Materials Chemistry and Physics 264 (2021) 124442

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Materials Chemistry and Physics

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

Calcination effect on structural, morphological and magnetic properties of

nano-sized CoFe2O4 developed by a simple co-precipitation technique
Munmun Basak , Md. Lutfor Rahman *, Md. Farid Ahmed , Bristy Biswas , Nahid Sharmin
Institute of Glass and Ceramic Research and Testing (IGCRT), Bangladesh Council of Scientific and Industrial Research (BCSIR), Dhaka, 1205, Bangladesh

H I G H L I G H T S

• Mixed alkali (10% NaOH & Na2CO3 aqueous solution) was used as precipitating agent.
• SEM, DLS & Laser diffraction method were used to observe particle size distribution.
• Highest saturation magnetization was 168 emu/gm and coercivity was 500 Oe.
• All the properties showed strong dependence upon calcination temperature.
• 800 ◦ C was the suitable calcination temperature for CoFe2O4 nanoparticle synthesis.

A R T I C L E I N F O A B S T R A C T

Keywords: A thorough analysis of the calcination effect upon structural, morphological and magnetic properties of nano-
Ferrites sized cobalt ferrite (CoFe2O4) particles synthesized by co-precipitation technique has been demonstrated. A
Calcination mixed alkali as precipitating agent (mixture of Sodium hydroxide and Sodium carbonate) was used. The
Nelson-Riley function
developed samples were calcined at six distinct temperatures. The crystallinity, chemical state, morphology,
Magnetic material
elemental composition and magnetic property of the developed ferrites were investigated by using XRD, FT-IR,
SEM, EDS and PPMS respectively. The evaluation of crystallite size and lattice parameter has been performed by
the Debye–Scherrer’s formula and Nelson-Riley function respectively using XRD data. Average crystallite sizes
were in between 12 and 123 nm revealed from XRD. Average particle sizes were between 84 and 139 nm
estimated from SEM images. The crystallite size, particle size and magnetic properties of the CoFe2O4 nano­
particles exhibited strong reliance upon calcination temperature as increased continually. The coercivity of the
sample primarily increased afterwards decreased with increased calcination temperature. The results suggest that
co-precipitation method might render a propitious option for preparing superior quality cobalt ferrite nano­
particles. The synthesized nano-sized CoFe2O4 are promising for liquid black pigment for the decoration of
ceramic products through digital printing and sensing materials in humidity sensor.

1. Introduction by tailoring the materials [5,6]. Among many magnetic nanoparticles,

cobalt ferrite which is a cubic spinel ferrite [7], has been zealously
Nano-sized materials have been widely contemplated at an investigated for its high coercivity (Hc), medium saturation magnetiza­
increasing rate around the world over the past few decades, because of tion (Ms) [8–13], high magnetic permeability [14], high magnetic
its distinctive properties and unique functional applications hence anisotropy (380 kJ/m3) [15], high chemical stability, elevated me­
exhaustively studied by the researchers [1]. The magnetic nanoparticles chanical stiffness [16–19] and low cost [20]. These properties have
have exceptional properties as contrasted with bulk on account of the made cobalt ferrite a prominent candidate in the development of new
higher surface area to volume ratio, which successively is liable for cell thawing agents [21], magneto-optical devices [22], ceramic pre­
various extraordinary properties [2] for instance, spin canting [3,4], cursors [23], noncontact torque sensors [24], antenna rods [25], sensors
high field irreversibility, surface anisotropy, superparamagnetism, dis­ [26], actuators [27], photo magnetic materials [19,28,29], microwave
locations [4] etc. This makes them quite flexible for specific applications absorbers [30], and biomedical applications e.g. hyperthermia [31],

* Corresponding author.
E-mail addresses: lutforrahman@bcsir.gov.bd, lutforju33@yahoo.com (Md.L. Rahman).

https://doi.org/10.1016/j.matchemphys.2021.124442
Received 8 December 2020; Received in revised form 21 January 2021; Accepted 20 February 2021
Available online 25 February 2021
0254-0584/© 2021 Elsevier B.V. All rights reserved.
M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Table 1 retentivity and coercivity.

