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International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056
Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072
One Day International Seminar on Materials Science & Technology (ISMST 2017)
4th August 2017
Organized by
Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India
© 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 110
SYNTHESIS & MAGNETIC PROPERTIES OF MAGNESIUM FERRITE
(MgFe2O4) NANOPARTICLES VIA SOL GEL METHOD
1M. Easwari, 2Dr. Sr. S .Jesurani.
1Assistant professor, Dept. of Physics, Thiravium College of Arts & Science for Women, Tamilnadu, India.
*Associate professor, Dept. of Physics, J.A. College for women (Autonomous), Tamilnadu, India.
---------------------------------------------------------------------***---------------------------------------------------------------------
Abstract - Magnesium Ferrite (MgFe2O4) nanoparticles
were prepared by citrate sol-gel method. The structure,
composition and magnetic properties of the gel precursor
characterized by powder SEM, FT-IR and VSM. The
functional groups were analyzed by FT-IR spectrum. XRD
confirmed the spinel cubic structure of MgFe2O4. The
average particle size was calculated approximately in the
range of 20-30 nm. The surface morphology studied by
SEM. The magnetic properties of the samples were
investigated using VSM.
Keywords: Magnesium ferrite nanoparticles, FT-IR,
XRD, SEM, EDAX, VSM.
1. INTRODUCTION
Recent research interests on spinel ferrites are
due to their unique optical, electrical, and magnetic
properties. These characteristics are strongly dependent
on their size, shape, and dispersion [1]. Study of spinel
ferrite MFe2O4 (where M = Fe, Mn, Zn, Co, Mg, Cu, Ni)
nanoparticles has great significance in modern
technologies such as contrast enhancement of magnetic
resonance imaging, high density data storage, and
magnetic carriers for site-specific drugs delivery [2].
Amongst the spinel ferrite families, magnesium ferrite
(MgFe2O4) is a soft magnetic n-type semiconducting
material [3, 4]. The spinel ferrite particles synthesized by
solid-state methods show an assembly of irregular
shapes and agglomerations [5, 6]. Magnesium ferrite
(MgFe2O4) is one of the most important ferrites. It has a
cubic structure of normal spinel-type and is a soft
magnetic n-type semiconducting material, which finds a
number of applications in heterogeneous catalysis,
adsorption, sensors, and in magnetic technologies [7].
Recently, nanostructures of magnetic materials have
received more and more attention due to their novel
material properties that are significantly different from
those of their bulk counter parts [8-12].
A wide variety of methods are being used to
synthesize spinel ferrite nanoparticles including citric
acid combustion method, sol-gel auto combustion
method, hydrothermal method, co-precipitation method,
thermolysis, wet chemical co precipitation technique,
self-propagating and microemulsion [13–17]. Among
these methods sol-gel method [18] is widely used for the
synthesis of nanoparticles of ferrite. This method has the
advantages of simple preparation, cost-effective and
gentle chemistry route resulting in fine and
homogeneous powder.
In the present investigation, MgFe2O4
nanoparticles are synthesized by sol-gel method. The
structure, composition, thermal and magnetic properties
of the gel precursor is characterized by powder XRD (X-
ray diffraction), FT-IR (Fourier transform Infrared
Spectroscope), SEM (Scanning Electron Microscope). The
magnetic properties of the samples were investigated
using VSM (Vibrating Sample Magnetometer).
2. MATERIALS & METHODS
2.1. Materials
Magnesium nitrate [Mg (NO3)2.6H2O], Ferric
nitrate [Fe (NO3)3.9H2O], ethylene glycol [C2H6O2] and
Citric acid [C6H8O7].
2.2. Methods
Magnesium ferrite nanoparticles are prepared
by sol-gel method. A small amount of metal nitrates are
first dissolved in a minimum amount of ethylene glycol.
Chelating agent added to it. The final solution is
magnetically stirred for 4h at room temperature & then
surplus water is removed in a vacuum rotary evaporator
at 60-80°C until a gel is obtained. For about 10h, the
obtained gel is dried in a hot air oven at 100, 150, 250°C
which are labeled as sample A, B & C.
International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056
Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072
One Day International Seminar on Materials Science & Technology (ISMST 2017)
4th August 2017
Organized by
Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India
© 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 111
3. RESULTS & DISCUSSION
3.1. FTIR
As shown in fig.1, 2, 3, the formation of MgFe2O4
structure in the synthesized samples are further
supported by FTIR spectrum. The band 3421 cm-1 could
be attributed the O-H stretching vibration of H2O
absorbed be by the sample. The peak at 2337 cm-1 is
described to H-O-H bending of the absorbed water. The
C=O stretching characteristic peak located at 1667 cm-1
in the PVA red shifts in the composite. At 14553cm-1
there is a significant change in the CH bending band. The
bands with the peak at 572, 462 cm-1 are assigned to the
deformation vibration of Fe-OH groups. The two main
metal-oxygen bands at 559, 466 cm-1 are observed in the
FT-IR spectrum of the synthesized Magnesium ferrite
samples. These two bands are usually assigned to
vibration of ions in the crystal lattices. This indicates the
presence of uniformly distributed ferrite particles.
