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A R T I C LE I N FO A B S T R A C T
Keywords: Pure NiO nanoparticles and NiO-CdO nanocomposite were prepared with different content of CdO by simple
Nanocomposite chemical precipitation method at 800 °C for 3 h. Crystal structure, surface morphology, elemental composition
XRD and function groups present in the prepared samples were characterized by XRD, SEM, EDX, Raman and FTIR
Raman analysis analysis, respectively. From XRD, preparation of pure NiO and formation of nanocomposite samples confirmed
Optical properties
by the presence of characteristic diffraction peaks of cubic phase structure of NiO and CdO. The particle size
Photocatalytic efficiency
increases from 26 to 34 nm with the increase of CdO content in the prepared samples. SEM images show the
spherical shape of NiO and plate like shape of nanocomposite samples. The EDX analysis revealed that the
absence of any impurity peaks indicates the high quality of prepared samples. Raman and FTIR spectra show the
fundamental peaks of NiO and CdO in the samples. The best photodegradation efficiency of methyl orange dye
i.e. 60% was achieved as a result of the decrease in the energy band gap from 3.42 to 2.92 eV at the optimum
content of CdO (0.12 wt%).
Introduction environment friendly nature [29–32]. One of the constraints facing the
use of nickel oxide as a phtocatalyst is the decreasing time of re-
Researches nowadays have been focused on the transition metal combination process between the electron and hole pairs because of its
oxide nanoparticles in single or composite form due to their distin- widely band gap (3.6–4.0 eV) [33]. It was reported that, a formation of
guishable optical, electrical, magnetic and catalytic properties [1–9]. the nanocomposite materials is the remarkable method to improve the
These properties make them more applicable in several fields such as photocatalytic properties of NiO by decreasing the rate of recombina-
photonics, electronics, biosensor, biomedical, biological and treatment tion process under light irradiation due to the presence of two dissim-
of environmental hazards [10–13]. The textile industries use coloured ilar energy-level systems which can play a significant role in attaining
dyes such as methylene blue, acid red 14, remazol red RR, reactive blue charge separation [11,34–37]. Due to high carrier concentration, high
19, methyl orange etc. Usage of these coloured dyes becomes a major electrical conductivity, greater chemical stability, wide spread avail-
source of environmental contamination. This leads to surface and ability, high transparency in the visible range of the electromagnetic
ground water contamination [14–23]. A nanoparticle nickel oxide spectrum and less cost material of n-type semiconductor cadmium
(NiO) as a p-type semiconductor used in catalysis process, energy sto- oxide (CdO), the decent combination between NiO and CdO would be a
rage, solar energy conversion, chemical, biological sensing and high- prominent composite for enhance the photocatalytic activity [38]. To
temperature superconductivity [24–28]. NiO was widely used as a study the role of CdO amount on the crystal structure, surface mor-
photocatalyst in the photodegradation process of some water pollu- phology, optical properties and photocatalytic efficiency of p-NiO/n-
tants, due to its low cost, environmental stability, efficiency and CdO nanocomposite, four nanocomposite samples were prepared by
Abbreviations: COD, Chemical oxygen demand ; EDX, Energy – dispersive X-Ray spectroscopy; Eg, Energy gap; FTIR, Fourier transform infrared; MO, Methyl
orange; NCs, nanocomposites; NPs, Nanoparticles; SEM, Scanning electron microscope; UV–Visible, Ultraviolet–Visible; VB, Valence band; Xe-Lamp, Xenone Lamp;
XRD, X-Ray Diffraction
⁎
Corresponding author.
E-mail addresses: esabozaid@yahoo.com, eabozaid@aun.edu.eg (E.F.A. Zeid).
https://doi.org/10.1016/j.rinp.2018.12.009
Received 30 September 2018; Received in revised form 21 November 2018; Accepted 2 December 2018
Available online 06 December 2018
2211-3797/ © 2018 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/BY/4.0/).
E.F.A. Zeid et al. Results in Physics 12 (2019) 562–570
chemical precipitation method in this work. The effect of CdO content achieve an adsorption-desorption equilibrium, then exposed to the light
was investigated using different analysis techniques. The photo- source. The concentration of MO dye after photodegradation was ana-
chemical degradation of methyl orange dye was used to evaluate the lyzed using a UV–Vis spectrophotometer (Shemadzu) by measuring the
catalytic efficiency of the samples. change in absorbance values at interval times for 2 h at a maximum
wavelength of the dye (464 nm). All photodegradation processes were
Methods evaluated at room temperature. Also, chemical oxygen demand (COD)
measurements were measured for all investigated samples which have
Materials different Ni-Cd catalyst ratio by using COD meter and multiparameter
photometer HI 83099. The COD percentages for removal of MO were
Nickel nitrate Ni (NO3)2·6H2O, Cadmium nitrate Cd (NO3)2.4H2, calculated by this equation:
Potassium hydroxide KOH and methanol absolute were purchased from
Sigma-Aldrich and used as received. All the aqueous solutions were COD0 − CODt ⎞
COD % = ⎛ ⎜ × 100
⎟
where CODo and CODt are the values of the chemical oxygen demand for
Preparation of catalysts
MO dye before and at interval times of irradiation.
