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Synthesis and characterization of nickel nanoparticles supported on aluminum oxide
D. Belfennache*1, D.Lakhdhari1, A.Belegane 1, N. Kaghouche2
1Research Center in Industrial Technologies CRTI Cheraga P.O. Box 64 Cheraga 16104 Algeries, Algeria
2Laboratory Microstructures and Defects in Materials (LMDM), from the Department of Physics of the University of Mentouri Constantine Brothers1 Algeria.
*d.belfenache@crti.dz
Abstract
Due to their peculiar qualities, metal-based nanostructures have been extensively used in applications such as catalysis, electronics, photography, and information storage, among others. New applications for metals in areas such as photonics, sensing, imaging, and medicine are also being developed. Significantly, most of these applications require the use of metals in the form of nanostructures with specific controlled properties. The properties of nanoscale metals are determined by a set of physical parameters that include size, shape, composition, and structure. In recent years, many research fields have focused on the synthesis of nanoscale-sized metallic materials with complex shape and composition in order to optimize the optical and electrical response of devices containing metallic nanostructures. In This work, we study nickel nanoparticles supported on aluminum oxide, prepared by impregnation with ionic exchange. In a first stage, the fixing conditions of the nickel precursor on aluminum oxide are optimized.
In the second stage, the samples are calcined at temperature (T= 750 °C). Several experimental techniques are used for the characterization of the samples at the various stages of their elaboration (SEM, DRX, and VSM). A change of morphology of the aluminum oxide grains was observed by Scanning Electron Microscope. The X-rays diffraction shows the formations of nanoparticles Al3Ni2 of near size 16.7 nm.The extracted magnetic measurements show the good and the easy magnetization
Keywords: Nanostructures, Ionic exchange, Nickel nanoparticles, Calcination.
I. Introduction
In addition to the simple miniaturization sought in the field of microelectronics, objects of nanometric size (whose size is between 1 nm and 100 nm) are at the heart of all attention for the development of materials with physical and chemical properties or original organic. The realization of nano-objects offers new perspectives from the fundamental point of view (Optics [1] and nonlinear optics [2], nanophotonic [3], plasmonic [4,5], local enhancement of the electromagnetic field [6], biosensing and molecular labeling [7, 8], spintronic [9],. . . ) that technological applications (high- density information storage [10], optoelectronic [11], chemical catalysts [12], etc.). All these applications require a speci fi city in the size, shape or organization of the nano-objects whose study passes beforehand by their elaboration.
Herein, we report a synthesis and characterization of nickel nanoparticles supported on aluminum oxide prepared by impregnation with ionic exchange. In a first stage, the fixing conditions of the nickel precursor on aluminum oxide are optimized. In the second stage, the samples are calcined at temperature (T=750°C).
II. Experimental
All reagents in this work were of analytical grades and used as received without further purification. NiSO4 (99.98%) was used as the nickel precursor, which was obtained from powder, used as a solid support for Ni was purchased from, whereas the Al2O3 (98%) and NH4OH (98.5%), All the aqueous solutions were prepared in double distilled water. For the preparation of supported nickel nanoparticles, we chose the method of impregnating the metal precursor with the support, in order first
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to promote the cationic exchanges between the negatively charged support and the positively charged metal. The method was chosen rather than the other methods because it makes it possible to obtain metal nanoparticles well dispersed on a substrate. The oxide support (α-Al2O3) is placed in the presence of an aqueous solution containing the metal precursor, of varying concentration and charge according to our choice. The pH of the solution is then adjusted with a suitable base (NaOH, NH2OH).
In order to promote the anchoring of the metal precursor on the support, the preparations are placed under magnetic stirring for a period of 24 hours. After the impregnation step, the prepared solutions are dried in an oven. Finally, the prepared samples were calcined in air in a furnace programmed for 3h.
III. Results and discussions:
III.1 Study of the aluminium oxide Al2O3
a) Structural properties
The diffraction X-ray spectrum of the Al2O3 support, shown in figure .1, This shows rays attributable to (ɑ) phase of aluminium oxide ( JCPDS No. 00-011-0661). The detected peaks correspond to the diffraction characteristics of the rhombohedral structure of Al2O3.
