IJE TRANSACTIONS B: Applications Vol. 33, No.

5, (May 2020) 877-884

International Journal of Engineering

Journal Homepage: www.ije.ir

Physical and Magnetic Properties Comparison of Cobalt Ferrite Nanopowder Using

Sol-gel and Sonochemical Methods
P. Puspitasari*a,b, L. S. Budia
a Department of Mechanical Engineering, Faculty of Engineering, State University of Malang, Indonesia
b Centre of Advanced Materials for Renewable Energy, State University of Malang, Indonesia

PAPER INFO A B S T R A C T

Paper history: Cobalt ferrite or CoFe2O4 has unique physical and magnetic properties depend on its synthesis method.
Received 18 February 2020 The application of cobalt ferrite as nanomedicine material become more interesting, however analysis
Received in revised form 20 March 2020 on physical and magnetic properties based on synthesis method have not been discussed. The cobalt
Accepted 10 April 2020 ferrite in this research was synthesised using two different methods: the sol-gel with duration sintering
variations of 500℃, 800℃, and 1100℃ and unsintered sonochemical. The phase identification
Keywords: analysis and crystal size used XRD and morphology analysis used SEM, the functional group bond
Phase Identification analysis used FTIR, and magnetic property analysis used VSM. The smallest crystal size from the XRD
Morphology result was 13.25 nm with 57.04% crystallinity. The morphology from the synthesized cobalt ferrite
Hysteresis Curve was mostly agglomerated. The FTIR showed functional group vibration at 601-636 cm-1 that signified
Hyperthermia the spinel structure of the cobalt ferrite. There was a change of hysteresis loop curve from hard
magnetic to soft magnetic, and there was a sample with a paramagnetic curve.
doi: 10.5829/ije.2020.33.05b.20

NOMENCLATURE
D Crystalline diameter (nm) A XRD diagram sample area
k Corrective Constants (0.9) R Remanence Ratio
λ Wavelength (1.5406 Å) Mr Magnetic Remanence (emu/g)
FWHM Full-width half maximum (the peak value in radians) Ms Magnetic Saturation (emu/g)
θ Peak angle (degree) HC Coercivity (Oersted)
It Crystalline peak intensity K1 Constant Anisotropy (erg/g)
Ia Amorphous area intensity μ0 Permeability of Free Space (H/m)
Acr Area of crystalline XRD diagram SLP Specific Loss Power (W/g)
CI Crystallinity Index

1. INTRODUCTION1 Nowadays, researchers pay attention to nanomaterial

ferrite because of its wide application such as in
In the recent years, the fast development of nanomaterial biotechnology, for catalyst, ferrofluid, and magnetic
and its application depends on synthesis methods for material [3]. Ferrite, as an excellent magnetic material,
desired properties than the base material at nanoscale attracts scientists and is continuously developed. Apart
compared to macro scale [1]. Industry always needs a from ferrite, cobalt also has some particular property as
cheap but high-quality material, and thus, research magnetic material, for example, medium magnetization
continues and progresses to produce advanced material saturation, strong anisotropy, high coercivity value at
or nanomaterial. The example is nanomaterial synthesis room temperature, stable chemical property and high
from the metal-oxide type that quickly develops due to curie temperature [2]. Hence, when combined into cobalt
its significant ability in its application [2]. ferrite (CoFe2O4), it has a unique magnetic property and
*
Corresponding Author Institutional Email: [email protected]
(P. Puspitasari)

Please cite this article as: P. Puspitasari, L. S. Budi, Physical and Magnetic Properties Comparison of Cobalt Ferrite Nanopowder Using Sol-gel
and Sonochemical Methods, International Journal of Engineering (IJE), IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-
884
878 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884

