Popova 2012 J. Phys. Conf. Ser. 345 012030

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IV Nanotechnology International Forum (Rusnanotech 2011) IOP Publishing
Journal of Physics: Conference Series 345 (2012) 012030 doi:10.1088/1742-6596/345/1/012030
Synthesis and Characterization of Iron-Cobalt Nanoparticles
A.N. Popova
Institute of Coal-chemistry and Material science of the RAS SB
650000, Russia, Kemerovo, Sovetskiy av., 18
E-mail: [email protected]
Abstract. Nanoparticles of iron-cobalt have attracted great interest in recent years because of
their unique physical and chemical properties because of their industrial importance in
preparing magnetic recording materials, pigments, catalysts, etc. With an objective to develop
magnetic materials with high saturation magnetization Fe-Co nanosysytems were synthesized
by method of chemical reduction reaction of salts aqua-solutions by hydrazine hydrate in
alkaline medium. The synthesized powders were characterized by XRD, SEM, EDX and
SQUID-magnetometry techniques. The steady-state grain size of 5-20 nm was calculated using
XRD line broadening and SEM. The maximum saturation magnetization of 207 and 215
A•m2/kg was achieved at 300 and 5 K, respectively.
1. Introduction
Nanocrystylline materials, because of the very fine grain sizes, exhibit a variety of properties, which
are different and often considerably improved in comparison with those of conventional coarse-
grained polycrystalline materials [1]. Therefore, nanosized materials are the subject of a large number
of studies in the last years from basic research and applications point of view. The high saturation
magnetic moment, Curie temperature, and high permeability properties of Fe-Co alloys make its
potential from magnetic recording head to drug delivery applications [2-4].
2. Materials and methods

Nanocrystalline Fe-Co alloys were synthesized by a chemical process involving the reduction of a
mixture of iron sulphate and cobalt chloride with hydrazine-hydrate added slowly to a predetermined
volume of water solution of the metal salt in reactor in the presence of magnetic field. The synthesized
samples were characterized by X-ray powder diffraction (XRD) using a BRUKER D8-Advance X-ray
diffractometer to identify the nanocrystalline state of the alloys and the phase of the crystalline grains.
Microstructural evaluation was studied with Scanning Electron Microscopy (SEM) of JEOL model
JSM-6390. Compositional analysis of the samples, carried out with an energy dispersive X-ray (EDX)
analyzer (in conjunction with SEM) shows no significant impurity except a small trace of 2-5 at.%
even smaller due to oxygen. The magnetic measurements were performed by a Quantum Design
superconducting quantum interference device (SQUID) magnetometer of the type MPMS-XL5 with a
maximum field of 2 T.
3. Results
Previously [5, 6], it was observed that for x ≤ 75 a single bcc Fe(Co) solid solution was formed.
Synthesis of Fe-Co alloys for Fe-rich region (x ≤ 25) shows formation of a well-defined ferrite spinel
Published under licence by IOP Publishing Ltd 1

(Fe2CoO4) and the bcc Fe(Co) solid solution. Synthesis for Co-rich region (x ≥ 95) were found leading
to the coexistence of two phases (fcc + hcp) end products while the fcc Co(Fe) solid solution is
observed for x ≥ 75. Thus, the phase formation by chemical reduction of Fe-Co appears to be similar
to what is observed in the well-known composition trend [7] of the bulk Fe-Co alloys at 650 K. Phase
portrait of Fe-Co nanosystems was designed (Figure 1).
Figure 1. Phase diagrams of Fe-Co nanosystems.
The average grain size of Fe-Co crystalline particles were estimated from the XRD patterns by
Scherrer analysis of the full widths at half maximum of the diffraction peaks. The grain size is
between 5 and 20 nm. It was found that the samples are characterized by morphology with multilevel
hierarchy. The crystalline particles form sphere-shaped ultrasonic disaggregation-resistant
agglomerates. The Fe-Co agglomerates form long chain-like structures. Figure 2 shows the typical
SEM images of Fe-Co samples.
Figure 2. SEM images of Fe-Co samples.
Figure 3 presents typical hysteresis loops of nanocrystalline Fe-Co alloys measured at 5 and 300 K.
One can see the hysteresis loop features small changes in shape at these temperatures.
2
Figure 3. Magnetic characteristics of nanocrystalline Fe-Co alloys at 300 K (1) and 5 K (2).
Figure 4 shows the cobalt composition effect on the evolution of saturation magnetization. A peak
value of saturation magnetization determined from magnetization curves is about 215 A•m2/kg.
Figure 4. Magnetic characteristics of nanocrystalline Fe-Co alloys at 300 K (1) and 5 K (2).
Table 1 shows the maximum magnetization (MS) level and the coercive force (Hc) of the nanosized
Fe-Co powders formed by reduction of salts mixture with hydrazine-hydrate. It was observed that
nanocrystalline Fe-Co have high saturation magnetization and high coercivity.
Table 1. Magnetic properties of nanocrystalline Fe-Co alloys
Sample T, K Ms, A•m2/kg Hc, kA/m

