Calcium and nickel-doped ferrites open a wide variety of applications in various fields. This work reports the synthesis and systematic investigation of the effect of nickel substitution in calcium ferrite powder. A series of NixCa1-xFe2O4 nanocrystalline powder (NixCa1-xFe2O4, x = 0, 0.1, 0.2...1) were prepared by co-precipitation method and sintered at 900 °C for 10 h. The samples were characterized using x-ray diffraction, x-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Vibrating sample magnetometry (VSM). XRD results revealed that the prepared samples were of cubic spinel structure with particle sizes ranging from 27 nm to 72 nm. A decreasing trend was observed in the particle size with an increase in nickel substitution. The saturation magnetization of the samples was found to increase with the increase in nickel substitution.
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