Synthesis route of CoFe2O4.
Samples Quantity/mol Co/Fe 2. Materials and methods
Ratio
Co Fe NaOH Na2CO3
(NO3)2⋅6H2O (NO3)3⋅9H2O Cobalt ferrite nanoparticles have been developed by co-precipitation
Calcined at 0.05 0.1 0.4 0.2 1:2
method using high purity Cobalt nitrate hexahydrate, Co(NO3)2⋅6H2O
300 ◦ C (Merck, Germany), Ferric nitrate nonahydrate, Fe(NO3)3⋅9H2O (Merck,
Calcined at 0.05 0.1 0.4 0.2 1:2 Germany), Sodium hydroxide pellets, NaOH (Merck, Germany) and
450 ◦ C Sodium carbonate, Na2CO3 (Merck, Germany) without any purification
Calcined at 0.05 0.1 0.4 0.2 1:2
and deionized water was used as prepared in the laboratory for the
600 ◦ C
Calcined at 0.05 0.1 0.4 0.2 1:2 preparation of aqueous solution. At first, a homogeneous mixture of
800 ◦ C Cobalt nitrate and Ferric nitrate was prepared by adding stoichiometric
Calcined at 0.05 0.1 0.4 0.2 1:2 amount of 0.5 M solutions of each ingredient with constant stirring using
900 ◦ C magnetic stirrer (Stuart, UC152D, UK). Thereafter, 10% NaOH and 10%
Calcined at 0.05 0.1 0.4 0.2 1:2
Na2CO3 solution were mixed homogenously which were used as
1000 ◦ C
precipitating agents and added dropwise to the salt solution. The num­
ber of moles with molar ratio of the precursors are shown in Table 1. The
medicine [32], magnetic resonance imaging (MRI) [33] and drug de­ reaction solution was thoroughly stirred and the pH increased to 13
livery [34,35]. The magnetization of cobalt ferrite nanoparticles de­ which indicates the completion of precipitation. The precipitate was
pends crucially on the magneto-crystalline anisotropy and particle’s then centrifuged and washed with deionized water for more than 10
size, shape and purity [36–39]. In case of CoFe2O4 nanoparticles, in the times to lower the pH at 7. Then, the precipitate was air dried at 110 ◦ C
presence of an applied magnetic field, the coercivity decreases towards for 16 h in a drying chamber (Binder, ED 53/E2, Germany). Finally, the
zero that means nanoparticles become superparamagnetic [40] after powder was calcined at 300 ◦ C, 450 ◦ C, 600 ◦ C, 800 ◦ C, 900 ◦ C and 1000
increased to a maximum coercivity value. When the applied magnetic ◦
C for 4 h in a muffle furnace (Nabertherm, LHT-8/16, Germany) to get
field is removed, the nanoparticles return to a non-magnetic state [41]. desired CoFe2O4 nanoparticles.
There are various techniques to synthesize nanoparticles out of
which co-precipitation method is the most promising for preparing nano 3. Results and discussions
ferrites in bulk scale because it produces homogeneous particles. Co-
precipitation is an inexpensive and straightforward route, where the 3.1. Structural analysis
control of size and distribution is attained by maintaining the relative
nucleation rates and growth while performing the preparation [41–43]. Crystallinity and phase identification of the CoFe2O4 have been
Co-precipitation reaction with controlled pH has been extensively studied by X-ray Diffractometer (model: Empyrean, PANalytical-
implemented as it gives highly crystalline and homogeneous materials Netherlands) with copper K-alpha radiation (λ = 1.540598 Å). It was
having rich textural properties [44]. In the current investigation, observed that all the diffraction pattern of the samples well matched
CoFe2O4 nanoparticles have been produced through co-precipitation with the spinel structure of cobalt ferrite (JCPDS Card # 22–1086) as
route and the consequences of thermal treatment have been observed shown in Fig. 1 and no impurity phases were identified in the XRD
by calcining the intermediate product at six distinct temperatures. The pattern. The XRD pattern exhibits 8 peaks appearing at 2θ = 18.28◦ ,
outcome of scrutinies have been studied in respect of crystallite size, 30.08◦ , 35.43◦ , 37.05◦ , 43.05◦ , 53.44◦ , 56.97◦ , 62.58◦ corresponding to
particle size, lattice parameter, zeta potential, saturation magnetization, the related miller indices [111], [220], [311], [222], [400], [422],

Fig. 1. X-ray diffraction pattern of CoFe2O4 samples calcined at distinct temperatures.

