Recebido em 15/1/09; aceito em 9/9/09; publicado na web em 22/2/10This work aimed at putting in evidence the influence of the pH on the chemical nature and properties of the synthesized magnetic nanocomposites. Saturation magnetization measurements evidenced a marked difference of the magnetic behavior of samples, depending on the final pH of the solution after reaction. Magnetite and maghemite in different proportions were the main magnetic iron oxides actually identified. Synthesis with final pH between 9.7-10.6 produced nearly pure magnetite with little or no other associated iron oxide. Under other synthetic conditions, goethite also appears in proportions that depended upon the pH of the synthesis medium.Keywords: magnetic nano-composites; magnetite; Mössbauer spectroscopy.
INTRODUCTIONNanotechnology is a field of growing interest for many physicists and chemists, because the reduced dimension of the solid system leads to peculiar physical and chemical properties that differ from the corresponding bulk materials. The origin of these distinguished properties is either the large surface-to-volume ratio in the particles or the quantum-mechanical nature of electronic structure, which imposes size-dependent modulations or modifications on the chemical behavior, when the size of the particles reaches dimensions of the wavelength of valence electrons in the solid.
1A main driving force for nanoparticle research is the large potential on technological applications. In the case of magnetic nanostructures, applications include data storage technology, 2 medical diagnostics as contrast enhancers in magnetic resonance imaging 3 and drug deliverer. 4 Among the iron oxides, magnetite (Fe 3 O 4 ) is a very promising candidate for biological applications for its biocompatibility 5 and suitable magnetic properties.6 Biomedical applications also require that iron oxide nanoparticles should be discrete and superparamagnetic with uniformly small particle sizes distribution.
7-9Reported methods for the synthesis of magnetite nanoparticles include reduction of hematite with CO/CO 2 10 or H 2 ; 11 co-precipitation from the solution of ferrous/ferric mixed salt solution in alkaline medium followed by aging and digestion in the temperature range of 90-150 °C; 12 microwave hydrothermal 13 and electrical discharge. 14 Qu et al. 15 reported a method for the direct preparation of spherically-shaped magnetite nanoparticles smaller than 10 nm, from aqueous solution of a ferric salt, which is stable in air. In such a method, the ferrous ions are formed by partial reduction of ferric ions with Na 2 SO 3 before the precipitation agent is added.In this work, it was studied the influence of the pH , on the chemical nature and properties of magnetic nanocomposites, prepared by precipitation from partially reduced ferric chloride aqueous solutions, via a modified route from that originally proposed by Qu et al.. 15 The chemical and magnetic properties of the formed nanomaterials were investigated in detail.
EXPERIMENTAL MaterialsFerric chloride...