Nickel zinc ferrite ͑NZFO͒ nanoparticles were synthesized via a reverse micelle method with a nonionic surfactant. Three different initial Fe 3+ / Fe 2+ ratios were employed along with three different firing temperatures ͑200, 500, 1000°C͒ to investigate the effects on the NZFO system. Extended x-ray absorption fine structure ͑EXAFS͒ results reveal zinc loss at high annealing temperatures; at 1000°C, the loss is nearly total for Fe 3+ / Fe 2+ ratios other than 10:90. Annealing at 500°C, however, appears necessary for fully incorporating the zinc and nickel into the spinel phase. The best nanoferrite was thus obtained using an initial Fe 3+ / Fe 2+ ratio of 10:90 and a moderate firing temperature of 500°C. This sample exhibits a room temperature saturation magnetization of 58 emu/g as measured via vibrating sample magnetometry, comparable with bulk values and greater than that of confirmed nano-NZFOs found in the literature. EXAFS also indicates that in all cases in which the elements adopted a spinel structure, the nickel occupies only octahedral sites and the zinc primarily tetrahedral sites.
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