International Journal of Trend in Scientific Research and Development (IJTSRD)

Volume 4 Issue 3, April 2020 Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470

Spinel Ferrite Nanoparticles:

Synthesis, Characterization and Applications
D. L. Chaudhari1, D. S. Choudhary2, K. G. Rewatkar3
1S.S.
Jaiswal College, Arjuni/Morgaon, Maharashtra, India
2D.
B. Science College, Gondia, Maharashtra, India
3Dr. Ambedkar College, Deekshabhoomi, Nagpur, Maharashtra, India

ABSTRACT How to cite this paper: D. L. Chaudhari |

Spinel ferrite nanoparticle have attracted a great attention due to its widely D. S. Choudhary | K. G. Rewatkar "Spinel
used in several areas such as in electronics devices, biomedical, catalyst and Ferrite Nanoparticles: Synthesis,
wastewater treatment. The synthesis, characterisation and application of Characterization and Applications"
spinel ferrite nanoparticles in various fields is focuses in this review paper. Published in
The most commonly used synthesis methods along with their advantages and International Journal
limitations were discussed. The most common characterisation techniques of Trend in Scientific
and their applications such as power applications, biomedical applications, Research and
inductors, high frequency and Electromagnetic Interference (EMI) Development
Suppression are briefly reviewed. (ijtsrd), ISSN: 2456-
6470, Volume-4 | IJTSRD30684
KEYWORDS: Spinel ferrites, Synthesis, Characterization, applications Issue-3, April 2020,
pp.973-978, URL:
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1. INTRODUCTION
The spinel ferrites are of great interest in basic science, ferrite, there are 64 tetrahedral and 32 octahedral positions
especially for addressing the fundamental relationships are available for cations, out of which only 8 tetrahedral and
between magnetic properties and their crystal chemistry 24 octahedral are occupied by cations. The distributions of
and structure. Crystal chemistry shows how the chemical each metal cations over both sites ( A and B sites) are
composition (chemical formula), internal structure and depend on their affinity for both positions. Which depends
physical properties of minerals are linked together. Spinel on the ionic radii of the specification, stabilisation energy,
ferrites have been investigated in recent years for their size of the interstices, the synthesis method and the
useful electrical and magnetic properties and applications in conditions employed during synthesis time. The cations
information storage systems, magnetic bulk cores, magnetic distribution at tetrahedral and octahedral sites have a
fluids, microwave absorbers and medical diagnostics. Ferrite significant effect on the physical and chemical properties of
nanoparticles belong to a major group of magnetic ferrite nanoparticles. For example, the magnetic properties
nanoparticles and have received a considerable attention of ferrite nanoparticles are directly proportional to the
due to their wide applications in different fields ranges from distribution and types of the cations at octahedral and
biomedical to industrial. tetrahedral sites of the spinel structure. Because, the net
magnetic moment of ferrite nanoparticles is the difference
Spinel ferrite nanoparticles are metal oxides with spinel between the two sites [1].
structure of general formula AB2O4, where A and B are
metallic cations located at two different crystallographic The spinel ferrites are unique materials exhibiting
sites, tetrahedral (A site) and octahedral (B site). The cations ferrimagnetic and semiconductor properties and can be
of both positions are tetrahedrally and octahedrally considered as magnetic semiconductors. These materials has
coordinated to oxygen atoms, respectively (Fig.1). The been extensively used in several applications including
chemicals to be named as ferrite, at least, there must be Fe recording heads, antenna rods, loading coils, microwave
(III) in the chemical formula. The common spinel ferrites are devices, core material for power transformers in electronics
MFe2O4 (where M = Fe, Co, Mn, Zn, Cu and Ni), and most of and telecommunication applications [2–4]. Nanosized
them show super paramagnetic properties at the size below ferrites may have extraordinary electric and magnetic
or about the 20 nm in diameter. In one unit cell of spinel properties that are comparatively different from

