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Archives of Applied Science Research, 2013, 5 (1):62-67


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ISSN 0975-508X
CODEN (USA) AASRC9

Structural, morphological and hydrophilic properties of nanocrystalline


NiFe2O4 by combustion route
Kiran V. Madhalea, Maheshkumar Y. Salunkheb and Sachin V. Bangalec*
a
Department of Physics, Walchand College of Engineering, Sangli (M.S.) India
b
Department of Physics, Institute of Science, Nagpur (M.S.) India.
c
Pratapsinh Mohite Patil Mahavidyalaya, Karmala, Solapur, (M.S.) India.
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ABSTRACT

Nano structured NiFe2O4 is synthesized by combustion method using glycine as a fuel. The synthesized material was
characterized by TG-DTA, XRD, EDS and SEM. The average particle size of the nanomaterial NiFe2O4 calculated
from XRD was found in the range 34 nm. The superhydrophilicity of the sintered oxides was investigated by wetting
experiments, by the sessile drop technique, were carried out at room temperature in air to determine the surface and
interfacial interactions.

Keywords: TG/DTA, XRD, NiFe2O4, combustion method.


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INTRODUCTION

The spinels compounds AB2O4, where A and B are metal cations and X is an anion have been extensively studied
for their magnetic properties [1-3]. Due to the unique physical and chemical properties, synthesis and application of
nanoparticles is the focaus of intense research.These materials are very attractive in view of both, their scientific and
technological importance. Nanocrystalline spinel ferrites with the common formula MFe2O4 ( M = Ni, Zn, Mn, Co,
Mg etc.) are the most significant magnetic materials [4]. The spinel structure belong to space group Fd3m. The cubic
unit cell is formed by 56 atoms, 32 oxygen anions dispersed in a cubic close packed structure, and 24 cations
occupying 8 of the 64 tetrahederal site (A site) and 16 of the 32 octahedral site (B site) [5]. Nickel ferrite powder,
one of the very important ferrite materials has been considered for many application such as high density magnetic
storage media, MRI contrast agent, colour imaging, ferro-fluids, high frequency devices, magnetic refrigerators,
catalysts, gas sensor, magnetic fludies, photomagnetic materials, site-specific drug delivery and microwave devices
[6-8]. The properties of the synthesized materials are influenced by the composition and microstructure, which are
sensitive to the preparation methodology used in the synthesis. Various methods such as citric acid combustion
methods [9], sol-gel autocombustion method[10], organic gel-thermal decomposition method [11], hydrothermal
method [12], co-precipation method [13], gel-assistant hydrothermal route [14], thermolysis [15], wet chemical co
precipitation technique [16], self-propagating [17], microemulsion [18] and microwave synthesis [19] have been
developed to prepare nanocrystallite nickel ferrite.

We report here the synthesis of nickel ferrites nanoparticles through combustion method which is a unique
combination of the ignition and the chemical gelatine processes. This method has the advantages of simple
preperation , cost effective and gentle chemistry route resulting in ultra fine and homogeneous powder. The ablity to

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Sachin V. Bangale et al Arch. Appl. Sci. Res., 2013, 5 (1):62-67
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obtain songle-phage nickel ferrites magnetic nanoparticle with controllable particle size and and size distribustion
improves its adequacy in a wide range of technological application.NiFe2O4 nanoparticle are prepred by combustion
method . the structural, thermal, morphological and hydrophlic properties are investigated.

MATERIALS AND METHODS

2.1. Preparation of materials


For the present study, polycrystalline NiFe2O4 powder was prepared by combustion route [20-22] using glycine as
fuel. The materials used as precursors were Nickel nitrate hexahydrate Ni(NO3)2 6H2O, Fe (NO3)26H2O Iron nitrate
hexahydrate (all these were procured from A.R. Grade of Qualligen) and Citric acid (Nuclear band). glycine
possesses a high heat of combustion. It is an organic fuel and provides a platform for redox reactions during the
course of combustion. Initially the Nickel nitrates, Iron nitrates and glycine are taken in the 1:1:4 stoichiometric
amounts and dissolved in 250 ml beaker slowly string with glass rod clear solution was obtained. Solution formed
was evaporated on hot plate in temperature range 700C to 800C gives thick gel. The gel was kept on a hot plate for
auto combustion and heated in the temperature range 1700C to 1800C. The nanocrystalline NiFe2O4 powder was
formed within few minutes and sintered at about 5000C for about 4 hours got brown colour shining powder of
nanocrystalline NiFe2O4 as shown in following sheet [20-22].

