You are on page 1of 3

IJSRD - International Journal for Scientific Research & Development| Vol.

3, Issue 11, 2016 | ISSN (online): 2321-0613

Synthesis and Characterization of NiO Nanoparticles by Thermal


Decomposition Method
E.Kumar1 D.Muthu Raj2 A.Jenufa Begam3 S.Karthiga Devi4
1
Assistant Professor 2Associate Professor 3,4Research Scholar
2,3,4
Department of Physics
1
Tamil Nadu Open University, Chennai, India 2,3,4The M.D.T. Hindu College, Tirunelveli, India.
Abstract Nickel oxide (NiO) nanoparticles were prepared
by Thermal Decomposition method. Thermal decomposition
or thermolysis is a chemical decomposition caused by heat.
Thermal decomposition was thoroughly studied in order to
control the particles size of the as-prepared NiO Nano
powders. Transition metal oxides and metals have been
researched extensively due to their interesting catalytic,
electronic and magnetic properties. It has more applications
like electro chromic coatings, plastics, textiles, nanowires,
Nano fibers and specific alloy and catalyst applications. It is
also used in active optical filters, ceramic structure, p-type
transparent conductive films and energy efficient smart
windows. The synthesized nickel oxide (NiO) nanoparticles
were subjects to various studies like X-ray diffraction
(XRD) technique and Fourier Transfer Infrared
spectroscopy (FTIR).
Key words: Nickel Oxide, Thermal Decomposition Method,
XRD, FT-IR

study on the as-received and decomposed specimens has


been made by using a powder X-ray diffractrometer with Cu
target and a secondary monochromator.
III. RESULTS AND DISCUSSION
A. Structural Characterization:
1) XRD:
The X-ray diffraction pattern of the synthesized Nickel
oxide nanoparticles is shown in fig.1&2 and the peak details
are in Table.1. The experimental XRD pattern agrees with
the JCPDS card no.89-7390 and the XRD pattern of NiO
nanoparticles other literature. The 2 at peak confirms the
NiO. Strong diffraction peaks at 37 and 43 indicating the
NiO. The intensity of XRD peaks of the sample reflects that
the formed nanoparticles are crystalline and broad
diffraction peaks indicate very small size crystallite

I. INTRODUCTION
Transition metal oxides and metals have been researched
extensively due to their interesting catalytic and electronic
properties. Nickel oxide (NiO) has a wide band gap [1] and
varied applications [2]. They include catalysis[3], lithium
ion batteries[4,5], smart windows[6], anti-ferromagnetic
film[7],
dye-sensitized
photocathodes[8,9],
photo
catalysis[10],
anti-microbial
activity[11],
thermal
conductivity[12] and field emission studies[13]. Varying the
particle size of NiO leads to novel and interesting magnetic
properties that range from nano sized to bulk like behavior
[14-30]. Nanoparticles have been prepared by different
methods such as solvo thermal process [31], Thermal
decomposition [32, 33], sol-gel [34] and reverse microemulsion method[35]. In the present study, metal oxide
Nanophases such as Nickel oxide have been synthesized by
the method of thermal decomposition using nickel oxalate
dehydrates. The products were characterized by powder Xray diffraction and Fourier Transform Infrared Spectroscopy
(FTIR).

Fig. 1: XRD pattern of NiO nanoparticle

II. EXPERIMENTAL PART


A. Materials:

Nickel oxalate ( AR grade MERCK)

B. Synthesis:

Synthesis of Nickel Oxide

A small amount of the nickel oxalate has been used with


alumina crucible for thermal treatment. Isothermal
treatments have been carried with a furnace at a temperature
of 450 C for two hours respectively. The temperature has
been recorded with an accuracy of better than 1 C. The
heating rate has been maintained at 10K/min. A structured

S.
No
1
2

Fig. 2: XRD pattern of NiO nanoparticle


Measur Standa FWH
2
Relative
ed drd dM
(degr
intensity
spacin
spacin
[degr
ee)
[%]
g[A ]
g[A ]
ee]
37.27 2.4126
0.217
2.4122
54.49
00
6
5
43.32 2.0884
0.167
2.0883
100.00
67
0
3

All rights reserved by www.ijsrd.com

Siz
e
[nm
]
38.
56
51.
12

99

Synthesis and Characterization of NiO Nanoparticles by Thermal Decomposition Method


(IJSRD/Vol. 3/Issue 11/2016/020)

3
4
5

62.92 1.4771
0.200
1.4759
56.31
01
6
7
75.39 1.2607
0.234
1.2594
20.80
24
8
2
79.40 1.2069
0.200
1.2044
16.99
01
1
7
Table 1: XRD data of NiO nanoparticles

Fig. 3: Plot of cos as a function of sin for the nickel


oxide specimen

46.
42
42.
89
51.
47

V. DISLOCATION DENSITY, MACROSTRAIN AND MICRO


STRAIN

A dislocation is an imperfection in a crystal associated with


the misregistry of the lattice existing in different parts of the
crystal. The dislocation density can be calculated using the
formula 4.
=1/ T2 (4)
The micro strain can be calculated using the
formula 5, and the macrostrain can be calculated using the
formula 6. The values of dislocation density, macrostrain
and micro strain are shown in the table 2.
= cos/4 (5)
Macrostrain= (dobs - dstd)/dstd (6)
where is the dislocation density of the material,
is the macrostrain and d & d are the observed and standard
interplaner spacing for different crystal planes with different
miller indices(hkl).
Dislocation
S.N
Microstrain
(hkl)
Macrostrain
density
-3
-4
o.
*10 [m ]
*1014[m-2]
1
(003)
0.8987
0.3876
6.7224
2
(012)
0.6780
4.7885
3.8260
3
(104)
0.7466
1.4760
4.6391
4
(015)
0.8081
0.1466
5.4349
5
(006)
0.6733
0.0416
3.7734
Table 2: Dislocation density, macrostrain and micro strain

