In this paper, the structural properties of nano manganese ferrite are synthesized by using environmental friendly co-precipitation method is reported. The structural parameters such as the lattice constant, average crystallite size (D), texture coefficients (TC), lattice strain (ε) and dislocation density (ρ) have been determined using X-ray diffraction data

Kapatkar, S.B.

Mathad, S.N.

Yattinahalli, S.S.

Journal of Nano- and Electronic Physics

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 7 No 4, 04096(3pp) (2015) Том 7 № 4, 04096(3cc) (2015) 
 
 
2077-6772/2015/7(4)04096(3) 04096-1  2015 Sumy State University 
Synthesis and Structural Characterization of Nanomanganese Ferrites 
 
S.S. Yattinahalli1, S.B. Kapatkar*, S.N. Mathad1 
 
1 Dept. of Physics, K.L.E. Institute of Technology, Hubballi-30, Karnataka, India 
2 Dept. of Physics, B.V.B. College of Engineering and Technology, Hubballi-31, Karnataka, India 
 
 (Received 24 June 2015; published online 24 December 2015) 
 
In this paper, the structural properties of nano manganese ferrite are synthesized by using environ-
mental friendly co-precipitation method is reported. The structural parameters such as the lattice con-
stant, average crystallite size (D), texture coefficients (TC), lattice strain (ε) and dislocation density () 
have been determined using X-ray diffraction data. 
 
Keywords: Nanoferrites, Spinel structure, Co-precipitation method, Cubic, Structural analysis. 
 
 PACS numbers: 61.46, 75.50Gg, 61.05.cp, 81.20.Fw 
 
 
                                                                
* sbkbvb@gmail.com 
1. INTRODUCTION 
 
The semiconductor spinel ferrite will have the 
chemical formula as AB2O4 (where A  divalent metal 
ion like Ni, Mn, Zn, etc and B  Iron metal ion Fe2 + and 
Fe3 +) and many studies have focused on the synthesis 
of nanomaterials because of extensive applications due 
to their novel properties. Magnetite and spinel ferrite 
nanocrystals are regarded as two of the most important 
inorganic nanomaterials because of their electronic, 
optical, electrical, magnetic, and catalytic properties, 
all of which are different from the properties of their 
bulk counterparts. [1-2] Among spinel ferrites, manga-
nese ferrite (MnFe2O4) nanoparticles are very im-
portant because they have proven to be useful in many 
magnetic applications, such as recording media devices, 
drug delivery, ferrofluid, biosensors, and contrast-
enhancement agents for MRI technology[3-4]. Also find 
extensive applications in microwave devices, radar, 
catalysis and magnetic refrigeration systems [5]. Fer-
rites are synthesized by several methods like ceramic 
method [6], chemical methods, solvothermal method 
[7], microwave combustion method [8], thermal treat-
ment method, sol-gel Method [9-10], EDTA-assisted 
hydrothermal method [11], oxalate co-precipitation 
technique [12]. Thus Chemical synthesis routes play a 
crucial role in designing the final product and also they 
are better and less cumbersome for the production of 
fine grained mixed oxide products. 
In this present work, we report the synthesis of 
nano manganese ferrite by environmental frieldly, low 
cost co precipitation method. The structural infor-
mation of manganese ferrite powder is done by XRD 
characterization. The current work also reports the 
Texture analysis (preferential orientation of planes), x 
ray density and crystallite size of manganese ferrite. 
 
2. EXPERIMENTAL 
 
2.1 Materials Method 
 
The manganese ferrite in nanosize is synthesized by 
environmental friendly and low cost chemical co-
precipitation method by choosing the AR grade precur-
sors like manganese chloride(MnCl2 .4H2O 99.5 %, Titan 
Biotech Ltd.), Iron chloride(FeCl3 98 %, Titan Biotech 
Ltd.). These precursors are weighed and mixed in de-
sired stiochiometric ratio in distilled water. The mixer is 
stirred for nearly one hour to get clean solution. Drop 
wise ammonia (NH3 25 %, extra pure Sp. gr. 0.91, 
SDFCL) is added to this solution for maintaining pH and 
again stirred for one hour. The reddish solution contains 
precipitate which is filtered to get the manganese ferrite 
using AR grade filter paper. The paste from precipitate 
is dried at room temperature and calcined around 800 C 
in muffle furnace for 5 hr which will yield the manga-
nese ferrite in nanosize. The process of synthesis of nano 
manganese ferrite by co precipitation method is sche-
matically as shown in Figure 1. The synthesized nano 
manganese ferrite is characterized by using Bruker AXS 
D8 Advance instrument (  1.5406 Å, detector Si(Li) 
PSD from STIC, Cochin) for XRD characterization. 
 
