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Two-phase nanocomposites comprised of Zn1−xNixO/NiO (0.05 ≤ x ≤ 0.3) were grown by using sol-gel process with hydrated metal acetates as precursors. Thermal decomposition of the co-precipitated oxalate α-ZnNi(C2O4) yields wurtzite h.c.p. Zn1−xNixO and f.c.c. NiO together. The X-band electron spin resonance spectra provide the signatures of anisotropic spin interactions with long-range magnetic ordering...