IJSTE - International Journal of Science Technology & Engineering | Volume 2 | Issue 12 | June 2016

ISSN (online): 2349-784X

Synthesis & Morphological Characterization of

Mixed Spinel Nano Ferrites
M. J. Gothe
Department of Physics
New English Junior College, Wardha

A. S. Kakde
Department of Physics
Dr .Ambedkar College, Deeksha Bhoomi, Nagpur

P. S. Sawadh
Department of Physics
Bapurao Deshmukh College of Engg., Sewagram, Wardha

K. G. Rewatkar
Department of Physics
Dr .Ambedkar College, Deeksha Bhoomi, Nagpur

Abstract
The nanoparticles of zinc substituted nickel spinel ferrite with generic formula Ni1-xZnxFe2O4 were synthesized by sol-gel auto
combustion route. The X-ray diffraction analysis confirms that the system exhibits polycrystalline mono phase cubic spinel
structure. Microstructure and morphological studies were carried out by using scaning electron microscope (SEM). The
transmission electron microscope (TEM) confirms the formation of cubic ferrite particles with the particle size lies between 1548 nm.
Keywords: Nanoparticles, cubic ferrite, sol-gel combustion, XRD, TEM etc
________________________________________________________________________________________________________
I.

INTRODUCTION

Nickel Zinc ferrites (NZF) play versatile role in the field of microwave devices because of their dielectric and low conductivity
property. In nanocrystalline forms ferrites are technologically important materials which are most useful in medical field such as
MRI, bio-seperation and magnetic sensors [1-4] etc. Among the various types of spinel ferrite Ni-Zn ferrite mostly knowing by
their magnetic material for general use. Also they have many applications in low and high frequency devices and play a
significant role in many technological applications such as microwave devices, power transformer in electronic, rod antenna as
read/write heads for high speed digital tape etc [5, 6].The individual cation formed in the sample leads to high conductivity when
such a material is cooled in an oxygen atmosphere, it is possible to form films of high resistivity over the constituents grains.
Such a ferrite in which the individual grains are separated by either air gap or low conducting layers behaves as in homogeneous
dielectric materials. The selection of appropriate method for synthesis is therefore the key to obtain good quality ferrites. For the
synthesis of nanosize ferrite various methods have been used. Such as hydrothermal, chemical, copreciptation sonochemical
reaction, mechanical ball milling, sol-gel auto combustion etc. Among all these synthesis method, sol-gel auto combustion seems
to be most convenient method because it possess high purity, chemical homogeneity, small, controlled and uniform particle size
[7].
II. EXPERIMENTAL
Synthesis of Nano Ferrites:
Powder of nickel zinc nanoferrites having the formula Ni1-xZnxFe2O4, (x = 0.5, 1) were prepared by sol-gel auto combustion
method [8]. Using analytical grade Ni(NO3)26H2O, Zn(NO3)26H2O and Fe(NO3)29H2O as starting materials the stoichimetric
proportions of above samples were dissolve in deionised water. The mixture of the solution was heated at 70 o C on magnetic
heating plate until the solution transform into gel. The obtained gel put in the specially designed microwave oven and then
ignited to microwave radiation to form ash powder. The as burnt ash powder grinded in the agate pestle mortar to have ultra-fine
particles and then calcined at 800o C in an electric furnace for 4 hours to remove any organic impurities.
Characterization Techniques:
XRD measurements of the samples were carried out by using Bruker AXE D8 advanced diffractometer with Cu-K radiation at
room temperature. The surface morphological studies have been done by using scanning electron microscopy (SEM-JSM7600F). TEM analysis is done using high resolution transmission electron microscopy (H-7500). The electric studies of
synthesized samples in palletize form were carried out between the temperature 30 o C to 400o C using precision impedence
analyser Wayn kerr 6500B.

All rights reserved by www.ijste.org

265

Synthesis & Morphological Characterization of Mixed Spinel Nano Ferrites

(IJSTE/ Volume 2 / Issue 12 / 048)

III. RESULTS AND DISCUSSION

Fig. 1: XRD pattern of Ni1-x Znx Fe2O4 system.

