Spectroscopy Letters

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Nickel doped copper oxide thin films prepared by

radiofrequency reactive sputtering: study of the
impact of nickel content on the structural, optical
and electrical properties

H. El Aakib, J. F. Pierson, M. Chaik, H. Ait Dads, C. Samba Vall, A. Narjis & A.

Outzourhit

To cite this article: H. El Aakib, J. F. Pierson, M. Chaik, H. Ait Dads, C. Samba Vall, A. Narjis &
A. Outzourhit (2019): Nickel doped copper oxide thin films prepared by radiofrequency reactive
sputtering: study of the impact of nickel content on the structural, optical and electrical properties,
Spectroscopy Letters, DOI: 10.1080/00387010.2018.1560335

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SPECTROSCOPY LETTERS
https://doi.org/10.1080/00387010.2018.1560335

Nickel doped copper oxide thin films prepared by radiofrequency reactive

sputtering: study of the impact of nickel content on the structural, optical and
electrical properties
H. El Aakiba, J. F. Piersonb, M. Chaika, H. Ait Dadsa, C. Samba Valla, A. Narjisa, and A. Outzourhita
a
Nanomaterials Laboratory for Energy and the Environment Faculty of Sciences Semlalia, Cadi Ayyad University, Marrakech, Morocco;
b
Campus ARTEM all
e Andr
ee Guinier, Institut Jean Lamour (UMR CNRS 7198), Universit
e de Lorraine, Nancy, France

ABSTRACT ARTICLE HISTORY

Nickel doped copper oxide thin films were grown on glass and silicon substrates using radiofre- Received 9 July 2018
quency sputtering in an argon–oxygen atmosphere. The impact of doping on the structural, Accepted 14 December 2018
optical, and electrical properties of copper oxide was examined for various contents of nickel. The
KEYWORDS
X-ray diffraction results revealed the polycrystalline monoclinic structure of copper oxide for the
Band-gap energy; nickel-
prepared films. Raman spectroscopy confirmed that only the copper oxide phase is evidenced in doped copper oxide; optical
nickel-doped copper oxide films. The band gap energy increased with increasing nickel content. properties; radiofrequency
All the sputtered films showed p-type conduction and the resistivity depends on the sputtering; resistivity;
nickel content. surface and compositional
properties; thin films

Introduction Indeed, the latter was shown to be a better physical

deposition technique for high purity films with a narrow
Recently, transition metal oxide films have attracted great
distribution of grain size when performed in the reactive
attention from the scientific researchers because of their
sputtering mode. In addition, this technique allows easy
suitable physical and chemical properties, environmental
friendless as well as suitability for various devices.[1–3] control of the elaboration of films with homogeneous surfa-
Among these various metal oxides, CuO has been inten- ces and properties close to those of bulk materials.
sively investigated due to its interesting properties, such as Moreover, RF sputtering has further advantages such as tun-
nontoxicity, abundance, its comparatively simple synthesis ing of internal stress which is easily controllable from com-
in thin films forms,[4] p-type conduction and direct band- pressive to tensile.[18] For all these reasons, the RF
gap energy which is between 1.2 and 1.9 eV.[5,6] These prop- sputtering method is used in various research fields rather
erties make CuO a promising candidate for various applica- than other conventional methods.[19]
tions such as anode interlayers for organic solar cells,[7] Up to now, Ni-doped CuO films grown by RF sputtering
photocatalysis,[8] selective absorbers,[9] and sensors.[10] technique have not yet been studied. Thus, in this paper,
To improve the performance of CuO thin films, the grain pure and Ni-doped CuO thin films were prepared using RF
size must be controlled as the physical and chemical proper- sputtering technique at room temperature and under highly
ties of the metal oxide films depend on the form and size of controlled conditions. The effect of nickel concentration on
the particles. Doping by different transition metals can also the structural and optical properties of CuO thin films was
be used to improve the properties of this semiconducting studied to understand the influence of Ni content on the
material. Among the various transition metals, nickel can be properties of the elaborated CuO films, which is essential
considered as a dopant to improve the structural, electrical, for the use of such Ni-doped CuO in the applications men-
magnetic and mechanical properties of CuO. tioned above.
Despite numerous studies of the doping of metal oxide
films, the ability to produce highly crystallized doped CuO
thin films with the desired physical and chemical properties Experimental details
is still challenging. For this reason, CuO thin films were Thin film elaboration
synthesized by different physical and chemical methods such
as sol–gel,[11] spin coating,[12] thermal evaporation,[13] elec- Undoped and nickel doped copper oxide thin films were
trodeposition,[14] spray pyrolysis,[15] chemical vapor depos- deposited on pre-cleaned glass and silicon substrates by RF
ition,[16] and radiofrequency (RF) sputtering technique.[17] reactive sputtering technique using a 99.99% purity metallic

