Available online at SciVerse ScienceDirect

J. Mater. Sci. Technol., 2013, 29(1), 34e38

Synthesis and Characterization of NiFe2O4 Magnetic Nanoparticles

by Combustion Method
M. Kooti*, A. Naghdi Sedeh
Chemistry Department, College of Science, Shahid Chamran University, Ahvaz 61357-43169, Iran
[Manuscript received April 17, 2012, in revised form June 9, 2012, Available online 24 December 2012]

Magnetic nanoparticles of nickel ferrite (NiFe2O4) have been successfully synthesized by microwave-assisted
combustion method using stable ferric and nickel salts as precursors and glycine as fuel. The as-synthesized
samples were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD),
transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and field emission scanning
electron microscopy (FESEM). The effect of different dose of glycine on the structural parameters and
magnetic properties of the prepared NiFe2O4 nanoparticles was also investigated. This study revealed that it
was possible to produce larger size of nanoparticles with lower saturation magnetization by using higher dose
of fuel.

KEY WORDS: Nanoparticles; Combustion; Microwave; Nickel ferrite; Glycine

1. Introduction The properties of the synthesized NiFe2O4 are influenced by

Magnetic spinel ferrite nanocrystals are regarded as one of the
most important inorganic materials because of their electronic,
optical, electrical, magnetic and catalytic properties, all of which
are different from their bulk counterparts. The spinel ferrites
have the general formula of MFe2O4 (M ¼ Co2þ, Ni2þ, Zn2þ or
other divalent metals) can be described as a cubic, closely-
packed arrangement of oxygen atoms, and M2þ and Fe3þ ions
can occupy either tetrahedral (A) or octahedral (B) sites[1,2].
Among various ferrites, nickel ferrite (NiFe2O4) is a typical
inverse spinel, where Fe3þ ions are located in the tetrahedral (A)
and octahedral (B) sites and Ni2þ ions are located in octahedral
sites only. The magnetic moments of the tetrahedral and octa-
hedral sublattices couple in an antiparallel manner and form
a collinear ferrimagnetic ordering (Neel type) with the Curie
temperature of about 870 K[3]. Powder of nanosized nickel ferrite
is a useful material due to its high electromagnetic performance,
excellent chemical stability and mechanical hardness, high
coercivity, and moderate saturation magnetization. These
unique properties of nickel ferrite make it a good contender for
the application as soft magnets and low loss materials at high
frequencies as well as ferro-fluids and biomedical material[4e7].
the composition, purity and microstructure, which are sensitive
to the preparation methodology used in their synthesis. In order
to achieve materials of the desired physical and chemical prop-
erties, the preparation of nickel ferrite nanocrystals through
different routes has become an essential part of research and
development. Many fabrication methods for preparation of
nickel ferrite nanocrystals have been employed, namely by co-
precipitation[8], hydrothermal methods[9], solegel methods[10],
reverse micelles[11], chemical method[12], etc[13e15]. Although
most of these methods have achieved particles of the required
sizes and shapes, they require complicated procedures, expensive
materials, high reaction temperatures, long reaction time, toxic
reagents and by-products and potential harm to the environment.
In this paper, we report the synthesis of nanosized nickel ferrite
particles by combustion method using microwave heating and
glycine as fuel. The employed combustion method can produce
fine, high-purity, stoichiometric nickel ferrite particles in very
short time. The nanostructure and magnetic properties of the as-
prepared nickel ferrite as well as the effect of different amounts
of fuel were also investigated.
2. Experimental

