Structural, Electrical, Dielectric, and Magnetic Properties of Cd<sup>2+</sup> Substituted Nickel Ferrite Nanoparticles

Devmunde, B. H.; Raut, A. V.; Birajdar, S. D.; Shukla, S. J.; Shengule, D. R.; Jadhav, K. M.

doi:https://doi.org/10.1155/2016/4709687

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Research Article | Open Access

Volume 2016 | Article ID 4709687 | https://doi.org/10.1155/2016/4709687

Structural, Electrical, Dielectric, and Magnetic Properties of Cd²⁺ Substituted Nickel Ferrite Nanoparticles

B. H. Devmunde,¹A. V. Raut,¹S. D. Birajdar,²S. J. Shukla,³D. R. Shengule,¹and K. M. Jadhav²

Academic Editor: Raphael Schneider

Received10 Oct 2015

Revised07 Jan 2016

Accepted13 Jan 2016

Published10 Feb 2016

Abstract

In the present investigation structural, electric, magnetic, and frequency dependent dielectric properties of ferrite nanoparticles (NPs) (where , , , and 0.8) prepared by sol-gel autocombustion method were studied. The crystallite size () (46.89~58.40 nm) was estimated from X-ray diffraction data with the postconfirmation of single phase spinel structure. Spherical shaped, fused grain nature with intergranular diffusion in NPs was observed in scanning electron micrographs. The value of loss tangent () decreases exponentially with an increasing frequency indicating normal Maxwell-Wagner type dielectric dispersion due to interfacial polarization. Decreasing values of Curie temperature () from 860°C to 566°C with increasing Cd²⁺ content in NPs were determined from AC-Susceptibility. Activation energy ranges within 0.03~0.15 eV. Decreasing magnetic saturation , coercivity , and magneton number values show the effect on nonmagnetic Cd²⁺ ions over magnetic Ni²⁺ and Fe ions.

1. Introduction

With the striking feature of “ferrimagnetism” nanocrystalline ferrites have attracted special attention of researchers in the field of electronic technology. Ceramics of ferrite have a wide temperature range of −40 to +225°C and greater values of specific resistivity and dielectric constant than that of the metals [1]. The unit cell contains eight formula units and is usually referred to as space group Fd3m () with the cations occupying special positions 8a and 16d. The ideal structure consists of cubic close packing of oxygen atoms (32e) in which one-eighth of the tetrahedral (A) and half of the octahedral [B] interstices are occupied [2]. The unit-cell geometry is controlled by only the metal-oxygen bond lengths for the tetrahedral (A–O) and octahedral [B–O] sites (Hill et al. 1979) [3]. In normal spinel structure the cation distribution is proposed as while inverse spinel has the general formula . The nonconvergent disorder of cations over the tetrahedral (A) and octahedral [B] sites can be described using an inversion parameter () and the formula , where for an extreme case and for a completely inverse spinel [3, 4]. NiFe₂O₄ NPs (cubic Å ± 0.002 Ǻ) ( number 227 in International Tables) [5], , JCPDS PDF-10-0325, is a semiconductor having a room-temperature resistivity ~1 kΩ cm and shows soft ferromagnetic order below 850 K with a relatively low magnetization of 2 per formula unit, that is, about 300 emu cm⁻³. Cd²⁺ is a nonmagnetic (0 ) divalent ion that shows almost similar substitution behaviour as that of Zn²⁺ substitution in ferrites [6]. Mixed Cd-ferrites (JCPDS-79-1155 [7]) are technically important due to their high resistivity, high permeability, and comparatively low magnetic losses making them more suitable for the electrical switching applications [8–10]. Cd²⁺ substituted NiFe₂O₄ NPs have widespread applications in recording heads, antenna rods, loading coils, microwave devices [1, 7], multilayer chip inductor (MLCI) [11], high frequency transformer cores, phase shifter, resonators, computers, TVs, and mobile phones [12–16]. The spinel structure of NiFe₂O₄ NPs is constructed by filling the FCC sublattice of relatively larger oxygen ions and the cation distribution is strongly dependent on ionic radii as well as concentration of the substituted divalent metal ions [17]. The entire Ni²⁺ cations occupy the [B]-site while the Fe³⁺ cations distribute equally between (A)-site and [B]-sites. Angle A–O–B is closer to 180° than the angles B–O–B and A–O–A; therefore, the AB pair (Fe–Fe) has a strong antiferromagnetic superexchange interaction [18]. Postsubstitution site preferences of Cd²⁺ ions are towards the tetrahedral (A) site suggesting the distribution of cations as Several possible cation distributions and various magnetic orders can be studied at A, B1, and B2 sites [19]. Nath et al. have studied the magnetic orders in Ni-Cd ferrite [6]. In recent days, variety of chemical and physical methods has been employed for the preparation of well-defined, magnetic Ni-Cd ferrite NPs with specific shape and size. Rafeek et al. have synthesised Ni-Cd NPs by sol-gel autocombustion method for the study of the antibacterial effects against microorganism [8, 20]. Nejati et al. have discussed the superparamagnetic nature of NiFe₂O₄ NPs synthesised by hydrothermal method [11, 21]. Drmota has discussed the precipitation in microemulsion method for the controlled size and morphology of magnetic nanoparticles [22]. Suresh et al. have prepared Ni-Cd NPs with crystallite size of 15~23 nm using chemical coprecipitation method [23]. Modi et al. have studied the pre- and postannealing particle size of the Ni-Cd ferrite NPs synthesis by wet-chemical technique [24]. Rahimi et al. have reported the synthesis of nanoscale ferrite powders by sol-gel autocombustion method using EDTA as a complexion agent [25]. In this investigation we have applied sol-gel autocombustion method for the production of fine powder of NPs. This preparation technique involves the exothermic and self-sustaining thermally induced anionic redox reaction of aerogel, which is obtained from aqueous solution [26].

