Nanoscale Reports 3(3) (2020) 37 -42

DOI:10.26524.nr.3.24
RESEARCH ARTICLE OPEN ACCESS

Exploring the Characteristics of the Nickel Oxide Nanoparticles

via Sol-gel Method
M. Jothi*1, K. Sowmiya1

A BSTRACT
Nickel Oxide (NiO) is an important transition metal oxide with cubic lattice structure. NiO is thermally stable that is suitable for tremendous
applications in the field of optic, ceramic, glass, electro-chromic coatings, plastics, textiles, nanowires, nanofibers, electronics, energy
technology, bio-medicine, magnetism and so on. In this present study, NiO nanoparticles were successfully synthesized by sol-gel
technique. Nano-sols were prepared by dissolving Nickel-Chloride [NiCl2.6H2O] in NaOH solvent and were converted into nano structured
gel on precipitation. A systematic change in preparation parameters like calcination temperature, time, pH value has been noticed in
order to predict the influence on crystallite size. Then the prepared samples were characterized by the X-ray Diffraction Spectroscopic
(XRD), UV-VIS Spectroscopy, Fourier Transform Infra-Red Spectroscopy (FTIR), Energy Dispersive X-ray Spectroscopy (EDX), Scanning
Electron Microscopy (SEM) and Particle Size Analyzer (PSA). From XRD, the average crystalline-size has been calculated by Debye-
Scherrer Equation and it was found to be 12.17 nm and the band gap energy of Nickel oxide (NiO) from UV studies reveals around 3.85
eV. Further, EDX and FTIR studies, confirm the presences of NiO nanoparticles. The SEM study exhibits the spherical like morp hology of
Nickel oxide (NiO). Further from PSA, the mean value of NiO nanoparticles has been determined.
Keywords: Nano-sols, Sol-gel, XRD, FTIR, EDX.
Author Affiliation: 1Department of Physics,Vellalar College for Women, Erode-12,Tamil Nadu, India.
Corresponding Author: M. Jothi. Department of Physics, Vellalar College for Women, Erode-12, Tamilnadu, India.
Email: [email protected]
How to cite this article: M. Jothi, K. Sowmiya. Exploring the Characteristics of the Nickel Oxide Nanoparticles via Sol-gel Method.
Nanoscale Reports 3(3), 37-40. Retrieved from https://nanoscalereports.com/index.php/nr/article/view/62
Source of support: Nil
Conflict of interest: None.
Received: 17 August 2020 Revised: 8 September 2020 Accepted: 9 September 2020

1. I n T RODU CTIO n fields. It is recommended that recycling of nickel is a value-

Nanotechnology is a scientific approach that includes added economic activity that supports communities and
the synthesis of nano structured materials ranging from 1 to governments, so the synthesis of nickel oxide is very essential.
100nm.[1] Further, the preparation of inorganic and chemical Further, NiO is a transition metal oxide and p-type
metal oxide nano-particles has gained concentration for the semiconductor which possess a wide energy gap (3.6 to 4) eV .[6]
past few decades, in physical, chemical, biological, medical, Hence the number of researches on synthesize of Nickel
optical, mechanical and engineering sciences, to explore and Oxide nanoparticles is increased in these recent years due to
handle single atom and molecules.[2] Thus, the nanomaterials, their magnetic properties and potential uses in many fields
so far discovered were well in economic circulation which including catalysis, memory - storage devices and sensors,
leads to the invention of many new products.[3,4] To ignore also used in medical applications such as magnetically
the use of poisonous chemical solutions which lead to controlled drugs delivery, magnetic resonance imaging
various dangerous reactions and to avoid such reactions, and hyperthermia treatment of cancer cells and so on.[7-9]
conditions such as temperature, pressure and time, It’s also plays a vital role in the fabrication of carbon-
have been investigated by introducing the prospect of nanotubes (CNTS),[10] and also exhibits potential applications
manufacturing nano- products in aqueous medium with the including electronics, magnetism, Energy-technology and
help of capping agents.[5] In the present work, NiO has been Bio-medicine.[11-13] Due to their high reactivity, operational
synthesized using sol-gel technique. As Nickel Oxide (NiO) simplicity and eco-friendly properties, they are used to
nanomaterials are quite good, cheap and are very stable. The catalyze various organic reactions including chemo selective
use of nickel oxide is to prevent the nickel deficiency which oxidative coupling of thiols, reduction of aldehydes and
has the interesting and essential applications in different ketones, hydrogenation of olefins, synthesis of stilbenes
© The Author(s). 2020 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http: //creativecommons.
org/licenses/by/4.0/), which permits unrestricted use, distribution, and non-commercial reproduction in any medium, provided you give appropriate credit to
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37
 M. Jothi et al. (2020)

