Processing and Application of Ceramics 8 [3] (2014) 137–143

DOI: 10.2298/PAC1403137K

Comparative studies on impact of synthesis methods on structural and

magnetic properties of magnesium ferrite nanoparticles
Navneet Kaur , Manpreet Kaur∗
Department of Chemistry, Punjab Agricultural University, Ludhiana-141004, India

Received 12 August 2014; Received in revised form 24 September 2014; Accepted 27 September 2014

Abstract
Magnesium ferrite nanoparticles (NPs) were synthesized by co-precipitation, sol-gel and solution combustion
methods. Polyethylene glycol (PEG), urea and oxalyl dihydrazide (ODH) were used as fuels for the combus-
tion. Various physicochemical techniques viz. X-ray diffraction (XRD), vibrating sample magnetometry (VSM),
Fourier transform infrared spectroscopy (FT-IR), BET surface analysis and transmission electron microscopy
(TEM) were utilized to study the effect of synthetic methodology on the properties of synthesized NPs. Differ-
ences in crystallinity, surface area, particle size and magnetic parameters of the ferrite NPs synthesized by
different methods were observed. XRD pattern of NPs obtained by sol-gel and combustion methods confirmed
phase purity where as in co-precipitation method α-Fe2 O3 was detected as impurity phase which also resulted
in greater value of physical density and lowering of magnetic parameters of the final thermolysis product.
TEM micrographs indicated that ferrite NPs are spherical with average diameter of 12–25 nm. Presence of
rectangular shaped crystallites of α-Fe2 O3 was clearly evident in the TEM images of the NPs synthesized by
co-precipitation method.
Keywords: Nano ferrite, combustion, co-precipitation, magnetic properties, calcination, structural properties

I. Introduction Magnesium ferrite is an important spinel ferrite

Nanomaterials play a pivotal role in physical, chemi- which finds applications in the fields of heterogeneous
cal and biomedical fields due to their high surface ener- catalysis, adsorption, sensors and magnetic technolo-
gies. Among these, spinel ferrites are useful magnetic gies [11]. Several methods are employed to synthesize
materials because of their low cost and high electro- ferrite nanoparticles. Ceramic method is economical for
magnetic performance over a wide frequency range as the bulk synthesis of ferrites but undesired non-uniform
compared to the pure metals [1]. Spinel ferrites are the particles are formed due to aggregation of nanoparti-
compounds having a general formula AB2 O4 , in which cles and phase purity is not completely achieved. High-
the A-site is tetrahedrally coordinated and occupied by energy milling can reduce the crystallite size but this
divalent cations and the B-site is octahedrally coordi- physical process not only requires greater energy con-
nated and occupied by trivalent ion Fe3+ [2]. High re- sumption but also easily induces structural disorder in
sistivity of ferrites greatly influences their dielectric and the crystallites [12]. In the recent past several chemical
magnetic behaviour [3]. They are widely used in elec- methods viz. co-precipitation [13], sol-gel [14], com-
tronic and magnetic devices due to their high magnetic bustion [15], micelle routes [3] and hydrothermal syn-
permeability and low magnetic losses [4]. In the recent thesis [16] have been employed to synthesize ferrite
years, ferrite nanoparticles have received applications in nanoparticles under moderate conditions. NPs synthe-
the diverse fields such as mineral separation, magnetic sized by these methods possess good chemical homo-
storage devices [5], catalysis [6], magnetic refrigeration geneity and high purity [17].
system, drug delivery system [7], magnetic resonance Studies pertaining to the effect of synthetic method
imaging [8], cancer therapy [9] and magnetic cell sepa- on the properties of ferrites are important in understand-
ration [10]. ing their inter relationship and need to be explored.
Properties of ferrite materials are strongly influenced by
∗
Corresponding author: tel: +91 814 6200711 the distribution of metallic ions among crystallographic
e-mail: manpreetchem@pau.edu lattice sites which in turn is sensitive to the synthetic

