Abstract: Experiments on preparation of iron oxide-mica nano-membrane materials were done to discuss some crucial parameters' influences on final pigment. Through these experiments, we gained the best preparation parameters of iron oxide-mica nano-membrane materials, and thought that the pearlescent effects of material was maily determined by the equality and superscription degrees of Fe₂O₃ particle-membrane, furtherly by the difference of preparation parameters. The final gained best parameters were: primary Fe³⁺ solution was 0.2 mol/l, the ration of Fe3+ solution volume to mica powder was 11:1; pH was about 3, reaction temperature was 70-80℃, titration velocity was 1.0-1.4ml/min; baked temperature were 650, 900℃ and time was 2 hours respectively.