在无模板、无催化剂、无表面活性剂的条件下，用溶剂热法合成了ZnIn₂ S₄光催化剂．通过X 射线衍射、扫描电子显微镜、能谱、X 射线光电子能谱、紫外－可见漫反射光谱分析等技术对样品进行了表征，研究了合成反应时间对ZnIn₂S₄催化剂晶体结构、形貌、光学性质及催化性能的影响． 结果表明: ZnIn₂S₄微球由大量的纳米薄片组成，呈现出花瓣状结构; 缩短合成反应时间导致ZnIn₂ S₄晶粒变大，同时样品的稳定性增加，产氢速率增大;ZnIn₂S₄的催化性能随着合成反应时间的延长而下降; 合成反应时间为1 h 时制备的样品具有最佳的光催化制氢活性，产氢率达745．8 μmol /( h·g) ．

Photocatalyst ZnIn₂S₄ was synthesized via the solvothermal method without templates,catalysts and surfactants,and the as-synthesized samples were characterized by means of XRD,SEM,EDS,XPS and UV-vis.Moreover,the effects of reaction time on the crystal structure,morphology,optical properties and photocatalyticactivity of ZnIn₂S₄ samples were discussed. The results indicate that ZnIn₂S₄ microspheres are composed of numerousnanosheets and present petaloid structure,and that,with the decrease of reaction time,the crystallite graduallyenlarges,the stability of the samples improves and the hydrogen production rate increases. However,with theincrease of reaction time,the photocatalytic activity of ZnIn₂S₄ decreases. In addition,after a solvothermal procedurefor 1h,the photocatalytic activity of ZnIn₂S₄ achieves the maximum and the hydrogen production rate is up to745.8 μmol /( h·g) .