from alcohol through witting type definition, i.e., by the changed into black colored nano powder. Thus, the black
strategy of simultaneous generation of ylides and aldehydes, colored Nickel Oxide (NiO) nanoparticle was prepared.
alcohols are directly transferred to olefins with no need of
preparation of either aldehydes or ylides, and α-alkylation NiCl2 + NaOH → Ni (OH) 2+Na-C l Ni (OH)2 → NiO + H2O
of methyl ketone.[14 -18] They also catalyze certain inorganic The prepared samples were characterized by UV-Vis
reactions like decomposition of ammonia.[19] Nano-crystalline Absorption, Fourier Transform Infrared (FTIR), X-Ray
NiO powder shows super-Para magnetism effects.[20] These Diffraction (XRD), Scanning Electron Microscope (SEM),
applications can be enhanced by decreasing the particle size Particle Size Analyzer (PSA), and Energy Dispersive X-ray
in Nanoscale. Thus, nanoparticles with smaller size will also Spectroscopy (EDX).
shows good anti-bacterial activity.[21]
Various synthesis techniques have been applied to prepare 3. R e s u lts and Discussion
Nickel Oxide nanoparticles such as Hydrothermal, Solid-state
reaction, Electro-chemistry, Micro- emulsions Spray-pyrolysis, 3.1 X-ray diffraction
Precipitation method and Co-precipitation method.[22 - 29] The X-Ray Diffraction is to measure of the average spacing
Among these sol-gel method gains more advantages over between layers or rows of atoms and to determine the
the other methods, as it requires relatively low temperature, orientation of a single crystal, size, shape and internal stress
can create very fine powder and produces composition not of small crystalline regions. The XRD pattern of the Nickel
possible by solid-state fusion, low cost and simple technique. oxide (NiO) nanoparticles after calcination is shown in Fig. 1.
Hence, the Sol-Gel process has been employed for the This pattern exhibits sharpened reflection peaks which
synthesis of “Nickel Oxide” (NiO) nanoparticles. In this process, indicates that the crystalline size of NiO nanoparticles. The
the solution evolves gradually towards the formation of a gel positions of peaks occurred at 2θ = 37.2611, 43.2826, 62.8354
like network containing both a liquid- phase and a solid- phase. has been indexed at (111), (200), (220) crystal planes of the NiO
[30]
Typical precursors are metal-alkoxides and metal-chlorides, respectively,[36] well match with the reported values.[37] The
which undergo hydrolysis and poly condensation reactions to sharpness and the intensity of the peaks indicate the well
form a colloid. The basic structure or morphology of the solid- crystalline size of the NiO sample. Further, the grain - size
phase can range anywhere from discrete colloidal particles to was calculated by Debye-Scherrer Equation. Table 1 shows
continuous chain- like polymer networks.[31] The applications the various structural parameters that were calculated from
areelectrophoresis,[32] inkjet[33] and their medical applications the obtained XRD pattern. The average crystalline size of the
are Wound-healer,[34] Scar-size decrease,[35] and Thrombosis Nickel oxide nanoparticles has been found to be 12.17 nm.
treatment is possible by developing a new family of "injectable
composites plasminogen" activator entrapped within alumina.

2. E x p e r i m e n tal P r o c e d u r e
Nickel-Oxide nano powder is prepared by dissolving 3
grams of NiCl2.6H2O in 70 ml of the distilled water. It was
allowed for stirring in the magnetic stirrer for 1 hour. Further,
the solution of NaOH is prepared by dissolving 1.0 grams of
NaOH pellets in100 ml of distilled water then the prepared
solutions was added drop wise (NiCl2+ NaOH) and stirred for
2 hours. After stirring, light green gel was formed and kept
in room temperature then, filtered and washed with water
and ethanol. Thus, the “Light green colored precipitate” was
obtained, dried at oven in 100˚C for 5 hours leads to light
green color powder which was calcinated at 300˚C for 2 hours
in the muffle furnace. Finally, the green color powder was Fig. 1: XRD pattern for nickel-oxide nanoparticles