0,5%Fe-99,5%Co 5 138,6 11,5
7%Fe-93%Co 5 157,9 15,1
20%Fe-80%Co 5 184,7 19,1
50%Fe-50%Co 5 214,7 8,3
60%Fe-40%Co 5 212,7 10,7
70%Fe-30%Co 5 196,1 9,1
50%Fe-50%Co 300 207,0 6,8
65%Fe-35%Co 300 203,1 7,0
3
4. Conclusions
With an objective to obtain alloys with highest possible MS value, the synthesis of nanocrystalline Fe-
Co alloys was investigated by characterization of the powders using SEM, EDX, XRD, and SQUID-
magnetometry. The results obtained show that the chemical synthesis by the reduction of a mixture of
iron sulphate and cobalt chloride with hydrazine-hydrate can lead to obtain Fe-Co nanoparticles with
chain-like structures, which present behaviour of hard magnetic materials.
References
[1] R. Birringer, H. Gleiter, H.P. Klein, P. Marquardt, 1984 Phys. Lett. 102A 365.
2] G. Schmid, Nanoparticles: From Theory to Application (New York: Wiley Interscience), 2004,
443 p.
[3] Tartaj P., Morales M.P., Veintemillas-Verdaguer S., Gonsalez-Carreno T., Serna C.J., 2003 J.
Phys. D, 36, R182-R197
[4] Manuel Arruebo, Rodrigo Fernández-Pacheco, M. Ricardo Ibarra, and Jesús Santamaría 2007
Nanotoday 2 (3) P. 22-32
[5] Yu. A. Zaharov, A. N. Popova, R. P. Kolmikov, V. M. Pugachev, V. G. Dodonov // 2008
Perspective Materials 6 249-254
[6] Yu. A. Zaharov, V. M. Pugachev, V. G. Dodonov, A. N. Popova 2010 Perspective Materials 3
60 – 72
[7] Binary Alloy Phase Diagrams, Massalski T. B., editor-in-chief (ASM INTERNATIONAL),
1986, 1086 p.
Acknowledgments
Author wishes to acknowledge assistance and encouragement from supervisor (Dr. Yuriy A. Zaharov)
and colleagues (Valeriy Pugachev, Vadim Dodonov). The work was supported by The Integration
Grant SB RAS.

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Journal of Physics: Conference Series

OPEN ACCESS Related content

- One-pot synthesis of Fe-Co nanospheres

- Investigation of fabrication of Mn-Ga-

- Phase Composition and Magnetic

This content was downloaded from IP address 14.187.196.47 on 29/02/2020 at 11:58

Synthesis and Characterization of Iron-Cobalt Nanoparticles

2. Materials and methods

Published under licence by IOP Publishing Ltd 1

Figure 1. Phase diagrams of Fe-Co nanosystems.

Figure 2. SEM images of Fe-Co samples.

Table 1. Magnetic properties of nanocrystalline Fe-Co alloys

Sample T, K Ms, A•m2/kg Hc, kA/m

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