IJE TRANSACTIONS C: Aspects Vol. 36 No.

06, (June 2023) 1034-1039

International Journal of Engineering

Journal Homepage: www.ije.ir

Investigating the Effect of Ultrasound Intensity on the Magnetic Properties of

Magnetite Nanostructures Synthesized by Sonochemical Method
A. Hassanjani-Roshana, M. R. Vaezib, H. Koohestani*a, F. Cheraghic
a Facultyof Materials and Metallurgical Engineering, Semnan University, Semnan, Iran
b Materialsand Energy Research Center (MERC), Karaj, Iran
c Department of material science and engineering, Sharif University of Technology, Tehran, Iran

PAPER INFO A B S T R A C T

Paper history: In this article, the synthesis of magnetite nanostructures was successfully carried out by the sonochemical
Received 02 February 2023
Received in revised form 02 March 2023
process. In this method, stoichiometric amount of iron chlorides (FeCl 3.6H2O and FeCl2.4H2O),
Accepted 03 March 2023 ammonia (NH3) and polyvinylpyrolidone (PVP) were used to synthesize pure Fe 3O4 nanoparticles. The
effect of initial sonication power of the ultrasonic device on the size and morphology of the final products
as one of the effective parameters was investigated. For this, the initial power of the sonicator was
Keywords: evaluated at 90, 70, 50 and 30 W at 40°C. Characterization of Fe3O4 nanoparticles was done by
Ultrasonic Irradiation transmission electron microscope (TEM) and X-ray powder diffraction (XRD) and its magnetic
Fe3O4 Nanostructures properties were investigated by vibrating sample magnetometer (VSM). Investigation of the XRD
Sonochemical Process pattern after annealing showed that pure Fe3O4 phase was successfully formed during the sonochemical
Magnetic Properties
process. TEM images determined the size of Fe3O4 nanoparticles to be 10-50 nm. The results showed
Sonication Power
that increasing the initial power of the system reduced the particle size and improved the magnetic
properties of nanoparticles.
doi: 10.5829/ije.2023.36.06c.01

1. INTRODUCTION1 have attracted much attention from researchers due to

their superparamagnetic properties, and containing both
The materials properties depend on the kind and situation Fe(II) and Fe(III) ions, which makes it superior to other
of atoms in the structure. When the materials dimension types of iron oxides [6].
approaches molecular and atomic size, the ratio of area Fe3O4 nanoparticles are also used in infectious
to volume increases considerably. Therefore, the diseases, encapsulating medicine, active drug delivery,
behavior of nanomaterials is substantially different from applied sensors, diagnostic cells, hyperthermia, making
bulk microstructures [1-3]. genes and imaging of the body and determining the
Iron oxide nanoparticles with various structures, diseases via increasing the image contrast in MRI as well.
known as very important nanomaterials, have been used This kind of particle ought to be enough small in order to
broadly in many fields such as electrical topics, prevent them to be deposited and also remaining invisible
magnetism, medicine, chemical, dying and the food against the phagocytosis systems [3, 7]. Despite the weak
industry. Fe3O4 nanostructures have various applications and strong points of iron oxides in practical applications,
in fabricating sensors, shape memory alloys, superparamagnetic iron oxides and super paramagnetic
rechargeable lithium batteries and drug delivery because iron nanoparticles are the only magnetic nanoparticles
of their unique chemical and magnetic characteristics [4, used in medical applications [8]. Materials magnetic
5]. These nanomaterials attracted to magnets have been properties result from the electrons magnetic moments.
studied as drug delivery factors. Fe3O4 nanoparticles Each electron has a magnetic moment in the atom that

*Corresponding Author Institutional Email:

[email protected] (H. Koohestani)