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Table 2 ( )
Effect of calcination temperature on crystallite size. 1 cos 2 θ cos 2 θ
f (θ) = + (3)
2 sin θ θ
Calcination Temperature (◦ C) Crystallite Size (nm)

300 12 Thereupon, the lattice parameters acquired from Bragg’s law are
450 16 plotted against the Nelson-Riley variables. The resultant data points
600 40 were investigated by a linear regression model where the y-intercept
800 72 gives the lattice parameter ‘a’ of the CoFe2O4 samples [55] as presented
900 92
in Fig. 2(a)-(f). Lattice parameter of all the samples were found close to
1000 123
the theoretical lattice parameter of cobalt ferrite which is 8.395 Å [56,
57]. The lattice parameter increases gradually and non-linearly during
[511], [440] respectively [35,45]. calcination up to 1000 ◦ C reaching a maximum value of 8.3818 Å.
The XRD spectra of as-synthesized particles calcined at 300 ◦ C ex­ The X-ray density “ρ”x of the prepared ferrites was calculated by
hibits broadened peaks, with insignificant intensity indicating the small equation (4).
crystallite size and ultra-fine nature of the particles as shown in Fig. 1(a).
8M
It may be assumed that the spinel cobalt ferrite phase initiation starts at ρx = (4)
NA a3
around 300 ◦ C.
The average crystallite sizes have been calculated from the highest where “M” is the molecular weight of the ferrites, “a” is the lattice
intensity [311] peaks utilizing the Debye–Scherrer’s formula [46,47] for parameter, “NA” is the Avogadro’s number and “8” is the number of
all the ferrites calcined at six distinct temperatures and the results were molecules per unit cell. The bulk density “ρ”b of the prepared ferrites was
recorded in Table 2. calculated by Archimedes’ principle. The percentage porosity “P” of the
kλ ferrite samples was calculated using equation (5).
D= (1)
βcosθ ρx − ρb
P= × 100% (5)
The gradual enhancement in intensity of diffraction peaks and nar­ ρx
rowing of the peak width is the manifestation of increase in crystallite Table 4 records the impact of calcination temperature on crystallite
size that demonstrate the improved crystallinity of the samples [48] size, lattice parameter, X-ray density, bulk density and porosity.
with the increase of calcination temperature [49,50]. This is often It is obvious that X-ray density decreases with increasing calcination
ascribed to the grain growth of the particles in the nano-region to reduce temperature as the lattice parameter increases. The bulk density of the
the surface energy. samples reflects the reverse behavior as of the X-ray density. Due to the
Lattice parameter was determined from the XRD pattern using presence of pores, X-ray density is higher than the bulk density which
Bragg’s Law [51]. The interplanar spacing is denoted by ‘d’, where ‘a’ is depends on the calcination conditions [58,59]. The porosity decreases
denoted as lattice parameter associated with the respective 2θ peak with calcination temperature as particles grow larger [60].
position value. The integers h, k and l are described as Miller indices [52, Fig. 3 shows the increase of crystallite size with calcination tem­
53]. perature for the CoFe2O4 samples. Crystallite size is the lowest at 300 ◦ C
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ and highest at 1000 ◦ C calcination temperature.
a = d h2 + k2 + l2 (2)
Fig. 4 presents the variation of lattice parameter with calcination
Moreover, the refined lattice parameter ‘a’ of the cobalt ferrite temperature for the CoFe2O4 samples. From the graph it is observed that
samples were calculated by using the Nelson-Riley function [54]. Using the lattice parameter is lowest at 300 ◦ C calcination temperature and
equation (3) a Nelson-Riley variable ‘f(θ)’ is calculated for 5 most highest at 1000 ◦ C calcination temperature.
intense peaks. The calculated results are recorded in Table 3(a)-(f).

Table 3
Calculation of lattice parameter by Bragg’s Law and Nelson-Riley function for the samples calcined at (a) 300 ◦ C, (b) 450 ◦ C, (c) 600 ◦ C, (d) 800 ◦ C, (e) 900 ◦ C, (f) 1000
◦
C.
(a) 300 ◦ C (b) 450 ◦ C

2θ ( )
◦
h k l a (Å) f(θ) 2θ (◦ ) h k l a (Å) f(θ)

