Cation distribution in CuFe₂O₄ nanoparticles: Effects of Ni doping on magnetic properties

The Cu_1−xNi_xFe₂O₄ nanoparticles (with x = 0, 0.3, 0.5, 0.7, and 1) were synthesized by using spray co-precipitation method at annealing temperature T_a = 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 T_C 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.