Preparation of pure NiO NPS
Results and discussion
0.5 mol of nickel nitrate Ni (NO3)2·6H2O was dissolved in 100 ml of
double distilled water with stirring for 30 min. A fresh solution from Structural investigations
potassium hydroxide KOH (1.5 mol dissolved in 100 ml of deionized
water) used as a precipitating agent added dropwise to a nickel solution The structural properties of pure NiO and NiO-CdO nanocomposite
under continuous stirring for 2 h at 60 °C. The obtained green pre- were obtained by X-ray powder diffraction Fig. 1. The recorded dif-
cipitate of Ni (OH)2 was filtered and washed by distilled water and fraction peaks of the cubic crystal structure of pure NiO NPs are mat-
absolute ethanol in several times. The formed sample was dried over- ched well with the standard JCPDS Card No: 04-0835 [39] at 2θ values
night at 100 °C in an air oven after that the product was grinding more 37.22°, 43.33°, 63.06°, 75.37° and 79.38° indexed to the (1 1 1), (2 0 0),
times. The calcination process occurred at 800 °C for 3 h using a muffle (2 2 0), (3 1 1) and (2 2 2) planes in Fig. 1. The analysis of XRD patterns
furnace to obtain the pure NiO NPS. of prepared nanocomposite provides the presence of the characteristic
diffraction peaks of both NiO and CdO cubic crystal structure with 2θ
Preparation of NiO-CdO NCs values at 33.08°, 38.31°, 55.42°, 66.07° and 69.38° indexed to the
(1 1 1), (2 0 0), (2 2 0), (3 1 1) and (2 2 2) planes which matched well
A simple chemical precipitation method has been used for the for- with JCPDS Card No: 05–0640 [40]. It was tentatively observed that,
mation of nanocomposite samples. For the preparation of the NC1 there is no peak shift in the main characteristic peaks of NiO, only the
sample, 0.08 M of Cadmium Nitrate tetrahydrate Cd(NO3)2·4H2O dis- intensity of the preferred diffraction peak (2 0 0) decreased in the
solved in 100 ml of deionized water was added to the Nickel Nitrate presence of CdO during the nanocomposite. The presence of diffraction
hexahydrate solution under stirring. The precipitating agent of po- peaks of CdO and NiO confirm the formation of NiO-CdO nano-
tassium hydroxide slowly added to the mixture solution at 60 °C with composite. The complete absence of new peaks attributed to there is no
stirring for 2 h. The obtained precipitate was filtered and washed with interaction between two transition metal oxides. The crystal properties
distilled water and absolute ethanol in several times to remove any of NiO cubic phase in the prepared samples was estimated at 2θ = 43°
impurities. The formed sample was dried overnight at 100 °C in an air with diffraction line (2 0 0).
oven after that the product was grinding more times. The calcination Debye-Scherer’s equation was used to estimate the crystallite size as
process occurred at 800 °C for 3 h using a muffle furnace. The same follows:
procedures were followed to prepare NC2, NC3 and NC4 samples using
0.1 M, 0.12 M and 0.14 M of Cadmium nitrate. 0.9λ
D=
βcosθ (2)
Physical characterization and measurements
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E.F.A. Zeid et al. Results in Physics 12 (2019) 562–570
Fig. 2. W–H plots obtained for: (a) NC0 (b) NC1 and (c) NC4 samples.
The slope value of the straight line from the relation between βcosθ
versus 4sinθ , Fig. 2, indicates the microstrain behavior of NiO phase in
the studied samples. The crystallographic properties were highly af-
fected by the presence of dislocation density. The crystallite size related
to the dislocation density by the relation:
δ = 1/ D 2 (4)
Sample Crystallite size Microstrain (ε) Dislocation density Energy The surface morphology of the prepared samples investigated by
D (nm) ×10-4 (δ) ×104 (lines/ band gap
nm2) Eg(ev)
SEM demonstrated in Fig. 4(a–c). The morphology structure of pure
NiO (NC0) identified spherical nanoparticles composed of irregularly
NC0 26.94 3.70 13.78 3.42 shaped grains agglomerated with each other Fig. 4a. The micrographs
NC1 29.22 3.85 11.71 3.05 of the nanocomposite samples with lower and higher content of CdO
NC2 29.70 3.37 11.34 2.95
(NC1 and NC4) indicate well-defined grains with increased size Fig. 4b
NC3 33.60 6.41 8.86 2.92
NC4 33.95 9.89 8.68 2.84 and c. A plate-like shape appeared in the NC1 and NC4 samples at-
tributed to the presence of CdO confirm the formation of a
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E.F.A. Zeid et al. Results in Physics 12 (2019) 562–570
Fig. 4. SEM images of (a) NC0 (b) NC1 and (c) NC4 samples.