Fig.1. FTIR for Sample-A.
Fig.2. FTIR for Sample-B.
Fig.3. FTIR for Sample-C.
3.2. XRD
The XRD pattern was compared with the
standard powder diffraction pattern (JCPDS card No.17-
464). The major planes correspond to (200), (311),
(222), (400), (422), (511) were found to be matched
which confirmed the presence of Magnesium ferrite. The
average particle size was calculated from line
broadening using the Debye - Scherrer equation,
D = Kαλ / β cos Ɵ
Where, λ = wavelength of the x-ray radiation.
kα = constant (0.91).
β = full width at half maximum.
θ = diffracting angle.
Fig.4. XRD patterns for Sample-A, B & C
Mg Fe 100
Wed Mar 1915:22:20 2014 (GMT+05:30)
406.94
422.26
438.76
466.17516.78
544.93
1084.44
1323.58
1435.15
1639.88
2337.41
3409.30
-2.0
-1.5
-1.0
-0.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
%T
5001000150020002500300035004000
Wavenumbers (cm-1)
Mg
Wed Jan 2917:31:58 2014 (GMT+05:30)
406.43
559.77
1324.72
1455.11
1667.49
2337.99
3421.35
-0.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
%T
500100015002000250030003500
Wavenumbers (cm-1)
Mg
Wed Jan 2917:31:58 2014 (GMT+05:30)
406.43
559.77
1324.72
1455.11
1667.49
2337.99
3421.35
-0.5
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
%T
500100015002000250030003500
Wavenumbers (cm-1)
International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056
Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072
One Day International Seminar on Materials Science & Technology (ISMST 2017)
4th August 2017
Organized by
Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India
© 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 112
3.3. SEM
Fig.5.SEM for Sample-B
The SEM micrograph of the magnesium ferrite
nanoparticles is shown in Fig.5. It shows that the ferrite
particles are spherical with average crystallite size of ~
20-30 nm.
3.4. VSM
The magnetic hysteresis loop and magnetic
property of the synthesized MgFe2O4 samples are studied
at room temperature using a vibrating sample
magnetometer (VSM) and is shown in Fig.6.
Fig.6. VSM curves for Sample-A, B & C.
The sample exhibits ferromagnetic behavior at
room temperature. The magnetic property of the
material has been known to be dependent on the sample
shape, crystallinity, magnetization direction etc [19]. The
saturation magnetization (Ms), remanent magnetization
(Mr), coercivity (Hc) is 25.4 emug-1, 1.48 emug-1 and 27.7
G for magnesium ferrite nanoparticles at 250°C,
respectively. The saturation magnetization (Ms) of the
sample is close to the reported bulk value, which is due
to the spin canting at the surface of ferrite nanoparticles
[20] and also due to the substitution of a part of Mg2+ in
the octahedral sites by fe2+ with higher magnetic
moment from the reported results it can be seen that
magnetic property are also influenced by the synthesis
process. The influence of this preparation method on
magnetic property is under study.
4. CONCLUSION
The sol-gel method is well suited for the
synthesis of nano-sized MgFe2O4. The powder XRD
reveals the purity of the sample. Average crystallite size
calculated from Scherrer’s equation. FT-IR spectroscopy
is a valuable method to identify the impurity free
nanocrystalline spinel MgFe2O4. SEM image confirmed
that particles have spherical shape. From these results
we conclude that the sol-gel process provides an
interesting synthesis technique with the advantages like
low cost and simple preparation.
