Effect of Ca²⁺ doping and annealing temperature on the structure, morphology and magnetic behavior of Ca_xCo_1-xFe₂O₄/SiO₂ nanocomposites

Co-doped ferrites are promising functional materials for many practical applications and their physical properties can be tailored by changing their composition. This study assesses the structure, morphology and magnetic properties of CaxCo1-xFe2O4/SiO2 (x = 0.0-0.5) nanocomposites (NCs) obtained by sol-gel method and annealed at different temperatures (400, 800 and 1200 degree celsius). The effect of Ca2+ doping on the properties of nano-structured Ca-Co ferrite embedded in the SiO2 matrix was investigated by thermogravimetry and differential thermal analysis, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, inductively coupled plasma optical emission spectrometry, atomic force microscopy (AFM) and magnetic measurements. The thermal analysis showed the formation of metal succinates up to 200 degree celsius and of ferrite above 280 degree celsius. The presence of poorly crystalline ferrite accompanied by silicates at low annealing temperatures and of highly crystalline ferrite accompanied by SiO2 and Ca silicates at high annealing temperatures was identified by XRD. The increased Ca2+ doping led to a decrease in the structural parameters estimated by XRD and the surface area. The AFM images revealed that the NCs have a crystalline core covered by a layer of amorphous SiO2. The hysteresis loop shape indicated the superparamagnetic-like and ferromagnetic behavior of the obtained NCs. The magnetic properties improved with the increase in annealing temperature and depended on the particle size and dopant content. The NCs with low Ca2+ content annealed at 800 degree celsius still show appreciable hysteresis, but doping with high Ca2+ contents drastically affects the magnetic properties.