30.2741 2 2 0 8.3435 3.6299 30.2419 2 2 0 8.3522 3.6343

35.7119 3 1 1 8.3319 3.0054 35.5821 3 1 1 8.3614 3.0182
43.4844 4 0 0 8.3179 2.3688 43.2127 4 0 0 8.3677 2.3875
57.5166 5 1 1 8.3194 1.6241 57.2522 5 1 1 8.3545 1.6351
63.2187 4 4 0 8.3138 1.4067 62.8812 4 4 0 8.3538 1.4187
(c) 600 ◦ C (d) 800 ◦ C
2θ (◦ ) h k l a (Å) f(θ) 2θ (◦ ) h k l a (Å) f(θ)
30.0672 2 2 0 8.3996 3.6579 30.1292 2 2 0 8.3827 3.6495
35.4760 3 1 1 8.3856 3.0288 35.4850 3 1 1 8.3835 3.0279
43.1397 4 0 0 8.3811 2.3926 43.1224 4 0 0 8.3843 2.3937
57.0315 5 1 1 8.3841 1.6444 57.0417 5 1 1 8.3828 1.6439
62.6682 4 4 0 8.3793 1.4262 62.6606 4 4 0 8.3802 1.4265
(e) 900 ◦ C (f) 1000 ◦ C
2θ (◦ ) h k l a (Å) f(θ) 2θ (◦ ) h k l a (Å) f(θ)
30.0693 2 2 0 8.3990 3.6576 30.1206 2 2 0 8.3851 3.6507
35.4307 3 1 1 8.3960 3.0333 35.4750 3 1 1 8.3858 3.0289
43.0861 4 0 0 8.3911 2.3963 43.1190 4 0 0 8.3850 2.3940
56.9942 5 1 1 8.3891 1.6459 57.0387 5 1 1 8.3832 1.6441
62.3797 4 4 0 8.3884 1.4365 62.6355 4 4 0 8.3832 1.4274

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Fig. 2. Determination of lattice parameter by Nelson-Riley function of cobalt ferrite samples calcined at distinct temperatures.

Table 4
Impact of calcination temperature on several parameters.
Calcination Temperature (◦ C) Crystallite Size (nm) Lattice Parameter (Å) Molecular Weight X-ray density Bulk density Porosity
“M” (gm/mol) “ρx” “ρ b ” “P” (%)
Kg/m3 Kg/m3

300 12 8.2957 234.62 5425.29 2899.63 46.55

450 16 8.3568 234.62 5307.16 3812.04 28.17
600 40 8.3687 234.62 5284.55 4097.01 22.47
800 72 8.3807 234.62 5261.89 4725.66 10.19
900 92 8.3809 234.62 5261.51 4849.31 7.83
1000 123 8.3818 234.62 5259.82 4971.97 5.47

3.2. FTIR analysis recorded by Fourier Transform Infrared Spectrometer (Model-

IRAffinity-1S, MIRacle 10, Shimadzu, Japan). FTIR spectra of co-
1
FTIR spectrum between 3500 and 400 cm− ranges have been precipitated CoFe2O4 calcined at 300–1000 ◦ C are presented in Fig. 5.

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

The two IR absorption bands are found at 594 and 447 cm− 1 owing to
the Metal-Oxygen stretching vibrations in the tetrahedral and octahe­
dral sites of spinel ferrites [61] respectively. The two bands observed at
594 and 447 cm− 1 for the CoFe2O4 are consistent with those reported in
literature [62,63]. No band have been observed between 3500 and 3000
cm− 1 for the stretching vibration of O–H bonds of physically adsorbed
H2O on particle surface as the samples were dried in oven before anal­
ysis. The FTIR results proved that the samples had a spinel structure of
CoFe2O4.

3.3. Morphological analysis

Scanning Electron Microscopy (MA15 VP-SEM, Carl Zeiss Evo, UK)

was used to analyze the morphology of CoFe2O4 nanoparticles. Fig. 6
shows the SEM micrographs of CoFe2O4 samples calcined at six distinct
temperatures.
From SEM pictures using Image J software, average particle size has
been calculated as listed in Table 5.
The particle size distribution histograms have been displayed as an
Fig. 3. Variation of crystallite size with calcination temperature. inset in Fig. 6(a)–(f). The average particle size was observed bigger than
the crystallite size achieved from the X-ray diffraction data [64]. Higher
surface area to volume ratio is responsible for the resulted agglomera­
tion [65] which yielded several crystallites to join together to form
larger particle and also because of the grain growth at higher calcination
temperature for the minimization of Gibbs free energy resulting from the
reduction of extended surface area of nanoparticle [65,66]. The particles
are found in a nearly spherical shape and some agglomeration is evi­
denced from the SEM micrographs. For the sample calcined at 1000 ◦ C,
the particle size distribution is found uniform and the particles are seen
to be closely compacted [60]. Therefore, the porosity of that sample is
lowest which is in agreement with the results recorded in Table 5.