Figure1: XRD spectra: Al2O3
b) Morphological properties
The observation by SEM of aluminium oxide Al2O3 is presented in Fig.1. It is in the form of size grains of the order of 5 μm. On the outer surface of these grains is smooth and clean, but with the presence of very small particles, clears contrast.
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Figure 2: SEM micrograph of the Al2O3
III.2. Study of the Ni/ Al2O3 after step impregnation a) Structural properties
After the impregnation step, the diffraction X-ray spectrum of Ni / Al2O3 is similar to that of the support alone. Indeed, no characteristic peak of Ni, or of a mixed phase (Ni-Al) is observable, which suggests a good dispersion of the (Ni) metal on the Al2O3.
Figure 3: XRD Ni / Al2O3 after step impregnation
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The morphology of the support by the metal precursor (Ni / Al2O3), an image of which is represented in Fig.4, shows a morphology different from that of the support alone (Fig.2). On the surface of these grains, one notices the presence of very small particles, indicating that probably the large grains consist of clusters of grains of much smaller size.
Figure 4: SEM micrograph of samples Ni /Al2O3 after step impregnation
III.3. Study of the Ni/ Al2O3 after calcination at 750 ° C.
a) Structural properties
The X-ray diffraction spectrum of Ni / Al2O3 after calcination at 750 °C shows the presence of three new peaks relative to the support spectrum (Fig.5), the new peaks are low intensity. The appearance of three peaks located at the respective angles at 2θ = 36.88 °, 53.05 ° and 74.20 ° indicates the formation of a new metallic phase based on nickel. The card (JCPDS N ° 03-065-9699) makes it possible to attribute these peaks to the phase Al3Ni2.
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20 30 40 50 60 70 80
0,0 0,2 0,4 0,6 0,8 1,0 1,2
Al3Ni
2
Al2O
3
(0 1 3 )
(0 1 2 ) (3 0 0 ) (2 1 4 )
(1 1 6 ) (0 1 8 )
(0 2 4 )
(1 1 3 )
(1 1 0 ) (1 0 4 )
(0 1 1 )
(0 1 2 )
I/ I
max2 (°)
Figure 5 : XRD Ni / Al2O3 after calcination at 750°C
The peak at 2θ = 36.88 ° were used to estimate the particle size for the phase Al3Ni2, the Scherrer relationship from the mid-width -Height of the relationship of X-ray diffraction peaks
Where β (2θ) is the width at half height of the peak, expressed in radians, λ is the wavelength of X- rays used (λ (KαCo) = 1.7891 Å) and θ the angle of diffraction.
b) Morphological properties
Observation in Scanning Electron Microscopy after calcination at 750 ° C. (Figure: 3 a ,b) shows the presence of bright contrast particles in spherical form, the finely dispersed nickel particles are attached to the α-Al2O3 grains, with a size smaller than the limit of resolution (about 50 nm) . In the latter case, in fact, the nickel ions are individually fixed, are reduced in situ, and fuse to a rather weak degree. The conditions are thus favorable to a high and lasting dispersion.
2θ (°) β (2θ) Ф (nm)
Ni/Al2O3 36.776 0.58 16.7
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Figure 6: SEM micrograph of samples Ni /Al2O3 after calcination: at 750°C III.4. Magnetic properties
For the magnetic behavior Figure(7) show the taken hysteresis loop for a sample Ni/Al2O3
with 750º C of calcinations temperature .For the first look it clearly seen the ferromagnetic behavior of the sample because of the presence of Ni2Al3 nanostructure on the powder .The extracted magnetic measurements show the good and the easy magnetization with a measured magnetization saturation value is Ms= 0.132384 emu/g and a soft magnetic character with a coercive field value is Hc=143Oe and saturation field is value Hs=3682.37 Oe. The remanant magnetization value is measured at Mr=0.017024 emu/g that show the high speed of demagnetization of our sample.
