Solid State Communications 147 (2008) 479–483

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Solid State Communications

journal homepage: www.elsevier.com/locate/ssc

Structural investigations and magnetic properties of cobalt ferrite nanoparticles

prepared by sol–gel auto combustion method
B.G. Toksha, Sagar E. Shirsath, S.M. Patange, K.M. Jadhav ∗
Department of Physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad: 431 004 (MS), India

article info a b s t r a c t

Article history: Morphological and magnetic characteristics of cobalt ferrite nanoparticles synthesized by sol–gel auto
Received 27 May 2008 combustion method using nitrates of respective metal ions have been studied. X-ray diffraction pattern
Received in revised form was indexed by a Rietveld program to calculate accurate unit cell dimension. A Transmission Electron
26 June 2008
Microscope (TEM) confirmed the formation of single phase cobalt ferrite nanoparticles in the range
Accepted 27 June 2008
by E.V. Sampathkumaran
11–40 nm depending on the annealing temperature and time. The size of the particles increases with
Available online 8 July 2008 annealing temperature and time while the coercivity goes through a maximum, peaking at around 25 nm.
A very large coercivity (10.2 kOe) is observed on cooling down to 77 K while typical blocking effects are
PACS: observed below about 260 K. The high field moment is observed to be small for smaller particles and
75.50Gg approaches the bulk value for large particles. Mossbauer spectra recorded at room temperature is a sextet
75.50Tt indicating that there is a strong magnetic coupling and increase in sintering temperature from 570 ◦ C to
75.70Rf 800 ◦ C do not affect Mossbauer parameters.
75.50.Vv © 2008 Elsevier Ltd. All rights reserved.
33.45._x

Keywords:
A. Magnetically ordered materials
B. Chemical synthesis
C. Scanning and transmission electron
microscopy

1. Introduction crucially on the size, shape and purity of these nanoparticles. The
particles should be single domain, of pure phase, should have high
Metal-oxide nanoparticles have been the subject of current coercivity and medium magnetization for using them in recording
interest because of their unusual optical, electronic and magnetic media.
properties, which often differ from their bulk counter-part [1, Techniques to produce nanoparticles include wet chemical
2]. Nanocrystalline magnetic particles are gaining attraction due co-precipitation, hot spraying, evaporation condensation, matrix
to many important applications such as ferrofluids, magnetic isolation, laser-induced vapor phase reactions and aerosols.
drug delivery, hyperthermia for cancer treatment [3–5]. Among Generally, in most types of nanoparticles prepared by these
the magnetic particles, cobalt ferrite (CoFe2 O4 ) is a well-known methods, control of size and size distribution is not possible [11].
hard magnetic material. The high coercivity [6] and moderate In order to overcome these difficulties, nanometer size reactors
magnetization [7] makes CoFe2 O4 a good candidate for many for the formation of homogeneous nanoparticles of cobalt ferrite
applications. The remarkable properties such as high saturation are used. To protect the oxidation of these nanoparticles from
magnetization, high coercivity, strong anisotropy along with good the atmospheric oxygen and also to stop their agglomeration,
mechanical hardness and chemical stability are not observed in the the particles are usually coated and dispersed in some medium
bulk sample [8]. These properties, along with their great physical like sodium dodecyl sulfate (NaDS) or oleic acid [12,13]. In
and chemical stability, make CoFe2 O4 nanoparticles suitable for general, the preparation methods for CoFe2 O4 nanoparticles have
magnetic recording applications such as audio and videotape been quite complicated requiring special techniques to prevent
and high-density digital recording disks etc. [9,10]. The magnetic agglomeration [14]. In this paper, we have presented the synthesis
character of the particles used for recording media depends of cobalt ferrite (CoFe2 O4 ) nanoparticles by sol–gel method
followed by heat treatment at 570 ◦ C.
The size and size distribution of the particles prepared by this
∗ Corresponding author. method was studied by XRD and TEM. The dependence of the
E-mail address: [email protected] (K.M. Jadhav). particle size on the annealing temperature and annealing time was
0038-1098/$ – see front matter © 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ssc.2008.06.040
480 B.G. Toksha et al. / Solid State Communications 147 (2008) 479–483

also studied. Finally, various magnetic properties of the particles

have been studied as functions of field, temperature and size.
60
Co Mossbauer spectroscopy is a nuclear-probe technique that
is very well suited for the investigation of the local symmetry,
the magnetic state, and the charge states of iron ions in iron-
containing materials. The Mossbauer analysis of prepared samples
is also presented in this paper.