Fig. 5. EDX spectra of (a) NC0, (b) NC1 and (c) NC4 samples.
FTIR analysis
Fourier Transform Infrared Spectral (FTIR) analysis used to de- Fig. 6. FT-IR spectra of (a) NC0, (b) NC1, (c) NC2, (d) NC3 and (e) NC4 sam-
termine the functional group present in the pure NiO (NC0) and na- ples.
nocomposite samples (NC1, NC2, NC3, and NC4) as shown in Fig. 6. For
the prepared samples the peaks obviously appeared at Raman analysis
3133–3138 cm−1, 1350–1450 cm−1, 1050–1060 cm−1, 820–880 cm−1,
and 700–705 cm−1 are attributed to stretching vibration of OH group Raman spectroscopy is a useful method to investigate the structural
which is contributed by water content, asymmetric stretching of C]O, phase and purity of prepared samples. Raman spectrum at room tem-
C–O stretching vibration of adsorbed CO2, C–H stretching and N–H perature of pure NiO and NiO-CdO nanocomposite within the range of
bending mode respectively. Stretching vibrations of Ni-O appeared at 200–1600 cm−1 was contain several characteristic bands as shown in
425 cm−1, 555 cm−1 and 670 cm−1. Fig. 7. For pure NiO vibrational band at 505 cm−1 can be assigned to
The main characteristic peak at 770–780 cm−1 appeared only in the one phonon (1P) first-order transverse optical (TO) mode. The peaks at
nanocomposite samples (NC1, NC2, NC3, and NC4) associated with Cd- 715 and 1058 cm−1 can be attributed to (2P) due to the mixing of
O bond [42,43]. This peak intensity increases with the increase of CdO (2TO) and longitudinal optical (2LO). Raman analysis of the nano-
in the nanocomposite. The presence of main characteristic peaks of the composite samples shows the appearance of fundamental two-magnon
two semiconductor oxides (Ni-O and Cd-O) confirms the nanocomposite peaks (2 M) of NiO which observed at 1441 cm−1. The presence of this
formation. peak reveals that the transformation of NiO from weak ferromagnetic to
ferromagnetic activity. The increase of magnetization with increase of
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Fig. 8. Kubelka-Munk plots of (a) NC0, (b) NC1, (c) NC2, (d) NC3 and (e) NC4 samples.
Fig. 9. Absorption spectra changes of methyl orange dye using (a) pure NiO (NC0) and (b) NiO/0.12 %wt CdO (NC3) after irradiation time under Xenone lamp. (For
interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
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E.F.A. Zeid et al. Results in Physics 12 (2019) 562–570
Table 2 respectively, thus improving the generation of the electric field (charge
Photodegration rates (K), COD % and degradation % for Methyl Orange de- separation process). The previous attitude of the movement is ther-
gradation in the presence of different catalysts. modynamically convenient due to larger conduction and valence band
Sample K (min−1) COD % Degradation % of CdO compared with NiO. Inhibition of the electrons-holes re-
combination process leads to increase quantum efficiency. In the trap-
–3
NC0 1.35 × 10 30.67 34 ping case, the generated electrons react with oxygen molecules and give
NC1 3.81 × 10–3 45.33 45
oxygen radical O2− which used to degradation of organic dye. After
NC2 4.00 × 10–3 57.33 48
NC3 5.29 × 10–3 72.00 60 that, the organic pollutant dye can be decomposed by the oxidation-
NC4 4.60 × 10–3 68.00 50 reduction reactions.
The surface reactions involved in methyl orange degradation given
in the following equations based on earlier reports [50,55,56].
Table 3
Comparison of photocatalytic activity of some nanocomposites against methyl NiO(e− + h+)/CdO(e− + h+) + hv → NiO(e− + e−)/CdO(h+ + h+) (7)
orange dye.
h+ + OH−→OH (8)
Sample Photodegradation efficiency (%) at Ref.
120 min
e− + O2 → ·O−2 (9)
ZnO/CuO (90/10) 28.3 [50]
WO3/Ag2CrO4 (4 wt 37 [51] H2 O+ ·O−2 → OOH·+OH− (10)
%/1)
ATT/TiO2 31 [52] 2OOH·→·O2 + H2 O2 (11)
Att/Fe2O3 20 [52]
Ag2CrO4/SnS2 (2 wt 61.9 [53]
%/1) H2 O2 + O−2 → ·OH + OH− + O2 (12)
ZnO/PANI 45.8 [54]
NiO/CdO (1/0.12 wt%) 60 Present work ·OH + ·O−2 + h+vb + organic dye → degrade organic dye (13)
Conclusion
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E.F.A. Zeid et al. Results in Physics 12 (2019) 562–570
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