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method employed. Selection of the method largely de- 2.4. Characterization techniques
pends on the targeted applications and desired proper- FT-IR spectra were recorded on Perkin Elmer, model
ties. Although magnesium ferrite NPs have been syn- RX-1 FT-IR spectrophotometer. The X-ray diffraction
thesized by different chemical methods under different measurements were carried out using Cu Kα radiation
temperature and sintering conditions, comparative eval- (λ = 1.5404 Å) with the Panlytical X’pert Pro. Mag-
uation of effect of different synthetic methodologies on netic properties of ferrite samples were studied by vi-
structural and magnetic properties of magnesium ferrite brating sample magnetometer model PAR-155. Trans-
NPs at constant calcination temperature and sintering mission electron micrographs (TEM) of end products
time are lacking. The objective of the present work is were recorded by employing transmission electron mi-
to assess the effect of these parameters on the struc- croscope model Hitachi Hi-7650 at 100 kV accelera-
tural and magnetic properties of spinel magnesium fer- tion voltages in HC mode using water as a dispersion
rite NPs prepared by different chemical routes viz. the medium. The lattice constant, or lattice parameter (a)
sol-gel, co-precipitation and combustion methods. was calculated employing the following relationship:
1/2
II. Experimental a = d h2 + k2 + l2

(1)
MgFe2 O4 NPs were synthesized employing three dif- where d is diffracting plane spacing and h, k and l Miller
ferent synthetic routes i.e. sol-gel, co-precipitation and indices of the diffracting plane.
combustion methods. All the chemicals used were of The XRD density (ρXRD ) was calculated by the for-
AR grade and all the solutions were prepared in double mula:
distilled water.
8M
2.1. Sol-gel method ρXRD = (2)
N a3
In the sol-gel method 2.0 mol of Fe(NO3 )3 ·9H2 O and
where, M is molecular weight of the sample and N is
1.0 mol of Mg(NO3 )2 ·6H2 O were dissolved in 20 ml
Avogadro’s number.
distilled water. Then 2.22 mol of citric acid was added
The crystallite size of the MgFe2 O4 NPs was based
in the aqueous mixture [18]. The mixture was magne-
on X-ray diffraction line broadening and calculated by
tically stirred at 60 °C and ammonium hydroxide was
using Scherrer’s equation [21]:
added into the mixture to adjust solution pH to 7.0 and
the mixture transformed into sol. After stirring for 8 h, Bλ
the sol turned into gel. The gel was dried at 100 °C for D= (3)
β cos θ
12 h with its volume expanding about five times. Finally,
the dried gel was ground and calcined at 500 °C for 3 h where D is the average crystallite size of the phase under
to get ferrite as final thermolysis product. investigation, B is the Scherrer’s constant (0.89), λ is the
wave length of X-ray beam used, β is the full-width half
2.2. Co-precipitation method maximum of diffraction peak and θ is the Bragg’s angle.
2.0 mol of Fe(NO3 )3 ·9H2 O and 1.0 mol of
Mg(NO3 )2 ·6H2 O were dissolved in 20 ml distilled III. Results and discussion
water. The pH of the solution was adjusted between
9 and 10 with 0.1 M NaOH resulting in the brown 3.1. FT-IR parameters
precipitates. The precipitates were filtered and washed FT-IR spectrum of ferrite NPs obtained using
repeatedly with distilled water till pH 7 was achieved. polyethylene glycol as fuel is shown in Fig. 1. The spec-
Finally, the precipitates were dried at 100 °C for 4 h and trum displayed two bands in the region 400–630 cm-1 .
subsequently calcined at 500 °C for 3 h to get ferrite as The higher frequency band (ν1 ) located in the region
end product. 520–630 cm-1 corresponds to stretching vibrations of
metal ions in the tetrahedral sites and some additional
2.3. Combustion method peaks observed in the region above 630 cm-1 were due
Three different complexing agents/fuels, i.e. poly- to the splitting of absorption band due to exchange of
ethylene glycol (PEG), urea and oxalyl dihydrazide ions between A and B sites. Similar results have been
(ODH), were used to prepare MgFe2 O4 NPs by combus- reported earlier [22]. The second lower frequency band
tion method. ODH required for the synthesis was pre- (ν2 ) observed in the region 400–482 cm-1 was due to
pared using hydrazine hydrate and diethyl oxalate [19]. the stretching vibrations of metal ions in the octahedral
Metal nitrates act as oxidizers (O) and PEG/Urea/ODH site [23]. The difference in band position was caused by
act as fuel (F). Equivalence ratio i.e. φe = (O/F) was difference in M–O distance in tetrahedral and octahe-
maintained unity by balancing the oxidizing (O) and re- dral sites [24]. Magnesium ferrite synthesized by other
ducing valency (F) of the reactants [20]. methods also displayed similar absorption bands.