 
 
Fig. 1 – Schematic Representation of Synthesis of Nano-
manganese ferrite 
 
3. EXPERIMENTAL RESULTS 
 
The cubic spinel structure of nano manganese fer-
rite is confirmed by X-ray diffraction pattern as shown 
 S.S. YATTINAHALLI, S.B. KAPATKAR, S.N. MATHAD J. NANO- ELECTRON. PHYS. 7, 04096 (2015) 
 
 
04096-2 
in Fig. 2.The X-ray diffraction pattern is indexed by the 
JCPDS card no (10-0319, 74-2403). The crystallite size 
of the nano manganese can be calculated using the De-
bye-Scherer equation [13] as shown in equation (1). 
 
 
0.9
cos
D

 
  (1) 
 
where  is the wavelength of used radiation,  is the 
full width half maximum (FWHM) of diffraction peak, 
and  is the Bragg angle. 
The average lattice parameter 'a' of nano manga-
nese ferrite found to be 8.63 Å and average crystallite 
size found to be 42 nm, also the crystallite size for (311) 
plane at glancing angle(2θ) is 36.83 nm. The measured 
values of d are in good agreement with the JCPDS card 
no 10-0319, 74-2403 as shown in Table 1. Table 2 
shows the average crystallite size, average lattice pa-
rameter, and volume of the nano manganese ferrite. 
 
 
 
Fig. 2 – X-ray Diffraction pattern of the Nano manganese ferrite 
 
Table 1 – Miller indices and lattice parameter 
 
d(obsverved) d(standard) δd (hkl) a (Å) 
2.66 2.58 0.08 (311) 8.82 
2.48 2.46 0.02 (222) 8.59 
2.17 2.13 0.04 (400) 8.68 
1.82 1.74 0.08 (422) 8.92 
1.67 1.64 0.03 (511) 8.68 
1.47 1.5 0.03 (440) 8.32 
1.44 1.44 0.00 (531) 8.52 
1.30 1.3 0.00 (533) 8.52 
1.25 1.23 0.02 (444) 8.66 
 
X-ray density (dx) was calculated by using the for-
mula [14] as shown in equation (2) 
 
 
2
8M
dx
Na
  (2) 
 
where M is the molecular weight of the nano manga-
nese ferrite, N is the Avogadro's number and a is the 
lattice parameter. The X-ray density of nano manga-
nese ferrite found to be 4.76 gm/cm3. 
The lattice strain is defined as the deformation of an 
object divided by its effective length. This lattice strain is 
widely utilized in material science which can be calcu-
lated by using the formula as shown in the equation (3) 
 
cos
4
 
   (3) 
 
 
 
Fig. 3 – Graph of a versus d 
 
Table 2 – Average lattice parameter and Crystallite size 
 
a (Å) a3 (Å3) D (nm) 
8.63 642.74 42 
 
Also the dislocation density can be calculated by us-
ing the formula as indicated in equation (4) 
 
 
2
1
D
   (4) 
 
The lattice strain and dislocation density for nano 
manganese ferrite found to be 0.082 and 7.37  1014 
respectively. 
Texture is perceived in almost all engineered mate-
rials which can have a great influence on properties of 
materials. Diffraction patterns from samples contain-
ing a random orientation of crystallites have predicta-
ble relative peak intensities. Texture frequently repre-
sents a pole figure, in which a defined axis (crystallo-
graphic) from each of a representative number of crys-
tallites is mapped in a stereographic projection [15]. 
The information regarding degree of orientation of the 
crystal plane is obtained from the calculation of texture 
co-efficient (TC) using the formula [16] as indicated in 
equation (5) 
 