2. Experimental Details

2.1. Synthesis of NPs

spinel ferrite NPs (where , , , and ) were prepared successfully by sol-gel autocombustion method using stoichiometric proportion of 99.9% pure AR grade ferric nitrate (Fe(NO₃)₃·9H₂O), nickel nitrate (Ni(NO₃)₂·6H₂O), and cadmium nitrate (Fe(NO₃)₂·4H₂O) (>99%) as starting materials. The metal nitrates were dissolved together in the presence of minimum amount of double distilled deionized water. Citric acid (C₆H₈O₇) is significantly used in wet-chemical methods compared to the other fuels, as it is characteristically weak organic acid having better complexing ability possessing a low ignition temperature (200–250°C). The molar ratio of metal nitrates to citric acid (C₆H₈O₇) was taken as 1 : 3. The pH of the solution was maintained at 7 with the drop by drop addition of ammonia solution. Continuous stirring of the mixed nitrate aqueous solution was performed on a magnetic hot-plate stirrer maintaining the temperature 90°C. During the evaporation stages, solution became viscous in colour and later on formed a viscous brown gel. Finally, a sticky mass began to bubble for few minutes in a same beaker. This gel got ignited automatically and burned with a glowing flint. The decomposition process would not stop before the whole citrate complex was consumed. As a yield product of this reaction, fluffy loose powder of brown coloured ash could be termed as presintered ferrite. The prepared samples were dried and annealed at 800°C for 12 h after thermogravimetric analysis (TGA). Some part of the annealed NPs was granulated with the addition of saturated PVA solution (polyvinyl alcohol ) as a binder. These granulated NPs were used to prepare disc shaped pellets of 10 mm diameter and 3 mm thickness using the hydraulic press by applying pressure of 5 tons/cm² for 5 min in a stainless steel die.

3. Results and Discussion

3.1. X-Ray Diffraction Study of NPs

X-ray diffraction patterns of NPs were recorded with the X-ray diffractometer (Philips). XRD of all samples were recorded in the range of 20–80° with Cu-K radiation ( a.u.) at room temperature. All the peaks were identified by comparing the “” spacing with that of JCPDS data of NiFe₂O₄ and CdFe₂O₄ in order to confirm the crystalline phases present. The major lattice planes (220), (311), (400), (422), (511), and (440) in Figure 1 confirm the formation of single phase with a face centred cubic spinel structure, space group Fd3m. Accordingly, minor lattice planes (222), (533), (622), and (444) in XRD pattern gave supporting agreement about the powder diffraction of the spinel cubic JCPDS [27]. Cation distribution was estimated from the comparison between observed intensity ratios () and calculated intensity ratios () by following the Bertaut method [12]. The values of structural parameters like peak intensity ratios, hopping length (), and bond length () are depicted in Table 1. Lattice constant () of NPs (Table 1) was determined from X-ray data analysis with an accuracy of ±0.002 Ǻ using the formula [28]:where is a lattice constant, ( ) represents the Miller indices, is a wavelength of X-rays, and is the glancing angle. It can be noticed from Figure 2 that the value of lattice parameter increased with the increase in Cd²⁺ content [29] from 8.350 Å to 8.491 Å (±0.002 Ǻ) which is attributed to the larger ionic radius of Cd²⁺ (0.97 Å) ions than that of Ni²⁺ (0.78 Å) ions obeying Vegard’s law [12]. Crystallite size () was determined by using the Scherrer formula [30]:where is a crystallite size (nm), is a full width at half maximum of strongest diffraction peak (311), is a wavelength of X-ray, and is the diffraction angle. Crystallite size of NPs was lying in the range of 46.89 nm to 58.40 nm (Table 2). There is a common trend of increasing crystallite size with increase in sintering temperature. Usually, increasing crystallite size in ferrite nanoparticles decreases the magnetic property because a large grain size leads to a low signal to noise ratio [31]. X-ray density () was calculated using the relation [32]: where is a molecular mass and is Avogadro’s number ( = 6.02 × 10²³). It was clear from Table 2 that X-ray density () of NPs increases with increasing Cd²⁺ content from 5.593 g/cm³ to 6.017 g/cm³. From X-ray density () and bulk density values () the pore volume distribution () was calculated (Table 2) using following relation:The values of percentage porosity “” ranges in between 38% to 40%. The variation in with increase in Cd²⁺ content in NPs is depicted in Table 2.