is applied as supercapacitor and anode in Li-ion battery glycol and was stirred for 2 hours with rotation speed of
[4]. Cobalt Ferrite can also be used in medical 200 rpm. Then, the solution was stirred and heated at
applications because of the magnetic properties. 80℃ with a rotation speed of 200 rpm until it turned to
Hyperthermia is one of a modality cancer treatments at gel. Gel formation occured in about 16.5 hours. After
elevated temperature between 41 ℃ and 45 ℃ and that, the sample was dried in the microwave oven for 7
treatment time of at least 30 minutes has been paid hours at 100℃. After drying process, the sample was
considerable attention due to its clinical efficacies, such grinded by agate mortar for 1 hour.
as minimizing clinical side effects and can selectively
destroy a localized or a deeply seated cancer tumor by 2. 3. The Sonochemical Method The base material
heating with magnetic field [5]. Well-dispersed cobalt in this research were 2.951 g Cobalt(II) nitrate
nanoparticles in the hyperthermia application give hexahydrate (Co(NO3)·6H2O with 99% purity, 8.08 g
effective and controlled heat generation [6]. Iron(III) nitrate nonahydrate (Fe(NO3)·9H2O with 99%
Cobalt ferrite (CoFe2O4) has unique physical purity that were bought from Merck and dissolved into
and mechanical properties and widely applicated in 100 ml DI Water. The mixture was stirred for 1 hours
nanomedicine [6], supercapacitor and anode in Li-ion with rotation speed of 200 rpm. Then, the solution was
battery [4]. Cobalt ferrite is a hard magnetic material with stirred and heated at 80℃ with the rotation speed of 200
high Curie temperature (520℃), high coercivity of rpm until it turned to gel. After, the sample was sonicated
around 4.3 kOe at room temperature for single domain for 30 minutes and titrated with 100 ml sodium hydroxide
with the size of 40 nm, medium saturation magnetization 10 M, washed with 750 ml distilled water for three times
of 80 emu/g for bulk material at room temperature, high and dried in the microwave oven at 100℃. The sample
anisotropy constant (2.65 x 106 – 5.1 x 106 erg cm-3) and was then grinding by agate mortar for 1 hour.
high magnetostrictive (-225 x 10-6). Besides, cobalt
ferrite shows excellent chemical stability, mechanical 2. 4. Characterization The powder from the sol-gel
hardness, wear resistance, easy to synthesis, and and sonochemical synthesis methods each had yellowish-
electrical isolation. The above properties make cobalt brown and darkish black colour. The cobalt ferrite from
ferrite as one of the promising candidates in various two methods then characterized to find the phase
applications. identification and crystallite size using the X-Ray
The magnetic property of CoFe2O4 depends on the Diffractometer (XRD) PAN Analytical Cu Kα (λ = 1.54
grain size and cation distribution in the form of Å), morphology of CoFe2O4 obtained from Scanning
tetrahedral and octahedral lattice [7]. Several synthesis Electron Microscopy of Phenom, the functional group
methods to produce CoFe2O4 nanomaterial in a right was observed using Fourrier Transform Infrared
nanometric scale are sol-gel and sonochemical [2, 8,9]. (Shimadzu) and the magnetic properties were obtained
To date the researcher still find the best synthesis from Vibrating Sample Magnetometer of OXFORD 1.2H
methods to obtain single phase CoFe2O4 resulted in the at room temperature.
best magnetic properties. This research surprisingly
describe how CoFe2O4 magnetic properties changing
from hard magnetic to soft magnetic material as the 3. RESULTS AND DISCUSSION
sintering temperatures varied and also study the
comparison of two synthesis methods which are sol-gel 3. 1. Phase Characterization The polycrystalline
and sonochemical in term of physical and magnetic material properties depend on the crystal size and this fact
properties.

2. MATERIALS AND METHODS

2. 1. Material Preparation Raw material for cobalt

ferrite is Cobalt(II) nitrate hexahydrate (Co(NO3)·6H2O
with 99% purity, Iron(III) nitrate nonahydrate
(Fe(NO3)·9H2O with 99% purity that were purchased
from Merck and ethylene glycol supplied from Merck.