3.4. Elemental analysis

The elemental analysis was conducted by Energy Dispersive Spec­

troscopy (EDS) (EDAX Team, EDAX, USA) for exploring the presence of
elements and their percentage composition [67] in the CoFe2O4 sam­
ples, which is shown in Fig. 7 and Table 6.
The nanoparticles calcined at different temperatures presented
composition with the Co/Fe atomic ratio very close to the stoichiometric
value of 0.5. It is menifested that the atomic ratios of Co:Fe are very close
to 1:2. The EDS spectra of the sample calcined at 300 ◦ C shows that the
Fig. 4. Variation of lattice parameter with calcination temperature. Co/Fe ratio is 0.39 which is relatively lower to the theoretical value.
These may be due to the incomplete formation of CoFe2O4 at 300 ◦ C
which is also evident from the XRD data. The leading signals of Cobalt,
Iron and Oxygen in the EDS spectra substantiate the successful pro­
duction of CoFe2O4 nanoparticles. No other signals were detected that
discloses the non-existence of contamination in the samples. The atomic
weight percentage of oxygen does not match the expected percentage
because EDS is not really suitable for light elements (like O). It can
detect the presence of oxygen, but the quantification is uncertain.

3.5. Electrical properties

The zeta potential of the prepared cobalt ferrite nanoparticles was

measured in water as dispersant at neutral pH by Zetasizer (SZ-100,
HORIBA Scientific Ltd, Japan). The samples for the measurement of zeta
potential were prepared by taking 10 mg of as prepared cobalt ferrite in
100 ml of deionized water. Then it was sonicated using an ultra­
sonication bath for 1 h. After settling down the solution was ready for
measuring zeta potential [68]. The stability state of cobalt ferrite
nanoparticles was studied by zeta potential values and displayed in
Fig. 8 and Table 7.
The zeta potential of cobalt ferrite samples calcined at 300 ◦ C, 450
Fig. 5. FTIR pattern of CoFe2O4 samples calcined at distinct temperatures.
◦
C, 600 ◦ C, 800 ◦ C, 900 ◦ C and 1000 ◦ C is − 38.5 mV, − 47.6 mV, − 39.2
mV, − 59.5 mV, − 46.4 mV, − 9.5 mV respectively. Particles having zeta

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Fig. 6. SEM image of CoFe2O4 nanoparticles calcined at distinct temperatures.

thus represents instability of the solution.

Table 5
SEM results of Cobalt ferrite particles calcined at different temperature.
Calcination Temperature (◦ C) Average Particle Size (nm) 3.6. Particle size analysis
300 C
◦
84
450 ◦ C 88
3.6.1. Particle size analysis by laser diffraction method
600 ◦ C 92 The particle size distribution as observed by particle size analyzer
800 ◦ C 94 (Mastersizer 3000, Malvern Instruments Ltd, UK) following wet
900 ◦ C 101 dispersion method using deionized water as dispersing agent is shown in
1000 ◦ C 139
Fig. 9.
This method is based on laser diffraction technique. The distribution
potentials value higher than +30 mV or lower than − 30 mV are regar­ seems to be closely symmetric. CoFe2O4 particles calcined at 300 ◦ C,
ded stable [69]. As zeta potential values are lower than − 30mV for 5 450 ◦ C, 600 ◦ C, 800 ◦ C, 900 ◦ C and 1000 ◦ C present highest peak value in
samples, the solutions are considered stable. The high negative value for the region between particle sizes of 29.1 μm and 43.4 μm. The specific
the ferrites obtained at 800 ◦ C calcination temperature proves the surface area were 81.89 m2/kg, 65.91 m2/kg, 65.68 m2/kg, 75.07 m2/
repulsion between the particles and thus increases the stability of the kg, 57.82 m2/kg, 59.15 m2/kg respectively. An elaborated particle size
solution [70]. The low negative value of − 9.5 mV for the sample ob­ analysis report of synthesized CoFe2O4 samples are recorded in Table 8.
tained at 1000 ◦ C indicates that the particles settle down rapidly and Particle size analyzer gives hydrodynamic diameter, so the results are
not in agreement with SEM results. Hydrodynamic diameter is always

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Fig. 7. EDS spectra of cobalt ferrite samples calcined at distinct temperatures.