* Corresponding author. Prof.; E-mail address: m_kooti@scu.ac.ir
(M. Kooti).
1005-0302/$ e see front matter Copyright Ó 2013, The editorial office of
Journal of Materials Science & Technology. Published by Elsevier
Limited. All rights reserved.
http://dx.doi.org/10.1016/j.jmst.2012.11.016
2.1. General
All materials were of commercial reagent grade and obtained
from Merck and Fluka. The combustion reactions were carried
out using solid state precursors and the heat for reactions was
supplied by a microwave oven with a nominal power of 1000 W.
 M. Kooti and A.N. Sedeh: J. Mater. Sci. Technol., 2013, 29(1), 34e38
Fig. 1 XRD patterns of NiFe2O4 nanoparticles: (a) S1, (b) S2, (c) S3
(- peaks for impurity).
X-ray diffraction (XRD) patterns of the samples were taken with
a PW1840 Philips X-ray diffractometer at room temperature
using CuKa radiation wavelength of l ¼ 0.15418 nm. The peak
position and intensity were obtained between 10 and 80 with
a velocity of 0.02 /s. The morphology and size of the particles
were examined by transmission electron microscopy (TEM)
using a Philips CM10-HT 100 KV microscope. The field emis-
sion scanning electron microscopy (FESEM) images were ob-
tained using a Hitachi Japan S4160 field emission scanning
electron microscope. Magnetic properties of nickel ferrite
nanocrystals were studied using vibrating sample magnetometer
(VSM) from Meghnatis Daghigh Kavir Company.
2.2. Procedure
The NiFe2O4 nanoparticles were synthesized by a combustion
method using glycine as fuel. In this synthesis calculated
proportions of nickel and iron nitrates with known amount of
glycine were thoroughly mixed. The obtained dark red liquid
was transferred into a porcelain crucible and then heated in
a microwave for 2 min with 30% power. During heating of the
mixture a great deal of foams produced and spark appeared
which spread through the mass, yielding a brown voluminous
and fluffy product in the container. The final product was washed
several times with deionized water and ethanol and dried at
100  C for 3 h. Three samples of NiFe2O4 have been prepared
using glycine: Ni(NO3)2$6H2O:Fe (NO3)3$9H2O in molar ratios
Table 1 Structural parameters of nickel ferrite calculated from XRD results
Glycine/mmol Structure Space group Crystallite size/nm
6 fcc Fd3m 34.7
8 fcc Fd3m 38
10 fcc Fd3m 42
35
of (6, 8 and 10):1:2, respectively. These samples are designated
as S1, S2 and S3.
3. Results and Discussion
Nickel ferrite nanoparticles were synthesized by the combus-
tion method using glycine as fuel. In this procedure, glycine
(CH2NH2COOH) was employed as the fuel due to its more
negative heat of combustion (3.24 kcal g1) as compared to
urea (2.98 kcal g1) and citric acid (2.76 kcal g1)[16].
The XRD patterns of samples are shown in Fig. 1. The
diffraction peaks observed at 2q ¼ 30.40 , 35.77 , 43.51 ,
53.98 , 57.39 and 63.04 correspond to the planes of (220),
(311), (222), (400), (422), (511) and (440), respectively. The
observed peaks for sample S3 have relative intensity (%) of
26.6, 100, 39.1, 15.9, 42.0, and 57.8, respectively. These
angles measured for the NiFe2O4 samples are in very good
agreement with the reported values (JCPDS card No. 44-
1485). The diffraction lines provide clear evidence for the
formation of cubic phase of pure inverse spinel structure of
nickel ferrite with Fd3m space group. The particle size of
NiFe2O4 samples has been calculated from the XRD line
broadening of (311) peak using DebyeeScherrer’s formula[17]
D ¼ Bl=bcos q
where D is the crystallite size (nm) of the phase under
investigation, B is the Scherrer constant (0.9), l is the
wavelength of X-ray (l ¼ 0.154 nm), b is the full-width at
half maximum (FWHM) of plane (311) and q is the Bragg’s
angle. The calculated crystallite size of NiFe2O4 for samples
S1, S2, and S3 are found to be 34.7, 38 and 42 nm,
respectively. These results revealed that increasing the amount
of glycine fuel, from samples S1 to S3 causes enlargement of
crystallite size of NiFe2O4 nanoparticles.
An X-ray analysis enable us to investigate the role of the
amount of fuel in the change of the structural parameters of
nickel ferrite such as the crystallite size (D), lattice constant (a),
unit cell volume (V) and density (d). The lattice constants of all
the samples are calculated using the following relation[17]