2. Experimental procedure

Nanocrystalline powder of CoFe2 O4 were prepared by sol–gel

auto-ignition method. The A.R. Grade citric acid (C6 H8 O7 · H2 O),
Cobalt nitrate (Co(NO3 )2 6H2 O) (>99% sd-fine) were used as
starting materials. Reaction procedure was carried out in air
atmosphere without protection of inert gases. The molar ratio of
metal nitrates to citric acid was taken as 1:3. The metal nitrates
were dissolved together in a minimum amount of double distilled Fig. 1. X-ray diffraction pattern (Cu Kα -radiation) of CoFe2 O4 nanoparticles
water to get a clear solution. An aqueous solution of citric acid was prepared by sol–gel method, after calcinations at 570 ◦ C for 4 h.

mixed with metal nitrates solution, then ammonia solution was

slowly added to adjust the pH at 7. The mixed solution was kept on
to a hot plate with continuous stirring at 90 ◦ C. During evaporation,
the solution became viscous and finally formed a very viscous
brown gel. When finally all water molecules were removed from
the mixture, the viscous gel began frothing. After few minutes,
the gel automatically ignited and burnt with glowing flints. The
decomposition reaction would not stop before the whole citrate
complex was consumed. The auto-ignition was completed within a
minute, yielding the brown-colored ashes termed as a precursor. It
is known that the pure CoFe2 O4 obtained by the sol–gel method can
be formed at 570 ◦ C and thoroughly crystallized at temperatures
above 570 ◦ C [15] The as-prepared powders of all the samples were
heat treated separately at 570 ◦ C for 4 h to get the final product.
The final product obtained was then confirmed by X-ray
diffraction (XRD). The Rietveld’s powder structure refinement Fig. 2. TEM micrograph of CoFe2 O4 nanoparticles prepared, after calcinations at
570 ◦ C for 4 h.
analysis of XRD data is adopted to obtain the refined structural
parameter and lattice parameter. Particle size and particle
and 28 ± 2 nm were obtained. Finally, on further annealing, at
size distribution is done by transmission electron microscopy
1000 ◦ C for 8 and 12 h, respectively, 32 and 40 ± 2 nm particles
(TEM). Vibrating sample magnetometer (VSM) gave the values
were obtained. Thus, the size variation has been achieved by the
of saturation magnetization and coercivity. Mossbauer spectra of
annealing conditions.
samples were used to identify magnetic phase of cobalt ferrite.
The TEM images (Fig. 2) of CoFe2 O4 nanoparticles calcined at
Mossbauer spectra were recorded at room temperature using
570 ◦ C for 4 h (with average crystallite size of about 15 nm. The size
a constant acceleration drive and a personnel computer analyzer distribution of these nanoparticles as observed in TEM images is
(PCA card with 1024 channel). The source was 60 Co in Rh matrix at shown in Fig. 3. The distribution seems to be symmetric (Gaussian)
room temperature with an initial activity of 25 mCi. The optimal about 15 nm, with particles of sizes 11–20 nm for this specimen.
weight of the absorber was approximately 10 mg/cm2 of natural The maximum number lie between 14–16 nm, peaking at 15 nm,
iron. Metallic iron spectrum was used for the calibration of both in good agreement with XRD crystallite size. Most of the parti-
observed velocities and hyperfine magnetic field. cles appear spherical in shape however some elongated particles
are also present. Some moderately agglomerated particles as well
3. Results and discussion as separated particles are present in the images. Agglomeration is
understood to increase linearly with annealing temperature and
The analysis of X-ray diffraction pattern of the calcined therefore agglomeration at this temperature appears unavoidable.
powder synthesized using this route shows that the final product Fig. 4 shows the correlation between the particle size and
is CoFe2 O4 with the expected inverse spinel structure. X-ray annealing temperature. The size of the particles is observed to
diffraction pattern was indexed by TREOR program to calculate be increasing linearly with annealing temperature. It appears that
accurate unit cell dimension. The data were processed to realize that increase in size with temperature becomes rapid between
the conditions of the software program FullProof for the structure 700–900 ◦ C and appears to be slowing down above 900 ◦ C.
refinement. The XRD pattern is shown in Fig. 1. The value of While annealing generally decreases the lattice defects and strains,
lattice constant is found to be 8.3731 Å ± 0.004 Å. The inversion however it can also cause coalescence of crystallites that results
parameter calculated from Rietveld refinement is 0.82 which is in in increasing the average size of the nanoparticles [18]. The Fig. 5
good agreement for values reported in literature [16,17]. The value shows the dependence of particle size on annealing time at a
of discrepancy factor is 6.31 and expected value is 3.62 and the fixed annealing temperature of 570 ◦ C. The particle size appears
goodness of fit index was 1.74. to increase almost linearly with annealing time, most likely due
The size of the particles was determined by Scherrer formula to the fact that longer annealing time enhances the coalescence
using most incense (311) peak. The average sizes of the particles process resulting in an increase in the particle size. Thus, it appears
calcined at 570 ◦ C were found to be 15 nm. By annealing 15 nm that particle size may be controlled by varying either of the two
particles at 800 ◦ C and 900 ◦ C for 10 h, particle sizes of 24 parameters i.e. annealing temperature and time.
 B.G. Toksha et al. / Solid State Communications 147 (2008) 479–483 481

