Solvothermal Synthesis Of Micro-porous Thiolates

Chalcogenidometalates is one kind of inorganic multifunctional materials. The design and synthesis of the chalcogenidometalates have been motived. Solvothermal (hydrothermal) synthesis is one of the important technique which is used to synthesize new inorganic solid, Some novel chalcogenidometalates can be produced by this techniques.This synthesis research on porous chalcogenidometalates were carried out. Some results obtained in the research are as follows: (1) The regularity of the synthesis of porous chalcogenidometalates was obtained. These results are helpful to design and synthesize solvothermally new porous chalcogenidometalates. (2) Some novel open-framework chalcogenidometalates were prepared by this technique, such as thiozincogermanate with a cristobalite topology, [(CH3)4N]2HgGe4S10 et al. This route is also characterized by mild reaction condition, and general utility to synthesis of other chalcogenides. In the meantime, the optimal conditions to prepare the porous chalcogenidometalates were obtained by adjusting the pH of reaction system, regulating the ratio of reactants and controlling the reaction temperature. Single-crystal X-ray diffraction shows that thioziocogermanate with a cristobalite topology crystallizes in the tetragonal system, space group I-42d; with a=11.0631(16)(A), c=19.146(4)(A), Z=16, V=2343.3(7)(A3), Dc=1.550(Mg/m3), U=5.776(Mg/m3), F(000)=1024, R=0.0542, wR=0.0957. [(CH3)4N]2HgGe4S10 crystallizes in the tetragonal system, space group 1-4; with a=9.2687(8XA), c=14.3739(12)(A), Z=2, V= 1234.84(18)(A3), Dc=2.183(Mg/m3), U=11.830(Mg/m3), F(000)=736, R=0.0982, wR=0.1512. These compounds were also characterized by XRD, SEM, TG-DSC, IR techniques.