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In this research a sol-gel auto-combustion route has been proposed to synthesize nickel-zinc ferrite nanocrystalline powder, using metal nitrates, citric acid as fuel and ammonia as pH adjusting agent. The influence of pH value of the solution on phase evolution, crystallite size and morphology of as-burnt powders were investigated by XRD, SEM and TEM techniques. The results revealed that with pH=7 the single phase nickel-zinc ferrite nanocrystalline powders with crystallite size of about 27nm were formed directly after auto combustion process.