Fig. 3. Size distribution of CoFe2 O4 nanoparticles from TEM images (570 ◦ C

calcinations for 4 h). Fig. 6. Hysteresis loops for 15 nm CoFe2 O4 nanoparticles at room temperature
(300 K) and 77 K at maximum applied field of 12 kOe.

found to be 67 emu/g and remanent magnetization (Mr) was

30.2 emu/g, while at 77 K the values for the same parameters
were 43 emu/g and 35 emu/g, respectively. The very large
coercivity and low saturation magnetization at 77 K are may
be related with a pronounced growth of magnetic anisotropy
inhibiting the alignment of the moment in an applied field. The
remanance ratios at these temperatures indicate the same feature,
rising from 0.45 to 0.81 at 77 K. The value of remanance ratio
of 0.45 is close to that expected (0.5) for a system of non-
interacting single domain particles with uniaxial anisotropy [19].
The existence of an effectively uniaxial anisotropy in magnetic
nanoparticles has been attributed to surface effects [20,21] as
evidenced by simulations of nanoparticles. Surface effects also tend
to lead to large anisotropies. Some reports argued that due to
the disorder near the surface, the typical two sublattice picture
for antiferromagnetic or ferrimagnetic nanoparticles appears to
Fig. 4. Particle size (nm) as a function of annealing temperature (570 ◦ C) for break down and multiple sublattice picture appears to hold [22].
CoFe2 O4 nanoparticles.
There appears to be a situation where several different spin
configurations e.g. 2, 4, 6 sublattice models have very similar
energies and hence multiple ground states are possible e.g. in a
spinglass. The interaction between the core and surface spins leads
to a variety of effects including large anisotropy and exchange bias
effects. It is common to find higher effective anisotropy values in
magnetic nanoparticles as compared to their bulk counterpart.
In a fine particles system where the dominant mechanism is
replaced by the rotation of magnetic moment, with the assumption
that the particles are randomly oriented and the strain distribution
is homogeneous in the samples, b is described as [23]
 