The XRD pattern of the Ni1-xZnxFe2O4 (x = 0.5, 1) it shows that the formation of single phase simple cubic structure of all the
samples. No other phase/impurity was detected in the obtained XRD pattern shown in the figure 1.The crystalline size for all the
samples has been calculated from the broadening line at high intensity peak corresponding (311) plane. The lattice parameter for
Ni0.5Zn0.5Fe2O4 and ZnFe2O4 are found to be 8.5194 and 8.4676 this value which is nearly equal to JCPDS card no.520278
(space group Fd3m) [9]. It is found that the lattice parameter decreases with increasing the Zn concentration of cations because
the ionic radius of Ni2+ ions (0.69 ) is small than the ionic radious of Zn2+ cation (0.82) and hence the replacement of Ni by
Zn in NZF causes a decrease in lattice constant obeying Vegards law.

Sample
Ni0.5Zn0.5Fe2O4
ZnFe2O4

Table 1
Various parameters calculated from XRD
X-ray Density x Bulk Density m Porosity
(g/cm3)
(g/cm3)
( p %)
8.5194
3.1412
38.51
8.4676
3.0687
38.18

Particlel size
D (nm)
21
22

Fig. 2: TEM pattern of Ni0.5Zn0.5 Fe2O4 system.

All rights reserved by www.ijste.org

266

Synthesis & Morphological Characterization of Mixed Spinel Nano Ferrites

(IJSTE/ Volume 2 / Issue 12 / 048)

Fig. 2 shows the TEM images of the samples calcinated at 800 C, from the micrographs we observe that the oxides particles
are finely dispersed and spherical in shape within narrow size range. The average size of the particle determine from TEM was
found to be in close agreement with that obtained from XRD studied [10].

Fig. 3: SEM pattern of Ni0.5Zn0.5 Fe2O4 system.

SEM images have a characteristic three dimensional appearance and are useful for judging the surface structure of Ni-Zn
ferrite. It is found that the powders were made up of particles with the size in the nano range as shown in fig.3.The shape of the
majority of the crystallities appeared to be spherical. The surface morphology of the sample as seen from the SEM consists of the
grains, with relatively homogeneous grain distribution, with an average grain size varying from 18 to 30 nm.
IV. CONCLUSION
The zinc substituted nickel nano spinel ferrites were successfully synthesized by sol-gel auto combustion route. The XRD
confirms the formation of single phase cubic structure with high degree of crystallinity. TEM studies reveals, the particles were
found to be exhibiting a spinel structure with sizes varying from 21nm - 33nm. It is observed from SEM image that it exhibits
cubic like features indicative of nano crystalline nature of the samples.
ACKNOWLEDGEMENTS
The authors gratefully acknowledge UGC, New Delhi (India) for financial assistance provided to carry out this work through
major research project File No. 42-851 (SR) 2013.
REFERENCES
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]

F. Li, H. Wang, J. Magn, Magn. Mater. 309, 295, 2007.

S. Y. Zhao, R. Qiao, X.L. Zhang, Y. S. Kang, J. Phys. Chem. C111, 7875, 2007.
H. Deng. X, Li, Q. Peng, X. Wang, J. Chen, Y. Li, Angew. Chem. Int. Ed. 44 , 782, 2005.
R. Lebourgeois, C. Coillot, Journal of Applied Physics, 103, 510-513, 2008
Z.Z.Lazarevic, C.Jovalekic, D. Sekulic, M Slankamenac, M. Romcevic, A. Milutinovic, N.Z. Romcevic, 44, 331-339, 2012.
E. Ranjithkumar, R.Jayaprakash, M.S. Seehra, T. Prakash, K. Sanjay, Journal of Physics and Chemistry of Solids 74, 943949, 2013.
S. R. Gawali, P. R. Moharkar, R. R. Kherani, K. G. Rewatkar., Bionano Frontier, vol.5, 2012.
K. G. Rewatkar, N. M. Patil, S. R. Gawali, Bulletin of Material Science, Vol. 28, No.6, 585-587, 2005.
Joint Committee on Powder Diffraction Standards (JCPDS) Powder Diffraction File (PDF): International Centre for Di_raction Data: Newton Square, PA
2003.
[10] L. Affleck, M.D. Aguas, I.P. Parkin, Q.A. Pankhurst, M.V. Kuznetsov, J. Mater. Chem. 10 (8), 2000.
[11] Z. Lazarevic, Jovalekic, A. Milutinovic, M. J. Romlevic and N. Romlevic ACTA PHYSICA POLONICA A Vol. 121 (2012).

All rights reserved by www.ijste.org

267