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Synthesis and Characterization of Erbium Doped Nickel Zinc Ferrites Nanoparticles
Synthesis and Characterization of Erbium Doped Nickel Zinc Ferrites Nanoparticles
Synthesis and Characterization of Erbium Doped Nickel Zinc Ferrites Nanoparticles
nanoparticles
1 Introduction
The properties of nanoparticles are different from the analogous bulk stable state
properties due to the reason is that it retains several chemical features and physical
physiognomies. It is due to the owing surface influence, dimensions, quantum
tunneling impact and quantum size effect (Naik et al., 2004; Search, Journals,
Contact, Iopscience, et al., n.d.). Until that time, metallic nanoparticles due to their
technical importance and theoretical significance have been systematically
inspected, also have been found wide variety of applications in microwave devices,
lubricants or catalysts, Ferro fluids and in magnetic materials etc. (Bhukal et al.,
2015; Kurian & Nair, 2014). The nanomaterials consist of interfaces as well as
nanosrystallites. The nanocrystallites interface displays neither short nor long
range order and it is just like a gas like material (R. De Oliveira et al., 2016). The
chemical as well as physical properties of nanocrystalline materials have been
affected by the interface volume and interfacial structure (Chandamma et al., 2017;
Prasad et al., 2015).
In the past, the history of ferrites and their applications have been well known for
many centuries. Mostly, ferrites consist of iron oxide which acts as a main
component and metal oxides. Depending upon the diverse crystal structure of
ferrites, it has been divided into different groups i.e., garnet, hexagonal ferrites,
ortho ferrite and spinel ferrite, but each of the ferrite have its own significance (M.
V. S. Kumar et al., 2019; A. Oliveira et al., 2019; Shevchenko & Barabash, 2019).
Conversely, in the advanced technology the substituted M-type hexaferrite retain
encouraging potential applications. Such type of ferrites exhibits ferromagnetic
1
nature i.e., having large total magnetic moment at ambient and operating
temperature and it comprises a hexagonal structure. In all over the world more than
90% permanent magnets are produced which is based on this composite.
At room temperature this compound acts as a deep semiconductor (~109 Ohm* cm)
Ohm comprises a total magnetic moment of 20 µB in the ground state and having
ferrimagnetic structure (M A Almessiere et al., 2019; Munirah Abdullah
Almessiere et al., 2019; Trukhanov et al., 2018). Moreover, multiferroic and large
spontaneous polarization properties recently revealed in barium hexaferrite at room
temperature which were replaced by diamagnetic cations (Kostishyn et al., 2015).
With this, if M-type hexaferrite having magnetoelectric properties and then
fabricated by using modified ceramic technique are considered more innovative in
contrast to renowned BiFeO3 orthoferrite multiferroic at room temperature (Search,
Journals, Contact, & Iopscience, n.d.).
Moreover, spinel type ferrite nanoparticle has got more importance because of its
thermal electrical, catalytic, unique magnetic and dielectric properties for advance
application in electric generator, disk recording, transformers, electrical devices,
microwave absorbers, ferrofluids, inductive as well as in industries (Majewski,
2021; Mathur et al., 2010). The structure of spinel permits various mixture of
mattelic ions without changing the structure of spinel crystal altering magnetic,
electrical structure and dielectric properties of ferrites spinel through replacing M 2
ions (Dias, 2000; Mathew & Juang, 2007; Vestal & Zhang, 2003; Zhao et al.,
2009). The structure of spinel ferrite is consist of [M +2]tet [Fe+3]octaO4. Therefore, the
entry of third metal ions specify the ions distribution in the spinel assembly. Thus
the dielectric, catalytically electrical and magnetic properties would be affected by
the concentration of third metal ions as it alters the distribution of M +2 and Fe+3
2
ions (Cekmece, 2009; Go, 2009; Köseoˇ, 2008). For high-tech applications several
ferrites systems are very important such as Mg-Mn, Ni-Zn, or Mn-Zn etc.,(Elahi et
al., 2015; Gao et al., 2015; Tsutaoka, 2003). The merely core materials which is
applicable to high frequency applications are Ni-Zn bulk ferrite nanomaterials.
