Ar气保护固相合成花状二硫化钼工艺研究

以三氧化钼和硫为原料,采用Ar气保护固相合成法,合成花状二硫化钼。采用XRD、SEM、TEM等手段对样品的结构和形貌进行表征。考察了原料比、反应温度、反应时间、升温速率对样品纯度的影响,制备出纯度较高的二硫化钼。结果表明:当MoO₃与S物质的量之比为1∶7.5,反应温度为450 ℃,反应时间为4 h,升温速率为15 ℃/min,可得到纯度为99.4%的花状二硫化钼,该花状结构由厚度为10 nm左右的翘曲片层组成,TEM照片中可见0.62 nm单层二硫化钼结构,具有较大的比表面积,使其在储能、催化等领域有广阔的应用前景。

Solid-State Synthesis of Flower-Like Molybdenum Disulfide by Argon Protection

Flower-like molybdenum disulfide was synthesized from molybdenum trioxide and sulfur by argon protection solid-state method. The structure and morphology of the products were characterized by XRD, SEM and TEM. The effects of raw material ratio, reaction temperature, reaction time and heating rate on the purity of the product were investigated, and molybdenum disulfide with high purity was prepared. The results show that when the molar ratio of MoO₃∶S is 1∶7.5, the reaction temperature is 450 ℃ and the reaction time is 4 h, heating rate is 15 ℃/min, the flower-like molybdenum disulfide with purity of 99.4% can be obtained. The flower-like structure is composed of warped thin plate with thickness of about 10 nm. 0.62 nm monolayer MoS₂ is observed by TEM. Flower-like molybdenum disulfide has large specific surface area, which has broad application prospects in the fields of energy storage and catalysis.