Synthesis and characterization of nanostructured cobalt ferrite by the microwave assisted hydrothermal method.
CoFe2O4; CoFe2; Core-Shell System; Hydrothermal Synthesis.
Cobalt ferrite is characterized by good magnetic moment saturation and considerable coercivity. The methods used in the production of CoFe2O4 that enable control of the particle size distributed are best suitable for different applications. The present study focused on the preparation and characterization, both structural and magnetic, of CoFe2O4 nanoparticles and CoFe2O4-CoFe2 core-shell system. CoFe2O4 ferrite was produced via the Hydrothermal Microwave Method and, subsequently reduced in flowing hydrogen atmosphere for the formation of the CoFe2O4-CoFe2 system. In the production of CoFe2O4, four series were produced individually using ammonia hydroxide, potassium hydroxide, sodium hydroxide and ethylene glycol. The structural characterization of the samples was performed by X-ray diffraction with Rietveld refinement and Transmission Electron Microscopy. Only the series using ammonia and potassium hydroxide depicted pure cobalt ferrite. Analyses of the diffractograms revealed that the average diameter of crystallites ranged from 5.2 to 21.3 nm. The potassium hydroxide series resulted in larger crystallites of mixed form (approximately spherical and cubic) whereas those of the ammonium hydroxide series were smaller and spherical. Samples of the sodium hydroxide and ethylene glycol series were characterized by the presence of hematite. The samples were also characterized by the magnetically vibrating sample method at room temperature and by physical property measurement system (PPMS) at low temperatures, in addition to Mössbauer spectroscopy. The results revealed the characteristic magnetically blocked behavior for samples with crystallites larger than 10 nm and superparamagnetic behavior for smaller crystallite sizes. The ratio MR:MHmax increased with increasing the crystallite size. In the production of CoFe2O4-CoFe2 system, a sample of the potassium hydroxide series was used after reduction in hydrogen atmosphere and stabilization at 350°C for 10 min. CoFe2 was obtained from this procedure. The reduced sample was analyzed. The XRD pattern and TEM images showed the formation of the core-shell system, indicating that the average diameter of crystallites was 33.7 nm (6.3 nm for CoFe2O4 and 27.4 nm for CoFe2). The magnetic properties, analyzed by the hysteresis plots and Mössbauer spectrum were also improved compared to the starting sample. The ratio MR:MHmax increased from 0.299 to 0.356.