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[5].H. Deng, H.Chen and H.Li, “Synthesis of crystal
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International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056
Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072
One Day International Seminar on Materials Science & Technology (ISMST 2017)
4th August 2017
Organized by
Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India
© 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 113
[7]. J. Rockenberger, E.C. Scher and A.P.Alivisatos “A new
nanohydrolytic single-precursor approach to
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nanoparticles”, Chemical Communications, vol.9, no.8,
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controlled magnetic (Cr, Mn, Fe, Co, Ni) oxide
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Synthesis & Magnetic Properties of Magnesium Ferrite (MgFe2O4) Nanoparticles Via Sol Gel Method

  • 1. International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 110 SYNTHESIS & MAGNETIC PROPERTIES OF MAGNESIUM FERRITE (MgFe2O4) NANOPARTICLES VIA SOL GEL METHOD 1M. Easwari, 2Dr. Sr. S .Jesurani. 1Assistant professor, Dept. of Physics, Thiravium College of Arts & Science for Women, Tamilnadu, India. *Associate professor, Dept. of Physics, J.A. College for women (Autonomous), Tamilnadu, India. ---------------------------------------------------------------------***--------------------------------------------------------------------- Abstract - Magnesium Ferrite (MgFe2O4) nanoparticles were prepared by citrate sol-gel method. The structure, composition and magnetic properties of the gel precursor characterized by powder SEM, FT-IR and VSM. The functional groups were analyzed by FT-IR spectrum. XRD confirmed the spinel cubic structure of MgFe2O4. The average particle size was calculated approximately in the range of 20-30 nm. The surface morphology studied by SEM. The magnetic properties of the samples were investigated using VSM. Keywords: Magnesium ferrite nanoparticles, FT-IR, XRD, SEM, EDAX, VSM. 1. INTRODUCTION Recent research interests on spinel ferrites are due to their unique optical, electrical, and magnetic properties. These characteristics are strongly dependent on their size, shape, and dispersion [1]. Study of spinel ferrite MFe2O4 (where M = Fe, Mn, Zn, Co, Mg, Cu, Ni) nanoparticles has great significance in modern technologies such as contrast enhancement of magnetic resonance imaging, high density data storage, and magnetic carriers for site-specific drugs delivery [2]. Amongst the spinel ferrite families, magnesium ferrite (MgFe2O4) is a soft magnetic n-type semiconducting material [3, 4]. The spinel ferrite particles synthesized by solid-state methods show an assembly of irregular shapes and agglomerations [5, 6]. Magnesium ferrite (MgFe2O4) is one of the most important ferrites. It has a cubic structure of normal spinel-type and is a soft magnetic n-type semiconducting material, which finds a number of applications in heterogeneous catalysis, adsorption, sensors, and in magnetic technologies [7]. Recently, nanostructures of magnetic materials have received more and more attention due to their novel material properties that are significantly different from those of their bulk counter parts [8-12]. A wide variety of methods are being used to synthesize spinel ferrite nanoparticles including citric acid combustion method, sol-gel auto combustion method, hydrothermal method, co-precipitation method, thermolysis, wet chemical co precipitation technique, self-propagating and microemulsion [13–17]. Among these methods sol-gel method [18] is widely used for the synthesis of nanoparticles of ferrite. This method has the advantages of simple preparation, cost-effective and gentle chemistry route resulting in fine and homogeneous powder. In the present investigation, MgFe2O4 nanoparticles are synthesized by sol-gel method. The structure, composition, thermal and magnetic properties of the gel precursor is characterized by powder XRD (X- ray diffraction), FT-IR (Fourier transform Infrared Spectroscope), SEM (Scanning Electron Microscope). The magnetic properties of the samples were investigated using VSM (Vibrating Sample Magnetometer). 2. MATERIALS & METHODS 2.1. Materials Magnesium nitrate [Mg (NO3)2.6H2O], Ferric nitrate [Fe (NO3)3.9H2O], ethylene glycol [C2H6O2] and Citric acid [C6H8O7]. 2.2. Methods Magnesium ferrite nanoparticles are prepared by sol-gel method. A small amount of metal nitrates are first dissolved in a minimum amount of ethylene glycol. Chelating agent added to it. The final solution is magnetically stirred for 4h at room temperature & then surplus water is removed in a vacuum rotary evaporator at 60-80°C until a gel is obtained. For about 10h, the obtained gel is dried in a hot air oven at 100, 150, 250°C which are labeled as sample A, B & C.
