The Cu1−xNixFe2O4 nanoparticles (with x = 0, 0.3, 0.5, 0.7, and 1) were synthesized by using spray co-precipitation method at annealing temperature Ta = 900 °C in air for 5 h. The crystal structure, microstructure, oxidation state, and magnetic properties of the samples were characterized by using X-ray diffraction, synchrotron X-ray diffraction, scanning electron microscopy, X-ray absorption spectroscopy, and vibrating sample magnetometer. It was shown that all the samples have cubic structure. Lattice constant and grain size decrease, while the Curie temperature TC increases with increasing of Ni2+ content. A small amount of Fe2+ was found in all the samples. Cation distribution was determined by using a combination of magnetization measurements, extended X-ray absorption fine structure analysis, and Rietveld refinement from synchrotron X-ray diffraction data. It was indicated that Ni2+ ions occupy in octahedral site only, while Cu2+ ions distribute in both tetrahedral and octahedral sites. The variation of magnetic parameters is discussed based on Ni2+ concentration, grain size, the cation distribution, surface effect, and the presence of Fe2+ ion in the samples.

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The MgFe 2 O 4 nanoparticles are synthesized by combustion method and annealed at different temperatures from 500 to 1000 C. Magnetic properties, morphology, valence states of iron, crystal structure, and microstructure of the samples are investigated systematically by vibrating sample magnetometer, field emission scanning electron microscope, transmission electron microscopy, X-ray absorption spectroscopy, and synchrotron X-ray diffraction. Cation distribution is determined from synchrotron X-ray diffraction data using Rietveld refinement combined with extended X-ray absorption fine structure spectroscopy. The results indicates that all the samples are phasepure with crystallite size ranging from 11 to 41 nm. By adjusting the annealing temperature, cation distribution and particle size can be changed, and consequently leading to the change in structure and magnetic properties. The saturation magnetization of the samples are enhanced significantly compared to that of the bulk material. The variation of magnetic properties is discussed based on cation distribution, particle size, valence state, surface effect, and spin canting.

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