Ni (NO3)2 6H2O Fe (NO3)2 6H2O glycine

Double distilled water

Magnetic stirring & drying at 70-800C

Sol Formed

Further heated at 170-1800C

Ignition in air

Nanoporous NiFe2O4

Characterization

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Sachin V. Bangale et al Arch. Appl. Sci. Res., 2013, 5 (1):62-67
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2.3 Characterization technique
The prepared NiFe2O4 samples were characterized using TG/DTA thermal analyzer (PERKIN ELMER, USA), X-
ray diffract meter (RIGAKU MINIFLEX-II) using CuKa radiation, Scanning Electron Microscope (FEI QUANTA
200) coupled with an Energy Dispersive Spectrometer.

RESULTS AND DISCUSSION

3.1 TGA Analysis


Figure 1 The first three intervals are entwined from 360C to 3500C with broad endothermic peaks and a weight loss
of 16%. These are attributed to the evaporation of residual water and burning of residual organic materials. The
second from 4000C to 6000C with a rapid weight loss of 40% and a broad exothermic peak around 6200C, this is
attributed to decomposition of the organic compounds. The synthesized powder was almost stable from the 6000C .

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Offset Y values

98

97

96
0 200 400 600 800 1000 1200 1400
Temperature 0C

Figure 1 Thermo gravimetric differential analysis curve of nickel ferrite sample.

3.2 X-Ray Analysis


The XRD pattern of the mixed precursor calcined in air at 5000C for 4 h is shown in Fig. 3. It exhibits the diffraction
peaks at 2 values of, 35.570, 37.160, 43.190, 57.110, 62.820 and 75.450 at 5000C which were attributed to the
formation of NiFe2O4 spinel structure in the calcined material. The calculated lattice parameter a = 8.3275 A was
in good agreement with the reported value for NiFe2O4 spinel (a = 8.3275, JCPDS # 74-2081). The crystallite size
was calculated by using the Scherrer equation t = K/ cos, where t is the average size of the crystallite, assuming
that the grain are spherical, K is 0.9, k is the wavelength of X-ray radiation, B is the peak full width at half
maximum (FWHM) and is the angle of diffraction. The crystalline size of the calcined mixed precursor is found to
be 5000C 34 nm.

3.3 EDAX result


TG-DTA curve indicates the phase formation of NiFe2O4 is just nearly 5000C therefore EDX carried out only at
5000C represented in Fig. 3, shows the energy dispersive X-ray spectrum of NiFe2O4. This was carried out to
understand the composition of nickel, iron and oxygen in the material. There was no unidentified peak observed in
EDX. This confirms the purity and the composition of the NiFe2O4 nanomaterial.

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Sachin V. Bangale et al Arch. Appl. Sci. Res., 2013, 5 (1):62-67
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400
2500
311 440
Intensity (arbitary unit)

222
2000
511 622

1500

1000

500
0 10 20 30 40 50 60 70 80 90 100

2 ( Degree)
Figure 2 Powder XRD pattern of the nickel ferrite sample

Figure 3 EDX pattern of mixed precursor NiFe2O4 at 5000C in air for 4 h.

3.4 Scanning electron micrograph analysis:


The microstructure of the sintered samples can be visualized from scanning electron microscope (SEM) tool. Figure
4 shown the particle morphology of high resolution, the particle are most irregular in shape with a Nanosize range.
Some particles are found as agglomerations containing very fine particles the particles shapes are not defined porous
nature and small and large core, spongy pores are seen in the micrograph.

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a b

Figure 4 SEM images of the self combustion product the powder annealed at 5000C at (a) and (b) high resolution.

4. SUPERHYDROPHILIC TEST
In to characterization:
Wetting experiment of synthesized pure nickel iron oxide evaluated by contact angle measurement were performed
by the sessile drop method using an Advanced goniometer (Model110, Ram hart Instrument Co., USA) apparatus
and distilled water droplets (0.01ml) were delivered to surface of nickel iron oxide material at different points

The wettability nature of our synthesized material is super hydrophilic in the Wenzel because of highly rough
surface nature clearly seen from SEM images with consideration given to the surface roughness. Figure 5 (a-b)
shows the image of contact angle on rough surface of nickel iron oxide material. It seen that contact angle of
material is =0, hence material in superhydrophilic (( 5) may be due to high energy surface and porous nature.

a b

Figure 5 (a-b) Photograph of measured contact angle on rough surface of nickel iron oxide materials.

CONCLUSION

Nanocrystalline NiFe2O4 has been synthesized by self combustion route. This synthesis route may be used for the
synthesis of other metal oxide.

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Sachin V. Bangale et al Arch. Appl. Sci. Res., 2013, 5 (1):62-67
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The phage formation of the NiFe2O4 is investigated by TG-DTA and XRD techniques. The synthesized product
shows single phage of inverse spinel structure with an average diameter 34 nm.
Elemental analysis confirmed by using EDX. Density can be carried out by different technique it was found to
approximately same.
Wetability of this material obtained from contact angle goniometer. The contact angle () is zero, which indicates
that oxide material was superhydrophilic.

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