Abstract: Results of XRD and Raman spectra show the successful preparation of lamellar structural materials Ni₂P₂S₆by 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 Ni₂P₂O₇and the existence of an intermediate metastable Ni₂P₂O₆phase of Ni₂P₂S₆thermo-oxidation in air.

Key words: Ni₂P₂S₆, Lamellar structure, Room temperature solid state reaction