CONTACT H. El Aakib [email protected] Nanomaterials Laboratory for Energy and the Environment Faculty of Sciences Semlalia, Cadi Ayyad
University, PO Box: 2390, Marrakech 40000, Morocco.
ß 2019 Taylor & Francis
2 H. EL AAKIB ET AL.

copper target with a diameter of 10 cm and a thickness of Table 1. Elemental composition of nickel-doped copper oxide thin films.
5 mm. The distance between the target and the substrates Surface coverage Nickel Copper Ratio
of nickel (%) (at. %) (at. %) nickel/copper
was fixed at 7 cm. Before the deposition, the base pressure
0 0 100 0
was in the range 2.10
4 Pa. For the deposition, the RF power 3 2.1 97.9 0.021
was fixed at 150 W, while the reactive atmosphere consisted 5 3.7 96.3 0.037
of 30% oxygen and 70% of argon with a total pressure of 7 4.5 95.5 0.047
1 Pa. The deposition duration was fixed at 2 h. The depos- The nickel atomic percentage (at. %) increases with increasing sur-
face coverage.
ition parameters were kept identical for undoped and Ni-
doped CuO thin films. In the case of Ni-doped CuO films,
the copper target was partially covered pure Ni with various
Table 2. Optical and electrical properties of undoped and nickel-doped cop-
surface coverages (0, 3, 5, and 7%). per oxide thin films.
Nickel doping Optical band Resistivity Thickness
(at. %) gap (eV) (X.cm) (nm)
0 1.62 21.70 416
Characterization techniques 2.1 1.68 23.02 402
3.7 1.72 48.86 299
The optical properties were investigated by using an UV- 4.5 1.76 69.80 296
Vis-NIR spectrometer (Varian Cary 5000). The thicknesses A increase in the optical band gap and in the resistivity was observed with
of the prepared films were measured using a tactile profil- increasing the atomic percentage (at. %) of nickel.
ometer. The structural properties were carried out using X-
ray diffraction (XRD) in Bragg Brentano configuration using
a Brucker D8 Advanced diffractometer with a CuKa1 radi- Optical properties
ation. The structural studies were complemented by Raman The optical transmittance spectra of the undoped and Ni-
spectroscopy using a Bruker–Senterra dispersive Raman doped CuO films were recorded in the wavelength range of
microscope which the wavelength of the laser is k ¼ 532 nm. 500–2500 nm and plotted in Fig. 1 as a function of the
The electrical resistivity of the films was deduced from sheet wavelength (k) for different Ni contents at room tempera-
resistance measurements using the 4-point probe method ture. The presence of well-contrasted interference fringes in
with a Keithley 6430 SUB-FEMTOAMP Remote Source these spectra suggest that the thin films are homogeneous
meter at room temperature. The elemental composition of and of high optical quality. The curves show that, for wave-
films was determined by using the Energy Dispersive X-Ray lengths greater than 800 nm, the highest value of the trans-
Spectroscopy (EDS-SSD Bruker). mittance for pure CuO is nearly 62.3%. The transmittance
values of the films increase significantly from 62.4% to
71.8% as the surface coverage of Ni increases from 0 to 7%,
i.e. for a Ni content ranging between 0 and 4.5 at. %. The
Results and discussion
domain k < 800 nm is characterized by a low transmission
Energy dispersive X-ray spectroscopy and consequently a strong absorption of light radiation by
the undoped and Ni-doped CuO layers. However, in this
Table 1 shows the Energy Dispersive X-Ray Spectroscopy
region, the average transmission increases with increasing
analysis of the elemental composition of nickel-doped cop-
percentage of Ni. This is clearly observed on the obtained
per oxide. These measurements have been performed by tak-
thin films as they become more transparent. The onset of
ing into account only the Ni and Cu elements. Indeed, the
significant absorption for all the samples remains below
EDS method is not accurate to determine the oxygen con-
k1000 nm ensuring excellent absorption across the UV-vis-
tent of oxide thin films. We notice that the nickel compos- ible range.
ition increases with increasing surface coverage. However, Fig. 2 shows the variation of the absorption coefficient a
the obtained values are smaller than the starting contents. of undoped and Ni-doped CuO films as a function of the Ni
This means that the sputtering of Ni atoms is lower than content. The absorption coefficient was obtained from the
that of Cu ones. Indeed, the sputtering yield of nickel is optical transmission in the absorption region using the
about 65% of that of copper. Lambert–Beer relation:


