Elsevier

Materials Research Bulletin

Volume 46, Issue 12, December 2011, Pages 2204-2207
Materials Research Bulletin

Preparation and properties of nickel ferrite (NiFe2O4) nanoparticles via sol–gel auto-combustion method

https://doi.org/10.1016/j.materresbull.2011.09.010Get rights and content

Abstract

Using nickel and ferric nitrates and citric acid, NiFe2O4 nanoparticles are prepared by a simple and cost-effective polyvinylpyrrolidone (PVP) assisted sol–gel auto-combustion method. The synthesised nanoparticles consist of single phase inverse spinel structure of NiFe2O4. The particles are in spherical shape with an average size of ∼8 nm. The vibrational properties show tetrahedral and octahedral sites of NiFe2O4 nanoparticles. The super-paramagnetism is observed with magnetic saturation (Ms) of 50.4 emug−1.

Graphical abstract

The synthesis of nickel ferrite nanoparticles through sol–gel auto-combustion method which is a unique combination of the ignition and the chemical gelatine processes. This method has the advantages of simple preparation, cost-effective and gentle chemistry route resulting in ultra fine and homogeneous powder. The ability to obtain single-phase nickel ferrite magnetic nanoparticles with controllable particle size and size distribution improves its adequacy in a wide range of technological applications.

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Highlights

► NiFe2O4 nanoparticles have been synthesised by a simple and cost-effective polyvinylpyrrolidone (PVP) assisted sol–gel auto-combustion method. ► The particles were in spherical shape with average size of ∼8 nm. ► The superparamagnetic properties were observed.

Introduction

The research in nano-science may be aimed to explore, synthesise and understand new nanomaterials and the related phenomena. Magnetic nano-materials have gained great interests in the past few years for their fascinating applications [1] like nano-magnetism [2] in mapping the scaling limits of magnetic information storage technology, antenna rod, drug targeting carrier, etc. Nanocrystalline ferrites which possesses a general formula MFe2O4 (M = divalent metal ion, e.g. Ni, Co, Cu, Mn, Mg, Zn, Cd, etc.) is one of the most attractive class of materials for technological applications. Nickel ferrite has been intensively investigated as one of the magnetic nanomaterials. Nickel ferrite (NiFe2O4) has an inverse spinel structure. The location of the divalent cations (Ni2+) in the crystal structure is closely related to the magnetic properties of the nickel ferrite. However, nickel ferrite shows super-paramagnetic behaviour and it has various applications such as gas-sensor, magnetic fluids, catalysts, magnetic storage systems, photomagnetic materials, magnetic resonance imaging, site-specific drug delivery and microwave devices [3], [4], [5], [6], [7], [8], [9], [10]. The properties of the synthesised 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 method [11], sol–gel autocombustion method [12], [13], organic gel–thermal decomposition method [14], hydrothermal method [15], co-precipitation method [16], gel-assistant hydrothermal route [17], thermolysis [18], wet chemical co recipitation technique [19], self-propagating [20], microemulsion [21], [22] and microwave synthesis [23], [24], [25] have been developed to prepare nanocrystallite nickel ferrite.

We report here the synthesis of nickel ferrite nanoparticles through sol–gel auto-combustion method which is a unique combination of the ignition and the chemical gelatine processes. This method has the advantages of simple preparation, cost-effective and gentle chemistry route resulting in ultra fine and homogeneous powder. The ability to obtain single-phase nickel ferrite magnetic nanoparticles with controllable particle size and size distribution improves its adequacy in a wide range of technological applications.

NiFe2O4 nanoparticles are prepared by PVP assisted sol–gel auto-combustion method. The structural, chemical composition, thermal, morphology and magnetic properties are investigated.

Section snippets

Materials

All the reagents are of analytical grade and are used as received but without further purification. Nickel nitrate [Ni(NO3)2·6H2O], ferric nitrate [Fe(NO3)3·9H2O], citric acid [C6H8O7] and polyvinylpyrrolidone (PVP) [C6H9NO]n are purchased from Sigma–Aldrich chemical reagent Co. (USA).

Synthesis of NiFe2O4 nanoparticles

The NiFe2O4 ferrite is prepared by the sol–gel auto-combustion method [26], [27], [28]. An appropriate amount of metal nitrates and citric acid are first dissolved in a minimum amount of de-ionized water. The

XRD study

The powder X-ray pattern recorded for the sample of NiFe2O4 is shown in Fig. 1. It is consistent with the standard pattern cubic spinel structure of bulk NiFe2O4 JCPDS (Card No. 10-0325). The lattice parameter of NiFe2O4 is a = 8.339 Å, which is close to the one reported in the previous literature [29]. Extra reflections are not detected in the X-ray diffraction pattern. The calculated average crystallite size, D is 7.3 ± 1.2 nm. Using Scherrer's equation [30],D=kλβcosθwhere D is the crystallite

Conclusion

A nitrate–citrate gel synthesised from metal nitrates and citric acid by sol–gel process with the molar ratio of 1:1, exhibits auto-combustion behaviour. The sol–gel auto combustion method proves good for the synthesis of nano-sized nickel ferrite. The PVP plays an important role in controlling the particle size in the synthesis process. The phase formation of the NiFe2O4 is investigated by XRD, FT-IR and microRaman techniques. The synthesised product shows single phase of inverse spinel

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