  
   
   
0
0
/
/
I hkl I hkl
TC hkl n
I hkl I hkl


 (5) 
 
where I and I0 are the observed and standard intensi-
ties and n is the number of reading obtained. 
In amorphous solids the crystallites are oriented in 
random, but each grain in a polycrystalline aggregate 
normally has a crystallographic orientation different 
from that of its neighbors that is in polycrystalline like 
metal oxide the crystals are oriented in particular 
planes. Hence the texture analysis is carried out by 
using diffraction technique to know the preferential 
orientation of the crystallite. So the texture analysis of 
material is very important factor to study the chemical, 
mechanical and physical properties of material. From 
the texture analysis the grain growth is observed at 
miller indices (311) plane is more dominant 
(TC(hkl)  1.56).The detailed TC(hkl) of all plains has 
been tabulated in Table 3. 
 SYNTHESIS AND STRUCTURAL CHARACTERIZATION… J. NANO- ELECTRON. PHYS. 7, 04096 (2015) 
 
 
04096-3 
Table 3 – Texture Coefficient of all planes of MnFe2O4 
 
hkl (311) (222) (400) (422) (522) (440) (531) (533) 
TC(hkl) 1.56 1.38 0.21 0.87 0.64 1.46 1.47 0.45 
 
4. CONCLUSION 
 
Nanosized manganese ferrite has been synthesized 
by cost effective and simple co-precipitation method. 
Synthesized nano manganese crystals had a cubic spinel 
structure with average lattice parameter a  8.63 Å and 
average crystallite size D  42 nm. Preferential orienta-
tion of grains in the (311) plane is predominant and lat-
tice strain and dislocation density for the same plane 
found to be 0.082 and 7.37  1014. Nano manganese fer-
rite may find its application in microwave devices, high 
capacity information storage, water treatment, sensors, 
inductor cores, and related implementations. 
 
ACKNOWLEDGEMENTS 
 
One of the authors, Suresh B. Kapatkar, gratefully 
acknowledges Management, and Principal B.V.B. Col-
lege of Engineering and Technology, Hubballi, for 
providing financial assistance under capacity building 
scheme. S.S. Yattinahalli is grateful to Management 
and Principal K.L.E. Institute of Technology, Hubballi, 
and all the authors are grateful to the Director, Sophis-
ticated Analytical Instruments Facility STIC, Cochin, 
for immediate help in characterization. 
 
REFERENCES 
 
1. S. Singhal, T. Namgyal, S. Bansal, K. Chandra, J. Electro. 
Anal. Appl. 2, 376 (2010). 
2. S.G. Dahotre, L.N. Singh, Arch. Phys. Res. 2 No 1, 81 
(2011). 
3. M.G. Naseri, E.B. Saion, H.A. Ahangar, M. Hashim, 
H.A. Shaari, J. Magn. Magn. Mat. 323, 1745 (2011). 
4. H. Yang, C. Zhang, X. Shi, H. Hu, X. Du, Y. Fang, Y. Ma, 
H. Wu, S. Yang, Biomaterials 31, 3667 (2010).  
5. Y.M.Z. Ahmed, Ceram. Int. 36, 969 (2010). 
6. S.A. Mazen, N.I. Abu-Elsaad, Condens. Matt. Phys. 2012, 
ID 907257 (2012). 
7. P. Guoa, G. Zhang, J. Yu, H. Li, X.S. Zhao, Colloid. Surf. 
A: Physicochem. Eng. Aspects 395, 168 (2012). 
8. M. Kooti, A. Naghdi Sedeh, Scientia Iranica 19 No 3, 930 
(2012). 
9. K.P. Chae, W.O. Choi, J.C. Lee, B.S. Kang, S.H. Choi. J. 
Mag. 18 No 1, 21 (2013). 
10. S.R. Kulkarni, Arch. Phys. Res. 3 No 2, 116 (2012). 
11. H. Kavas, N. Kasapoglu, A. Baykal, Y.H. Koseoglu, Chem. 
Paper. 63 No 4, 450 (2009). 
12. S. Kumar, T.J. Shinde, P.N. Vasambekar, Adv. Mat. Lett. 
4 No 5, 373 (2013). 
13. S.S. Yattinahalli, S.B. Kapatkar, N.H. Ayachit, 
S.N. Mathad, Int. J. Self-Propag. High-Temp. Synth. 22 
No 3, 147 (2013). 
14. A.T. Pathan, S.N. Mathad, A.M. Shaikh, Int. J. Self-
Propag. High-Temp. Synth. 23 No 2, 112 (2014). 
15. S.N. Mathad, V. Puri, Int. Scholarly Res. Notice. 2014, ID 
683986 (2014). 
16. T. Mahalingam, V. Dhanasekaran, R. Chandramohan, 
Jin-Koo Rhee, J. Mater. Sci. 47, 1950 (2012). 
 