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microstructured materials, tailoring them to modern solutions, which containing the mixture of divalent and
technologies, as well as providing novel applications such as trivalent transition metals, were mixed together in mole
ferrofluids [4], magnetic drug delivery [5], high density ratio of 1:2, respectively. Salts containing Fe(III) are usually
information storage [6], photocatalysis [7], gas sensors [8], used for the source of trivalent metal ions and the
etc. experiment is normally conducted in an alkaline medium .By
adjusting and controlling the pH of the solution may
Ni–Zn spinel ferrites are magnetic materials that are mostly synthesized super quality ferrite nanoparticles. The pH of
used in the modern electronics industry. This is due to their the solution is usually adjusted using ammonium solution.
high electrical resistivities, which implies low eddy current The co-precipitation method used in several research
losses that becomes significant at higher frequencies of studies, for the synthesis of spinel ferrite nanoparticles [11].
electromagnetic fields. Nickel–zinc ferrites also have a very
high values of saturation magnetization (Ms) and magnetic 2.2. Hydrothermal
permeability, high mechanical strength, low coercivities, low In this synthesis method, soluble salts containing divalent
dielectric losses and good chemical stability .The current and trivalent transition metals are dissolved separately and
interest in making nanosized nickel- zinc ferrite particles is mixed in the mole ratio of 1:2, respectively [12]. Then add
to reduce energy losses linked with bulk powders. Also more drop-wise organic solvents such as ethylene glycol or
electronic applications require these materials be pressed ethanol in the mixtures of aqueous solutions and under
into larger shapes with near theoretical density, which is continuous stirring in order to made homogeneous solution.
difficult to obtain if the particles have a wide size After that the solution is heated under the high pressure in
distribution.[9]. an autoclave. The hydrothermal method is one of the most
promising methods for the large-scale production of ferrite
nanoparticles. The synthesis of a good quality of nanferrites
with controlled size and size distribution can be obtained by
selecting the proper mixture of solvents and varying
parameters such as pressure, temperature and reaction time.

2.3. Sol-gel Method

The sol–gel method is widely used for the synthesis of the
spinel ferrite nanoparticles, in which metal alkoxide solution
undergoes hydrolysis and the condensation polymerization
reactions to formed gel and any volatile impurities were
removed by the heat treatment after the synthesis reaction.
The advantages of this method is, it is low-cost, simple,
achievable of narrow particle size distribution, carried out at
Fig.1. Crystal structure of Spinel ferrite showing also at low temperature without the need of any special
tetrahedral and octahedral sites equipment. However, care is taken for a better control of
reaction parameters such as concentration of sol, stirring
2. Synthesis methods of ferrite nanoparticles rate and annealing temperature. The major limitation is the
Recently, a number of synthesis techniques have been lack of purity in the final product and thus required thermal
developed for the preparation of ferrite nanoparticles, but to treatment after the synthesis of ferrite sample to attain high
date there is no anyone universal method of synthesis of purity. Nevertheless, composition control, particle size,
spinel ferrite nanoparticles and each synthesis methods has homogeneity and particle distribution can be achieved by
advantages and also disadvantages. These synthesis methods sol–gel method. The detailed process for synthesis of Ni-Zn
are grouped into two broad categories namely ‘‘top-down” Spinel ferrite can be described as follows (Fig. 2)[13].
and ‘‘bottom-up”. During the ‘‘top-down” technique
materials are pulverised to form tiny particles while in 2.4. Thermal decomposition Method
‘‘bottom-up” the ions are chemically combined to form the The thermal decomposition method is one of the simplest
particles. There are several synthesis methods for the method for the synthesis of spinel ferrite nanoferrites. This
‘‘bottom up” option includes co-precipitation, solvothermal, method involves thermal decomposition of organometallic
hydrothermal, sol-gel, flame spray pyrolysis, thermal precursors such as metallic acetylacetonates and carbonyls
decomposition, vapour deposition, sonochemical, in the presence of organic solvents and surfactants for the
microwave-assisted, polyol and microemulsion, techniques. synthesis of ferrite nanoparticles. On the basis of type of
The ‘‘top-down” synthesis techniques common for, the precursor materials, the high or low temperature can be
mechanical milling and pulsed laser ablation. These used. The shape and size of ferrite nanoparticles can be
synthesis techniques have a great advantages such as higher controlled by adjusting the temperature [14].
yields, shorter reaction time, improved selectivity, milder
reaction conditions and clean reaction [10]. Some of these
synthesis techniques are reviewed by Kefeni et al. [1].

2.1. Co-precipitation
Synthesis of spinel ferrite nanoparticles by co-precipitation
method is the most convenient, economic, and less time-
consuming, has high mass production, and is frequently
employed among all other methods in order to achieve
uniform-sized particles. In this method, an aqueous

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Typically, the temperature ranges in microwave-assisted
synthesis method from 1000C to 2000C and with the shorter
reaction time. Vapour produced during the heating time can
be eliminated by means of an exhaust drain. The microwave-
assisted synthesis method offers an opportunity to
synthesize ferrite nanoparticles on a large scale but due to
low yield compared to thermal or hydrothermal
decomposition methods and coprecipitation method [17].