3.2. Scanning Electron Microscopy

Surface morphology and average grain size of Cd²⁺ substituted NPs were determined by using analytical scanning electron microscope by selecting 10,000 magnification range. SEM images (Figure 3) of typical samples ( and ) shows the nanocrystalline nature of NPs with vivid pores suggesting it as more advantages for the gas sensing applications. Voids and pores present in NPs can be attributed to the release of gases during the combustion process and lesser the dense nature. Intergranular diffusion can be clearly seen in SEM images of the NPs. Fused grain nature can be seen in , whereas looks comparatively more crystalline affecting the spin coupling in NPs which is at the base of the magnetic behaviour.

3.3. DC-Resistivity

The resistivity of ferrites ranges from 10⁵ Ω cm to 10⁹ Ω cm at room temperature. The DC-resistivity in NPs arises from the contribution of crystallite resistivity as well as the resistivity of crystalline boundaries. This phenomenon can be described by Vervey’s hopping mechanism. The electrical conduction in a material takes place due to the ions migration and when an external agency makes the activation of charge carriers. As the (A)-site and [B]-site are energetically not equivalent, conductivity is mostly dependent upon electron exchange between [B]-site cations [33]. The temperature dependence DC-resistivity of NPs was measured by two-point probe technique within the temperature range of 300–900 K and calculated using Arrhenius relation [34]:where is an activation energy and is Boltzmann constant (1.38066 × 10⁻²³ J K⁻¹). In ferrites, the mobility of electron is temperature dependent and it is characterized in terms of activation energies. The values of activation energy in paramagnetic () and ferrimagnetic region () with respect to Cd²⁺ content were calculated from the plots of versus using following relation [35]:The low value of activation energy in Ni-Cd ferrites may be attributed to the creation of small number of oxygen vacancies after doping of Cd²⁺ content and the decreasing activation energy may be due to the dominant role of Cd²⁺ in electrical resistivity of NPs [36]. Several researchers have justified such behaviour in nickel cadmium ferrites on the basis of role of ferrous ion content in exchange interactions [37]. The minimum value of ferrous ion concentration in octahedral [B] site plays an important role in exchange interaction, which is significantly responsible for the maximum electrical resistivity and low activation energies in this ferrite [38]. It was found that the activation energy in paramagnetic region is maximum compared to that of the ferrimagnetic region. A break separating the curve (Figure 4) in ferromagnetic and paramagnetic region indicates the change in magnetic order which is termed as Curie point (). The substitution of nonmagnetic Cd²⁺ ions in place of magnetic Ni²⁺ ions reduces the active linkage with increase in Cd²⁺ content ; therefore, Curie temperature of the system decreases with increasing Cd²⁺ substitution which is depicted in Table 2. The value of AC-Susceptibility decreases from 860°C to 566°C with increase in Cd²⁺ content . An electrical property based application of NPs includes transformer cores, inductors, (SMPS), converters, EMI filters, picture tube yoke, rotator, circulator, and phase shifter.