Synthesis and Structural Characterization of Nanomanganese Ferrites

Electronic Sumy State University Institutional Repository

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ Vol. 7 No 4, 04096(3pp) (2015) Том 7 № 4, 04096(3cc) (2015)   2077-6772/2015/7(4)04096(3) 04096-1  2015 Sumy State University Synthesis and Structural Characterization of Nanomanganese Ferrites  S.S. Yattinahalli1, S.B. Kapatkar*, S.N. Mathad1  1 Dept. of Physics, K.L.E. Institute of Technology, Hubballi-30, Karnataka, India 2 Dept. of Physics, B.V.B. College of Engineering and Technology, Hubballi-31, Karnataka, India   (Received 24 June 2015; published online 24 December 2015)  In this paper, the structural properties of nano manganese ferrite are synthesized by using environ-mental friendly co-precipitation method is reported. The structural parameters such as the lattice con-stant, average crystallite size (D), texture coefficients (TC), lattice strain (ε) and dislocation density () have been determined using X-ray diffraction data.  Keywords: Nanoferrites, Spinel structure, Co-precipitation method, Cubic, Structural analysis.   PACS numbers: 61.46, 75.50Gg, 61.05.cp, 81.20.Fw                                                                   * sbkbvb@gmail.com 1. INTRODUCTION  The semiconductor spinel ferrite will have the chemical formula as AB2O4 (where A  divalent metal ion like Ni, Mn, Zn, etc and B  Iron metal ion Fe2 + and Fe3 +) and many studies have focused on the synthesis of nanomaterials because of extensive applications due to their novel properties. Magnetite and spinel ferrite nanocrystals are regarded as two of the most important inorganic nanomaterials because of their electronic, optical, electrical, magnetic, and catalytic properties, all of which are different from the properties of their bulk counterparts. [1-2] Among spinel ferrites, manga-nese ferrite (MnFe2O4) nanoparticles are very im-portant because they have proven to be useful in many magnetic applications, such as recording media devices, drug delivery, ferrofluid, biosensors, and contrast-enhancement agents for MRI technology[3-4]. Also find extensive applications in microwave devices, radar, catalysis and magnetic refrigeration systems [5]. Fer-rites are synthesized by several methods like ceramic method [6], chemical methods, solvothermal method [7], microwave combustion method [8], thermal treat-ment method, sol-gel Method [9-10], EDTA-assisted hydrothermal method [11], oxalate co-precipitation technique [12]. Thus Chemical synthesis routes play a crucial role in designing the final product and also they are better and less cumbersome for the production of fine grained mixed oxide products. In this present work, we report the synthesis of nano manganese ferrite by environmental frieldly, low cost co precipitation method. The structural infor-mation of manganese ferrite powder is done by XRD characterization. The current work also reports the Texture analysis (preferential orientation of planes), x ray density and crystallite size of manganese ferrite.  2. EXPERIMENTAL  2.1 Materials Method  The manganese ferrite in nanosize is synthesized by environmental friendly and low cost chemical co-precipitation method by choosing the AR grade precur-sors like manganese chloride(MnCl2 .4H2O 99.5 %, Titan Biotech Ltd.), Iron chloride(FeCl3 98 %, Titan Biotech Ltd.). These precursors are weighed and mixed in de-sired stiochiometric ratio in distilled water. The mixer is stirred for nearly one hour to get clean solution. Drop wise ammonia (NH3 25 %, extra pure Sp. gr. 0.91, SDFCL) is added to this solution for maintaining pH and again stirred