1=2
a ¼ dhkl h2 þ k 2 þ l2
The values are in good agreement with earlier reported values of
0.833 nm for nano NiFe2O4[18] and 0.8339 nm for the bulk
NiFe2O4[19], which prove the efficiency of our synthesis
technique. The calculated values of various structural
parameters are given in Table 1. Furthermore, in both samples
S1 and S2 a peak at 2q ¼ 33.42 , attributed to a-Fe2O3 phase
impurity is seen but in sample S3, where a high dose of
glycine was used, this peak disappeared.
The FT-IR spectrum of the as-prepared NiFe2O4 is presented
in Fig. 2. A broad absorption band at about 3400 cm1
represents a stretching mode of H2O molecules and OH
Lattice constant/nm Density/(g/cm3) Volume/nm3
0.8322 5.404 0.5760
0.8294 5.459 0.570
0.8321 5.405 0.5761
36 M. Kooti and A.N. Sedeh: J. Mater. Sci. Technol., 2013, 29(1), 34e38
Fig. 2 FT-IR spectrum of NiFe2O4 nanoparticles.
[15]
groups . Two other principle absorption bands in the range of
400e600 cm1 are also observed in the FT-IR spectrum. The
first band (n1) is around 459 cm1 and the second one (n2) is
around 563 cm1, attributed to the long bond length of oxygene
metal ions in the octahedral sites and shorter bond length of
oxygenemetal ions in the tetrahedral sites in the spinel structure,
respectively[20]. Three samples S1, S2, and S3 show the same IR
spectra and Fig. 2 is the IR spectrum of S1.
The morphology and particle sizes of the as-prepared nickel
ferrite nanoparticles were determined by FESEM and TEM
techniques. As it can be seen from Fig. 3, the FESEM images
show the presence of voids and pores in the samples. This is
attributed to the release of large amount of gases during
combustion process. The samples have spongy structure and
the formation of multigrain agglomerations consisting of very
fine crystallites. In sample S3 (Fig. 3(c)), where a high molar
ratio of glycine was used, most of pores on the surface have
smaller size and the particles are more packed. This is due to
the release of more heat during the combustion, which causes
the fusion of the NiFe2O4 nanoparticles.
The TEM micrographs of the as-fabricated NiFe2O4 nano-
particles (sample S3) is given in Fig. 4 showing almost
homogeneous and uniform distribution of these particles in the
powder sample. The particles consisted of some regular and
irregular polyhedrons with mean sizes of about 35 nm, which
is in close agreement with the size obtained from XRD analysis.
Magnetic measurements of as-prepared NiFe2O4 were carried
out at room temperature using vibrating sample magnetometer
(VSM) with a peak field of 10 kOe and the hysteresis loops for
samples S1, S2, and S3 are shown in Fig. 5. As it can be seen,
the variation of magnetization as a function of applied field
presents a narrow cycle and the observed hysteresis loops are
characteristic behavior of soft magnetic material.
Saturation magnetization (Ms), remanence magnetization (Mr)
and coercivity (Hc) values of these ferrites are given in Table 2.
The saturation magnetization of NiFe2O4 samples nearly
Fig. 3 FESEM images of NiFe2O4 nanoparticles: (a) S1, (b) S2, (c) S3.
Fig. 4 TEM image of as-prepared NiFe2O4 nanoparticles (sample S3).
approaches the value of bulk NiFe2O4 (56 emu g1)[21]. For
most magnetic nanoparticles, the saturation magnetization is
much lower than bulk value due to the surface spin
disorder[22,23] and decreases with decreasing particle size[24].
Among the three synthesized nickel ferrite samples, sample
S3, which was prepared using higher dose of fuel, has the least
value of Ms. The magnetic saturation of the synthesized NiFe2O4
with pure phase (sample S3) is 48.75 emu g1, which is an
acceptable value for this size as reported in literature[25e28] and
relatively low in comparison with the corresponding bulk
NiFe2O4. A similar decrease in the saturation magnetization was
observed for cobalt ferrite, which is also an inverse spinel with
collinear ferrimagnetic spin structure in the bulk form[29]. Nickel
ferrite is a typical soft ferromagnetic material, whose magnetic
behavior depends significantly on the synthesis route and the
particle size. For relatively larger particles, magnetic domains
are formed to reduce the static magnetic energy. The number
of domains diminishes with decreasing particle size. The
particles turn into single domain ones with their size under
a critical radius (for nickel ferrite, this parameter is about
100 nm), resulting in the increase of coercive force due to
vanishing of the magnetization caused by the movement of
domain walls. Back to our finding of the variation of Ms from
samples S1 to S3, the higher value of Ms for samples S1 and
S2 compared to sample S3 could be attributed to the presence
of some Fe2O3 impurities in samples S1 and S2 as shown in
the XRD patterns of these samples. These paramagnetic
impurities may have some contribution to the magnetization
that resultantly increases the saturation magnetization of nickel
ferrite nanoparticles. In addition to this parameter, the variation
of saturated magnetization and coercivity of NiFe2O4
nanoparticles may be also explained on the basis of various
factors such as cation redistribution, surface spin, formation of
spin glass structures, and magneto crystalline anisotropy.
 M. Kooti and A.N. Sedeh: J. Mater. Sci. Technol., 2013, 29(1), 34e38 37