(Rao & Rao, 2003; Tsutaoka, 2003; J. Wang et al., 2012).
Due to the high frequencies and eddy current, its performance is inhibited to 100
MHz and it is considered as main drawback of Ni-Zn ferrite nanomaterials.
However, by keeping the higher saturation magnetization and improving the
material electrical resistivity this problem can be resolved. Higher electrical
resistivity can be achieved with the processing material in the ultra-fine particles
and eradication of inter granular domain wall (Ahmed & Okasha, 2008; Zaag et al.,
2010). The reduction in eddy current might be occurred, when the ultra-fine grain
produces grain boundaries which in turns acts as a barrier for the flow of electrons
thus reduced the losses of current (Introduction, 1992; Search et al., 2008; Verma
et al., 1998, 1999).
For the preparation of ferrites, traditional methods have undeniable drawbacks like
higher grain size, higher time consumption and at high temperature it has long
heating schedule etc. In the preparation of these materials, the experimental
environments used play a significant role in the particle size and the properties of
the ferrite nano particles produced. Due to this reason, in the production of nano
particles a several types of experimental methods have been used such as co-
precipitation method(Arulmurugan et al., 2005; Date et al., 2004; Kim et al., 2001),
refluxing method, the sol–gel techniques (Gatelytė et al., 2011; Gruskov et al.,
2009), microwave sintering method (Sorescu et al., 2004), hydrothermal method
(H. Wang & Kung, 2004), spray-spin-heating-coating method (M. Liu et al., n.d.),
hydrothermal method (H. Wang & Kung, 2004), auto combustion method (Fe,
3
2010) and pulsed wire discharge method. Sol–gel and co-precipitation methods out
of above mentioned methods are the assuring techniques on bulk scale for
preparing nano ferrites due to the production of homogeneous particles.
The Co-precipitation method has been commonly used with constant pH because
of the homogeneity, high crystallinity and good textural properties of the materials
formed. Due to the high chemical homogeneity, the chances of controlling
morphology and size of particles, the sol–gel technique has become very common
for the preparation of a variety of nanomaterials, mixed-metal oxides and nano
porous oxides recently. It has been shown that excellent chemical homogeneity in
the final product and improved mixing of the starting materials are the significant
advantages of the sol–gel process (Veith et al., 2005).
4
band were assigned due to the octahedral complex and higher frequency band were
allocated due to the tetrahedral complexes. (Kurian & Nair, 2013)
Due to the broad range of potential applications of the nanocrystalline nickel zinc
magnetic particles like transformer cores, high-density information storage
devices, NEM/MEMs, microwave devices, magnetic fluids, etc. these particles
have attracted much attention by the researchers. (Costa et al., 2003; Verma et al.,
1999; Virden & Grady, 2005). In comparison to the bulk, the surface to volume
ratio of these nano-magnetic materials is very large. Due to this they show extra
ordinary properties like surface anisotropy, superparamagnetism and spin canting,
etc. (Caruntu et al., 2007).
Different authors from the field of science has been publicized several thesis,
publications etc., however the actual information on the erbium doped nickel zinc
ferrites nanoparticles were either limited, few or simply overcharged. So it can
provide more enthusiasm to an individual to take up this contest and took this topic
for the research paper.
2 Literature review
Currently, owed to its exclusive characteristics, nano type ferrite has been utilized
in many kind of technical branches which are biosensor, magnetic recording,
microwave devices, biomedicine, magnetic drug delivery and catalysis (Thakur et
al., 2017). Iron oxide and rare earth type group of oxide are mainly called ferrite;
these are consisting of composites oxide. The spinel ferrite mainly has chemical
formula of MeFe2O4, and in this formula Me is actually a divalent type metal ion,
which consists of Co+2, Fe+2, Ni+2, Mn+2, Mg+2 etc., (Morelli, n.d.). Soft ferrite is
typically representing magnetic properties of nickel-zinc ferrite (NZF) and zinc
5
ferrite. NZF is a type of functional material which are mostly utilized in internet,
biomedical, communication, anti-electromagnetic interference technology,
electrical appliances and computer circuit (Bazuev et al., 2016; Mattei et al., 2017;
Nag et al., 2018; Shinde et al., 2013).