IV. PARTICLE SIZE CALCULATION


From this study, considering the peak at degrees, average
particle size has been estimated by using Debye-Scherer
formula. The results show that the value for the average
particle size is 46nm for the nickel oxide specimen. Interplanar spacing between atoms (d-spacing) is calculated
using Braggs law and enumerated in Table.1.
D= 0.9/ cos (1)
2d sin = n (2)
The values of particle size have also been
computed by using the Hall-Williamson method.
Subsequently, plot of cos as a function of sin as per
equation (3) for the nickel oxide specimen is shown in fig
3.The results show the value of particle size obtained by this
method is 71.84nm which is higher than those obtained by
the Scherrer method as from equation 3.
cos = (0.9/D)+ sin (3)
Where, is wavelength of X-Ray (0.1540nm), is
FWHM (full width at half maximum), is diffraction angle,
d is d-spacing and D is particle diameter size and n is the
order of diffraction, is a function of lattice strain in the
specimen.

VI. FT-IR SPECTRAL ANALYSIS


Fig 4. Shows the FTIR spectra for the nickel oxide
specimen. The spectrum has one profile 425 cm-1 due to
stretching mode of vibrations of Ni-O bonds which confirms
decomposition of the as-received specimen. The observed
bands in the spectra are also presented in table 3.

-1

S.
N
o.

Adekunle
et al(2014)
[1]
-1

Transmittance bands (cm )


Saghar Foroush[2]
El-Kemary et
et al(2012) and K.Anandan[3] et
al(2013) [4]
al(2012)
-1

-1

Present
Study

Band assignment

-1

1.
Stretching Vibrtion of Ni-O
435.93cm
430cm
425cm
425cm
Table 3: FTIR spectroscopy data for the Nickel Oxide specimen along with the band assignments and a comparison with
literature

Fig. 4: FTIR spectra for the nickel oxide specimen

All rights reserved by www.ijsrd.com

100

Synthesis and Characterization of NiO Nanoparticles by Thermal Decomposition Method


(IJSRD/Vol. 3/Issue 11/2016/020)

VII. CONCLUSION
NiO nanoparticles were prepared by using thermal
decomposition method. The synthesized nanoparticles were
characterized by XRD, FTIR spectroscopy. The XRD
pattern showed that the synthesized NiO nanoparticles were
crystallite in nature and they have Rhombhohedral structure
and the average particle size is 46nm. The FTIR study
confirmed the functional groups appeared at 425 cm-1 in
NiO Nano particles were due to the stretching of NiO.
REFERENCES
[1] F.Reinert, P.Steiner, H.Hufner, J.Schimtt, J.Fink,
M.Knupper,
P.Sandal,
E.Bertel,
Z.Phys.
B97(1995) 83-93.
[2] K.Anandan,
V.Rajendran,
Nanosci.Nanotechnol:Int.J.2(2012) 24-29.
[3] S.Berchmans, H.Gomathi, G.P.Rao, J.Electronal, Chem.
394 (1995) 267-270.
[4] P.Poizot, S.Laruelle, S.Grugeon, L.Dupont, J.M.
Tarascon, Nature 407 (2000) 496-499.
[5] M.V.Reddy,
G.V.Subbarao,
B.V.R.Chowdari,
Chem.Rev.113 (2013) 5364-5457.
[6] C.G.granqvist, Handbook of inorganic Electrochromic
Materials Ed. Elsevier, Amsterdam, 1995.
[7] J.C. Loudon. Phy.Rev.Lett.109 (2012) 267404-267408.
[8] J.He, H.Lindstrom, A.Hagfeldt, S,-E. Lindquist, J.Phys.
Chem B 103 (1999) 8940-8943.
[9] Z.Ji, G. Natu, Y,.Wu, ACS Appl.Mater. Interfaces 5
(2013) 8641-8648.
[10] C.Nitin, S.Sunayana, M.K Sharma, R.K Chaturvedi,
Int.J.Res.Chem.Environ. 1 (2011) 66-70
[11] Y.W.Back, Y.J.An, Sci.Total Environ. 409 (2011)
1603-1608.
[12] P.Sahoo,
D.Misra,
G.S.Chaubey,
J.Salvadaor,
N.J.Takas, P.F.P.Poudeu, MRS Proc.(2010) 1256.
[13] B.Varghese,
M.V.Reddy,
Z.Yanwu,
C.S.Lit,
T.C.Hoong, G.SubbaRao, B.V.R.Chowfari, A.T.S.Wee,
C.T.Lim, C.H.Sow, Chem.mater.20 (2008) 3360-3367.
[14] N. Rinaldi-Montes, P. Gorria, D. Martinez-Blanco, A.B.
Fuertes, L. Fernandez Barquin, J. Rodriguez Fernandez,
I. De Pedro, M.L. Fdez-Gubeida, J. Alonso, L. Olivi, G.
Aquilianti,
J.A.
Blanco,
Interplay
between
microstructure and magnetism in NiO nanoparticles:
breakdown of the anti ferromagnetic order Nanoscale 6
(2014) 457.

All rights reserved by www.ijsrd.com

101