Table 1: Structural parameters of NiO nanoparticles

Interplanar- Crystalline- Size Dislocation-Density Micro- Strain
S. No 2° (deg)
distances (d) (D*10-8m) (δ*1015) (ε*103)
1. 37.2611 2.4122 1.17157 7.2855 3.0902
2. 43.2826 2.0889 1.22938 6.6164 2.9448
3. 62.8354 1.4776 1.25084 6.3913 2.8944

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3.2 Scanning Electron Microscope (SEM) Analysis 46.57% of O-content without the presence of any other type
The SEM is used to determine the particle size and the of elements in Fig. 3.
surface morphology of the synthesized nanoparticles by 3.4Fourier Transform Infrared Spectroscopy (FTIR)
using a focused beam of high-energy electrons to generate analysis
a variety of signals at the surface of solid specimens. Typical
FTIR is a technique used to determine quantitative
SEM images of the Nickel oxide (NiO) nanoparticles were
and qualitative features of IR- active molecules in organic
shown in Fig: 3.2, which shows the morphology of the
or inorganic solid, liquid or gas samples.[41] The FTIR was
synthesized powder at different magnifications of 55,000
employed to identify the functional groups of the synthesized
with particle sizes. The results indicate that particles are
material. Fig. 4 shows the FTIR Spectra of explored Nickel
in spherical shaped nano clusters with agglomeration are
oxide nanoparticles prepared by sol – gel method. The peaks
formed.[39]
at 3828.70 cm-1 and 3531.66 cm-1 represent the stretching
of [O–H] band. The Alkyne group [C≡C and C≡N] observed
3.3 Energy Dispersive X-Ray Analysis (EDX)
at 2358.94 cm-1. The peak 1423.47 cm-1 corresponds to the
The composition of NiO nano powder was examined bending of C–H Alkane group. The bending [=C–H] Alkene
by the Energy Dispersive X-ray Spectroscopy (EDX), a micro group peak observed at 991.41 cm-1.[42]
analytical technique used in association with SEM.[40] The The characteristic absorptions functional groups and
EDX examine the X-ray emitted from the synthesized sample, type of vibrations with intensity were listed in the Table 2.
when electrons bombarded on the surface of the sample. By
measuring the intensity and energy of the signal, data about 3.5 Ultra-Violet Visible Spectroscopy studies
the chemical composition was detected. The EDX spectrum UV Spectroscopy refers to absorption spectroscopy
shows frequency of X-rays in count of each energy-level. or Reflectance spectroscopy in the ultra-violet region
The peak's intensity determines the amount of the element and visible region. UV- VIS spectroscopy is commonly
in the sample. Since the EDX, demonstrated that explored preferred technique for estimating the optical properties
NiO nano-powders consists of 53.43 % of Ni-content and of the prepared samples. It states that the absorbance of

Fig. 2: SEM images of NiO nanoparticles

Fig. 3: EDX spectrum of NiO nanoparticles Fig. 4: FTIR spectrum of NiO nanoparticles

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 M. Jothi et al. (2020)

Table 2: Functional groups in IR spectra of NiO

Functional- Groups Wave number (cm-1) Type of Vibrations Intensity
Alcohol O-H 3828.703531.66 Stretch, Free Strong, Sharp
Alkyne C≡C and C≡N 2358.94 Stretch Variable, not present in symmetrical
Alkane -C-H 1423.47 Bending Variable
Alkene =C-H 991.41 Bending Strong

Fig. 5: UV visible spectra of NiO nanoparticles Fig. 6: Distributions of NiO nanoparticles

Table 3: Particle size distributions with diameter 4. C o n c lu s i o n

Distribution Diameter X Nanoparticles of Nickel oxide (NiO) have been successfully
Q (%) (μm) explored by low temperature sol gel method. The XRD
pattern indicates nano crystalline size of the particles that
25 % 2.725
was found to be 12.17 nm. The SEM image exhibits NiO
50% 7.125 nanoparticles with spherical shape morphology in nanoscale.
The EDX indicates the compositions of NiO nanoparticles
75% 16.368
i.e., 53.43% of Ni-content and 46.57% of O-content. The FTIR
shows the corresponding functional groups of synthesized
a solution is directly proportional to the concentration NiO nanoparticles. The PSA reveals the average particle size
of the absorbing species in the path length. UV Visible of NiO nanoparticles and found to be 7.125 μm.
absorption spectra of Nickel oxide (NiO) are shown in
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