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Magnetic properties of materials with frustrated structure excite the interest of scientific community for decades. Usually the frustrated magnetic structure is generated in ferrites with spinel structure as a result of diluting of both octahedral and tetrahedral sublattices by non-magnetic ions. Lately, it was discovered that the spinels don’t have to be diluted to reveal frustrated magnetic structure. Injecting of relatively large amount of Cr3+ ions leads to the same effect [1,2]. In our study, the samples of Ni ferrite-chromite nanoparticles were synthesized and comprehensively studied by the means of X-ray diffraction, TEM and SEM spectroscopy and Mössbauer spectroscopy, also FC and ZFC magnetization measurements were performed. Magnetic and crystal structure of the samples and the influence of annealing temperature in the process of synthesis were defined.