Results of XRD and Raman spectra show the successful preparation of lamellar structural materials Ni2P2S6 by a new synthetic route - room temperature solid state reaction, Compared with the traditional high temperature solid state reaction, the preparation method adopted here has the following advantages: fast reaction rate, low energy cost, high homogeneity of final products and the facility of preparation in quantity, Study of TG-DTA shows the final product Ni2P2O7 and the existence of an intermediate metastable Ni2P2O6 phase of Ni3P2S6 thermo-oxidation in air