2.8. Microemulsion Method

In the microemulsion synthesis technique,
thermodynamically stable isotropic dispersion of two
immiscible liquids stabilised by surfactant molecules is
usually used. For example, use of polyoxyethylene ethers as a
non-ionic surfactant, n-butanol as a co-surfactant and n-
hexane as an oil phase. One of the main advantage of the
microemulsion synthesis technique is, it offers the possibility
of synthesis diversity of ferrite nanoparticles by changing
the nature of surfactant, co-surfactant, reaction conditions
and oil water ratio. [18].

2.9. Electrochemical
The electrochemical synthesis method of nanoparticles is
similar to coprecipitation method, the difference between
Figure2. Schematic of synthesis of Ni-Zn Spinel ferrite these two methods is that the ion sources are due to the
by sol-gel route scarification of anode electrode through oxidation process.
Once the electrode (anode) is oxidised and released into
2.5. Solvothermal Method surfactant solution, ions are interacting between electrode-
In solvothermal synthesis method, an aqueous or non- electrolyte interface and formed the corresponding ferrite
aqueous solvents are used to synthesise nanoparticles with nanoparticles. The highly pure product and the particle size
precise control over the crystalline phases shape and size control are the some advantages of electrochemical method
distribution. These physical characteristics are altered by over the other synthesis methods. Purity of the sample and
changing certain parameters, such as the reaction time, the particle size achieved by optimising the distance
recation temperature, surfactant, solvent and precursors. A between the electrodes or controlling the current [15].
number of spinel ferrites and their composites have been Particularly, in an aqueous solution, current density and the
synthesized using the solvothermal method. The distance between the electrodes considerably influence
solvothermal method is useful where the preparation of crystallinity and the particle size. The crystallinity of the
spinel ferrites with improved chemical and physical synthesized particles could be improved by reducing the
properties applicable to both biomedical and industrial areas distance between the electrodes. Hence, either by increasing
is required. Due to its simplicity in terms of its reaction, the current or by decreasing the distance between the
solvothermal method use for the scalable production of electrodes, particle size tends to enhance. However, factors
spinel ferrites with controlled size and shape [15]. such as pH, current density, electrolyte concentration,,
distance between the electrodes should be properly and
2.6. Sonochemical electrode choice calculated in order to obtained the required
The sonochemical route is widely used for the synthesis of quality of ferrite nanoparticles intended to be synthesised
spinel ferrite nanoparticles due to facile control of reaction [19-20].
conditions. This method mainly used for controlling the
particle size distribution and the achieving homogeneous 2.10. Mechanical milling Method
mixing. Therefore, the temperature and intensity of Mechanical milling is a typical method for the preparation of
ultrasonic waves are the major factors which have a direct nanoferrites by using a high-energy shaker, tumbler mills or
impact on the particle size of spinel ferrites. During the planetary balls. This method is an example of the‘‘top-down”
synthesis process, due to ultrasonic wave, the bubbles are approach for the synthesis of spinel ferrite nanoparticles.
formed in solvent medium and spinel ferrites undergo in situ The major advantage of mechanical milling method is that it
calcination due to induced high-energy collisions between offers the possibility of scaling up to tonnage quantities of
the ferrite particles. Due to ultrasonication, mixing at the the materials for various applications while its major
atomic level can be achieve, so that formation of crystalline drawback is that the contamination of nanoparticles during
phase is achievable by annealing at relatively low milling [21]. This synthesis method is significantly used in
temperatures [16]. order to obtain nanoferrites with a wide size distribution of
35nm –85 nm.
2.7. Microwave assisted Method
The microwave-assisted synthesis method is the recent 3. Characterization
technique, for the preparation of ferrite nanoparticles. In a There are so many techniques are used to characterized the
microwave system, energy is directly delivered to materials nanoferrites. These techniques are varying in sensitivity and
through the molecular interaction with EMR. Conversion of they provide quality of the information about the sample.
electromagnetic energy into thermal energy generate heat. The characterization techniques which are most common

