra of pure ZnO, Ag:ZnO and logical progression with the variation of doping nature. In
Ag-Fe:ZnO thin films, respectively. The A1 (LO) mode was addition Figs. 4d) and e) shows the ZnO nanowires diame-
noticed in every sample. The A1 phonon, which is polarized ter distribution of pure ZnO and Ag doped ZnO thin films.
perpendicular to the c-axis of the wurtzite structure of ZnO, Figure 4a) shows that the pure ZnO films had nanoparticles

Rev. Mex. Fis. 69 051004

 ELABORATION AND CHARACTERIZATION OF PURE ZNO, AG:ZNO AND AG-FE:ZNO THIN FILMS:. . . 5

F IGURE 3. Raman spectra of a) pure ZnO, b) Ag:ZnO and c) Ag-Fe:ZnO thin films.

F IGURE 4. SEM images of a) ZnO, c) Ag:ZnO and e) Ag-Fe:ZnO thin films. ZnO Nanowires diameter distribution of b) pure ZnO and d)
Ag:ZnO thin films. EDS spectra of f) Ag-Fe:ZnO, g) Ag:ZnO and h) pure ZnO thin films.

Rev. Mex. Fis. 69 051004

6 F. LEKOUI et al.,

with batonnets-like shapes covering the whole surface; the

average of batonnets diameter is ∼ 150.68 nm. According to
Fig.4c), Ag doped ZnO films have a silver shape resembling
a microsphere that is embellished with ZnO nanowires. The
average diameter of these nanowires are reduced compared to
the pure ZnO films, it is ∼ 75.18 nm. The apparition of the
silver micro-spherical structure probably inhibited the growth
of ZnO nanowires. In the other hand, for the Ag-Fe co-doped
ZnO films [Fig. 4e)], it can be noticed the disappearance of
the nanowires. Iron caused a significant alteration in the sur-
face morphology, making it smoother.
The EDS results for the ZnO, Ag:ZnO, and Ag-Fe:ZnO
films are displayed in Figs. 4f), g), and h), respectively. The
results contain varying levels of zinc, silver, iron, and oxy-
gen. All of the samples’ observed silicon peaks are thought to
F IGURE 6. The refractive index n dispersion for the whole wave-
have originated from glass substrates. What was previously
length range for pure ZnO films.
indicated about the XRD data is validated by the iron found
in the Ag-Fe:ZnO EDS analysis, showing that iron is incor-
porated in these films at interstitial or replacement locations.
The decrease in oxygen concentration between Ag:ZnO and
Ag-Fe:ZnO samples further indicates that the insertion of Fe
atoms increases the number of oxygen vacancies.

3.4. Optical properties

Figure 5 displays the optical transmission spectra of thin

films made of pure ZnO, Ag:ZnO, and Ag-Fe:ZnO. It is clear
that pure ZnO films have the maximum transmittance, at 88
% at wavelengths below λ = 600 nm. In addition, with val-
ues of about 80% and 73.8%, respectively, the transmittance
of Ag:ZnO and Ag-Fe:ZnO films is lower than that of ZnO
layer. For films with Ag and Ag-Fe doping, the rise in oxy-
gen vacancies and the distortion of the ZnO mesh are what F IGURE 7. Example of extrapolation of linear part of (αhν)2 ver-
cause this difference in transmittance. The optical transmis- sus hν plot to αhν = 0 to determine Eg of the samples.
sion is altered by a distortion at the level of the ZnO lattice,
notably along the c axis, as seen in the XRD and Raman anal- Using our method, that is based on the ABC algorithm
ysis sections. In the other hand the presence of silver in the [18]. The optical band gap, the refractive index n, and the
ZnO lattice favorite the absorption of light which reduces the thicknesses of the films were computed. The films’ predicted
values of the transmittance in particular in the visible range. thickness d was around 140 nm. Ag:ZnO and Ag-Fe:ZnO
films had a refractive index of 1.86 and 1.92, respectively. It
is higher than that of pure ZnO films, which have a refractive
index of 1.6. This fall in refractive index n is probably due to
oxygen deprivation, caused by doping and co-doping.
The calculated band gap for pure ZnO is 3.92 eV. When
ZnO is co-doped with Ag and Ag-Fe, the calculated band gap
decreases to 3.82 eV and 3.78 eV. Additional defects includ-
ing shallow donor buildup (Oxygen vacancies) and shallow
acceptor buildup (Zn interstitials and Zn vacancies) at the va-
lence band and near to the conduction band are to blame for
this decrease [31]. These results are in good agreement with
that found in XRD, Raman and EDS analysis. In the other
hand, residual strain in the films has also an impact on semi-
conductor band gap. The band gap will change due to the
tensile and compressive strains in opposite ways. After an-
F IGURE 5. Transmission spectra of pure ZnO, Ag:ZnO and Ag- nealing, the band gap Eg of the films can be described in
Fe:ZnO thin films. terms of the stain εc [32]:

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 ELABORATION AND CHARACTERIZATION OF PURE ZNO, AG:ZNO AND AG-FE:ZNO THIN FILMS:. . . 7

XRD and EDS investigations, this will cause the ZnO mesh
TABLE III. Sheet resistance and the calculated resistivity of the to become damaged and the amount of oxygen vacancies de-
films. crease [33].
Thin films ZnO Ag:ZnO Ag-Fe:ZnO
7 4
Sheet resistance [Ω/¤ ] 10 10 103 4. Conclusion
−3
Resistivity [Ω.cm] 1.4 1.4*10 1.4*10−4
In conclusion, pure ZnO, Ag:ZnO and Ag-Fe:ZnO thin films
Transmittance at λ = 600 nm 88% 80% 73.8%
were elaborated on glass substrates using rapid thermal evap-
oration. All of the produced films have a wurtzite mesh and
a polycrystalline structure. Ag:ZnO and Ag-Fe:ZnO doping
Eg = 3.28 − 0.045εc . (16) induce a distortion in the structure and a change in the oxy-
For tensile strain, the film’s band gap will increase; for gen vacancies, according to XRD and Raman analysis. SEM
compressive strain, it will decrease. In our situation, εc has images showed that ZnO and Ag:ZnO films have nanostruc-
positive values, indicating compressive strain, which causes tured surfaces, however with Fe addition the surface tends to
Eg decrease. besmooth and the nanoparticles disappeared. With average
transmittances ranging from 73.8% for Ag-Fe:ZnO films to
3.5. Electrical properties 88% for pure ZnO films at λ = 600 nm, the prepared films
showed high refractive indexes of 1.6, 1.86 and 1.92 for pure
The measured values of the films’resistivity are shown in Ta- ZnO, Ag:ZnO and Ag-Fe:ZnO films, [Link] opti-
ble III for comparison. They are around 1.4 Ω.cm for pure cal band gap Eg of the films were in the range of 3.80 eV for
ZnO, 1.4 × 10−3 Ω.cm and 1.4 × 10−4 Ω.cm for Ag:ZnO pure ZnO, 3.78 eV and 3.70 eV for Ag:ZnO and Ag-Fe:ZnO
and Ag-Fe:ZnO thin films, respectively. These results indi- films, respectively. Finally, Ag:ZnO and Ag-Fe:ZnO films
cate that ZnO films are semiconductors by nature and be- were found to have an excellent conductivity confirmed by
come conductors when doped with Ag and Ag-Fe. The dif- the four point probe [Link] latter property, in combina-
ference in electrical resistance when doping ZnO films can be tion with their high transparencysuggest that these TCO films
connected to the change in oxygen vacancies. According to are potential candidates for solar applications.

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