Table 6
EDS results of Cobalt ferrite particles calcined at different temperature.
Calcination Temperature (◦ C) Atomic Weight (%) Co/Fe

Co Fe O

300 ◦ C 6.27 15.74 77.99 0.39

450 ◦ C 10.85 18.43 70.72 0.59
600 ◦ C 11.34 17.80 70.85 0.63
800 ◦ C 10.31 18.63 71.01 0.55
900 ◦ C 10.44 18.64 70.92 0.56
1000 ◦ C 10.30 17.89 71.81 0.57

much larger than the size estimated by SEM [71].

3.6.2. Particle size analysis by dynamic light scattering

The size distribution of the particles were also observed by Zetasizer
(SZ-100, HORIBA Scientific Ltd, Japan) which is based on dynamic light
scattering is shown in Fig. 10.
The distribution also appears to be closely symmetric. It can be noted
that CoFe2O4 calcined at 300 ◦ C, 450 ◦ C, 600 ◦ C, 800 ◦ C, 900 ◦ C and
1000 ◦ C present highest peak in the region 316 nm, 394 nm, 451 nm,
460 nm, 554 nm, 675 nm respectively. It is clearly demonstrated from
the curve that the mean particle size distribution curve shifts towards
larger particle size as the calcination temperature increases which is
concomitant with overall experimental finding. An elaborated investi­
gation report of the CoFe2O4 nanoparticles is recorded in Table 9. The
zetasizer also gives hydrodynamic diameter which is achieved including
the hydration layer and other molecules linked to the layer. But from
SEM, obtained particle diameter i.e., particle size is related to the
dehydrated sample [72] so the particle size is lower than the size esti­
mated by zetasizer.
Fig. 8. Zeta potential pattern for CoFe2O4 nanoparticles calcined at distinct
temperatures.

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Table 7
Zeta potential report of the CoFe2O4 samples.
Calcination Temperature (◦ C) Zeta potential (mV)

300 C◦
− 38.5
450 ◦ C − 47.6
600 ◦ C − 39.2
800 ◦ C − 59.5
900 ◦ C − 46.4
1000 ◦ C − 9.5

Fig. 10. Particle size distribution by dynamic light scattering method of

CoFe2O4 nanoparticles calcined at distinct temperatures.

Table 9
Particle Size Analysis report by dynamic light scattering method of the CoFe2O4
samples.
Calcination Temperature (◦ C) Average Particle Size (nm)

300 ◦ C 316
450 ◦ C 394
600 ◦ C 451
800 ◦ C 460
900 ◦ C 554
Fig. 9. Particle size distribution by laser diffraction method of CoFe2O4
1000 ◦ C 675
nanoparticles calcined at distinct temperatures.

Table 8
Particle size analysis report by laser diffraction method of the CoFe2O4 samples.
Calcination 10% Particles 50% Particles 90% Particles
Temperature (◦ C) Size (μm) Size (μm) Size (μm)

300 ≤5.55 ≤29.1 ≤115

450 ≤7.29 ≤38.8 ≤189
600 ≤7.11 ≤40.3 ≤165
800 ≤6.41 ≤33.4 ≤126
900 ≤7.49 ≤43.4 ≤301
1000 ≤8.23 ≤35.2 ≤110

3.7. Magnetic properties

Magnetic measurements of the CoFe2O4 samples was performed by

Physical Property Measurement Systems (PPMS) at room temperature
under the applied magnetic field of 20 kOe. Magnetic measurements for
all the samples were performed and the hysteresis loops are presented in
Fig. 11.
Saturation magnetization (Ms), retentivity (Mr) and coercivity (Hc) of
the samples are recorded in Table 10. The magnetic measurement at
room temperature show that the coercivity primarily rises and after­ Fig. 11. Magnetic hysteresis loops of CoFe2O4 nanoparticles calcined at distinct
wards drops with increased calcination temperature after 800 ◦ C while temperatures.
the saturation magnetization and retentivity continuously increases
linearly. Particle size is directly proportional to magnetic domain size magnetization and coercivity attributed to the escalation of magnetic
[73]. As the magnetic domain size increases, the atomic spin numbers anisotropy of the ferrite particles which hinder the magnetic moment
increase correspondingly towards applied magnetic field, thus the from aligning in an applied field. The magnetic anisotropy (K) values are
saturation magnetization increases. The saturation magnetization and calculated by equation (6) [74] and listed in Table 10.
retentivity of the samples increase with increasing particle size as the
MS × HC
calcination temperature increases, which arise from the spin K= (6)
non-collinearity at the crystal surface. The raise in saturation 0.96