2. 2. The Sol-gel Method The base material in this

research was 1.4505 g Cobalt(II) nitrate hexahydrate
(Co(NO3)·6H2O with 99% purity, 4.4 g Iron(III) nitrate
nonahydrate (Fe(NO3)·9H2O with 99% purity that were Figure 1. Phase Identification of CoFe2O4 with Different
bought from Merck and dissolved into 50 ml ethylene Sintering Temperature and Methods
 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884 879

TABLE 1. Intensity, FWHM, d-spacing, Crystallite Size of CoFe2O4 and Cristalinity

X-Ray Diffraction Corresponding to [311] peak
Sample Material Crystallinity (%)
Intensity (counts) FWHM (rad) d-spacing (Å) Crystallite Size (nm)
CoFe2O4 Sonochemical 24.74 0.0034 2.35897 42.71 44.17
CoFe2O4 Sol-Gel Sintering 500℃ 69.05 0.0101 2.51587 13.25 57.04
CoFe2O4 Sol-Gel Sintering 800℃ 226.88 0.0024 2.52141 60.5 57.67
CoFe2O4 Sol-Gel Sintering 1100℃ 428.55 0.0021 2.52602 70.64 57.71

triggered several decades of research to find the size material until 70.64 nm at sintering temperature
nanomaterial with the best crystal size. Therefore, it is 1100, but it did not happen with the crystallinity in the
essential to measure the crystallite size of the range of 500 to 1100℃ sample. The crystallinity of the
polycrystalline material accurately. The crystallite size sample was saturated for 57% from 500℃ until 1100℃
was calculated using the Scherrer equation [10,11]. but increasing the crystallinity unsintered sample which
𝑘× 𝜆 was 44.17% crystallinity to 57.04%.
𝐷= (1)
𝐹𝑊𝐻𝑀×cos 𝜃
3. 2. Morphological Characterization The
Crystallinity percentage in the samples were taken
observation and comparison of morphology form were
into consideration because crystallinity influences the
conducted using SEM. This analysis aimed to find the
phase and physical property. Crystalinity percentage or
morphological change of CoFe2O4 from different
Segal CI (Crystallinity Index) was found by Segal et al.
synthesis method and different sintering temperature.
[12] and formulated as peak crystalline area divided by
the amorph area as shown below [13]:
𝐼𝑡−𝐼𝑎
𝐶𝐼 = × 100% (2)
𝐼𝑡

Or,
𝐴𝑐𝑟
𝐶𝐼 = × 100% (3)
𝐴

Figure 1 shows the significant crystallinity difference

between both methods. As-sintered CoFe2O4 displays
better crystallinity chart whereas the unsintered sample
has lower crystallinity. Unsintered CoFe2O4 crystallinity
percentage was 44.17% while the sintered samples had
around 57% crystallinity. Although the sintered samples
had different temperatures, but the percentage did not Figure 2. Crystallinity Area Measurement of CoFe2O4 with
significantly change since at 500℃ temperature. Figure 500℃ Sintering Temperature
2 presents the calculation using Equation 3 above and
calculated using OriginPro software. There are peaks on
Figure 1: 220, 311, 400, and 511, that were the phase
identity of CoFe2O4 [14]. The same peak of 311 from
sintered samples showed that the crystallinity was single
phase [12].
Table 1 shows the crystal size and crystallinity index
of CoFe2O4 that were synthesized using unsintered
sonochemical and sintering sol-gel for 2 hours and
holding temperature variations (500℃, 800℃, and
1100℃). The smallest crystal size was found in the
CoFe2O4 sample sintered at 500℃ with the value of
13.25 nm. The most significant crystallinity percentage
was found in the CoFe2O4 sample sintered at 1100℃,
with a value of 57.71%.
Based on Figures 3(a) and (b), an increase in the
temperature of sintering causing grown to the crystallite (a)
880 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884

(a)

(b)
Figure 3. Comparison Effect of Sintering CoFe2O4 Samples,
(a) Sintering Temperature and Crsytallite Size, (b) Sintering
Temperature and Crystallinity