1 8 4 3 4
b= K12 + 2
Ksh + λ2 σ 2 + Ksf2
MS2 105 15 5 15

where, K1 is the magneto-crystalline anisotropy constant, Ksh

the shape anisotropy constant, Ksf the surface anisotropy, λ =
|λS | the magnetostriction constant and σ the internal strain.
For simplicity and comparison with the bulk materials, here the
Fig. 5. Correlation between particle size and annealing time in hrs (at 570 ◦ C). effective magnetic anisotropy KE is defined as
9
Magnetic characterization of the particles was done using KE2 = Ksh
2
+ λ2 σ 2 + Ksf2 ,
vibrating sample magnetometer (VSM), at room temperature and 4
at 77 K, with maximum applied field up to 12 kOe (Fig. 6). so,
For the 15 nm size particles the coercivity at room temperature  
1 8 4
was 1215 Oe while at 77 K it had increased to ∼10.2 kOe. The b= K12 + KE2 .
saturation magnetization (MS ) obtained at room temperature was MS2 105 15
482 B.G. Toksha et al. / Solid State Communications 147 (2008) 479–483

In the approaching saturation region, b can be determined from

the approximation M = MS (1 − b/H 2 ) and MS can be obtained by
extrapolation of the line to the axis. From a fit of the magnetization
data at high fields using the law of approach to saturation

∂ M ∼ α Keff
2
χ= = .
∂H MS H 3
In the present study the value of the anisotropy constant is
Keff = 3.7 × 107 ergs/cc, where α = 0.524 for uniaxial
anisotropy and the value of anisotropy constant for 800 ◦ C is Keff =
3.2 × 106 ergs/cc. For the samples sintered at 570 ◦ C the value of
anisotropy constant is higher by one order of magnitude than the
value for bulk cobalt ferrite [24]. The value for samples sintered
at 800 ◦ C is very close to that of bulk samples. The coercivity
of the nanoparticles was also studied as a function of particle
size. Fig. 7. shows the coercivity as a function of particle size at
room temperature (300 K). The Gaussian fit to the data shows the
Fig. 7. The correlation between the coercivity (HC ) and mean particle diameter
coercivity increases with size rapidly, attaining a maximum value (nm), at room temperature and applied field of 15 kOe and saturation magnetization
of ∼1215 Oe at 25 nm and then decreases with size of the particles. (MS ) as function of particle size (nm) at maximum applied field of 15 kOe.
This decrease at larger sizes could be attributed to either of two
reasons. Firstly, it may be due to the expected crossover from single
domain to multidomain behavior with increasing size. Secondly
such an effect can arise from a combination of surface anisotropy
and thermal energies. The former effect is expected in CoFe2 O4
particles for a size close to 40 nm [25] that is significantly higher
than the critical size of 25 nm that we observed. The latter source
of the effect is therefore considered as a more likely explanation
for the peak. The initial increase of the coercivity with decreasing
size can be understood due to the enhanced role of the surface and
its strong anisotropy, as opposed to the weaker bulk anisotropy.
This rise is followed by a decline at small enough sizes when the
product of the anisotropy energy and volume becomes comparable
to the thermal energy, leading to thermally assisted jumps over
the anisotropy barriers. It is also likely that the two processes are
operating simultaneously and the single domain effects may not
be excluded, however the dominant role will be of the surface
effects for smaller particles. The decrease of Hc at d ≥ 40 nm may
very well have a contribution from the development of domain
Fig. 8. Temperature dependence of magnetic susceptibility for zero-field cooled
walls in the nanoparticles. Fig. 7 also shows the dependence of (ZFC) CoFe2 O4 nanoparticles at applied field of 5 kOe.
saturation magnetization on particle size. The MS values obtained
for the samples are in the range 50–76 emu/g. The maximum value shows the effect of size on the blocking temperature. There is
of saturation magnetization is 76 emu/g for 40 nm particles which a clear increase in the blocking temperature with size, it is also
is close to the bulk value for CoFe2 O4 . The saturation magnetization observed that this increase is very rapid in the beginning (at
increases consistently with particle size. For small particles the smaller sizes) and thereafter the increase becomes very slow
value of Ms is significantly lower than the bulk value of 80 emu/g appearing to reach a maximum at T ∼ 272 K. The larger particles
while for the size of ∼40 nm the magnetization value approaches seem to be blocked at high temperatures as compared to the
to the bulk value. A very sharp increase in the magnetization smaller particles at the same field. For larger particles, the larger
between the sizes of 10–25 nm is observed while there is a volume causes increased anisotropy energy which decreases the
slower increase thereafter, as in the case of coercivity and blocking probability of a jump across the anisotropy barrier and hence
temperature. The decrease in MS at small particle sizes is related the blocking is shifted to a higher temperature. From the data it
with the effects of the relatively non-reactive surface layer that appears that above about 25 nm the particle blocking becomes
has low magnetization. This surface effect becomes less significant relatively insensitive to size.
with increasing sizes and above 40 nm seems to be no longer The analysis of the Mossbauer spectra provides very important
relevant to the bulk magnetization. information about the chemical, structural and magnetic proper-
The magnetization of different size nanoparticles is shown as ties of ferrite samples from hyperfine interaction, isomer shift and
a function of temperature in Fig. 8. The samples were zero field quadrupole splitting. Mossbauer absorption spectra measured at
cooled (ZFC) to 77 K. After cooling a field of 5kOe was applied room temperature for cobalt ferrite powders annealed at 570 ◦ C
and magnetization was recorded as function of temperature up and 800 ◦ C temperatures are shown in Fig. 10. The Mossbauer spec-
to 300 K. A peak in the magnetization is evident in each case tra of samples are fitted with two six-line sub-patterns that are as-
with the exact position of the peak depending on the size. It signed to A-ions in tetrahedral sites and B-ions in octahedral sites
is understood that in the ZFC mode the magnetization of a of a typical spinel crystal structure. The value of average line width
collection of nanoparticles may go through a peak as the particles’ (mm/s) for samples sintered at 570 ◦ C hereafter called as sample
moments become blocked along the anisotropy axes. The blocking (a) and for samples sintered at 800 ◦ C hereafter called as sample
temperature (TB ) is defined as the temperature at which maximum (b) is found to be 0.539 ± 0.003 and 0.548 ± 0.003. It may be
magnetization is achieved. This temperature is a function of concluded from these values that increase in sintering tempera-
applied field and typical time scale of measurement. The Fig. 9 ture from 570 to 800 ◦ C do not much affect the site symmetry [26].
 B.G. Toksha et al. / Solid State Communications 147 (2008) 479–483 483

