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Volume 10, Issue 4, 2020, 6015 - 6019
ISSN 2069-5837
Biointerface Research in Applied Chemistry
www.BiointerfaceResearch.com
https://doi.org/10.33263/BRIAC104.015019
Original Research Article
Open Access Journal
Received: 24.03.2020 / Revised: 23.04.2020 / Accepted: 24.04.2020 / Published on-line: 29.04.2020
Structural, morphological, and magnetic properties of copper zinc cobalt ferrites systems
nanocomposites
Arthur Charles Prabakar 1, Govindarasu Killivalavan 1, Dhananjayan Sivakumar 2, K. Chandra Babu
Naidu 3, Balaraman Sathyaseelan 4,* , Krishnamoorthy Senthilnathan 5, Iruson Baskaran 6, Elayaperumal
Manikandan 7, B. Ramakrishna Rao 8, M.S.S.R.K.N. Sarma 3 , A. Ratnamala 8
1
Research and Development Center, Bharathiar University, Coimbatore-641046, India
Department of Physics, Sree Krishna College of Engineering,Unai,Anaicut-632101,Tamilnadu,India
3
Department of Physics, GITAM Deemed to be University, Bangalore-562163, Karnataka, India
4
Department of Physics, University College of Engineering Arni , Anna University Chennai, Arni 632326, Tamil Nadu, India
5
Photonics Division, School of Advanced Sciences, VIT University, Vellore, 632014, Tamil Nadu, India
6
Department of Physics Arignar Anna Government Arts College, Cheyyar 604407, Tamil Nadu, India
7
Department of Physics, Thiruvalluvar University College of Arts and Science, Thennangur Village, Vandavasi Taluk, Tiruvannamalai District 604408, India
8
Department of Chemistry, GITAM Deemed to be University, Bangalore-562163, Karnataka, India
*corresponding author e-mail address: bsseelan03@gmail.com | Scopus ID 35734996700
2
ABSTRACT
In this study, by the method of co-precipitation with PEG as surfactant as agent nanocomposite of the Copper Zinc Cobalt ferrites systems
(CuZnCoFO NCs) are prepared. The X-ray diffraction (XRD), transmission electron microscopy, and field emission scanning electron
microscopy of the samples are carried out. To analyse the magnetic measurements the samples are subjected to the vibrating sample
magnetometer (VSM). The results of the paramagnetic properties formed out of chemical precipitation method are effective at room
temperature. These ferrite system nanoparticles with magnetic fields could have effective application. The photocatalyst activity when
annealed at 600ºC at 2h NPs is also evaluated by Methylene Blue degradation when exposed to ultraviolet light irradiation.
Keywords: Ferrite, nanocomposite, XRD, TEM, magnetic properties.
1. INTRODUCTION
Spinel ferrite particles in nano dimension exhibit appealing
and extraordinary properties compared to their bulk samples [1].
The reduction of organic dopants through the Photocatalytic
degradation on the surface of semiconductor is the most promising
and reliable technique.In comparison with iron oxide many large
catalytic phenomenon. The obtained ferrite systemwas also ferrite
nanoparticles performperoxidase-like activity towards Mg, Co, and
Cu ferrite system which yield excellent catalysts and possess
excellent potential with chemical compositions that leads doping of
non-metal [6-8], transition metal [9, 10] and noble metal [11-13].
Also it is possible to develop unique properties to the
nanocomposites by different ferrite oxides with spinel structures
[14]. Spinel structures have the general formula AB2O4, with A as
a divalent cation (Co2+, Zn2+) and B as a trivalent cation (Fe3+,
Cr3+) [15-16]. Ferrites are spinel structure in which B sites are
occupied with Fe3+ cations to form ferromagnetic compound.
The Spinel ferrites (MFe2O4) perform extremely well during
advanced oxidation processes (AOPs), due to their narrow energy
band gap (2 eV) [19], and is also used to alter the properties of the
catalyst by using a metal with strong magnetic properties.
In this way, the catalyst is easily recovered during
wastewater management [20]. Moreover, ferrites in the spinel
structure, formed by multiple metals, decide the permanent
properties of the catalyst [21].
He et al. reported the photo degradation of Methylene blue
dye using catalyst Zn1-xCoxFe2O4 [22], due to its strong magnetic
field influence the Zn and Co-ferrite phase and narrow energy band
gap. The nanoparticles have a wide applications that are prepared
by methods like, co-precipitation [23], ultrasound-assisted
emulsification [24], hydrothermal [25], sol-gel [26] and microwave
solid - state techniques [27]. Among the various type of spinel
ferrite Nanoparticles, zinc ferrite nanoparticles exhibit endearing
magnetic properties [28] and its performance mostly depends on
their stoichiometric ratio and structures (micro), which vary by the
methods of synthesizing.
In the present work, the preparation, depiction, evaluation
and photo catalytic performances of the new removal catalyst
Copper Zinc Cobalt ferrites systems (CZCFO NCs) for the removal
of Methylene blue dye using solar irradiation is studied. To achieve
the desired properties and to ensure strong magnetic properties of
ferrites systems Copper Zinc Cobalt's unification was made.