  • 2. International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 111 3. RESULTS & DISCUSSION 3.1. FTIR As shown in fig.1, 2, 3, the formation of MgFe2O4 structure in the synthesized samples are further supported by FTIR spectrum. The band 3421 cm-1 could be attributed the O-H stretching vibration of H2O absorbed be by the sample. The peak at 2337 cm-1 is described to H-O-H bending of the absorbed water. The C=O stretching characteristic peak located at 1667 cm-1 in the PVA red shifts in the composite. At 14553cm-1 there is a significant change in the CH bending band. The bands with the peak at 572, 462 cm-1 are assigned to the deformation vibration of Fe-OH groups. The two main metal-oxygen bands at 559, 466 cm-1 are observed in the FT-IR spectrum of the synthesized Magnesium ferrite samples. These two bands are usually assigned to vibration of ions in the crystal lattices. This indicates the presence of uniformly distributed ferrite particles. Fig.1. FTIR for Sample-A. Fig.2. FTIR for Sample-B. Fig.3. FTIR for Sample-C. 3.2. XRD The XRD pattern was compared with the standard powder diffraction pattern (JCPDS card No.17- 464). The major planes correspond to (200), (311), (222), (400), (422), (511) were found to be matched which confirmed the presence of Magnesium ferrite. The average particle size was calculated from line broadening using the Debye - Scherrer equation, D = Kαλ / β cos Ɵ Where, λ = wavelength of the x-ray radiation. kα = constant (0.91). β = full width at half maximum. θ = diffracting angle. Fig.4. XRD patterns for Sample-A, B & C Mg Fe 100 Wed Mar 1915:22:20 2014 (GMT+05:30) 406.94 422.26 438.76 466.17516.78 544.93 1084.44 1323.58 1435.15 1639.88 2337.41 3409.30 -2.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 %T 5001000150020002500300035004000 Wavenumbers (cm-1) Mg Wed Jan 2917:31:58 2014 (GMT+05:30) 406.43 559.77 1324.72 1455.11 1667.49 2337.99 3421.35 -0.5 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 %T 500100015002000250030003500 Wavenumbers (cm-1) Mg Wed Jan 2917:31:58 2014 (GMT+05:30) 406.43 559.77 1324.72 1455.11 1667.49 2337.99 3421.35 -0.5 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 %T 500100015002000250030003500 Wavenumbers (cm-1)
  • 3. International Research Journal of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 112 3.3. SEM Fig.5.SEM for Sample-B The SEM micrograph of the magnesium ferrite nanoparticles is shown in Fig.5. It shows that the ferrite particles are spherical with average crystallite size of ~ 20-30 nm. 3.4. VSM The magnetic hysteresis loop and magnetic property of the synthesized MgFe2O4 samples are studied at room temperature using a vibrating sample magnetometer (VSM) and is shown in Fig.6. Fig.6. VSM curves for Sample-A, B & C. The sample exhibits ferromagnetic behavior at room temperature. The magnetic property of the material has been known to be dependent on the sample shape, crystallinity, magnetization direction etc [19]. The saturation magnetization (Ms), remanent magnetization (Mr), coercivity (Hc) is 25.4 emug-1, 1.48 emug-1 and 27.7 G for magnesium ferrite nanoparticles at 250°C, respectively. The saturation magnetization (Ms) of the sample is close to the reported bulk value, which is due to the spin canting at the surface of ferrite nanoparticles [20] and also due to the substitution of a part of Mg2+ in the octahedral sites by fe2+ with higher magnetic moment from the reported results it can be seen that magnetic property are also influenced by the synthesis process. The influence of this preparation method on magnetic property is under study. 4. CONCLUSION The sol-gel method is well suited for the synthesis of nano-sized MgFe2O4. The powder XRD reveals the purity of the sample. Average crystallite size calculated from Scherrer’s equation. FT-IR spectroscopy is a valuable method to identify the impurity free nanocrystalline spinel MgFe2O4. SEM image confirmed that particles have spherical shape. From these results we conclude that the sol-gel process provides an interesting synthesis technique with the advantages like low cost and simple preparation. REFERENCES [1].J.Hu.T.W.Odom, and C.M.Liber, “chemistry and physics in one dimension: synthesis and Properties of nanowire and nanotubes” Chemical research, Vol.32, no.5, pp. 435-445, 1999. [2].Z.L.Wang, Y.Liu and Z.Zhang, Handbook of nanophase and nanostructured materials, vol.3, Kluwer Academic/Plenum, New York, NY, USA, 2003. [3].R.J.Willey, P.Noirclerc and G.Busca, “Preparation and characterization of magnesium chromite and magnesium ferrite aero gels”, Chemical Engineering Communications, vol.123, pp. 1-16. [4].N.Sivakumar, A.Narayanasamy, J.M.Greneche, R.Murugaraj and Y.S.Lee, “Electrical and magnetic behavior of nanostructured MgFe2O4 spinel ferrite”, Journal of Alloys and Compounds, vol.504, no.2, pp. 395-402, 2010. [5].H. Deng, H.Chen and H.Li, “Synthesis of crystal MFe2O4 (M=Mg, Cu, Ni) microsperes”, Materials chemistry and physics, vol101, no.2-3, pp 509-513, 2007. [6].S.H.Yu and M.Yoshimura, “Direct fabrication of ferrite MFe2O4 (M=Zn, Mg)/Fe composite thin films by soft solution processing”, Chemistry of Materials, vol.12, no.12, pp. 3805-3810, 2000.
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