(a)
(b)
Nickel nanoparticles
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-10000 -5000 0 5000 10000
-0,15 -0,10 -0,05 0,00 0,05 0,10 0,15
M a g n et iz a ti o n ( em u /g )
Aplied field (Koe)
Figure. 6: hysteresis cycle 4. Conclusion
Our study of the impact of the adsorption step of the metal precursor on the properties of nickel nanoparticles. Indeed, on one hand, by ion exchange interaction allows uniform fixing metal precursor on metal oxides to form ferromagnetic nanostructures. The setting conditions of the metal precursor on the oxide are optimized. These conditions provide a wide dispersion of money. Our results demonstrate, after calcination at 750°C the formation of Al3Ni2 phase of the size of neighboring particles of 16.7 nm. In order to analyze the extracted magnetic measurements show the good and the easy magnetization
References
[1] S.Kumar, N. Ganapathy, M. Sharmila, S. Shankar, M. Vimalan, M. & Vetha Potheher “ZnO/Ni(OH)2 core- shell nanoparticles: Synthesis, optical, electrical and photoacoustic property analysis”. Journal of Alloys and Compounds, 703, 624–632 (2017).
[2] Yuvaraj, S. Manikandan, N. & Vinitha, G. “Structural and nonlinear optical properties of nickel substituted manganese ferrite nanoparticles”. Ceramics International 44, 22592-22600 (2018)
[3] M. Sun, H. Dong, A. W. Dougherty, Q.Lu, D.Peng, W.T.Wong, B.Hung, L.D.Sun, C.H.Yan. “Nanophotonic energy storage in upconversion nanoparticles”. Nano Energy 56, 473-481(2019)
[4] G.S.Pawar, A.Elikkottil, B.Pesala, A.A.Tahir, T. K.Mallick. “Plasmonic nickel nanoparticles decorated on to LaFeO3 photocathode for enhanced solar hydrogen generation” International Journal of Hydrogen Energy 44, 578-586(2019)
[5] J. Zeng, W. Zeng, H,Zeng. “In situ plasmonic Au nanoparticle anchored nickel ferrite: An efficient plasmonic photocatalyst for fluorescein-sensitized hydrogen evolution under visible light irradiation”.
Journal of Solid State Chemistry 253, 294-304 (2017)
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[6] B.Quan, G.Xu, H.Yi, Z.Yang,J.Xiang, Y.Chen, G.Ji “Enhanced electromagnetic wave response of nickel nanoparticles encapsulated in nanoporous carbon”. Journal of Alloys and Compounds, 769, 961-968 (2018).
[7] S.Alim, J.Vejayan, M. M.Yusoff, A.K.M.Kafi “Recent uses of carbon nanotubes & gold nanoparticles in electrochemistry with application in biosensing: A review” Biosensors and Bioelectronics 121, 125-136 (2018)
[8] B.Golichenari, K.Velonia, R.Nosrati, A.Nezami, A.F.Fard, K.Abnous, J.Behravan, A. M.Tsatsakis. “Label- free nano-biosensing on the road to tuberculosis detection”. Biosensors and Bioelectronics 113, 124-135 (2018)
[9] K.Jeyasubramanian;R.V.William, P.Thiruramanathan, G.S.Hikku, M.Vimal Kumar, B.Ashima, P.Veluswamy, H. Ikeda. “Dielectric and magnetic properties of nanoporous nickel doped zinc oxide for spintronic applications”. Journal of Magnetism and Magnetic Materials 485, 27-35(2019)
[10] G.X.Pan, F.Cao, D.Xie, Y.J.Zhang, X.H.Xia, “Nickel nanoparticles activated highly porous carbon for excellent sodium storage”. Electrochimica Acta 292, 935-941(2018)
[11] R.Chen, B.Fan, M.Pan, Q.Cheng, C.Chen. “Room-temperature optoelectronic response of Ni supersaturated p-type Si processed by continuous-wave laser irradiation”. Materials Letters 163, 90-93(2016)
[12] S. N.V. Mahlaba, J. Valand, A. S. Mahomed, H.B. Friedrich. “A study on the deactivation and reactivation of a Ni/Al2O3 aldehyde hydrogenation catalyst: Effects of regeneration on the activity and properties of the catalyst”. Applied Catalysis B: Environmental, 224, 295–301(2018)
