Onsite magnetic moments through cation distribution and magnetocrystalline anisotropy studies of NiFe2−xRxO4 (R = Y and Lu; x = 0, 0.05, and 0.075) compounds were investigated, and the results are discussed and presented in this paper. All the compounds were prepared by solid state reaction, and the compounds formed in the cubic inverse spinel phase with the space group Fd3¯m. The cation distribution, bond lengths, u-parameter, etc. were estimated through the Rietveld refinement of XRD patterns. Increment in the lattice constant was observed upon partial substitution of Fe3+ by Y3+/Lu3+. The presence of all elements and their ionic states were confirmed from X-ray photoelectron spectroscopy studies. Analyses of Mössbauer spectra revealed that the hyperfine fields and the magnetic moments at the B-site (and hence net moment) decreased with increasing Y3+/Lu3+ occupancy and that the compounds exhibited a Néel-type, collinear ferrimagnetic structure. Magnetization measurements revealed that the magnetic moment decreased with Y3+/Lu3+ substitution. The high field regimes of the magnetization curves were modeled using the law of approach to the saturation magnetization equation, and the first order cubic anisotropy constants (K1) were calculated. The temperature variation of K1 and effects of Y3+/Lu3+ substitution are explained.

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