The researcher N.Boda (Boda et al., 2018) has studied that nickel ferrite synthesis
exposed about the superparamagnetic performance and on the other hand cobalt
ferrite exposed about the soft magnetic performance. Moreover, this type of
material is mostly utilized in soft magnetic production industries. In the ferrite,
magnetism is found due to the spin exchange of direct electron in between the
adjacent type magnetic atoms. The spin ferrite have structural formula which is
shown as [Znx+2Fe1-x+3]A[Me1-x+2 Fe1+x+3 ]BO4 and the subscripts that are present in
their structural formula are (A) represents the tetrahedron and (B) represents the
octahedron as shown in figure 1.
6
For the preparation of ferrites, the following compounds like ferric chloride
hexahydrate (FeCl3.6H2O), sodium hydroxide (NaOH), zinc chloride (ZnCl2),
nickel chloride (NiCl2), anhydrous ethanol and rare earth chloride are required. No
purification is required in these compounds because all chemicals are of analytical
grade. Throughout the experiment deionized water is used. The solutions of NiCl 2
(3 M), ZnCl2 (3 M), ScCl3 (0.3 M) and FeCl3. 6H2O (3 M) were diluted in
deionized water (100 ml) using appropriate amount in stoichiometric ratio and
subsequently mixed the solutions than for 30 minutes stirred it in order to obtain a
homogenous solution. In a magnetic stirrer the mixed homogenous solution was
kept then at 80 oC heated it and continuously stirred the solution. Into the mixture
of salt solution sodium hydroxide (3 M) was added drop by drop.
By the suction filtration process the slurry type substance was obtained which is
dried for one day and one night in drying oven. After that the slurry powder was
grounded and used to perform for further study (Shiwen, n.d.).
7
By X-ray diffraction (XRD) the crystal structures of nanoparticles were inspected.
The X-ray diffractometer instrument (RIGAKUD/max 2500 V) was used for the
structural and compositional analysis of the samples by using Cu-Kα1 having
wavelength of 0.154 nm at room temperature. For the X-ray tube there is some
specifications i.e., the X-ray tube current is 150 mA, the voltage of X-ray tube is
40 kV and scanning angle and scanning speed is 20 o to 90o and 10 o
/min
respectively. Using coupled plasma atomic emission spectrometry (ICP-AES) the
chemical constituents of the formulated ferrites were investigated. By Fourier
transform infrared spectroscopy (FTIR) the measurement of the intrinsic vibrations
of the metal complexes were examined.
For the characterization of elemental analysis of the particles exploited the energy
dispersive spectroscopy (EDS). By exploiting a physical property measurement
system (PPMS-9) i.e., vibrating sample Magnetometer (VSM), the magnetic
examination of the sample was conceded out. Additionally, under the magnetic
field of 2 T the temperature sensitivity of the sample was examined within the
range of 225-400 K (Kaman & Kohout, 2021).
8
considered to be best choice if compared to the bulk ferrites (Guo et al., 2009; K.
Kondo et al., 2012; N. M. K. Kondo et al., 2006), due to of their low eddy current
loss, high permeability and relatively high resistivity (Monitor et al., 2009;
Science, 2009). These magnetic material have the soft properties and easily
crystallize in its spinal structure having a type of (Zn1-xFex) (NixFe2-x) O4, so its
metallic type cation Fe+3/Zn+2 which capture the tetrahedral A sites and other
octahedral B sites is capture by the other metallic cations of Fe +3/Ni+2
(Albuquerque & Macedo, 2000; Cullity & Graham, n.d.).