2. MATERIALS AND METHODS
2.1. Material Synthesis.
The sample is meticulously prepared. The characteristic
behaviour of the nanocomposites has great impact on the
preparation process. [29]. Ferric nitrate (98%), cupric nitrate
(99.5%), zinc nitrate (96%), cobalt nitrate (99%), salts are taken
and the required sample is arrived by modifying the co-precipitation
method.
Two solutions of molarity 0.1 are mixed well using a stirrer
maintained at a temperature of 80ºC until the mixture turns into dark
brown. Polyethylene glycol oxide powder of 0.2 g is added gently
Page | 6015
Arthur Charles Prabakar, Govindarasu Killivalavan, Dhananjayan Sivakumar, K. Chandra Babu Naidu, Balaraman
Sathyaseelan, Krishnamoorthy Senthilnathan, Iruson Baskaran, Elayaperumal Manikandan, B. Ramakrishna Rao,
M.S.S.R.K.N. Sarma, A. Ratnamala
to the product in order basicity; excess of NH3 is later added. The
extracted paste is sintered in an oven at 150ºC for 24 h. Then the
prepared sample is annealed at temperature 500 and 600º C under
thermal control which is finally well ground.
2.2. Instrumentation and Apparatus.
The structure and phase purity of Copper Zinc Cobalt ferrites
systems(CZCFO NCs)Nano composite was observed by X-ray
powder Diffractometer. The morphology and selected area electron
diffraction pattern are analyzed by the transmission electron
microscopy. In addition Copper Zinc Cobalt ferrites systems
(CZCFO NCs) nanocomposites photo catalytic activity was
examined through MB in UV light irradiation by photoreactor
(HML MP88,).
Fourier transform infrared spectra (FTIR) of Copper Zinc
Cobalt Ferrites Systems (CZCFO NCs) nanocomposites were
developed in the range of 2000 – 400 cm-1 wavenumber. For
improved physical and magnetic character, the sample is annealed
at 600ºC sample and analysed through Vibrating Sample
Magnetometer.
3. RESULTS
3.1. Structure and crystalline nature of the obtained copper zinc
cobalt ferrites systems (CZCFO NCs) nanocomposite.
Figure 1 exhibits that the XRD pattern of the
nanocomposites at room temperature possesses a cubic spinel
structure [29]. In the XRD pattern the intensity of (311) reflections
is strong, indicating the preferred orientation along the (311)
direction. The other peaks (111), (200),(220), (400), (411), (422)
and (511) are also observed.
3.2. Microstructural analysis through scanning electron
microscopy (SEM) and fundamental attributes of the copper
zinc cobalt ferrites systems (CZCFO NCs) Nano composite.
Figures 2 show the SEM images of Copper Zinc Cobalt
ferrites systems (CZCFO NCs) Nano composites. The SEM images
emphasize the collection of particles with some residue. Porosity is
formed at the junctions. It could be observed from the graph that the
grains of the Zn-Cu –Co are rigid and paves for oxygen adsorption
on its surface.
Figure 2. SEM images of copper zinc cobalt ferrites systems (CZCFO
NCs) nanocomposites at (a) as-prepared(b) annealed at 500ºC(c) annealed
at 600ºC.
Figure 1. Powder XRD of copper zinc cobalt ferrites systems (CZCFO
NCs) nanocomposites.
The X-ray diffraction also confirms the fcc spinel structure
with a single phase for all the samples, and the broad lines
acknowledge the nano size of the samples. The estimated final
contents agree with the initial ratio and the broad lines acknowledge
the nano size of the samples. From the (3 1 1) plane using Debye–
Scherrer formula, the particles size is measured.
During TEM imaging the EDX spectra were recorded at
multiple positions of the sample to confirm the chemical
constituents of the (CZCFO NCs) nanocomposites (Fig 3). The
chemical attributes match with the experimental data. The
stoichiometric proportions of Cu, Co, Zn, Fe, and O elements are
identical with the ferrite crystallites in the sample. The presence of
Na arises from the grid, supports carbon film. The EDX for the
heated sample also exhibits synonyms composition.
All these studies acknowledge that the synthesized material
obtained by co-precipitation protocol were particles of (CZCFO
NCs) nanocomposites.
Page | 6016
Structural, morphological, and magnetic properties of copper zinc cobalt ferrites systems nano composites
and (440) planes. The sample once again confirms the ED profile
analysis.
3.4. FTIR study of copper zinc cobalt ferrites systems (CZCFO
NCs) nanocomposite.
The extensive metal-oxygen bands are shown by the FTIR
spectra (Fig-5). The vibration of metal in tetrahedral site has wave
number in the range 400 cm-1 to 500 cm-1. The bands in the range
of 500 cm-1 to 600 cm-1 are identified as octahedral stretching. The
Mtetra ↔ O bands are observed at 478 cm-1,509 cm-1, 586 cm-1
and 393 cm-1. The absorption bands found at 3404cm-1 indicates
the presence of adsorbed water on the surface of the ferrite nano
particles.
Figure 3. EDX spectra of Copper Zinc Cobalt Ferrites Systems (CZCFO
NCs) Nanocomposites at (a) annealed at 600ºC.
