Controlled preparation of unsupported binary and ternary sulfides with high surface area from tetraalkylammonium thiosalts

Unsupported MoS2, WS2 and Ni–MoS2 sulfides have been successfully prepared by decomposition of tetraalkylammonium thiosalts, which were synthesized by using an aqueous solution of tetraalkylammonium halide and ammonium thiosalts at room temperature. The as-prepared samples were characterized by N2 physorption, thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results showed that structures and properties of unsupported binary and ternary sulfides depended on tetraalkylammonium thiosalts and decomposition conditions. The samples formed by decomposition of methyl and cetyltrimethyl substituted ammonium thiosalts exhibited high specific surface areas of above 100 m2/g, indicating the organic ligand in the precursor can tune the structure of the binary and ternary sulfides. MoS2 and Ni–MoS2 prepared from TMetATM and Ni/TMetATM had a relative narrow distribution in mesoporous range. TEM and XRD results revealed that the unsupported binary and ternary sulfides consisted of few-stacked layers and Ni was well-dispersed on MoS2.