Ni2FeV3O11-.delat samples have been synthesized by the solid-state reaction method using two different heat treatment processes (samples of the type A and B). The XRD measurements have shown the same diffraction patterns for both types of samples. The temperature dependences of the electron paramagnetic resonance (EPR) spectra have been recorded for the two types of thermal annealing processes of Ni 2FeV3O11-.delta. Strong differences have been observed in the EPR spectra of both types of Ni2FeV3O 11-.delta. An intense EPR line has been recorded at high temperatures; it is suggested that the line is associated with oxygen-vanadium clusters (ferromagnetic ordering). The linewidth, resonance field and integrated intensity of the EPR spectra have shown a strong temperature dependence down to 200 K. Additionally, in one sample a very broad EPR line of Fe3+ ions appeared at low temperatures while at high temperatures this line was overlapped by the other line. The temperature dependence of the integrated intensity of this broad line has shown the Curie-Weiss behaviour. In the vanadate oxide materials with two strong magnetic ions in the structure (iron(III) and nickel(II)), the spectrum of the Fe3+ ions is not observed. Different oxygen deficiency processes could explain the differences in the EPR spectra of both types of Ni2FeV3O 11-.delta compounds.
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