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only due to the crystalline domain size [27]. The crys-

tallite size of the samples prepared by different meth-
ods was in the range of 8–16 nm respectively. The dif-
ference in crystallite size was due to different prepara-
tion conditions for ferrite synthesis. NPs synthesized by
the sol-gel method (Fig. 2) displayed the most intense
XRD peaks, indicating their highest crystallinity among
the synthesized NPs. Lattice constant obtained using the
XRD data is found to be in the range 8.308 Å to 8.351 Å.
X-ray diffractogram of NPs obtained by the chemical
co-precipitation method (Fig. 2) displayed weak diffrac-
tion peaks corresponding to α-Fe2 O3 along with sharp
peaks for spinel ferrite component due to the low crys-
tallinity, which indicates that in co-precipitation method
Figure 1. FT-IR spectrum of MgFe2 O4 NPs synthesized by phase purity is not completely achieved. Fe2 O3 impurity
PEG-metal nitrate combustion method phase was previously reported in MgFe2 O4 NPs synthe-
sized by co-precipitation method [28] and it is clearly
3.2. XRD parameters evident that the phase purity is determined by prepara-
X-ray diffractograms of MgFe2 O4 NPs synthesized tion method. Physical density of sol gel, co-precipitation
by different chemical methods are shown in Fig. 2 and and combustion derived NPs are shown in Table 1. Fer-
XRD parameters are given in Table 1. The diffraction rite NPs synthesized by combustion and sol-gel meth-
patterns of MgFe2 O4 consisted of peaks correspond- ods displayed lower values than the corresponding XRD
ing to crystallographic planes (220), (311), (400), (422), density which was expected due to the presence of
(511) and (440). All the observed peaks and Miller in- pores created in the powders during the sintering pro-
dices (hkl) of the fcc lattice were in agreement with cess, whereas greater value of physical density of fer-
the reported values [25,26] for MgFe2 O4 and also con- rites synthesized by co-precipitation method and their
firmed by matching with ASTM Data Card No. 17- non-porous nature can be attributed to the presence of
465. The peak broadening of the diffraction patterns α-Fe2 O3 impurity. It has been reported that the density
is mainly attributed to four factors: faulting (extended of bioactive glass-ceramics increased with increase in
defects), micro strains (deformation of the lattice) and Fe2 O3 content [29], moreover Fe2 O3 containing sam-
crystalline domain size distribution. If the samples are ples have improved hydration resistance due to their
free from strains and faulting, the peak broadening is larger grain size compared to Fe2 O3 free samples [30].
3.3. Magnetic studies
Hysteresis plots showing the variation of magnetiza-
tion (M s , emu/g) as a function of applied magnetic field
(H, Oe) are shown in Fig. 3 and magnetic parameters
are presented in Table 2. All the samples displayed nor-
mal (S-shaped) narrow hysteresis loops. Narrow loop
indicated low coercivity values which indicate that the
prepared sample can be easily demagnetized. Magnetic
parameters like saturation magnetization (M s ), remnant
magnetization (Mr ) and coercivity (Hc ) of the samples
depend upon a number of factors viz. anisotropy den-
sity, grain growth and A–B exchange interactions. M s
values of NPs synthesized by PEG, sol-gel, ODH and
urea combustion methods were 13.55, 13.22, 13.25 and
10.73 emu/g, respectively. Although urea has greater
combustion heat (−2.98 kcal/g) as compared to citric
acid (−2.76 kcal/g) [31] the observed M s has higher
value for the later. This could be explained on the ba-
sis of better complexion power of the citric acid and
greater amount of heat evolved when equimolar amount
of citric acid is used. Polymerization is favoured upon
heating and the resultant citrate gel is a polymeric net-
work with metal ions uniformly distributed throughout
the organic matrix. Autocatalytic combustion of poly-
Figure 2. X-ray diffraction patterns of MgFe2 O4 synthesized
by different chemical routes
meric gel and polyethylene glycol also favours greater