4. Conclusion

Combustion method with microwave heating was used to

synthesize nickel ferrite nanoparticles in high yield and purity. A
mixture of Fe (III) and Ni (II) nitrates with glycine as fuel was
heated in a microwave to afford nanosized NiFe2O4, which was
characterized by various techniques, mainly XRD, FT-IR,
FESEM, TEM and VSM. The effect of different amounts of
fuel, i.e. glycine, on the size and purity of the prepared nickel
Fig. 5 Hysteresis loops of as-prepared NiFe2O4 nanoparticles.
ferrite nanoparticles was also investigated. The microwave
combustion method can be considered as a facile and rapid route
for the preparation of nanoscale NiFe2O4. Moreover, there is no
need for expensive precursors or complicated treatments in this
Table 2 Magnetic properties of the as-fabricated NiFe2O4 nanoparticles method.
Sample Ms/(emu/g) Mr/(emu/g) Hc/Oe
Acknowledgment
S1 60.87 17.44 112.62 The authors are grateful for the financial support provided by
S2 51.86 18.36 137.12 the Research Council of Shahid Chamran University, Ahvaz,
S3 48.75 18.95 177.55 Iran.

REFERENCES
Therefore, the magnetic behavior of nanosized nickel ferrites can
be a collective effect of these interactions[30,31]. It is worth noting
[1] B. Aslibeiki, P. Kameli, H. Salamati, M. Eshraghi, T. Tahmasebi,
that the magnetic properties of similar ferrite nanoparticles of the J. Magn. Magn. Mater. 322 (2010) 2929e2934.
same particle size differ depending on the preparation method [2] S.C. Tsang, V. Caps, I. Paraskevas, D. Chadwick, D. Thompsett,
used. As stated by Naseri et al.[9], pairs of similar spinel ferrite Angew. Chem. Int. Edit. 43 (2004) 5645e5649.
nanoparticles of the same particle size have different saturation [3] B.D. Cullity, S. Graham, Introduction to Magnetic Materials, Wiley,
magnetization values and coercivity fields. This fact indicates New York, 2009.
that, the magnetic properties of ferrites are related primarily to [4] L.Y. Chen, H. Dai, Y.M. Shen, J.F. Bai, J. Alloys Compd. 491
the preparation methods. (2010) L33eL38.
The Ms value of sample S3 also supports the fact that in this [5] D.S. Mathew, R.S. Juang, Chem. Eng. J. 129 (2007) 51e65.
sample Ni2þ ions (almost) entirely locate in B sites because due [6] I. Sharifi, H. Shokrollahi, S. Amiri, J. Magn. Magn. Mater. 324
(2012) 903e915.
to the lower spin moment of Ni2þ (S ¼ 2 mB/ion) compared to
[7] M.R. Phadatare, V.M. Khot, A.B. Salunkhe, N.D. Thorat, S.H.
that of Fe3þ (S ¼ 5 mB/ion), the occupation of Ni2þ ions in A Pawar, J. Magn. Magn. Mater. 324 (2012) 770e772.
sites would result in an increase of the net magnetization [8] M.S. Niasari, F. Davar, T. Mahmoudi, Polyhedron 28 (2009)
according to the Neel configuration. 1455e1458.
Finally, to give an idea about the advantage of the method for [9] M.G. Naseri, E.B. Saion, H.A. Ahangar, M. Hashim, A.H. Shaari,
synthesizing NiFe2O4 nanoparticles, we compared our method Powder Technol. 212 (2011) 80e88.
with those reported earlier, listed in Table 3. As can be seen in [10] M. Mozaffari, Z. Abooalizadeh, J. Amighian, J. Magn. Magn.