Please cite this article as: A. Hassanjani-Roshan, M. R. Vaezi, H. Koohestani, F. Cheraghi, Investigating the Effect of Ultrasound Intensity on the
Magnetic Properties of Magnetite Nanostructures Synthesized by Sonochemical Method, International Journal of Engineering, Transactions
C: Aspects, Vol. 36, No. 06, (2023), 1034-1039
 A. Hassanjani-Roshan et al. / IJE TRANSACTIONS C: Aspects Vol. 36 No. 06, (June 2023) 1034-1039 1035

comes from two sources: one is related to the orbital TABLE 1. The process conditions of ultrasonic device for
motion around the nucleus (electron orbit magnetic synthesizing magnetite nanoparticles
moment), and another is associated with the electron Sample Initial
Ultrasonic Imported Energy
spinning around its axis (electron spin magnetic moment) Waves Intensity into the Solution
Code Power (W)
(W/cm2) (kJ)
[9]. Furthermore, each electron can be a small permanent
magnet using its orbit and spin magnetic moments [10]. I 30 52 123
The relation between the properties and the grain size is II 50 65 150
a very important issue in magnetic materials. In the case
III 70 78 185
of soft magnetic materials, the area under the hysteresis
curve significantly decreases with reducing the size of IV 90 94 202
grains even if it can be disappeared completely [11, 12].
So far, various synthesis methods have been
mentioned for the synthesis of magnetite nanoparticles, centrifuge system at 1000 rpm for 15 min to separate
including the sol-gel process, chemical vapor deposition precipitations containing nanoparticles. After collection,
(CVD), hydrothermal technique, pulsed laser the final precipitated particles were filtered and washed
evaporation, electron irradiation, and reactive sputtering with methanol and distilled water to remove by-products.
[12-15]. However, chemical processes are often used Then all the samples were air-dried at room temperature
because it is an easy, repeatable and cost-effective and calcined at 500 °C for 60 min to obtain crystalline
methods, and among them, chemical bath deposition iron oxide nanoparticles.
(CBD) and sonochemical processes are more useful [16-
18]. In previous works, Fe3O4 nanoparticles have been 2. 3. Characterizations Crystal phases of Fe3O4
synthesized by the sonochemical method. The results nanoparticles were characterized by X-ray diffraction
have shown that ultrasonic radiation causes cavitation in (Siemens D-5000, with Cu Kα radiation). The
an aqueous medium, which leads to the formation, morphology of the synthesized samples was studied by
growth, and collapse of microbubbles [19, 20]. TEM analysis (ZEISS, Germany). Their magnetic
Therefore, the quality and properties of the synthesized properties were measured with a vibrating sample
product will be affected. In this work, the effect of magnetometer system (AGSM model, ± 0.001 emu/g).
ultrasound intensity on the structural and Fe3O4
properties of magnetite nanoparticles synthesized by the
sonochemical method will be investigated. 3. RESULTS AND DISCUSSIONS

The primary product without annealing has a completely

2. MATERIALS AND EXPERIMENTS amorphous structure [18, 21]. This is due to the collapse
of high-temperature bubbles in some parts of the solution
2. 1. Materials In this work iron chlorides where the bubbles are present, so as the temperature
(FeCl3.6H2O, FeCl2.4H2O), ammonia (NH3) and decreases rapidly, the particles do not have enough time
polyvinylpyrrolidone (PVP) were purchased from to crystallize. Under these conditions, the reactants carry
Merck. out intense interactions in a very short period of time.
Cavitation events lead to increased heating and cooling
2. 2. Synthesis The synthesis of magnetite rates to more than 1010 Ks-1 [22, 23]. Hence, after
nanoparticles was done according to the previous method TGA/DTA analysis in previous work and determining
[18]. In this method, FeCl3.6H2O (0.4 M, 50 ml) and the crystallinity temperature, the samples were heat-
FeCl2.4H2O (0.2 M, 50 ml) are used as starting precursors treated at 500 C for about 1 h to gain a calcined powder
and PVP as a surfactant, and ammonia (0.8 M, 50 ml) is and also to get the required peaks for phase and structure
also used. NH3 was added dropwise to the resulting analysis [18]. It can be seen in Figure 1 which is related
aqueous solution. Process sonication was provided using to the diffraction of Fe3O4 nanoparticles, all peaks are
the Misonix sonicator model S-4000 sonicator through associated with Fe3O4 nanoparticles and there are not any
direct ultrasonic irradiation with an initial power of 10, peaks associated with impurities. The sharp peaks with
30, 50 and 70 W for about 30 min and a temperature of high intensity show the high crystallinity of the prepared
40 °C. Then the solution was exposed to ultrasound for nanopowder via sonochemical method.
60 min to complete the sonochemical process. The Considering the pattern, it can be found that there is a
influence of ultrasonic power on the structure and direct relation between ultrasonic intensity and flatness
morphologic properties of nanoparticles has been studied of peaks. As much as the initial power is raised, flatness
and samples I, II, III, and IV are prepared under different of peaks is also increased, although the crystallite size
conditions listed in Table 1. will be decreased, in sequence. Using the XRD patterns
After completing the procedure and appearing and Scherer equation, the size of the crystals was
precipitations, the obtained solution is put in the determined [24]:
1036 A. Hassanjani-Roshan et al. / IJE TRANSACTIONS C: Aspects Vol. 36 No. 06, (June 2023) 1034-1039