was no agglomeration and that the size distribution of the prepared

nanoparticles was small. The Rietveld-refined inversion parameter
value shows the cobalt ferrite in the present study have partially
inverted spinel structure. The size of the nanoparticles increase
linearly with annealing temperature and time most probably due
to coalescence that increases as annealing temperature increases.
The very large coercivity and low saturation magnetization at
77 K in comparison with room temperature appear to be due to
a pronounced growth of magnetic anisotropy at low temperatures.
The observed magnetization remanance ratio of 0.45 at room
temperature is close to the value of 0.5 typical of a system of
non-interacting single domain particles suggests that CoFe2 O4
nanoparticles exhibit an effective uniaxial anisotropy. The effective
uniaxial anisotropy in magnetic nanoparticles has been explained
as arising from surface effects that also lead to large anisotropy
energy in nanoparticles. The coercivity shows maxima with
particle size at a value much smaller than the single domain range
Fig. 9. Dependence of blocking temperature (TB ) on particle size (nm). and is attributed to the thermal effects which are prominent at
small particle sizes. For smaller particles the value of saturation
magnetization was significantly lower than the bulk value while
for the larger size particles the values were approaching to those
of the bulk. The smaller value of MS in smaller particles is attributed
to the greater fraction of surface spins in these particles that
tend to be in a canted or spin glass like state with a smaller net
moment. The coercivity of ferrite powder strongly depended on the
annealing temperatures and can be directly related to the variation
of cobalt ferrite particle sizes. The Mossbauer patterns of both
the samples (a) and (b) are sextet indicating there is a magnetic
coupling. Therefore, no doublet could be observed which is the
significance of the superparamagnetic state.

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