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Current Applied Physics 8 (2008) 758–760

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Synthesis and characterization of magnetite nanopowders

a,d,1
Ki-Chul Kim , Eung-Kwon Kim b, Jae-Won Lee c, Sung-Lyul Maeng d,
Young-Sung Kim c,*
a
BK 21, Physics Research Division, Institute of Basic Science, Sungkyunkwan University, Suwon 440-746, Republic of Korea
b
School of Information and Communication Engineering, Sungkyunkwan University, Republic of Korea
c
Advanced Material Process of Information Technology, Sungkyunkwan University, Republic of Korea
d
Cambridge-ETRI Joint R&D Centre, Electronics and Telecommunications Research Institute, Daejeon 305-350, Republic of Korea

Received 27 July 2006; received in revised form 15 January 2007; accepted 27 April 2007
Available online 1 October 2007

Abstract

We have synthesized the iron oxide nanoparticles using the newly developed mechanical ultrasonication method with the FeS-
O4 Æ 7H2O. We have also investigated the crystallographic structural properties, morphology, and magnetic properties of the nanopow-
ders. According to the high resolution X-ray diffraction result, the as-synthesized iron oxide nanoparticles were magnetite (Fe3O4). The
particle size of the magnetite nanoparticles was about 6 nm confirmed by transmission electron microscopy image. The particle shape was
almost a sphere confirmed by scanning electron microscopy image. The coercivity and saturation magnetization of the as-synthesized
iron oxide nanopowders were 114 Oe, and 3.7 emu/g, respectively.
Ó 2007 Elsevier B.V. All rights reserved.

PACS: 61.46.Df; 75.75.+a; 87.80.Ek

Keywords: Synthesis of magnetic nanoparticles; Magnetite; Iron oxide; Mechanical ultrasonication method

1. Introduction
The synthesis of the iron oxide particles has been a field
intense study due to the novel properties and potentiality on
the practical applications to ferrofluids, rotary shaft sealing,
oscillation damping and position sensing [1–3]. The sub-
10 nm iron oxide nanoparticles exhibit superparamagnetic
behavior, because each particle can be considered as a single
magnetic domain. Superparamagnetic nanoparticles offer a
high potentiality for biomedical applications, such as med-
ical diagnosis with contrast enhancement of magnetic reso-
nance imaging (MRI) [4], AC magnetic field-assisted cancer
therapy, magnetic cell separation [5], and magnetically con-
trolled transport of anti-cancer drugs [6].
*
Corresponding author. Tel.: +82 31 299 6702; fax: +82 31 290 5644.
E-mail address: youngsk@skku.edu (Y.-S. Kim).
1
Present address: Department of Information Communication Engi-
neering, Mokwon University, Daejeon 302-318, Republic of Korea.
There are several techniques have been used for the syn-
thesis of iron oxide nanoparticles, which including copre-
cipitation of ferrous (Fe2+) and ferric (Fe3+) ions by a
base, usually NaOH in an aqueous solution [1,7], thermal
decomposition of iron pentacarbonyl (Fe(CO)5) in the
presence of oleic acid followed by oxidation [6], thermal
decomposition of alkaline solution of Fe3+ chelate in the
presence of hydrazine [8], and direct decomposition of
FeCup3 [9]. Organic solution-phase decomposition of the
iron precursor at high temperature has been widely used
in iron oxide nanoparticle synthesis [3]. In this study, we
have synthesized the iron oxide nanoparticles using the
newly developed mechanical ultrasonication method with
the FeSO4 Æ 7H2O. The FeSO4 Æ 7H2O is a low cost resid-
uum of synthesis process of TiO2. The low cost, mass pro-
duction and clean environmental process are very
important issues to practical applications. Our mechanical
ultrasonication method is very economic and environmen-
tally-friendly simple process. The crystallographic

1567-1739/$ - see front matter Ó 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.cap.2007.04.021
 K.-C. Kim et al. / Current Applied Physics 8 (2008) 758–760 759

structural properties, morphology, and magnetic properties
of the as-synthesized iron oxide nanopowders were investi-
gated with various analyses including X-ray powder dif-
fraction (XRD) analysis, scanning electron microscopy
(SEM), low resolution transmission electron microscopy
(TEM) and vibrating sample magnetometer (VSM)
measurement.
2. Experiment
To prepare iron oxide nanoparticles, especially magne-
tite (Fe3O4), 2.0 g of FeSO4 Æ 7H2O dissolved in 225 ml of
the deionized (DI) water, and 60 mg of KNO3 and 0.56 g
of NaOH dissolved in 90 ml of the DI water. The two solu-
tions were heated to 75 °C and mixed the two solutions
while stirring which was used a stirring rod not a magnetic
stir bar. A green suspension formed and rapidly turned
black. The mixed solution was heated to 90 °C for
respectively. The particle size is about 6 nm confirmed
from TEM image, and the particle shape is almost a
sphere confirmed by SEM and TEM images. According
to the SEM and TEM images, the agglomeration is
occurred very strong in the iron oxide nanopowders.
The agglomeration is due to the van der Waals force
between the particles. According to TEM image, the as-
synthesized iron oxide nanopowders are not monodi-
spersed particles. There exist various sizes of iron oxide
nanoparticles.
The X-ray powder diffraction patterns of the as-synthe-
sized iron oxide nanopowders and JCPDS reference pat-
terns of the magnetite (Fe3O4) (No. 19-0629) are shown
in Fig. 2. The XRD peaks of the as-synthesized powders
are compared with those of standard magnetite data. The
X-ray powder diffraction patterns of the as-synthesized
500