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includes: X-ray diffraction (XRD), scanning electron 3.2. Morphological Study
microscopy (SEM), transmission electron microscopy (TEM), The surface morphology of spinel ferrite nanoparticles could
superconducting quantum interference device (SQUID, be investigated by scanning electron microscopy (SEM) and
vibrating sample magnetometer (VSM),), UV- Visible, energy Transverse electron microscopy (TEM). These techniques
dispersive X-ray spectroscopy (EDS), Fourier transform are used in large scale to measure their diameter and to
infrared (FTIR) spectroscopy, X-ray photoelectron visualise the morphology of ferrite nanoparticles.
spectroscopy (XPS), Mössbauer spectroscopy (MS), thermo Particularly, TEM is a more informative technique in
gravimetric analysis (TGA), dielectric magnetic force providing morphological, compositional, and crystallite of
microscopy (MFM) and electron paramagnetic resonance. In ferrite nanoparticles. TEM provide the better resolution
this review paper the major characterisation techniques down to atomic scale. Scanning electron microscopy is a
were briefly discussed based on their application areas. surface sensitive imaging technique. It utilizes the electrons
generated due to interaction of beam with the sample
3.1. XRD surface. It is commonly used to study the aggregation state
X-ray diffraction (XRD) is a powerful nondestructive and the surface morphology of nanoparticles. SEM is used
technique for characterizing crystalline materials. It frequently than TEM but resolution of SEM is poorer than
provides information on structures, phases, preferred crystal the TEM shown in fig.3(a) and 3(b)[25].
orientations (texture), and other structural parameters, such
as average grain size, crystallinity, strain, and crystal defects.
X-ray diffraction peaks are produced by constructive
interference of a monochromatic beam of X-rays scattered at
specific angles from each set of lattice planes in a sample.
The peak intensities are determined by the distribution of
atoms within the lattice. XRD used CuKα as radiation source
for extracting XRD patterns of samples. The site radii,
hopping bond length, shared and unshared edges are the
structural parameters which were also calculated using the
X-ray diffraction data.

The crystallite size is estimated by using the Debey

Scherrer’s formula [24].

D= (1)

Where D is the particle size, β is the full-width at half- Figure 3.(a) TEM image of Ni0.65Zn0.35Gd0.25Fe1.75O4
maximum, λ is the wavelength of x-ray (1.5406 Å); and θ the
angle of diffraction.

Induced strain in the NiZn ferrite for different concentration

of Gd was calculated from Williamson –Hall method [9].

βcosɵ= 4ɛsinɵ + λ/D (2)

Where D is particle size, λ is wavelength of X-ray, β is FWHM

measure in radian, ɛ is the induced lattice strain and ɵ is the
Bragg Angle. The induced lattice strain obtained using above
formula

The X-ray density (ρx), bulk density (ρm) and porosity (P) of
the samples were calculated using the following equations
[4].
ρx (3) Figure 3.(b)SEM image of
Ni0.65Zn0.35Gd0.25Fe1.75O4

ρm (4) 3.3. Surface area

BET is the characterization technique used for the surface
area determination of ferrite nanoparticles. This method
P 1- (5) involves drying of powder ferrite nanoparticles in a vacuum
and then measure the adsorption of nitrogen gas on the
Where (M) is the molar mass, (m) is the mass of pellets, (r) is surface and micropores. The fundamental assumption in BET
the radius of the pellets, NA the Avogadro's number, Z is the characterization technique is that nitrogen gas access to the
number of molecules per unit cell (Z = 8 for Spinel ferrites ), whole surface of the particles [26].
and (V) is the volume of unit cell.
3.4. Magnetic properties
The common techniques were used to investigate and
measure the magnetic properties of ferrite nanopartcles are