Figure 4(a) displays that unsintered sonochemical

CoFe2O4 has morphological magnification of 25k. The
grains are not homogenous but agglomerated and
covered by cylindrical shape that extends into taper in
various sizes, from the smallest of 34.63 nm up to the
largest of 42.48 nm. Figure 4(b) presents the sintered
CoFe2O4 at 500℃ with 10k magnification, and the (b)
easiest spotted grain sizes are 65.94 nm up to 74.92 nm.
Meanwhile, Figure 4(c) shows the sintered CoFe2O4 at
800℃ with 10k magnification. The observed grains are
between 59.79 nm until 73.72 nm. Figure 4d displays the
sintered CoFe2O4 at 1100℃ with 10k magnification. The
grain sizes start from 50.98 nm up to 56.98 nm.
The SEM image analysis present that agglomeration
in all samples was still high as observed the decreasing
agglomeration from the sintering at 500°–1100℃ due to
the crystalline development in the sintering process [15].
The crystalline growth caused the grain size in SEM
morphology to be small. The sintered CoFe2O4 at 500℃
had crystal size of 13.25 nm and SEM results around 70
nm, the crystal size continued to grow up to 70.64 nm (c)
with the grain size from SEM results was 52 nm for
sintered CoFe2O4 at 1100℃. The sonochemical CoFe2O4
had a crystal size of 42.71 nm, and the SEM grain results
were around 27 nm. However, it had the lowest
crystallinity percentage than the other three samples with
a value of 44.17%. Sintering causes crystal size to grow
and lower the agglomeration, as shown in Figure 4d
where the agglomeration was reduced compared to other
samples. High agglomeration was a possibility caused by
Van der Waals forces that weaken the bonds between
particle [16]. In general, the SEM grain was spherical, but
some was elongated.
(d)
3. 3. FTIR Analysis The FTIR spectrum was used to Figure 4. Morphology of CoFe2O4, (a) Sonocehmical
identify the chemical compound structure and found the without Sintering, (b) Sol-gel 500℃ Sintering, (c) Sol-gel
spinel phase formation of the synthesized CoFe2O4 [16]. 800℃ Sintering, (d) Sol-gel 1100℃ Sintering
 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884 881

Figure 5 shows the comparison of the FTIR spectrum other molecules and thus make the intensity to decrease
from four samples with three main zones analysis. There [19]. Also different methods proved that sol-gel samples
are several peaks based on various treatments in the first had higher water content as seen from the peak intensity
zone, 636 cm-1 for sonochemical method, sol-gel 500℃ of the second zone and the third zone because the
sintering 601 cm-1, sol-gel 800℃ sintering 619 cm-1and synthesis process form sol then followed by liquid
sol-gel 1100℃ sintering 623 cm-1.The first zone was compaction into a gel that will not be separated easily
indicated the area stretching vibration from the metal- from the content of water molecules in it.
oxygen (M–O, where M = Co or Fe) that showed identity 𝑀𝑟
and finger print zone from the CoFe2O4 absorption band 𝑅= (4)
𝑀𝑠
[17].
The difference in the absorption position in the first 3. 4. Magnetic Properties Analysis The magnetic
zone that was the fingerprint of CoFe2O4 due to the property of CoFe2O4 that was synthesized was obtained
crystal size are variated. The variated crystal size will from the VSM test such as magnetic saturation (Ms),
make difference distance between Fe3+-O2- then the magnetic remanence (Mr), and coercivity (Hc) [20]. Ms is
absorption will slightly difference between the samples. the maximum value of magnetization that is received
The second zone compound several peaks based on the from the given magnetic field. The value of Mr can be
samples, there are 1456 cm-1 for sonochemical method, taken from the intersection of curves that intersect with
sol-gel 500℃ sintering 1531 cm-1, sol-gel 800℃ the vertical axis. Hc is the magnetic field intensity needed
sintering 1427 cm-1, sol-gel 1100℃ sintering 1409 cm-1. to make the magnetic sample reach zero magnetization
The second zone indicated bending vibration and after achieving magnetization saturation. Remanence
stretching vibration from the hydroxyl (-OH) functional ratio is the ability of magnetic material to change the
group as one of the characteristics of water absorption curve in the hysteresis loop curve after the magnetic field
bands [18] the adsorbed water is featured by the bands at is removed [21]. The value of parametere above was
1409-1531 cm-1assigned to the δ H-O-H bonding mode described in Table 2. Remanence ratio can be formulated
[19]. From the second zone, we can imply that water [22].
molecules does not get totally remove from the sample
although there are several heat treatments applied to the
samples.
The third zone had several differences, but for the
sonochemical CoFe2O4, peak 3423 cm-1 and 3412 cm-1
could not be observed as well as the spectrum of the
sintered sample at 1100℃. The both peaks have been
assigned to antisymmetric and symmetric O-H stretching
vibration of lattice water. Thus, this situation followed
the sintering process that omits water content because the
sample was sintered at 1100℃.
Meanwhile the sonochemical sample lost the peak
due to the long duration of drying. The second zone
peak’s appeared on all synthesised samples because this
is the water molecule identity. This peak experienced
intensity decrease along with the increasing sintering Figure 5. FTIR Spectra Analysis of CoFe2O4 with Different
temperature that proved the sintering temperature Sintering Temperatur and Methods
reduces water molecule as well as water absorption by

