The research paper published by IJSER journal is about Synthesis and Characterization of nanocrystalline Ni-Co-Zn ferrite by Sol-gel Auto-Combustion method. 1

ISSN 2229-5518

Synthesis and Characterization of nanocrystalline Ni-Co-Zn ferrite by Sol-gel Auto-Combustion method.

R. B. Bhise1*, S. M. Rathod2, A. K. Supekar3.

1 Department of Physics, JJT University, Jhunujhunu, Rajasthan (India).

2 Department of Physics, Abasaheb Garware College, Pune(MH)

3 Department of Physics, Balasaheb.Jadhav.College, Ale( Pune ).

Email: bhiseramesh@gmail.com

Abstract:

The structural properties of nanocrystalline NiFe2O4 (NF), CoFe2O4 (CF) and ZnFe2O4 (ZF) ferrites were synthesized by Sol-gel auto combustion method. The powders were sintering at Normal temperature,

400oc and 700oc for 2hrs to densify properly. The samples were characterized by X-RD, SEM and FT-IR.

The X-RD used to analyze phase structure and lattice parameters. The FT-IR spectra confirmed that synthesis material is ferrite. Morphology of ferrite powders were investigated by using SEM. Porosity of synthesis ferrite is measured.

Key Words: Nano crystalline, Structural Properties, Sol-gel Auto Combustion method, X-RD, FT-IR Spectra, SEM.

1. Introduction

Ferrite of the type NiFe2O4 (NF), Co Fe2O4 (CF) and ZnFe2O4 (ZF) with the spinal structure are magnetic ceramics of great importance in the production of electronic and magnetic components. The electric and magnetic properties of ferrite are depends on various parameters such as processing conditions, sintering temperature and time as well as on their chemical composition [1]. Several attempts have been made by researchers to deposited ferrite films by a variety of techniques including alternative sputtering technology [2], Pulse-Laser deposition [3], and spin- spray plating [4]. However most of them cannot be economically applied on a large scale because they required high vacuum system, complicated experimental steps and high reaction temperatures. In this study, chemical synthesis route called sol-gel auto combustion method has been applied synthesize NF, CF and ZF [1-4]. This method is useful to achieve the fabrication of magnetic nano ferrites at low annealing temperature. In recent years very few studied based on different composition of Ni Co and Zn have been carried out. The size and morphology
of nano particles and their properties may be controlled by modifying the composition of the nano composites and by thermal treatment conditions [5]. Due to the small size of the nano crystals, an important part of the atoms are located at the surface this is the reason why the sol-gel synthesis method gone on intensive development [6]. Up to this stage the research work on Ni CO Zn Ferrite is very limited. The sol-gel method was used for synthesis of this nano ferrite material. This method involves hydrolysis [7].
In this paper we present a study on the synthesis of Ni0.6CO0.2Zn0.2Fe2O4, Ni0.4CO0.2Zn0.4Fe2O4 and Ni0.2CO0.2Zn0.6Fe2O4 nano composites of different composition. The composition, crystal structure, morphology, and size distribution of Ni, Co, Zn-Ferrite nano crystals can be controlled by adjusting the synthesis route and molar ratio of materials in the initial mixtures. The synthesized nano crystals have been characterized by X-RD, SEM, and FT-IR, presented below are the
details of investigation.

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The research paper published by IJSER journal is about Synthesis and Characterization of nanocrystalline Ni-Co-Zn ferrite by Sol-gel Auto-Combustion method. 2