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VSM, EPR and SQUID. EPR is a sensitive method in high-density storage, computer components, microwave
identification and detection of free radicals and the absorbing materials, sensors and biosensors, transformer
paramagnetic centres such as F-centre in the chemicals and core, magnetic recording media [29].
chemical reactions. This is a alternative method to find the
4.1. Inductors.
physical properties of ferrite nanoparticles and their
Inductors are used as elements in frequency selective
behaviour under the influence of external magnetic field.
circuits. spinel ferrites are primarily used as inductive
EPR is based on the interaction of an external magnetic field
components in a large variety of electronic circuits such as
with the magnetic moments of an unpaired electrons in
filters ,low noise amplifiers, impedance matching networks,
ferrite sample. Vibrating sample magnetometer(VSM) and
voltage-controlled oscillators. The basic components to
Superconducting quantum interference device(SQUID) used
produce the inductance are a very soft ferrite and a metallic
where high sensitive measurements of magnetisation are
coil. To provide high permeability at the operating frequency
required, sensitivity limit of VSM is about 10-6 emu [27]. VSM
the ferrite film synthesized by the process compatible with
study investigate the Saturation magnetization (Ms),
the integrated circuit manufacturing process [29].
Coercivity(Hc), Remenance (Mr), squareness ratio(SQR). The
variation of saturation magnetization with applied external 4.2. High Frequency
magnetic field illustrated in Fig. 4. SQUID measures different Ferrites have low losses and relatively high permeabilities
sample types such as crystals, powders, thin films, gases and varies with polarizing fields The magnetic materials having a
liquids. The samples under investigation packed into a more demands for high-frequency applications such as
gelatin capsules. By using SQUID technique it is possible to telecommunication systems and in radars, as microwave
determine Ms, Hs and residual magnetisation of ferrite technology requires higher frequency range and bandwidths
nanoparticles at applied external magnetic field and up to 100 GHz. Ferrites are nonconducting oxides and
temperature. therefore allow the total penetration of electromagnetic(EM)
fields, in contrast with metals, where the skin effect strictly
limits the penetration of high-frequency field [30]. At these
frequencies, the domain walls are unable to follow the fields
and the absorption of microwave power take place by the
spin dynamics.
4.3. Power Application
Spinel ferrites were used in Power applications. Power
supplies is an integral part of a large variety of devices such
as computers, all kinds of peripherals, TV, video systems, all
types of small and medium instruments. A compact and
efficient power unit is obtained called as switched-mode
power supplies (SMPSs). For this application, the mains
power signal is first rectified as regular pulses (typically
rectangular) at a high frequency and feed into a ferrite
transformer, and finally it is rectified again to provide the
required power to the given instrument. An increase in
power delivery and efficiency can be obtained by increasing
the working frequency of the transformer. [29].
Figure4. Variation in magnetization of Ni0.65Zn0.35Fe2O4
and Ni0.65Zn0.35Gd0.25Fe2O4 Ferrites 4.4. Electromagnetic Interference (EMI) Suppression.
The considerable increase in the amount of electronic
3.5. Dielectric properties equipment such as high-speed digital interfaces in
Dielectric behaviour is one of the most important properties computers and notebooks, scanners, digital cameras and so
of ferrites which markedly depend on the preparation forth, in small areas, has seriously enhanced the possibility
conditions, e.g. sintering time, and temperature, type and of disturbing each other by electromagnetic interference
quantity of additives. The study of dielectric properties (EMI). In particular, the fast development in wireless
produces valuable information on the behaviour of localized communications has led to interference induced by electric
electric charge carriers leading to greater understanding of and magnetic fields. Electromagnetic interference can be
the mechanism of dielectric polarisation in these studied defined as the degradation in performance of an electronic
ferrite samples. The dielectric properties were studied as a system caused due to an electromagnetic disturbance [31].
function of temperature, frequency and composition for a The noise from electric devices is usually produced at
spinel ferrites. An “abnormal” behaviour of the dielectric frequencies higher than circuit signals. To avoid, or to
constant is found and also the loss factor as a function of minimize EMI, suppressors should work as a low-pass filters,
frequency and temperature in comparison with the “normal” that is, circuits block signals with higher frequency value.
behaviour of spinel ferrites [28]. 4.5. Biomedical applications
4. Applications of ferrite nanoparticles The spinel ferrites finds application in the field of
Transition metal oxides, particularly, spinel ferrite nanomedicine is targeted drug delivery using magnetic
nanoparticles has been attracted the researchers due to their metal oxide nanoparticles by applying an external magnetic
useful electrical, magnetic, chemical and optical properties. field at the target tissue. The magnetic property of these
Their application ranges from biomedical to the modern structures allows controlling the orientation and location of
information technologies which include but not limited to particles by changing the direction of the applied external
satellite communication, antenna cores, memory devices, magnetic field. Pharmaceutical design and research in the
field of nanotechnology offer novel solutions for diagnosis

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 International Journal of Trend in Scientific Research and Development (IJTSRD) @ www.ijtsrd.com eISSN: 2456-6470
and therapies. The magnetic nanoparticles and magnetic [10] I. Safarik., K. Horska, K. Pospiskova, Z. Maderova, M.
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@ IJTSRD | Unique Paper ID – IJTSRD30684 | Volume – 4 | Issue – 3 | March-April 2020 Page 978