以升华硫粉为原料，采用液相沉积法在水溶液体系下制备纳米硫材料。采用激光粒度分析仪和扫描电镜，对纳米硫的合成条件进行分析与优化；通过恒流充放电测试、电化学阻抗分析等方法对所制备纳米硫的电化学性能进行表征。结果表明：在以甲酸为沉淀剂、PEG-400为分散剂、多硫化钠溶液浓度为0.2 mol/L的合成条件下，可制备出粒径范围为50~80 nm、平均粒径约65 nm且分散性较好的类球形纳米硫材料。基于该纳米硫组装的锂/硫电池在0.054 mA/cm2电流密度下，首次放电比容量达1050 mA?h/g，经10次循环后，放电容量仍可保持初始容量的70%左右(700 mA?h/g)。本方法工艺简单、操作方便、成本低廉，适合锂/硫电池用纳米硫材料的工业化制备。
Sulfur nanomaterial was prepared in aqueous solution by liquid phase precipitation method with sublimed sulfur as the raw material. The synthesis conditions of the material were analyzed and optimized by laser size analysis device (LSA) and scanning electron microscopy (SEM). The electrochemical performances of the materials were studied by charge-discharge test and electrochemical impedance spectroscopy (EIS). The results show that spherical sulfur nanomaterial with good dispersion is synthesized under the condition of using formic acid as the precipitant, PEG-400 as the dispersant and 0.2 mol/L sodium polysulfide solution. The range and average value of particle size are about 50?80 nm and about 65 nm, respectively. Also, the initial specific capacity of the Li/S battery assembled of sulfur nanomaterial can reach 1 050 mA?h/g at a current density of 0.054 mA/cm2, and the discharge capacity retains 70%(700 mA?h/g) of the initial capacity after 10 cycles. This method is simple and low cost to prepare sulfur nanomaterial used in lithium sulfur batteries.
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