溶剂热法制备石墨烯/Sb2S3纳米复合材料及其光催化性能  

Solvothermal Synthesis and Photocatalytic Performance of Graphene/Sb_2S_3 Nanocomposites

作　　者：朱启安[1] 王建霞[1] 胡耐根[2] 魏明扬[1] 杜寒宇 蒋叔立 

机构地区：[1]湘潭大学化学学院,环境友好化学与应用省部共建教育部重点实验室,湖南湘潭411105 [2]新余学院新能源科学与工程学院,江西新余338004

出　　处：《湘潭大学自然科学学报》2016年第4期34-42,共9页Natural Science Journal of Xiangtan University

基　　金：国家自然科学基金项目(21276215)

摘　　要：以天然鳞片石墨为原料,通过改进的Hummers法制备了氧化石墨（GO）,然后以GO、三氯化锑（SbCl3）和硫代乙酰胺（CH3CSNH2,TAA）为反应物,1,2-丙二醇为溶剂,通过溶剂热法制备了石墨烯/Sb2S3（RGO/Sb2S3）纳米复合材料.用XRD、FT-IR、SEM、UV-Vis DRS、PL光谱等手段对复合材料的物相、官能团、形貌和光学性能进行了表征;并通过降解罗丹明B（RhB）对其光催化活性进行了考察.结果表明：所制备的复合材料中Sb2S3为正交晶相;Sb2S3与复合材料对可见光均有较强吸收,其能带间隙分别为1.55eV和1.43eV;PVP和GO的浓度对材料的形貌、复合效果和光催化活性有重要的影响,当GO浓度为0.5mg/mL时,所制备复合材料（RGO/Sb2S3-0.5）的复合效果最好,有很多粒径为85-100nm的硫化锑纳米颗粒附着在石墨烯片层表面及片层之间,其在PL谱中的发射峰最低,光生电子-空穴对的分离效果最好,光催化效率最高,在300 W氙灯照射下,9h后其降解率达90%以上,是纯Sb2S3的1.3倍.另外,以对苯二甲酸（TA）为荧光探针,证明了光催化过程中羟基自由基（·OH）的存在;通过加入·OH消耗剂维生素C（Vc）,进一步证明了在光催化过程中·OH起了非常重要的作用.Graphite oxide（GO）was prepared with natural flake graphite powder as raw material by a modified Hummers method,and then graphene/Sb2S3（RGO/Sb2S3）nanocomposites were successfully synthesized via solvothermal method,using GO,antimony sulfide（SbCl3）and thioacetamide（CH3CSNH2,TAA）as the reactants,1,2-propanediol as solvent.The crystal phase,functional groups,morphologies,and optical performance of the composites were characterized by XRD,FT-IR,SEM,UV-Vis DRS and PL spectra.The photocatalytic activity was investigated through the degradation of rhodamine B（RhB）.The results show that,the Sb2S3 of the as-prepared composites are of orthorhombic-phase.Both Sb2S3 and composites have strong absorption to visible light,and the band gap of them is1.55 eV and 1.43 eV,respectively.PVP and the concentration of GO have great influence on the morphologies,composite effects and photocatalytic performance of the materials.When the concentration of GO is 0.5 mg/mL,the as-prepared composite（RGO/Sb2S3-0.5）,on the surface and between the graphene flake layers of which many antimony sulfide nanoparticles with the particle diameter of 85-100nm are loaded,has the best composite effect,the lowest emission peak in the PL spectra,best separation effect of photo-generated electron-hole pairs and the highest photocatalytic efficiency.The degradation rate reaches more than 90% after 9hunder 300 W xenon-lamp irradiation,which is 1.3times higher than Sb2S3.In addition,the existence of hydroxyl radicals（·OH）in the process of photocatalysis is proved using terephthalic acid（TA）as fluorescent probe.It is proved that·OH plays a very important role in the photocatalytic degradation process by adding·OH scavenger vitamin C（Vc）.

关 键 词：硫化锑 石墨烯 复合材料 光催化 

分 类 号：O627.8[理学—有机化学] O613.62[理学—化学]