ISSN 2229-5518

2. Experimental:

The Ni0.6CO0.2Zn0.2Fe2O4, Ni0.4CO0.2Zn0.4Fe2O4 and Ni0.2CO0.2Zn0.6Fe2O4 ferrite powders were prepared by co-precipitation and hydro thermal technique using iron nitrate, zinc nitrate, cobalt nitrate, and nickel nitrate as reaction agent. To obtain Ni0.6CO0.2Zn0.2Fe2O4, Ni0.4CO0.2Zn0.4Fe2O4 and Ni0.2CO0.2Zn0.6Fe2O4 ferrite powders we have mixed AR grade iron nitrate, zinc nitrate, cobalt nitrate, and nickel nitrate with double distilled water. Citric acid was used as a chelating agent because it plays an important role in homogeneous mixture formation of metal cations. Reaction procedure was carried out in air atmosphere at room temperature. The composition was well shake and pH of solution is maintained as 7
by adding ammonia. The prepared solution was
sintered ferrites specimens, evaluated by X-RD analysis are shown in table (1) along with their composition, density, crystalline size, Porosity. There was a minor increase in lattice parameter which may be due to increasing concentration of Ni and Zn. But lattice parameter increases with in increasing annealing temperature. Decreasing densification may be due to the evolution of excess Ni, and Zn in the composition for Fe at Room Temp., 4000C and 7000C respectively. Decreasing in density may be due to vary with concentration of Ni and Zn. Increasing porosity is depends on increasing temperature. The X-RD patterns are shown as in fig 1(a), (b), and (c).
Table No. 1
stirred on magnetic stirrer at low temperature 800C to form a gel. The prepared ferrite samples were annealed for 4000C and 7000C. The general chemical reaction involves in synthetic process can be written as
(x-0.8)Ni(NO3)2.6H2O+(0.2)Co(NO3)2.6H2O+ (x)Zn
(NO3)2.6H2O+2Fe(NO3)3.9H2O+3C6H8O7→Nix-0.8
CO0.2Znx Fe2O4+4N2↑+18CO2↑+12H2O.

ture C

gm/cc

4.91x10

The synthesized nano crystalline samples were characterized by X-Ray Diffraction techniques at room temperature by using Philips powder X-Ray Diffractometer (model PW3710) with CuKα radiations having wavelength 1.5406 A0. The morphological behavior of the investigated samples was determined by using Scanning Electron Microscopy (SEM) techniques (model HITACHI Japan). Fourier Transform Infrared (FT-IR) spectra were recorded in the range of 4000-400 cm-1 at room temperature by using Brukar Spectrometry.

3.Result and discussion:

2000

1800

1600

1400

1200

1000

800

600

30.1851

35.552

43.2078

57.0592

62.6628

3.1 X-Ray Diffraction.

To identify the possible formation of phase in Ni Co Zn Ferrite an X-RD analysis was done. The most intense peaks in all the specimens were found to match well with spherical spinel ferrite
(JCPD). Lattice parameters and crystalline sizes of

25 30 35 40 45 50 55 60 65

2θ

Fig-1(a) X-RD Pattern of Sintered Ni0.6CO0.2Zn0.2Fe2O4 Ferrites. Of peaks (210,211,311,411,421.)

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The research paper published by IJSER journal is about Synthesis and Characterization of nanocrystalline Ni-Co-Zn ferrite by Sol-gel Auto-Combustion method. 3

ISSN 2229-5518

3000

2500

2000

35.4534

used a reducing agent in reaction. The of Ni0.6CO0.2Zn0.2Fe2O4 IR curve fig2(a) of sintered powder shows strong absorption band 1598.699Cm-1 to 1345.10Cm-1 indicates N-H Bending structure, the strong absorption band at 2342.11Cm-1 indicating C
triple bond N- Stretched. The band at 724.13 Cm-1
indicating C-H out of plane bending carbohydrates which is very weak and shifted to low frequency.

1500

30.0865

56.9605

62.5839

100

1000

53.4089

1345.1057

80 8.6991

30 40 50 60

2θ

60 2342.123

40

Fig-1(b) X-RD Pattern of Sintered

Ni0.4CO0.2Zn0.4Fe2O4 Ferrites of

peaks (300,222,410,510,520,530) 20

0 724.1393

4000 3500 3000 2500 2000 1500 1000 500

16000

35.38

Wavenumber (Cm-1)

Fig-2(a) FT-IR Pattern of Sintered

14000

Ni0.6CO0.2Zn0.2Fe2O4

Ferrites.

