Electron paramagnetic resonance studies have been carried out over 3.7‐300 K on micropowders of Ni1‐xZnxFe2O4 ferrites, obtained by high temperature synthesis and preliminary characterized by X‐ray diffraction and differential scanning calorimetry in a wide range of tempera‐tures. Complimentary, scanning probe microscopy, compris‐ing atomic and magnetic force microscopies has been applied to polycrystalline Ni1‐xZnxFe2O4thin films. The correlation between X‐ray and differential scanning calorimetry data has been observed. Deconvolution of the obtained paramagnetic resonance spectra into Gaussian components and their further analysis have allowed retrival of the compensation points of the magnetc momenta of the sublattices of Ni1‐xZnxFe2O4, as well as of superparamagnetism effect and g‐factors dispersion verified by studies on polycrystalline thin films. (© 2015 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

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