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Table 1. XRD parameters of ferrite nanoparticles

Lattice constant X-Ray density Physical density Porosity Average particle diameter
Method
[Å] [g/cm3] [g/cm3] [%] [nm]
Sol-gel 8.351 3.819 2.586 32.28 16.0
Co-precipitation 8.321 3.837 5.431 - 13.5
PEG 8.314 3.843 3.235 15.82 16.0
Urea 8.312 3.844 3.017 21.51 8.0
ODH 8.308 3.848 1.852 51.87 11.0

Table 2. Magnetic parameters of ferrite nanoparticles synthesized by different chemical methods

Saturation magnetization, M s Retentivity, Mr Coercivity, Hc

Method
[emu/g] [emu/g] [Oe]
Sol gel 13.22 3.62 130.55
Co precipitation 1.95 - 2.59
PEG 13.55 0.89 55.47
Urea 10.73 1.36 112.02
ODH 13.25 3.45 66.05

is a measure of its magneto-crystalline anisotropy. The

values of Hc have no direct relationship with the prepa-
ration temperature and/or crystalline size. These values
are altered by Mr values. Higher remanent magnetiza-
tion favours increase in coercive field. NPs synthesized
by PEG method displayed high M s values coupled with
low coercivity which is an essential requirement for a
good electromagnet. The lower values of magnetic pa-
rameters as compared to bulk counterparts are attributed
to the smaller particle size of the ferrite NPs [34] and
existence of spin canting, which has been reported in
several nanometer-sized ferrites and is dependent upon
surface structural disorder [35].

3.4. TEM and BET studies

Particle morphology and size distribution of the fer-
Figure 3. Hysteresis loop of MgFe2 O4 synthesized by rite powder calcined at 500 °C were investigated using
different chemical methods TEM micrographs. Figure 4 displays the TEM micro-
graphs and particle size distribution histograms of the
crystallinity for NPs synthesized by these methods. NPs NPs synthesized by sol-gel, co-precipitation and com-
prepared by co-precipitation method had lowest M s bustion methods. NPs synthesized by sol-gel method
value of 1.948 emu/g. Presence of ferric oxide phase (Fig. 4a) show average particle diameter of 25 nm and
along with ferrite phase due to incomplete precipita- these results are corroborated with the XRD results
tion resulted in the observed decline in magnetic be- where sharp peaks confirmed greater crystallinity.
havior. Another possible reason for the diminution in In case of co-precipitation derived ferrites (Fig. 4b)
the value of M s may be attributed to the incomplete the particle size distribution displayed large variation
crystallization of MgFe2 O4 which is undetectable by and rectangular shaped α-Fe2 O3 particles (as depicted
XRD technique. The higher saturation values for NPs by arrow) are clearly visible in the TEM micrograph.
obtained from the PEG, sol-gel and ODH methods may Average particle diameter of ferrite NPs was 12 nm.
be due to the fact that the anisotropic features of these Similar results were reported in case of nickel ferrite
nanocrystals have enhanced dipole-dipole interaction, synthesized by co-precipitation method [36].
favouring a head-to-tail orientation [32]. The second TEM micrographs of ferrite NPs synthesized by com-
factor favouring increase in the value of M s and Mr bustion methods (Figs. 4c,d) confirm nanocrystalline
for sol-gel and PEG synthesized NPs is the increase in nature of combustion derived ferrite NPs with average
crystalline size. It was also observed that MgFe2 O4 NPs particle diameter of 14.5 and 17.3 nm respectively for
prepared by combustion method at calcination temper- PEG and ODH derived NPs. Spherical shape of the NPs
ature 900 °C had a crystalline size of 78.8 nm and M s was clearly visible and impurity phase was not detected
value of 30.6 emu/g [33]. Hc of the magnetic material in sol-gel and combustion derived NPs. Agglomeration