Over the last few years, a significant importance has given in the synthesis
processes of these substances and therefore has been developed. To the preparation
parameters, starting materials and preparation methodology, the dielectric,
structural and electrical properties of NZFOs are extremely sensitive (Dimri et al.,
2006; Science, 2009). By employing several wet-chemical processes such as
hydrothermal process (Tamaura et al., 1990)(Yutaka et al. 1990), co-precipitation
method (Arulmurugan et al., 2005), microemulsion (Giesche, 2001; Lee et al.,
2005) and sol-gel process (Chatterjee1993.Pdf, n.d.; Chimiche et al., 2004), which
turns in synthesizing the ultrafine powders, though there are many drawbacks in
each of the method. The processes which are stated above have some common
difficulties such as coarser particle size, high calcinations temperature and
chemical inhomogeneity etc., (Dimri et al., 2006; X. Liu et al., 2007). In the
synthesis of mixed ferrites nanomaterials, very lately an aqueous organic gel
method was introduced by Pechini et al. in 1967 and this process accomplished
great significance thus involves the reaction of single or multiple metal ions by
citric acid which is a ploy functional organic acid.
9
along with narrow size distribution. From the decomposition of the ploynuclear
coordination compound, the pure Ni-Zn ferrite nanoparticles have been formed by
using sol-gel auto-combustion method and can be easily scaled up at 180 oC
temperature. For the formation of nanocrystalline, stoichiometric and mixed ferrite
powders, this method considered to be economically eco-friendly and have
reproducible chemical pathway.
The aqueous solution of 1 M Fe(NO3)3. 9H2O, Zn(NO3)2. 6H2O 0.25 and 0.25 M
solution of Ni(NO3)2. 6H2O was firstly formed in 10 mL of deionized water. The
molar ratio of the total nitrate to citric acid turns out to be unity, so the amount of
the citric acid was reserved in such a way. At the temperature of 60 to 80 oC, the
mixture was stirred for 30 min continuously thus the deep brown colored sol was
produced. At this condition, the ethylenediamine (EDA) was added drop by drop
and at a pH of 4.5-5 a semisolid mass was formed from the stirring the mixture.
At temperature of 180 oC the resulting mass was then subjected to in a hot plate
autocombustion for 30 min, then the resulting quantity was then transformed into
brown fluppy ash which was subsequently powdered for furthest structural
characterizations and heat treatment. The schematic diagram for the preparation
method of the nickel zinc ferrite nanoparticles was shown in figure 2.
(Bhattacharjee et al., 2011)
10
Figure: 1 Schematic diagram of the preparation of nickel zinc ferrite
nanoparticles
By the X-ray diffraction technique, the phase purity of the solid solutions was
examined. By field emission scanning electron and high resolution transmission
electron microscopy were performed for the morphological characterizations of the
formulated samples. For the identification of the possible mechanism of the
synthesis method has been done by the characterization using extensive Fourier
transformed infrared spectroscopy.
The electrical properties of the synthesized solid solution which depend upon
composition such as dielectric constant and resistivity of the prepared sample have
been examined. With respect to composition a non-linear variation in the dielectric
permittivity has been examined. The dielectric permittivity and electrical resistivity
of Ni0.5Zn0.5Fe2O4 with respect to room temperature was acquired to be decrease as
the particle size decrease. (Susceptibility, Magnetization and M6ssbauer Studies
of the Mg-Zn Ferrite System, 1986; Taylor et al., 2010)
11
The features of the particular dopant ion like electronic configuration, site
preference and ionic radii specifically control the degree of modification are the
properties of the doped ferrites (Peng et al., 2011). Internal lattice type strain
always produced when the rare earth (RE +) ions are added in the spinel ferrites,
which cause disorderness in the structure (Jacob et al., 2012). That leads to mostly
effects on magnetic, transport and dielectric properties (Avazpour et al., 2016;
Iorgu et al., 2015; Junaid et al., 2016) of substance. The spinal lattice containing
octahedral site of RE+ ions having affinity to cause the Fe+2 ions conduction, which
in turns increase the resistivity (Wu et al., 2015). The lanthanide ions series have
net magnetic moments which is rule by the unpaired type of f-orbital electrons. By
rare earth impurity, the doping of spinel ferrites gives 4f-3d coupling, which in
results of definite changes in the sample regarding its magnetic crystalline
anisotropy.