TABLE 2. Magnetic Saturation, Magnetic Remanence, Coercivity and Remanence Ratio

Magnetic Magnetic Remanence/Mr Remanence Coercivity/HC
Sample Material
Saturation/Ms (emu/g) (emu/g) Ratio/ R T Oe
CoFe2O4 Sonochemical 1.29 0.06 0.046 0.0012 12
CoFe2O4 Sol-Gel Sintering 500℃ 89.02 41.83 0.469 0.1032 1032
CoFe2O4 Sol-Gel Sintering 800℃ 113.51 23.4 0.206 0.472 472
CoFe2O4 Sol-Gel Sintering 1100℃ 4.18 0.17 0.040 0.0066 66
882 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884

Figure 6 shows the comparison of the hysteresis loop In the application of hyperthermia, it requires several
curve from the synthesized CoFe2O4. The hysteresis loop important parameters, such as high Ms and Hc values so
curve of the sintered sample at 500℃ indicated hard that it can quickly kill cancer cells but dissolved particles
magnetic material, sintered sample at 800℃ indicated must be small in size. Based on reported data by
soft magnetic material, while the sintered sample at Yadavalli et al. [28] nanomaterials CoFe2O4 with
1100℃ and sonochemical sample indicated crystallite size 19.8 nm have Ms and Hc about 59 emu/g
paramagnetic material [23]. The change from hard and ± 300 Oe, which was the best results for their
magnetic into soft magnetic occurred in 500℃ to 800℃ experiment to hyperthermia study. Darwish et al. [29]
sintering temperature. Changes in the curve are thought reported nanomaterials CoFe2O4 with crystallite size
to be due to the sintering temperature which has exceeded 32.46 nm have Ms about 50.61 emu/g with applicate to
its temperature (520℃) [7] thereby reducing Mr and HC; hyperthermia have SLP value about 552 W/g. Rashad et
the change was due to the transition from a single domain al. [30] reported nanomaterials CoFe2O4 with crystallite
to multi-domain [14]. The transition change was caused size 10.7 nm have Ms and Hc about 36.2 emu/g and 513.2
by the critical diameter of CoFe2O4 that was 40 nm Oe with applicate to hyperthermia have SLP value about
according to Figure 7, and thus, after passing the critical 302 W/g. Nam et al. [31] reported nanomaterials
diameter, the coercivity was reduced [24, 25]. CoFe2O4 with crystallite size 11 nm have Ms about 58
With the decrease of Hc, there was an increase of Ms emu/g which is applicable to hyperthermia have SLP
from 89.02 emu/g to 113.5 emu/g following the Brown’s value about 297 W/g. Yasemian et al. [32] also reported
equation as follows [14, 27]: nanomaterials CoFe2O4 having crystallite size 11.1 nm
2𝐾1 have Ms and Hc about 42.94 emu/g and 169.19 Oe with
𝐻𝑐 = (5)
𝜇0𝑀𝑠