for one hour. The reddish solution contains precipitate which is filtered to get the manganese ferrite using AR grade filter paper. The paste from precipitate is dried at room temperature and calcined around 800 C in muffle furnace for 5 hr which will yield the manga-nese ferrite in nanosize. The process of synthesis of nano manganese ferrite by co precipitation method is sche-matically as shown in Figure 1. The synthesized nano manganese ferrite is characterized by using Bruker AXS D8 Advance instrument (  1.5406 Å, detector Si(Li) PSD from STIC, Cochin) for XRD characterization.    Fig. 1 – Schematic Representation of Synthesis of Nano-manganese ferrite  3. EXPERIMENTAL RESULTS  The cubic spinel structure of nano manganese fer-rite is confirmed by X-ray diffraction pattern as shown  S.S. YATTINAHALLI, S.B. KAPATKAR, S.N. MATHAD J. NANO- ELECTRON. PHYS. 7, 04096 (2015)   04096-2 in Fig. 2.The X-ray diffraction pattern is indexed by the JCPDS card no (10-0319, 74-2403). The crystallite size of the nano manganese can be calculated using the De-bye-Scherer equation [13] as shown in equation (1).   0.9cosD   (1)  where  is the wavelength of used radiation,  is the full width half maximum (FWHM) of diffraction peak, and  is the Bragg angle. The average lattice parameter 'a' of nano manga-nese ferrite found to be 8.63 Å and average crystallite size found to be 42 nm, also the crystallite size for (311) plane at glancing angle(2θ) is 36.83 nm. The measured values of d are in good agreement with the JCPDS card no 10-0319, 74-2403 as shown in Table 1. Table 2 shows the average crystallite size, average lattice pa-rameter, and volume of the nano manganese ferrite.    Fig. 2 – X-ray Diffraction pattern of the Nano manganese ferrite  Table 1 – Miller indices and lattice parameter  d(obsverved) d(standard) δd (hkl) a (Å) 2.66 2.58 0.08 (311) 8.82 2.48 2.46 0.02 (222) 8.59 2.17 2.13 0.04 (400) 8.68 1.82 1.74 0.08 (422) 8.92 1.67 1.64 0.03 (511) 8.68 1.47 1.5 0.03 (440) 8.32 1.44 1.44 0.00 (531) 8.52 1.30 1.3 0.00 (533) 8.52 1.25 1.23 0.02 (444) 8.66  X-ray density (dx) was calculated by using the for-mula [14] as shown in equation (2)   28MdxNa  (2)  where M is the molecular weight of the nano manga-nese ferrite, N is the Avogadro's number and a is the lattice parameter. The X-ray density of nano manga-nese ferrite found to be 4.76 gm/cm3. The lattice strain is defined as the deformation of an object divided by its effective length. This lattice strain is widely utilized in material science which can be calcu-lated by using the formula as shown in the equation (3)  cos4    (3)    Fig. 3 – Graph of a versus d  Table 2 – Average lattice parameter and Crystallite size  a (Å) a3 (Å3) D (nm) 8.63 642.74 42  Also the dislocation density can be calculated by us-ing the formula as indicated in equation (4)   21D   (4)  The lattice strain and dislocation density for nano manganese ferrite found to be 0.082 and 7.37  1014 respectively. Texture is perceived in almost all engineered mate-rials which can have a great influence on properties of materials. Diffraction patterns from samples contain-ing a random orientation of crystallites have predicta-ble relative peak intensities. Texture frequently repre-sents a pole figure, in which a defined axis (crystallo-graphic) from each of a representative number of crys-tallites is mapped in a stereographic projection [15]. The information regarding degree of orientation of the crystal plane is obtained from the calculation of texture co-efficient (TC) using the formula [16] as indicated in equation (5)          00//I hkl I hklTC hkl nI hkl I hkl (5)  where I and I0 are the