Preparation and characterization of magnetic nanoparticles

Thesis Type: Postgraduate

Institution Of The Thesis: Orta Doğu Teknik Üniversitesi, Faculty of Arts and Sciences, Department of Chemistry, Turkey

Approval Date: 2009




Magnetite (Fe3O4) and Maghemite (γ-Fe2O3) are well-known iron oxide phases among magnetic nanoparticles due to their magnetic properties, chemical stability, and nontoxicity. They have gained acceptance in several fields of application of nanomaterials such as magnetic recording systems, magnetic refrigeration, magneto-optical devices, magnetic resonance imaging, magnetic separation techniques and separation and purification of biological molecules. Recently, there is a growing interest in the synthesis of magnetic iron oxide nanoparticles in a polymeric, glassy or ceramic matrix since the preparation of pure phase iron oxide composite material involves, presently, some difficulties partially arising from different oxidation states of iron which can lead to the presence of various oxides. Matrix support, in principle, modifies the properties of nanomaterials, thus opening new possibilities for the control of their performance. In addition, the chosen matrix, polymer or sol-gel, provides binding of the functional groups and also prevents grain growth and agglomeration. Therefore, extensive research is conducted on this subject. Sonochemical technique is an effective method to synthesize magnetic nanoparticles with many unique properties due to extreme reaction conditions. Besides, a microscopic mixing in the synthesis procedure is obtained because of the microjet effect which comes from the collapse of the bubbles. This effect creates relatively uniform reaction conditions. Thus, well-dispersed and stable nanoparticles are obtained by using ultrasound. In this study, γ-Fe2O3, maghemite nanoparticles are accommodated in an inert, inorganic, transparent and temperature resistant sol gel matrix to achieve stabilization. The nature and concentration of the salt used, evaporation conditions of the sols, the following heat treatments had been investigated and shown that they had great influence on the particle size and the final iron oxide phase in the sol-gel. The Fe2O3/SiO2 nanocomposites were characterized using X-ray diffraction (XRD) and vibrating sample magnetometry (VSM) techniques. In addition, magnetite (Fe3O4) nanoparticles were synthesized via co-precipitation in the presence of poly(methacrylic acid) (PMAA) in aqueous solution. PMAA, which was used as the coating material, prevents magnetite nanoparticles from oxidation towards a lower saturation magnetization iron oxide phases. In order to achieve small particle size and uniform size distribution of the magnetite nanoparticles in PMAA matrix, ultrasonic irradiation was applied during co-precipitation. The polymer coated Fe3O4 nanoparticles were characterized using scanning electron microscopy (SEM), laser particle sizer, X-ray diffraction, (XRD) and vibrating sample magnetometry (VSM) techniques and zeta potential measurements.