An increase in sintering temperature from 500℃ to

800℃ made the Hc value changed from 1032 Oe to 472
Oe and thus narrow down the curve. This phenomenon
made the grain size uneven and agglomerated, as shown
in Figure 4 where agglomeration decreases following the
decreasing Hc. An increase in sintering temperature
around 500℃ to 800℃ caused the crystal grain to grown
from 13.25 nm to 60.5 nm, and the Hc value decreased
[23]. Sintered CoFe2O4 at 1100℃ had paramagnetic
curve caused by the sintering temperature that passed the
Curie temperature and made the magnetic property to
dissolve, whereas the sonochemical sample was thought
to have paramagnetic curve because the NaOH titration
that has not entirely disappeared in the sample. All
samples had remanence ratio below 0.5, thus if R <0.5, Figure 6. Magnetic Hysteresis Curve of CoFe2O4, (black)
there was a static magneto interaction between the Sol-gel 500℃ Sintering, (red) Sol-gel 800℃ Sintering,
granules [27]. (blue) Sol-gel 1100℃ Sintering, (light green) Sonochemical
Figure 8 explains the relationship between crystal size without Sintering
with Ms and Hc. Comparison of crystallite size to Ms
shows that there is the largest Ms value in crystallite size
of 60.5 nm and 113.51 emu/g. The 13.25 nm crystal size
has a Ms value of 89.02 but has the greatest coercivity
value of all samples, which is 1032 Oe. This phenomenon
occurs because the crystal size has a magnetic domain in
the form of a single domain, this phenomenon has been
explained in the explanation above. From Figure 8 we
can say that after critical diameter the magnetic curve of
Ms and Hc will be downward curve due the transiton from
single domain to multi domain magnetic. From the
results above we can also conclude that cobalt ferrite sol-
gel with sinterring 500℃ have a high magnetic saturation
and high coercivity also smaller crystallite size that can Figure 7. Dependence of coercivity with particle diameter
be applied to Hyperthermia. for cobalt ferrite [25].
 P. Puspitasari and L. S. Budi / IJE TRANSACTIONS B: Applications Vol. 33, No. 5, (May 2020) 877-884 883

sintered samples at 500℃ and 800℃ from hard magnetic

into soft magnetic material. The curve difference was due
to the high temperature that passed the Curie temperature
and due to the transition from the single domain into
multiple domains as shown by the Brown equation. The
SEM results displayed the decreasing agglomeration
because of the sintering temperature that passed the Curie
temperature and decreased the magnetic property. Based
on research that already mentioned, cobalt ferrite sol-gel
sintering 500℃ had big potential to applicate on
hyperthermia.

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Persian Abstract
‫چکیده‬

‫ استفاده از فریت کبالت به عنوان ماده نانومواد جالب‬.‫ دارای خواص فیزیکی و مغناطیسی منحصر به فردی هستند که به روش سنتز آن بستگی دارد‬CoFe2O4 ‫فریت کبالت یا‬
‫ فریت کبالت در این تحقیق با استفاده از دو روش مختلف‬.‫ اما تجزیه و تحلیل خواص فیزیکی و مغناطیسی بر اساس روش سنتز مورد بحث قرار نگرفته است‬، ‫تر می باشند‬
‫ و‬XRD ‫ تجزیه و تحلیل شناسایی فاز و اندازه کریستال‬.‫ و سونوشیمیایی بدون هدف‬1100 ℃‫ و‬800 ، 500 ‫ژل با مدت زمان تغییرات تغییرات پراکندگی‬-‫ سل‬:‫سنتز گردید‬
XRD ‫ کوچکترین اندازه بلور از نتیجه‬.‫ استفاده شده است‬VSM ‫ و تجزیه و تحلیل خاصیت مغناطیسی از‬FTIR ‫ آنالیز پیوند گروهی کاربردی‬، SEM ‫آنالیز مورفولوژی از‬
‫ نشان داد که‬601-636 cm-1 ‫ ارتعاش گروه عملکردی را در‬FTIR .‫ مورفولوژی حاصل از فریت کبالت سنتز شده بیشتر آگلومره بود‬.‫ بود‬٪57.04 ‫ نانومتر با بلوریت‬13.25
.‫ تغییری در منحنی حلقه هیسترزیس از مغناطیسی سخت به مغناطیسی نرم وجود دارد و نمونه ای با منحنی پارامغناطیسی وجود دارد‬.‫حاکی از ساختار ا سپینل فریت کبالت است‬