Sains Malaysiana 43(4)(2014): 611–616

 

Effect of FeCl2 Concentration on the Properties of Magnetic
Nanoparticles by Using Massart’s Procedure
(Kesan Kepekatan FeCl2 terhadap Sifat Nanozarah Magnetik dengan Menggunakan Prosedur Massart)


B.C. ANG1*, I.I. YAACOB2& C.S. CHEW3
1Center of Advanced Materials, Department of Mechanical, Faculty of Engineering
University of Malaya, Lembah Pantai, 50603 Kuala Lumpur, Malaysia

2Department of Manufacturing and Materials Engineering, Kuliyyah of Engineering
International Islamic University Malaysia, P.O. Box 10, 50728 Kuala Lumpur, Malaysia

3Faculty of Engineering and Science, Department of Mechanical and Materials Engineering
Universiti Tunku Abdul Rahman Jalan Genting Kelang, Setapak, 53300 Kuala Lumpur Malaysia

Received: 7 June 2012 /Accepted: 31 July 2013

 

ABSTRACT

The effect of variation of FeCl2 concentration on the properties of magnetic nanoparticles produced by Massart’s procedure was investigated. Samples with different FeCl2 concentration of 0.1, 0.8, 1.0, 1.2 and 1.5 M were produced. In this technique, an aqueous mixture of ferrous and ferric chloride was co-precipitated under controlled conditions to yield magnetic iron oxide nanoparticles. Thermogravimatric analysis (up to 700oC) showed a continuous weight loss from room temperature to 200oC that was mainly due to evaporation of water from the sample. Above 230oC, no more weight loss was observed indicating the stability of the maghemite nanoparticles. The lattice parameter of the samples obtained from X-ray diffraction analysis showed that the nanoparticles formed were maghemite (?-Fe2O3). The crystallite sizes calculated from the broadening of XRD peaks were 6.79, 6.56, 6.15, 6.72 and 7.24 nm for FeCl2 concentration of 0.1, 0.8, 1.0, 1.2 and 1.5 M, respectively. The magnetization curves showed no hysteresis indicating that the particles were superparamagnetic. The least upper bound of the ‘magnetic’ sizes calculated were 7.53, 6.29, 5.92, 6.41 and 8.04 nm and the physical sizes measured from TEM images were 5.97, 6.02, 4.98, 5.35 and 5.98 nm, respectively. The crystallite, magnetic and physical sizes were similar, indicating that the particles are monocrystals.

Keywords: Maghemite; magnetic nanoparticles; Massart’s procedure

 

ABSTRAK

Kesan kepekatan FeCl2 yang berlainan ke atas sifat nanozarah magnet yang dihasilkan oleh prosedur Massart telah dikaji. Lima sampel telah dihasilkan dengan kepekatan FeCl2 yang berlainan iaitu 0.1, 0.8, 1.0, 1.2 dan 1.5 M. Dalam teknik ini, campuran akueus ferus dan ferik klorida akan mendak di bawah dalam keadaan terkawal untuk menghasilkan nanozarah ferrum oksida. Analisis termogravimetri menunjukkan kehilangan berat sampel yang turun berterusan daripada suhu bilik ke 200oC yang disebabkan oleh penyejatan air daripada sampel. Pada suhu melebihi 230oC, tiada kehilangan berat sampel diperhatikan, menunjukkan kestabilan nanozarah maghemit. Parameter kekisi sampel yang diperoleh daripada analisis belauan sinar-X menunjukkan nanozarah yang terhasil adalah maghemit. Saiz hablur yang dikira dari pelebaran puncak XRD adalah 6.79, 6.56, 6.15, 6.72 dan 7.24 nm untuk kepekatan FeCl2 0.1, 0.8, 1.0, 1.2 dan 1.5 M, masing-masing. Lengkung pemagnetan yang tidak menunjukkan histerisis menunjukkan bahawa nanozarah adalah superparamagnet. Saiz AGM ialah 7.53, 6.29, 5.92, 6.41 dan 8.04 nm manakala saiz TEM yang diperoleh dari TEM adalah 5.97, 6.02, 4.98, 5.35 dan 5.98 nm untuk sampel 0.1, 0.8, 1.0, 1.2 dan 1.5 M masing-masing. Saiz XRD, AGM dan TEM di atas menunjukkan keputusan yang agak sama dan menunjukkan nanozarah ini adalah terdiri daripada monokristal.

Kata kunci: Maghemit; nanozarah magnet; prosedur Massart

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*Corresponding author; email: amelynang@um.edu.my