(a)

(b)

(c)

(d)

3.4. Dielectric Properties

In general, the dielectric behaviour of a material depends on the strength of electromagnetic interactions between constituent phases, the relative predominance of one phase over the other, and micro structure of phases [39]. The dielectric constant () and dielectric loss tangent () were determined as a function of frequency (100 Hz ≤ ≤ 10 MHz). In the present investigation Figures 5 and 6 show that decreases and decreases exponentially which corresponds to the decrease in AC-conductivity. More dielectric depression can be observed at the lower frequency region. The dielectric behaviour of NPs can be explained on the basis of Maxwell-Wagner interfacial polarization which is in agreement with Koop’s phenomenological theory [40–42]. In Figure 6, the shoulder-like peaks observed in the variation of with logarithmic frequency range from 3.5 to 4. This behaviour reveals that the resonance occurs between applied frequencies and hopping frequencies of charge carries. The maximum values of dielectric constant at lower frequencies may be attributed to the polarization due to inhomogeneous dielectric structure, namely, porosity and grain boundaries [43]. The decrease in polarization with increase in frequency may be due to the fact that beyond a certain frequency of electric field the electron exchange cannot follow the alternating field and therefore the real part of the dielectric constant decreases with increase in frequency [24].

3.5. Magnetic Properties

Room-temperature magnetic properties of NPs were measured using pulse field hysteresis loop tracer technique by applying a magnetic field of 1000 Oe. Using plots (see Figure 7) of NPs the saturation magnetization (), remanence magnetization (), coercivity (), and squareness ratio () were determined. From Table 3 it is evident that magnetic parameters of NPs decrease as a function of cadmium content which is associated with linkage between (A) and [B] sites. It may be due to the fact that nonmagnetic Cd²⁺ ions (0 ) replace magnetic Ni²⁺ ions (2 ) [44]. The magneton number increases up to and then decreases with increasing Cd²⁺ content . According to Neel’s two-sublattice model of ferrimagnetism magnetic moment per formula in , is given bywhere and are the [B] and (A) sublattice magnetic moment in and the values of magnetic moments of Fe³⁺, Ni²⁺, and Cd²⁺ were taken as 5 , 2 , and 0 , respectively. Neel’s model of two sublattices does not hold good for the variation in magneton number with Cd²⁺ content . According to the Yafet-Kittel model, where is a angle. In the samples with Cd²⁺ content and 0.2 was found zero. From to 0.8. increases from 29°30′ to 77°55′ which is attributed to the increased triangular spin arrangements on octahedral [B] sites [6]. These dilutions of spin moments weaken the in A-B interaction as Cd²⁺ content increases. Fe³⁺ ions have no magnetic neighbours and hence spins become uncoupled decreasing the saturation magnetization () from 94.22 to 13.73 (emu/g) which is in agreement with Suresh et al. [23]. This shows the size dependent behaviour of NPs [45]. Behaviour of coercivity can be explained on the basis of Brown relation [46] . For = 0.2–0.6 increases which is attributed to the uniform grain growth of single domain particle in which the absence of domain wall makes the magnetization process more difficult [4]. The values of magneton number (saturation magnetization per formula unit in ) are depicted in Table 3. For maximum value of was recorded; otherwise, decreasing nature of was observed for other samples from 2.58 to 0.42 with Cd²⁺ content which is associated with a decrease in A-B interaction.

4. Conclusions

spinel ferrite nanoparticles (NPs) were successfully prepared by sol-gel autocombustion technique using citric acid as a fuel. X-ray diffraction results showed the presence of all characteristic reflections (220), (311), (222), (400), (422), (511), (440), (222), (533), (622), and (444) which confirmed the formation of single phase, cubic spinel structure. Lattice constant (), X-ray density (), and crystallite size () increase with Cd²⁺ substitution. DC-resistivity decreases continuously with the increasing temperature, revealing the semiconducting nature of the prepared Ni-Cd samples. decreases from 860°C to 566°C with increase in Cd²⁺ content . SEM images show the fused grain nature with intergranular diffusion in NPs. The dielectric constant () and dielectric loss tangent () decrease exponentially which correspond to the decrease in AC-conductivity. Size dependent behaviour of magnetic parameters shows the decrease in saturation magnetization () from 94.22 to 13.73 (emu/g).

Highlights

(i) NPs are synthesised by sol-gel autocombustion method.(ii)X-ray diffraction pattern confirmed the formation of spinel structure.(iii) decreases with frequency and decreases exponentially.(iv)SEM confirmed the nanocrystalline nature with intergranular diffusion.(v)Magnetic parameters decrease with increasing Cd²⁺ substitution.

Conflict of Interests

The authors declare that there is no conflict of interests regarding the publication of this paper.

Acknowledgment

The authors would like to thank Dr. K. M. Jadhav for his valuable guidance and research facility for the present investigation.

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Copyright © 2016 B. H. Devmunde et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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