Figure 2. TEM images of Fe3O4 nanoparticles at initial

powers: (a) I, (b) II, (c) III, (d) IV

The gained size of nanoparticles is shown in Table 2.

Cavitation promotes the local reaction, heating, and
severe stirring through the heat transfer of gas bubbles.
Therefore, by accelerating the nucleation process, the
concentration of seeds increases. This phenomenon leads
to the relaxation and interface defects and the formation
of nanoparticles [22].
Since the temperature and solution concentration are
constant for all samples in this research, these factors
have not influenced the results and the only effective
factor is ultrasonic wave intensity. By increasing the
initial power, the bubbles are formed with more energy.
Furthermore, the sonochemical influences of this kind of
Figure 1. XRD patterns of the samples (a) I, (b) II, and (c)
bubbles will increase. These bubbles have more energy
IV
so they have more sonochemical influences on the
solution [26-28].
According to Table 1, by increasing the initial power
k . from 30 to 50 W at constant temperature of 40 C, the
D= (1)
 . cos intensity of the ultrasonic waves has increased from 52
W/cm2 to 94 W/cm2. This increase is due to the
where k is constant (0.89 for spherical particles), D is the
expansion of energetic bubbles or the increase in the
crystallite size (nm),  is the wavelength of the X-ray
solution viscosity due to precipitation formation.
beam (= 0.15406 nm for Cu Kα radiation),  is the full The VSM analysis is used in order to determining the
width at half maximum for the diffraction peak under effect of the ultrasonic waves intensity on the magnetic
consideration (in radians), according to measurements, properties of the prepared nanostructures via
the mean size of crystals is about 8 nm, 14 nm, and 17 sonochemical technique. Figure 3 shows the hysteresis
nm for initial powers of 90, 50 and 30 W, respectively. curves of the prepared nanostructures, and their results
Ultrasonic waves disperse the suspension solution into are listed in Table 3.
smaller droplets. In this way, it reduces the kinetics of
particle growth and the amount of aggregation and stops
crystal growth. This leads to reduced crystallinity, cluster TABLE 2. The average size of obtained Fe3O4 nanostructure
decomposition [25]. The ultrasonic process is more measured from TEM images
effective than the magnetic field in the particle growth Sample Code The size of particles (nm)
step, and the bubbles formed in this process break more
particles into smaller particles [23]. I 50
Figure 2 shows TEM images of Fe3O4 nanostructures II 35
prepared via sonochemical process with different III 20
powers. Fe3O4 nanoparticles have spherical morphology
with smooth geometry and high degree of crystallinity. IV 10
 A. Hassanjani-Roshan et al. / IJE TRANSACTIONS C: Aspects Vol. 36 No. 06, (June 2023) 1034-1039 1037

