| 水热法合成球花状二硫化钼及其电化学性能 |
| Hydrothermal Synthesis of MoS2 Flower-like Spheres with Electrochemical Performances |
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| 摘要: 采用二水钼酸钠（Na2MoO4·2H2O）和硫脲（CS（NH2）2）分别作为钼源和硫源，通过水热合成法获得球花状二硫化钼，其较佳的水热条件为：180℃下反应48 h，钼硫原子比为1：4，反应物浓度为0.001 mol·L-1， 在100 mL反应釜中的填充体积为90 mL。采用X射线衍射（XRD）、扫描电镜（SEM）和透射电镜（TEM）、对样品的物相和形貌进行了表征，并利用低温氮吸附BET模型测试了样品的比表面积。结果表明，合成的二硫化钼结晶性良好，平均粒径约为1 μm，比表面积约为87 m2·g-1，分布均匀且无明显团聚。通过循环伏安（CV）曲线、恒电流充放电曲线（GCD）、阻抗谱图（EIS）表征其电化学性能，测试表明：在3 mol·L-1 KOH水相电解液中，单电极比电容可达130.6 F·g-1（扫速为5 mV·s-1）和110.9 F·g-1（电流密度为0.1 A·g-1），界面转移电阻Rct为0.33 Ω；循环 1 000圈后比电容损失为14.7%。说明采用该水热法合成的二硫化钼可以成为超级电容器电极的理想材料。 |
| 关键词: 二硫化钼 水热法 电化学性能 |
| 基金项目: 湖北省自然科学基金项目（No.2014CF258）资助项目。 |
| Abstract: A simple but useful hydrothermal method is developed to prepare molybdenum disulfide (MoS2) flower-like spheres by sodium molybdate dehydrate (Na2MoO4·2H2O) and thiocarbamide (CS(NH2)2). In this work, the appropriate hydrothermal condition is at 180℃ reaction temperature for 48 h and the atomic ratio of S and Mo is 1:4 in 0.001 mol·L-1 aqueous solution. The morphologies and microstructures of as-prepared MoS2 are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area test method (BET). Results indicate that the average diameter of as-prepared products is about 1 μm with good crystallinity and dispersibility, and their specific surface area is about 87 m2·g-1. In order to character the electrical properties of MoS2, the electrochemical performance was studied by cyclic voltammetry (CV), galvanostatic charge-discharge cycling (GCD) and electrochemical impedance spectroscopy (EIS). Analysis results show that in 3 mol·L-1 KOH electrolyte, the specific capacitance of single electrode is 130.6 F·g-1 at 5 mV·s-1 scan rate and 110.9 F·g-1 at 0.1 A·g-1 current density. The charge-transfer resistance (Rct) is of 0.33 Ω. The loss of specific capacitance is 14.7% after 1 000 cycles. These electric properties illustrate the MoS2 prepared by hydrothermal processing can act as an ideal material for supercapacitor electrode. |
| Keywords: molybdenum disulfide hydrothermal method electrochemical performances |
| 投稿时间：2017-05-07 修订日期：2017-07-28 |
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| 李美娟,沈舒宜,罗国强,张联盟.水热法合成球花状二硫化钼及其电化学性能[J].无机化学学报,2017,33(9):1521-1526. |
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