Nanoparticle Ni 1−x Zn x Fe 2 O 4 (x = 0.35, 0.45) samples were prepared successfully via microwave assisted combustion method. Synthesis of nanosize materials at a low temperature using a domestic microwave oven is the unique feature of this method and is being tried for the first time to produce NiZn ferrites. Single-phase formation of the samples was confirmed from X-ray analysis and IR spectrum. XRD data reveals that lattice parameter increases with Zn content 'x'. Particle sizes calculated from XRD analysis are in good agreement with TEM results. Extent of spin canting at octahedral B-site is deduced from Yafet-Kittel angles. Surface properties and reduced particle size affects the Curie temperature.

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