Therefore, by controlling the particle size in the nano

dimension, it is possible to change the coercivity easily.
After removing the magnetic field, the magnetic
properties are disappeared approximately in this kind of
nanostructure. If permanent magnets will be necessary,
nanopowders should keep their magnetite properties
even in absence of a magnetic field. Consequently, the
hysteresis loop should be large, which means that Hc and
Mr should be high, but the hysteresis loop of the
nanostructures obtained via the sonochemical process is
small. It is an important point that declares a good
relationship between the properties and the grain size of
materials. In soft magnetic materials decreasing the grain
Figure 3. VSM spectra of the synthesized samples: (a) I, (b) size tends to reduce the area under the hysteresis graph
II, (c) III, (d) IV significantly, even if it may disappear completely such as
in sample IV. Fuentes-García et al. [31] synthesized
magnetite nanoparticles by a one-step sonochemical
TABLE 3. Magnetic properties of the samples synthesized via method. The results showed that the obtained
sonochemical processing with different intensity of ultrasonic
waves
nanomaterials with improved properties have a good
potential to be used as magnetic hyperthermia agents.
Sample Code Initial power (W) M (emu/g) HC (Oe)
I 30 38 1100
II 50 43 1000 4. CONCLUSIONS
III 70 47 800
In this work, the sonochemical process was used as a new
IV 90 50 - and advanced technique with direct ultrasonic waves
irradiating on the solution for the synthesis of iron oxide
(Fe3O4) nanostructures. Then, the effect of the intensity
It can be seen that by increasing the power and the of ultrasonic waves on the properties of Fe3O4
intensity of ultrasonic waves, the magnetism of particles nanoparticles was investigated. The obtained
has decreased. Reduction in the particle size results in nanoparticles have an amorphous structure resulting
raising coercivity to a maximum amount (IV), then it will from the collapse of cavitation bubbles as enormous
be decreased until it will be closed to zero. Yadav et al. cooling rate. Because it prevents their crystallization
[29] showed that increasing of the ultrasonic power input during quenching and also the quick decrease of
in the synthesis of MnFe2O4 increases the saturation temperature around the nanoparticles. Therefore, to
magnetization and negligible surface spin canting. obtain crystallite nanoparticles, they must be calcined.
The main reason for this situation is that the The significant results of this work relate to the size,
magnetization of the multi-domain nanoparticles can be morphology, structure, purity and magnetic properties of
changed with the motion of the domain walls. In this the prepared materials. The size of crystallites is about 8
case, nanoparticles with small sizes consist of one nm to 17 nm and the particle size considering the average
domain, but larger particles that are composed of several size of particles is 10-50 nm which put them in a super
domains minimize the static magnetization energy. The small iron oxide nanoparticles group with a diameter of
approximate range for the critical particle size above less than 50 nm. It can be seen that increasing the initial
which the magnetic nanoparticle is not single-domain is power of the system reduces the grain size with which the
from a few to several tens of nanometers, which is higher magnetic properties of particles have increased.
than the typical domain wall dimension in the magnetic Synthesized magnetite nanoparticles have a spherical
material. The nature of the domain structure has a strong morphology with smooth geometry and a degree of
influence on the hysteresis behaviour of magnetic crystallinity, which are very useful and practical in
nanoparticles. By decreasing the ultrasonic frequency, various fields.
the nucleation rate accelerates due to an increase in the
magnitude of the shock wave caused by the cavitation
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‫‪Persian Abstract‬‬
‫چکیده‬
‫در این مقاله‪ ،‬سنتز نانوذرات مگنتیت با فرآیند سونوشیمیایی با موفقیت انجام شد‪ .‬در این روش از مقدار استوکیومتری کلریدهای آهن (‪ )FeCl3.6H2O‬و (‪،)FeCl2.4H2O‬‬
‫آمونیاک (‪ )NH3‬و پلی وینیل پیرولیدون (‪ )PVP‬برای سنتز نانوذرات خالص ‪ Fe3O4‬استفاده شد‪ .‬تاثیر توان امواج آلتراسونیک اولیه بر اندازه و مورفولوژی محصوالت نهایی‬
‫به عنوان یکی از پارامترهای موثر مورد بررسی قرار گرفت‪ .‬برای این کار‪ ،‬توان اولیه دستگاه سونیکاتور در ‪ 50 ،70 ،90‬و ‪ 30‬وات در دمای ‪ 40‬درجه سانتیگراد ارزیابی شد‪.‬‬
‫شناسایی نانوذرات ‪ Fe3O4‬با استفاده از میکروسکوپ الکترونی عبوری (‪ )TEM‬و پراش پرتو ایکس (‪ ) XRD‬و خواص مغناطیسی آن توسط مغناطیس سنج نمونه ارتعاشی‬
‫(‪ )VSM‬بررسی شد‪ .‬بررسی الگوی ‪ XRD‬پس از کلسینه کردن نشان داد که فاز ‪ Fe3O4‬خالص با موفقیت در فرآیند سونوشیمیایی تشکیل شد‪ .‬تصاویر ‪ TEM‬اندازه نانوذرات‬
‫‪ Fe3O4‬را ‪ 10-50‬نانومتر تعیین کردند‪ .‬نتایج نشان داد که افزایش توان اولیه سیستم باعث کاهش اندازه ذرات و بهبود خواص مغناطیسی نانوذرات میشود‪.‬‬