Table 3, the reaction conditions of our method are much Mater. 323 (2011) 2997e3000.
superior to the methods illustrated in this table. The properties [11] A. Kale, S. Gubbala, R.D.K. Misra, J. Magn. Magn. Mater. 277
of our fabricated NiFe2O4 sample appear to be either better (2004) 350e358.
[12] P. Deb, A. Basumallick, S. Das, Solid State Commun. 142 (2007)
than some of those presented in this table or comparable with
702e705.
those reported by Umare et al[33]. [13] L. Chen, Y. Yuan, H. Peng, X. Lu, Z. Luo, Mater. Lett. 67 (2012)
311e314.
[14] J. Wang, F. Ren, R. Yi, A. Yan, G. Qiu, X. Liu, J. Alloys Compd.
Table 3 Comparison of reaction conditions and properties of our 479 (2009) 791e796.
NiFe2O4 sample with those reported earlier [15] V.K. Sankaranarayana, C. Sreekumar, Curr. Appl. Phys. 3 (2003)
205e208.
Method of Conditions Grain Ms/ Hc/Oe Reference [16] C.C. Hwang, J.S. Tsai, T.H. Huang, Mater. Chem. Phys. 93 (2005)
preparation size/nm (emu/g) 330e336.
[17] B.D. Cullity, Elements of X-ray Diffraction, second ed., Addison-
Solegel 70  C/3 h, 45 31 93 [19]
Wesley, London, 1978.
700  C/10 h
[18] J. Huo, M. Wei, Mater. Lett. 63 (2009) 1183e1184.
Co-precipitation 80  C/40 min, 28 40.5 89 [27]
[19] M. Srivastava, S. Chaubey, A.K. Ojha, Mater. Chem. Phys. 118
600  C/10 h
(2009) 174e180.
Hydrothermal 180  C/10 h 65 49.6 30 [32]
[20] P. Laokul, V. Amornkitbamrung, S. Seraphin, S. Maensiri, Curr.
Combustion 80  C/2 h, 35 42.5 112.3 [33]
Appl. Phys. 11 (2011) 101e108.
800  C/2 h
[21] V. Sepelak, K. Tkacova, V.V. Boldyrev, S. Wibmann, K.D. Becker,
Hydrothermal 180  C/10 h 80 53.6 68 [18]
Physica B 234e236 (1997) 617e619.
Thermal 80  C/24 h, 47 29.05 51 [9]
[22] S. Rana, R.S.M. Srivastava, M. Sorensson, R.D.K. Misra, Mater.
treatment 821  C/3 h
Sci. Eng. B 119 (2005) 144e151.
Combustion Microwave/2 35 48.75 177.5 This work
[23] R.D.K. Misra, S. Gubbala, A. Kale, W.F. Egelhoff Jr., Mater. Sci.
min
Eng. B 111 (2004) 164e170.
38 M. Kooti and A.N. Sedeh: J. Mater. Sci. Technol., 2013, 29(1), 34e38
[24] A.H. Morrish, K.H. Haneda, J. Appl. Phys. 52 (1981)
2496e2498.
[25] T.F. Marinca, I. Chicinas, O. Ismard, V. Pop, F. Popa, J. Alloys
Compd. 509 (2011) 7931e7936.
[26] A. Azizi, S.K. Sadmezhaad, Ceram. Int. 36 (2010) 2241e2245.
[27] K. Maaz, S. Karim, A. Mumtaz, S.K. Hasanain, J. Liu, J.L. Duan,
J. Magn. Magn. Mater. 321 (2009) 1838e1842.
[28] A.C.F.M. Costa, A.P.A. Diniz, A.G.B. de Melo, R.H.G.A. Kiminami,
D.R. Cornejo, A.A. Costa, L. Gama, J. Magn. Magn. Mater. 320
(2008) 742e745.
[29] K.V.P.M. Shafi, Y. Koltypin, A. Gedanken, R. Prozorov, J. Balogh,
J. Lendvai, I. Felner, J. Phys. Chem. B 101 (1997) 6409e6414.
[30] M.A. Gabal, Y.M. Al Angari, M.W. Kadi, Polyhedron 30 (2011)
1185e1190.
[31] Y. Cheng, Y. Zheng, Y. Wang, F. Bao, Y. Qin, J. Solid State Chem.
178 (2005) 2394e2397.
[32] T. Prabhakaran, J. Hemalatha, J. Alloys Compd. 509 (2011)
7071e7077.
[33] S.S. Umare, R.S. Ningthoujam, S.J. Sharma, S. Shrivastava,
S. Kurain, N.S. Gajbhiye, Hyperfine Interact. 184 (2008) 235e243.