ln 1 =T
a ¼ (1)
d
Thickness measurements
where T is the optical transmission, and d is the thickness
The thickness values of all the prepared thin films were of the film. It was found that the absorption coefficient
determined using the tactile profilometer and presented in decreases with increasing Ni content in the visible range
Table 2. It was shown that the thickness decreases with (400–800 nm). The high value of the absorption coefficient a
increasing Ni content for all the sputtered thin films. This is (>104) reflects the effective absorption of the solar spectrum
due to the decrease in the growth rate of CuO as a result of in the visible range, then the value a starts to decrease with
the increasing surface coverage of the Cu target with Ni. increasing the Ni content.
 SPECTROSCOPY LETTERS 3

Figure 1. Optical transmittance spectra as a function of the wavelength of the undoped and nickel-doped copper oxide thin films deposited on glass by radiofre-
quency sputtering. The obtained thin films are homogeneous with a high optical quality. The sputtered thin films become more transparent with increasing nickel
content. at. %: atomic percentage.

Figure 2. Absorption coefficient spectra as a function of the wavelength of the undoped and nickel-doped copper oxide thin films deposited on glass by radiofre-
quency sputtering. A decrease in the absorption coefficient was observed with increasing nickel content in the visible range (400–800 nm). A: absorption coefficient;
k: wavelength; at. %: atomic percentage.

The extinction coefficient has been also calculated using where h is the Planck’s constant,  the frequency of the
the following equation[20] and plotted in Fig. 3: irradiation, Eg is the optical band gap energy, and C is a
ak constant. As a consequence, the band gap energy of all the
k ¼ (2) sputtered films can be obtained by the extrapolation of
4p
straight line to (aht)2 ¼ 0 as shown in Fig. 4. The obtained
For direct band gap materials, as in the case of CuO, the optical band gap of pure CuO film is 1.62 eV which is in
optical absorption coefficient and the incident photon good agreement with the literature.[21] Fig. 4 reveals that the
energy (ht) are related by the Tauc relation:[21] optical band gap of Ni-doped CuO films increases with
ðahtÞ ¼ Cðht
Eg Þ1=2 (3) increasing the Ni content. The Eg values are given in
4 H. EL AAKIB ET AL.

Figure 3. Extinction coefficient spectra as a function of the wavelength of the undoped and nickel-doped copper oxide thin films deposited on glass by radiofre-
quency sputtering. A decrease in the extinction coefficient was observed with increasing nickel content in the visible range (400–800 nm). at. %: atomic percentage.