observed and standard intensi-ties and n is the number of reading obtained. In amorphous solids the crystallites are oriented in random, but each grain in a polycrystalline aggregate normally has a crystallographic orientation different from that of its neighbors that is in polycrystalline like metal oxide the crystals are oriented in particular planes. Hence the texture analysis is carried out by using diffraction technique to know the preferential orientation of the crystallite. So the texture analysis of material is very important factor to study the chemical, mechanical and physical properties of material. From the texture analysis the grain growth is observed at miller indices (311) plane is more dominant (TC(hkl)  1.56).The detailed TC(hkl) of all plains has been tabulated in Table 3.  SYNTHESIS AND STRUCTURAL CHARACTERIZATION… J. NANO- ELECTRON. PHYS. 7, 04096 (2015)   04096-3 Table 3 – Texture Coefficient of all planes of MnFe2O4  hkl (311) (222) (400) (422) (522) (440) (531) (533) TC(hkl) 1.56 1.38 0.21 0.87 0.64 1.46 1.47 0.45  4. CONCLUSION  Nanosized manganese ferrite has been synthesized by cost effective and simple co-precipitation method. Synthesized nano manganese crystals had a cubic spinel structure with average lattice parameter a  8.63 Å and average crystallite size D  42 nm. Preferential orienta-tion of grains in the (311) plane is predominant and lat-tice strain and dislocation density for the same plane found to be 0.082 and 7.37  1014. Nano manganese fer-rite may find its application in microwave devices, high capacity information storage, water treatment, sensors, inductor cores, and related implementations.  ACKNOWLEDGEMENTS  One of the authors, Suresh B. Kapatkar, gratefully acknowledges Management, and Principal B.V.B. Col-lege of Engineering and Technology, Hubballi, for providing financial assistance under capacity building scheme. S.S. Yattinahalli is grateful to Management and Principal K.L.E. Institute of Technology, Hubballi, and all the authors are grateful to the Director, Sophis-ticated Analytical Instruments Facility STIC, Cochin, for immediate help in characterization.  REFERENCES  1. S. Singhal, T. Namgyal, S. Bansal, K. Chandra, J. Electro. Anal. Appl. 2, 376 (2010). 2. S.G. Dahotre, L.N. Singh, Arch. Phys. Res. 2 No 1, 81 (2011). 3. M.G. Naseri, E.B. Saion, H.A. Ahangar, M. Hashim, H.A. Shaari, J. Magn. Magn. Mat. 323, 1745 (2011). 4. H. Yang, C. Zhang, X. Shi, H. Hu, X. Du, Y. Fang, Y. Ma, H. Wu, S. Yang, Biomaterials 31, 3667 (2010).  5. Y.M.Z. Ahmed, Ceram. Int. 36, 969 (2010). 6. S.A. Mazen, N.I. Abu-Elsaad, Condens. Matt. Phys. 2012, ID 907257 (2012). 7. P. Guoa, G. Zhang, J. Yu, H. Li, X.S. Zhao, Colloid. Surf. A: Physicochem. Eng. Aspects 395, 168 (2012). 8. M. Kooti, A. Naghdi Sedeh, Scientia Iranica 19 No 3, 930 (2012). 9. K.P. Chae, W.O. Choi, J.C. Lee, B.S. Kang, S.H. Choi. J. Mag. 18 No 1, 21 (2013). 10. S.R. Kulkarni, Arch. Phys. Res. 3 No 2, 116 (2012). 11. H. Kavas, N. Kasapoglu, A. Baykal, Y.H. Koseoglu, Chem. Paper. 63 No 4, 450 (2009). 12. S. Kumar, T.J. Shinde, P.N. Vasambekar, Adv. Mat. Lett. 4 No 5, 373 (2013). 13. S.S. Yattinahalli, S.B. Kapatkar, N.H. Ayachit, S.N. Mathad, Int. J. Self-Propag. High-Temp. Synth. 22 No 3, 147 (2013). 14. A.T. Pathan, S.N. Mathad, A.M. Shaikh, Int. J. Self-Propag. High-Temp. Synth. 23 No 2, 112 (2014). 15. S.N. Mathad, V. Puri, Int. Scholarly Res. Notice. 2014, ID 683986 (2014). 16. T. Mahalingam, V. Dhanasekaran, R. Chandramohan, Jin-Koo Rhee, J. Mater. Sci. 47, 1950 (2012).  

Synthesis and Structural Characterization of Nanomanganese Ferrites

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