Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Abstract

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)