Figure 4. Estimation of energy band gaps of the copper oxide doped by different nickel contents. Inset: band gap energy as function of nickel content. The optical
band gap of nickel-doped copper oxide films increases from 1.68 to 1.76 eV with increasing the nickel. A: absorption coefficient; h: the Planck constant; : the fre-
quency of the irradiation; at. %: atomic percentage.

Table 2 and were found to be 1.68, 1.72, and 1.76 eV in the CuO lattice. Therefore, Ni doping can be used to
respectively for 2.1, 3.7, and 4.5 at. % of Ni content. The tune the band gap of CuO films for specific applications.
observed increase in the optical band gap of CuO after Ni Fig. 5 shows the FTIR spectra, in the range of
doping may be attributed to the Ni substitution at Cu sites 400–800 nm, of an undoped CuO sample and another being
 SPECTROSCOPY LETTERS 5

Figure 5. Fourier transform infrared spectra of undoped and 3.7 atomic % nickel-doped copper oxide thin films deposited on glass by radiofrequency sputtering. In
the nickel-doped copper oxide sample, the band at 618 cm
1 is assigned to nickel–oxygen stretching mode suggesting the incorporation of nickel in the films. at.
%: atomic percentage.

doped with 3.7 at. % of Ni. For both samples, the absorption the Scherrer’s equation:[22]
bands at 418, 453, 511, and 668 cm
1 correspond to Cu–O 0:89k
vibration mode.[22] In the Ni-doped CuO sample, the band D ¼ (4)
b cos H
at 618 cm
1 is assigned to Ni–O stretching mode[23] suggest-
ing the incorporation of Ni in the films. where k ¼ 1.5406 Å is the X-ray wavelength, H is the Bragg
diffraction angle and b is the full width at half maximum
(FWHM) corrected by the instrumental broadening. As shown
X-ray diffraction study in Table 3, the crystallites size decreases with from 17 to 12
Fig. 6a–d displays the X-ray diffractograms of undoped and nm with increasing the Ni content. The decrease of crystallite
Ni doped CuO films with the considered contents. size may come from the substitution of Cu2þ by Ni2þ that lim-
The XRD diffractograms evidence that all films are poly- its the growth of the oxide grains during the film deposition.
crystalline, with a monoclinic structure ref (80-0076). The Another source of broadening of the XRD peaks is the
diffractions peaks at 32.62 , 35.4 , 38.1 , 61,5 , and 74.8 strain e in the films, which was evaluated by using the fol-
lowing equation:[25]
correspond to (110), (111), (111), (200) and (311) lattice
planes, respectively. The substitution of Cu by Ni into CuO b cos H
e ¼ (5)
leads to a slight shift towards high 2h angles and conse- 4
quently in the d-spacing and the lattice parameters since the The strain corresponds to the relative error in the lattice
effective ionic radius of Ni2þ (0.69 Å) is smaller than that of parameter, it’s then given as a dimensionless quantity or
Cu2þ (0.73 Å).[24] In addition, the intensities of the diffrac- expressed in %.
tion peaks as well as the crystallite sizes decrease with We notice that the strain increases with the increasing Ni
increasing Ni content as a result of the random substitution content as shown in Table 3.
of Cu by Ni. However, the crystal structure of CuO films is
not affected by these levels of substitution.
The structural parameters of sputtered thin films are listed Raman study
in Table 3. As shown in this table, the d-spacing value of the The structural properties of pure CuO and Ni-doped CuO
obtained films decreases with increasing the Ni content. This were also studied by Raman spectroscopy as shown in
effect can be attributed to the deformation of the lattice which Fig. 6. CuO has 12 optical phonon modes as follows:[26]
is consistent with the effect observed in the XRD characteriza-
C ¼ 4Au þ 5Bu þ Ag þ 2Bg (6)
tion that we attributed to the substitution of Cu by Ni.
The crystallite sizes D of Ni-doped and undoped CuO where Raman active modes are Ag and 2Bg and the infrared
films were calculated from the X-ray diffractograms by using modes are 4Au and 5Bu. The Raman spectra of undoped
6 H. EL AAKIB ET AL.