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M. Basak et al. Materials Chemistry and Physics 264 (2021) 124442

Table 10
Effect of calcination temperature on saturation magnetization (Ms), retentivity (Mr), coercivity (Hc), magnetic anisotropy (K) and rectangular ratio (RS).
Calcination Temperature (◦ C) Saturation magnetization Retentivity Coercivity Magnetic anisotropy Rectangular ratio RS
Ms (emu/gm) Mr (emu/gm) Hc (Oe) K × 103 (erg cm− 3) Mr/Ms

300 31 3 180 5.81 0.097

450 53 12 400 22.08 0.226
600 97 22 450 45.46 0.227
800 109 29 500 56.77 0.266
900 112 32 480 56.00 0.286
1000 168 33 330 57.75 0.196

values indicate that the ferrites are soft magnet with characteristic of
single domain nanoparticles [73]. As the RS value is less than 0.5, the
particles interact by magnetostatic interactions [76]. The magnetostatic
interactions are responsible for the agglomeration [77] of CoFe2O4
nanoparticles which is manifested from SEM images as well.
The growth in particle size from single domain size with the increase
of calcination temperature is responsible for the primary increase in
coercivity. The decrease in coercivity on further calcination after 800 ◦ C
is owing to the development of multi-domains beyond the critical size i.
e., single-domain size limit of CoFe2O4 nanoparticles. Fig. 12 and Fig. 13
shows the changes in saturation magnetization and coercivity with ris­
ing calcination temperature respectively.

4. Conclusion

Cobalt ferrite nanoparticles have been developed successfully by

using co-precipitation route and calcined at 6 different temperatures.
The XRD spectra of CoFe2O4 samples possessed the cubic spinel ferrite
structure, supported by FTIR results. The size and shape of CoFe2O4
nanoparticles and incorporation of cobalt and iron content were
Fig. 12. Variation of Saturation magnetization with calcination temperature. confirmed with the help of SEM and EDS experiments, respectively. The
SEM images, Zetasizer and Particle size analyzer give a clear idea
regarding the particle size and distribution of spinel nanoparticles and
the results are in good agreement with each other. At 800 ◦ C calcination
temperature, crystallite size of 72 nm, particle size of 94 nm and highest
zeta potential of − 59.5 mV having high coercivity value of 500 Oe were
achieved. So the optimum sample can be obtained at calcination tem­
perature 800 ◦ C. This analysis recommend that high quality CoFe2O4
nanoparticles can be prepared by using mixture of alkali (Sodium hy­
droxide and Sodium carbonate) as precipitating agent.

CRediT authorship contribution statement

Munmun Basak: Investigation, Data curation, Formal analysis,

Software, Writing – original draft, Writing – review & editing. Md.
Lutfor Rahman: Conceptualization, Methodology, Supervision, Project
administration, Visualization, Writing – review & editing. Md. Farid
Ahmed: Validation, Writing – review & editing. Bristy Biswas: Vali­
dation, Writing – review & editing. Nahid Sharmin: Project adminis­
tration, Supervision, Writing – review & editing, Funding acquisition.

Declaration of competing interest

Fig. 13. Variation of coercivity with calcination temperature. The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
The magnetic anisotropy is dependent on nanoparticles’ degree of the work reported in this paper.
crystallinity [75], surface area to volume ratio and modification in
interparticle interactions. Acknowledgements
The rectangular ratio (RS) calculated from equation (7) which is a
measure of how easy the direction of magnetization re-orient after The work has been carried out in Ceramic Raw Materials & Ceramic
withdrawal of the magnetic field to the closet easy axis. Materials Testing Division, Institute of Glass and Ceramic Research &
Mr Testing (IGCRT), Bangladesh Council of Scientific and Industrial
RS = (7) Research (BCSIR), Dhaka, Bangladesh. The authors thank Glass
Ms
Research Division, IGCRT, BCSIR, Dhaka, Institute of Fuel Research &
Rectangular ratio (RS) is obtained within the range of 0.09–0.28. The Development, IFRD, BCSIR, Dhaka for providing technical supports.

9
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