12
elements but it has greater magnetic moment i.e., 7 µB affects greatly on structural,
transport and magnetic properties of the sample (Ahmad et al., 2014; Kakade et al.,
2016). Therefore, many efforts were done for preparing the doped spinel ferrites
using rare earth (Ahmad et al., 2014; Kakade et al., 2016; Peng et al., 2011),
although the basic hurdle in its synthesis is due to the segregation of its impure
phase i.e., hematite, metal monoxide and orthoferrite (Ahmad et al., 2014; Kakade
et al., 2016; Rahman et al., 2014).
By employing citric acid assisted sol gel auto combustion methodology, there were
many reports on the synthesis of Er3+ doped nickel zinc ferrite nanocomposites.
2.5 Different Methods for the Preparation of Erbium based Nickle Zinc
ferrites nanoparticles
13
i.e., citric acid was added. The ratio among citric acid to metal salt was reserved
2:1. In 10 ml of deionized water the mixture was dissolved and thus the resulting
solution i.e., cationic in nature was formed which then continuously stirred to
increase the homogeneity of the solution.
14
With double distilled water the obtained precipitated particles were washed out
many times in order to clean the impurities and other salt residues. To obtained the
powder form it was further dried at 80 oC. (Shahane et al., 2010)
15
(TEM) (JEOL, JEM-2011), the analysis of the morphology of the samples were
characterized.
To calibrate the spectrometer, a 12 m natural iron foil of high pureness was used.
To attain both low temperature i.e., 5 K and room temperature i.e., 300 K
dependent magnetic hoops (M-H hoops), the samples were also explored by a
superconducting quantum interference device (SQUID) having magnetometer
MPMS XL-7. (Nag et al., 2018)
The mixed metal oxide system Ni0.5Zn0.5Fe2O4 was prepared by two co-
precipitation methods as well as two sol–gel auto combustion methods. In the first
co-precipitation method, calculated amounts of Fe(NO3)3Æ9H2O,
Zn(NO3)2Æ6H2O and Ni (NO3)2Æ6H2O were weighed accurately and dissolved
in doubly distilled water. The precipitation was carried out at a controlled pH of
9.5 using 1:1 NH3 solution. It was then hat 95 C with constant stirring for 4 h
followed by oxidation using 30% H2O2. The precipitated ferrite was washed well,
dried in an air oven at 120 C and crushed well. In the second co-precipitation
method, the precipitation was done by 10 M NaOH using the same procedure as in
the previous method with the exclusion of H2O2 addition. In the first sol–gel auto
16
combustion method, nano particles were produced through the metal nitrate–citrate
gel auto combustion method. i.e., an aqueous solution of citric acid was mixed with
metal nitrate solution; appropriate amount of ammonia solution was added until a
pH of 7 was reached. This solution was then heated on a magnetic stirrer at 90 C
with constant stirring until the resulting gel foams. It was then heated in a mantle at
150 C for spontaneous ignition and the loose powder was then crushed well. In the
second method, the metal nitrates were dissolved in a minimum amount of
ethylene glycol and the rest was the same as explained in the above sol–gel
method. All the ferrite samples prepared were calcined at 550 and 800 C for 4 h
and hereafter are designated as CPA-I, CPA-II, CPS-I, CPS-II, SGC-I, SGC-II
SGE-I and SGE-II, respectively for ferrite samples at 550 and 800 C obtained from
the above methods. The prepared NZF samples were characterized with respect to
phase identification, crystalline size, lattice parameter and bulk density
determination by using a Bruker AXS D8 Advance model X-ray diffractometer
with Cu Ka (1.5406 A˚ ) as a radiation source. The Fourier Transform Infra Red
studies were carried out in KBr medium using Thermo Nicolet, Avatar 370 model
FTIR spectrometer in the range of 400–4000 cm 1 with a resolution of 4 cm1 . The
particle size and morphology of various nanoparticles were confirmed by using a
PHILIPS Model CM 200 Transmission Electron Microscope with a resolution of
2.4 A.
17
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