Figures 6. X-Ray spectra of undoped and nickel-doped copper oxide thin films deposited on glass by radiofrequency sputtering at different nickel contents (a)
undoped copper oxide; (b) 2.1 atomic % of nickel; (c) 3.7 atomic % of nickel; (d) 4.5 atomic % of nickel. All obtained films exhibit polycrystalline and monoclinic
character. H: Bragg angle;  : degree; at. %: atomic percentage.

Table 3. Structural parameters derived from XRD measurements of undoped and nickel-doped thin films.
Nickel doping (at. %) Orientation 2H ( ) FWHM ( ) d-spacing (Å) Crystallite Size (nm) Strain (10
3)
0 (111) 35.39 0.47 2.5239 17 1.95
2.1 (111) 35.39 0.59 2.5239 14 2.45
3.7 (111) 35.39 0.61 2.5236 13 2.77
4.5 (111) 35.39 0.70 2.5236 12 2.90
FWHM: Full Width at Half Maximum; at. %: Atomic percentage; d-spacing: interplanar spacing.

CuO exhibit three phonon modes at 283, 334, and substitution at Cu sites in CuO which can contribute to cre-
620 cm
1, corresponding to the Ag, Bg1, and Bg2 modes ate defects in the CuO nanostructure. Another possible rea-
respectively.[27] Fig. 7 shows that the intensity of the peak son for the shift and the broadening of the Raman peaks
located around 283 cm
1 decrease while its FWHM increases may be the decrease of crystallites size with increasing Ni-
as the Ni content of the films increases. Both parameters doping. The presence of a short peak around 320 and
depend on the crystallinity of the films. Their variations 525 cm
1 corresponds to random cosmic Rays spikes.
with the doping level suggest a decrease in crystallinity,
which further supports the results of the XRD measure-
Electrical properties
ments. In addition, one can notice the broadening and the
shift of the Raman peaks towards higher wavelengths with The electrical properties of the undoped and Ni-doped CuO
increasing Ni content. This may be due to the Ni thin films were studied at each percentage of doping by
 SPECTROSCOPY LETTERS 7

using the 4-point probe resistivity method at room tempera-

ture. Fig. 8 and Table 2 shows the variation of resistivity for
the undoped and Ni-doped CuO films with various Ni dop-
ing content. The resistivity value of the pure CuO thin film
was 21.7 X.cm and starts to increase with increasing Ni con-
tents, reaching a maximum value of 69.8 X.cm at a Ni con-
tent of 4.5 at. %. The increase in resistivity with increasing
Ni content can be attributed to two factors. The first one is
the decrease in the mobility of the holes[28] as Ni impurity
scattering increases with the Ni content. The second one is
the increase of the grain boundary contribution since the
grain size decreases with increasing doping level[29] as
revealed by the XRD measurements.

Conclusion
Homogenous and crystalline undoped and nickel-doped
copper oxide thin films were deposited by the radiofre-
quency sputtering technique. The effect of nickel doping on
the structural, optical and electrical properties was explored.
It was found that all obtained films exhibit polycrystalline
structure with dominant peak along (111) direction. The
crystallite size, strain and electrical resistivity have been
found to depend on the nickel content. The energy band
gap increases from 1.62 to 1.76 eV with increasing the nickel
content from 0 to 4.5 at. %. The Raman spectroscopy results
Figure 7. Raman spectra of copper oxide thin films for different nickel contents. confirm the formation of nickel-doped copper oxide. All
The broadening and shifting of the Raman peaks towards higher wavelengths
was observed with increasing nickel content. at. %: atomic percentage. obtained films show p-type conduction and exhibit good
properties to be involved as conductive oxides in solar cells
nanotechnology.

Figure 8. Variation of the resistivity of the undoped and nickel-doped copper oxide thin films deposited on glass by radiofrequency sputtering. The resistivity value
increases with increasing nickel content, reaching a maximum value of 69.8 X cm. at. %: atomic percentage.
8 H. EL AAKIB ET AL.

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