12000

10000

8000

6000

30.04

42.96

53.3

56.84

62.4

100

80

60

2339.2305

16194.819231.42042.619415

30 35 40 45 50 55 60 65

2θ 40

Fig-1(c) X-RD Pattern of Sintered 20

Ni0.2CO0.2Zn0.6Fe2O4 Ferrites of

peaks (200,211,220,222,321,410) 0

693.2839

3.2 FT-IR Spectra:

In the present study Ni0.6CO0.2Zn0.2Fe2O4, Ni0.4CO0.2Zn0.4Fe2O4 and Ni0.2CO0.2Zn0.6Fe2O4 ferrite

4000 3500 3000 2500 2000 1500 1000 500

Wavenumber Cm-1

Fig-2(b) FT-IR Pattern of Sintered

Ni0.4CO0.2Zn0.4Fe2O4 Ferrites.

has been synthesized at room temperature, 4000C,
The of Ni
CO Zn
Fe O
IR curve fig2(b)

0.4

0.2

0.4 2 4

and 7000C.The synthesis process is carried out using
sol-gel auto combustion method. The citric acid was
of sintered powder shows strong absorption band
1619.91Cm-1 to 1344.14Cm-1 indicates N-H Bending

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ISSN 2229-5518


structure, the strong absorption band at 2339.23Cm-1
indicating C triple bond N- Stretched. The band at
693.28 Cm-1 indicating C-H out of plane bending carbohydrates which is very weak and shifted to low frequency.

100

80

60 2339.2305

40

20

1619.9122

Fig-3(a)SEM Morphology of Sintered

Ni0.6CO0.2Zn0.2Fe2O4 Ferrites.

0

715.4612

4000 3500 3000 2500 2000 1500 1000 500

Wavenumber ( Cm-I )

Fig-2(c) FT-IR Pattern of Sintered

Ni0.2CO0.2Zn0.6Fe2O4 Ferrites

The of Ni0.2CO0.2Zn0.6Fe2O4 IR curve fig2(c)
of sintered powder shows strong absorption band
2339.23Cm-1 to 1619.91Cm-1 indicates N-H Bending structure, the strong absorption band at 2341.15Cm-1 indicating C triple bond N- Stretched. The band at
715.46 Cm-1 indicating C-H out of plane bending
carbohydrates which is very weak and shifted to low frequency.

3.3 SEM Morphology:

Performing SEM we analyzed the structure of Ni0.6CO0.2Zn0.2Fe2O4, Ni0.4CO0.2Zn0.4Fe2O4 and Ni0.2CO0.2Zn0.6Fe2O4 shows typical morphology in fig3(a,b,c). For samples synthesized by sol-gel method the surface has compact structure with smallest particle size typically less than 100 nm. The micrograph of samples sintered at 4000C and 7000C indicating that microstructure is completely form these temperature. The grain size increases with increase in temperature.

Fig-3(b) SEM Morphology of Sintered

Ni0.4CO0.2Zn0.4Fe2O4 Ferrites.

Fig-3(c) SEM Morphology of Sintered

Ni0.2CO0.2Zn0.6Fe2O4 Ferrites

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The research paper published by IJSER journal is about Synthesis and Characterization of nanocrystalline Ni-Co-Zn ferrite by Sol-gel Auto-Combustion method. 5

ISSN 2229-5518

5. References:

4. Conclusion:

The NiCoZn Spinel ferrite nano particles were successfully synthesized by sol-gel auto combustion method. By varying the concentration of NiFe2O4 (NF), and ZnFe2O4 (ZF) at constant Co Fe2O4 (CF), there is increase in Lattice Constant, Inter planer distance and Porosity and decrease in Density, at increasing temperature. The FT-IR investigation shows strong absorption of Ni and Zn ions. The nano crystalline natures confirm from SEM and X-RD. SEM shows spherical structure. X-RD pattern confirm the formation of spherical spinel phase. The lattice parameters, Porosity and Density of ferrite materials are changes for different
concentration and different temperature.
1) K.C.Varma et al(2011), Strl, Microstrl.,Mag. Prop. Of NiCoMn Ferite thin film, J.Of Mag.and Mat.,323,3271-3275.
2) J.H.Gao, et al.(2004), Mat. Sci.Eng.B.,
110,111.
3) P.C.Dorsey,etal,(1997), J.Of Appli. Phy.,81,6884.
4) K.H.Buschow,(1995),Hnd.bk Of Mag. Mat,8,198.
5) M.Stefanescu,(2009), Prepn. Of Ni Zn Micro Comp. Powd. By S-G, j of Mat. Chem. And app. Phy.,113,342-348.
6) P.K.Roy,(2008),Chr. Of nano Cryst. Ferritr, J. of Mat. Process Tec.,197,279-283.
7) Xqi,J.Zhou,(2002), Key Eng. Mat.,593,224.

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