The chemical constituents of the composites were also
viewed by an energy dispersive spectroscopy (EDX). The Na, O,
Zn, Cu, Co and Fe peaks in EDX spectra confirm the presence of
sodium, oxygen, Zinc, copper, cobalt and ferrite system.
3.3. Morphological study of the copper zinc cobalt ferrites
systems (CZCFO NCs) nanocomposite by transmission electron
microscopy and selected area electron diffraction (SAED).
The morphology and shape of the nanocomposite were
examined. When examined using high-resolving transmission
electron microscopy due to nano size, single-field the particles are
permanently magnetized and experience a magnetic moment
proportional to their volume. The particles with size less than 15nm
are grouped. After crystallinity, the sample with cubic spinel crystal
structure confirms the electron diffraction (ED) profile. (Fig.4).
Figure 5. FTIR spectra of copper zinc cobalt ferrites systems (CZCFO
NCs) nanocomposites.
Figure 6. Copper zinc cobalt ferrites systems (CZCFO NCs)
nanocomposites annealed at 600⁰C under UV-light irradiation (a)
Absorption of MB solution during the photo degradation (b) Photo
degradation percentage.
Figure 4. TEM images of copper zinc cobalt ferrites systems (CZCFO
NCs) Nano composites (a) annealed at 600ºC (b) SAED.
The selected area electron diffraction (SAED) picture of the
sample estimated the d-spacing as 2.541 Å indicates that the initial
concentric ring corresponds to (311) plane of Copper Zinc Cobalt
ferrites systems (CZCFO NCs) nanocomposites. (JCPDS powder
diffraction) Similarly, other fringes were assigned as (422) (511)
3.5. Photocatalytic analysis of copper zinc cobalt ferrites
systems (CZCFO NCs) Nano composite
The absorbance versus wavelength graph and degradation
efficiency with respect to time of (CZCFO NCs) nano composites
during photocatalytic degradation of MB dye under UV light
irradiation is shown in Fig.6. Thirty (30) mg of Copper Zinc Cobalt
ferrites systems (CZCFO NCs) nano composites catalyst was
dispelled in 10 ppm of MB dye and photo degradation was
evaluated with 10 mg/L. Using photochemical reactor, the solution
was irradiated by UV radiation and from the resultant, 2 mL were
withdrawn at every 20 mins intervals in 300 mins duration.
The photo degradation of the collected aqueous solution was
measured using a UV - Visible spectrometer [31]. Generally light
absorbing catalyst generate electron-hole pair which produce H and
O2– ions at the surface of the catalyst. The degradation efficiency
of MB under UV light irradiation is determined to be 72% with
enhanced time interval.
3.6. Magnetic parameters of copper zinc cobalt ferrites systems
(CZCFO NCs) nanocomposite at room temperature.
Page | 6017
Arthur Charles Prabakar, Govindarasu Killivalavan, Dhananjayan Sivakumar, K. Chandra Babu Naidu, Balaraman
Sathyaseelan, Krishnamoorthy Senthilnathan, Iruson Baskaran, Elayaperumal Manikandan, B. Ramakrishna Rao,
M.S.S.R.K.N. Sarma, A. Ratnamala
The hysteretic loop obtained in fig.7. reveals the magnitude found to be greater than 5 the sample is considered to be in single
of the magnetic features such as magnetic saturation (Ms), magnetic domain. If the squareness is smaller than 5, the material
coercivity (Hc) and remanence (Mr) for the prepared synthesized has multiple fields [33,34]. The sample in our project
nanocomposites. The results exhibit that the samples having smaller has squareness less than 5.
grains are estimated to have low coercivity, and vice versa. The size
may be the general reason for the reduction in the coercivity of the
ferrites system [30, 31]. It can be noticed the value of coercivity
(Hc) of the ferrite samples, thereby indicates that these materials are
soft magnetic materials.
The reason for the reduction in saturation magnetization is
due to the movement of ferric ions from B to A region [32]. In our
study ‘Ms’ magnetic saturation (36.818 emu/g) and ‘Hc’ coercivity
values (99.738 G) found to be high and the value of Hc seems to be
low. Hence the synthesized Copper Zinc Cobalt Ferrites Systems
(CZCFO NCs) Nanocomposites are apt for low core losses on
Figure 7. Magnetic hysteresis characterization of copper zinc cobalt
transformers.
ferrites systems (CZCFO NCs) nano composites.
The value of Squareness of Copper Zinc Cobalt ferrites
systems (CZCFO NCs) is estimated to be 0.1. If the ratio Mr/Ms is
4. CONCLUSIONS
The Spinel Copper Zinc Cobalt ferrites systems (CZCFO
NCs) Nanocomposites were carefully prepared by chemical
precipitation method with necessary precautions. The cubic inverse
spinel structures of the prepared sample were confirmed by X-ray
diffraction. The crystalline nature of the nanocomposites is
acknowledged by (SAED) profile. The specific absorption rate is
found to be inversely proportional to the concentration of the
sample. The degradation efficiency of MB, under UV light is 72%
with an increase in time duration.
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