(311)
10 min. while stirring with a stirring rod. The ultrasonica- a
tion performed to prevent agglomeration which was 400
induced from van der Waals force in the initial stage of
nanoparticles formation with Ultrasonic Homogenizer 300

(220)
(Han. Tech. Co.) at frequency 28 kHz ± 200 Hz. The black

(440)
(400)

(511)
suspension was cooled to room temperature and added 200
H2O2 for oxidation. The sodium hydroxide added to the
cooled solution to neutralize and rinsed with the DI water. 100
The suspension was dispersed and milled with the basket-
Intensity (CPS)

milling machine. Finally the suspension was rinsed with 0

20 30 40 50 60 70 80
the DI water and dried in a vacuum chamber at 80 °C
for 2 h. 2θ (degree)
The crystallographic structure of the as-synthesized iron 0
oxide nanoparticles was characterized by high resolution
b
XRD analysis (Bruker AXS, D8 Discover). The surface 20
morphology of the powders was observed by the SEM
(Philips, XL30 ESEM-FEG) and TEM. The magnetic 40
properties of the as-synthesized nanopowders were ana-
lyzed by a VSM (Princeton Measurements, MicroMag 60
3900).
80
3. Results and discussion
100

The SEM image and TEM image of the as-synthesized Fig. 2. XRD patterns of the (a) as-synthesized iron oxide nanopowders
iron oxide nanopowders are shown in Fig. 1a and b, and (b) JCPDS reference patterns of the Fe3O4 (No. 19-0629).

Fig. 1. (a) SEM and (b) TEM images of the as-synthesized magnetite nanopowders.
760 K.-C. Kim et al. / Current Applied Physics 8 (2008) 758–760

5 as-synthesized iron oxide nanoparticles were magnetite

4 (Fe3O4). According to the TEM image, the particle size
was around 6 nm, and particle shape was almost a sphere.
Magnetization (emu/g)

3
2
The saturation magnetization of the iron oxide nanopow-
ders was 3.7 emu/g.
1
0
Acknowledgement
-1
-2 This work was supported by the Korea Research Foun-
-3 dation Grant funded by the Korean Government
-4 (MOEHRD) (KRF-2005-005-J11901, KRF-2005-005-
-5 J11903).
-8000 -6000 -4000 -2000 0 2000 4000 6000 8000
Magnetic Field (Oe) References
Fig. 3. Hysteresis curve of the as-synthesized magnetite nanopowders. [1] Fong-Yu Cheng, Chia-Hao Su, Yu-Sheng Yang, Chen-Sheng Yeh,
Chiau-Yuang Tsai, Chao-Liang Wu, Ming-Ting Wu, Dar-Bin Shieh,
Biomaterials 26 (2005) 729–738.
iron oxide nanopowders are matched well with standard [2] Yong-kang Sun, Ming Ma, Yu Zhang, Ning Gu, Colloids Surf. A:
magnetite (Fe3O4) XRD patterns [1]. Physicochem. Eng. Aspects 245 (2004) 15–19.
The hysteresis loop of the as-synthesized iron oxide [3] Shouheng Sun, Hao Zeng, J. Am. Chem. Soc. 124 (2002) 8204–8205.
nanopowders is shown in Fig. 3, which is measured at [4] Ho-Taek Song, Jin-sil Choi, Yong-Min Huh, Sungjun Kim, Young-
wook Jun, Jin-Suck Suh, Jinwoo Cheon, J. Am. Chem. Soc. 127 (2005)
room temperature with a vibrating sample magnetometer. 9992–9993.
The coercivity and saturation magnetization of the as-syn- [5] Hyun-Seok Kim, Oh-Taek Son, Kunhong Kim, Ki-Chul Kim, Sung-
thesized magnetite nanopowders are 114 Oe and 3.7 emu/g, Lyul Maeng, Hyo-Il Jung, in: The 8th Korean MEMS Conference
respectively. Proceedings, April 6–8, 2006, pp. 108–111.
[6] Taeghwan Hyeon, Su Seong Lee, Jongnam Park, Yunhee Chung,
Hyon Bin Na, J. Am. Chem. Soc. 123 (2001) 12798–12801.
4. Conclusions [7] Tcipi Fried, Gabriel Shemer, Gil Markovich, Adv. Mater. 13 (2001)
1158–1161.
We have synthesized the iron oxide nanopowders using [8] R.S. Sapieszko, E.J. Matijevic, J. Colloid Interface Sci. 74 (1980) 405.
the newly developed mechanical ultrasonication method [9] J. Rockenberger, E.C. Scher, A.P. Alivisatos, J. Am. Chem. Soc. 121
with the FeSO4 Æ 7H2O. The XRD patterns indicated that (1999) 11595–11596.