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(a) (b)

(c) (d)

(e)

Figure 4. Transmission electron micrographs and particle size distribution histograms of calcined MgFe2 O4 synthesized by:
a) co-precipitation method, b) sol-gel method, c) PEG method and d) Urea method and e) ODH method

phenomenon was also observed as small particles ag- accordance with the observed average particle size trend
gregated in order to achieve lower free energy state. of the TEM studies.
NPs synthesized using urea as a fuel (Fig. 4e) showed
greater agglomeration of the primary particles and av- IV. Conclusions
erage size of 21 nm. This trend was also observed by
Wu et al. [37] during synthesis of SiO2 doped Ni-Zn MgFe2 O4 NPs are synthesized by sol-gel, co-
ferrites by using different fuels. TEM images of these precipitation and combustion methods keeping uniform
NPs clearly reveal self alignment of NPs. The particle calcination temperature and sintering time. Differences
size estimated from TEM was greater than the parti- in crystallinity, surface area, particle size and magnetic
cle size calculated from XRD using Scherrer’s formula. parameters of the ferrite NPs synthesized by differ-
This is because X-ray diffraction gives the informa- ent methods were observed. TEM micrographs showed
tion of the crystalline region only and the contribution that NPs exhibited agglomeration phenomenon and had
from the amorphous grain surface does not contribute. an average diameter of 12–25 nm. Rectangular shaped
On the other hand TEM images display the complete nanocrystals of α-Fe2 O3 were observed in the TEM
morphology of the nanoparticles. MgFe2 O4 NPs synthe- images of NPs synthesized by co-precipitation method
sized by sol-gel, co-precipitation, PEG and urea method which was confirmed by the XRD pattern. Magnesium
displayed BET surface area of 3.8, 67.2, 17.1 and 27.5 ferrite synthesized PEG, ODH and sol-gel methods
and 26.5 m2 /g, respectively. The large surface area of displayed M s values ranging from 13.22–13.55 emu/g
co-precipitation derived ferrites was due to hindrance whereas NPs synthesized by urea method had lower
in the growth of particles due to incomplete ferritiza- M s value of 10.73 emu/g which was in accordance with
tion and presence of α-Fe2 O3 in the final thermolysis the observed lower crystallinity. The lowest value of
product. The results of BET surface area study were in M s 1.95 emu/g for NPs synthesized by co-precipitation

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method confirmed the effect of impurity phase on the Prasad, “Co-precipitation method of synthesis and
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Acknowledgment: Manpreet Kaur acknowledges the 14. M. Kaur, B.S. Randhawa, P.S. Tarsikka, “Synthesis
financial assistance (grant number 42-337/2013) pro- of Mg0.3 Zn0.7 Fe2 O4 nanoparticles from thermolysis
vided by University Grants Commission, India. of magnesium zinc tris maleatoferrate (III) heptahy-
drate”, Ind. J. Eng. Mater. Sci., 20 (2013) 325–328.
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