(1. 东北大学 材料各向异性与织构教育部重点实验室，沈阳 110819；
2. 东北大学 材料科学与工程学院，先进陶瓷材料研究中心，沈阳 110819)
摘 要: 本文以绿色、环境友好的没食子酸(GA)为还原剂，一步水热合成制备出纳米颗粒自组装成的ZnSe微米球。同时研究了水热反应中GA添加量、反应温度及时间等参量对产物组成与形貌的影响以及ZnSe微球生长机制。利用XRD、SEM、TEM、XPS、UV-Vis DRS、FTIR等手段表征了样品物相组成、形貌、光谱特征。利用紫外光催化降解罗丹明B(RhB)溶液评价ZnSe微球的光催化性能。结果表明，在GA的还原作用下，Se被有效还原为Se2-，并与Zn2+反应形成闪锌矿ZnSe。GA添加量和水热温度是控制产物组成与形貌的关键。ZnSe一次颗粒尺寸随GA添加量的增加而逐渐减小；只有温度达到150 ℃及以上时，产物才为单相ZnSe。在15 mmol GA、200 ℃、24 h优化条件下制备的ZnSe微球具有优异的光催化性能，紫外光照2.5 h后，ZnSe微球对RhB的光催化降解率达98.1%。
关键字: 没食子酸；ZnSe；微米球；水热法；光催化
（1. Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), Northeastern University, Shenyang 110819, China;
2. Advanced Ceramics Research Center, School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China）
Abstract:In this paper, ZnSe microspheres self-assembled by nanoparticles were synthesized by one-step hydrothermal using green, environmentally friendly gallic acid (GA) as reducing agent. Meanwhile, the effects of GA amount, reaction temperature and time on composition and morphology of the products, and growth mechanism of the ZnSe microspheres were also studied. XRD, SEM, TEM, XPS, UV-Vis DRS and FT-IR were used to characterize phase composition, morphology and spectral features of the prepared samples. Photocatalytic property of the ZnSe microspheres was evaluated by photocatalytic degradation of Rhodamine B (RhB) solution under UV irradiation. The results show that, using GA as reductant in hydrothermal synthesis, Se element could be effectively reduced to Se2- and then react with Zn2+ to form ZnSe. The amount of GA and hydrothermal reaction temperature play a key role in controlling composition and morphology of the products. With the increase of GA, the primary particle size of ZnSe gradually decreases, and only when the hydrothermal temperature is 150 ℃ or above, the single-phase ZnSe can be obtained. Under the optimized conditions of 15 mmol GA, 200 ℃ and 24 h, the obtained ZnSe microspheres show superior photocatalytic performance, e.g., the photocatalytic degradation efficiency of RhB for ZnSe microspheres achieves 98.1% after UV irradiation for 2.5 h.
Key words: gallic acid; ZnSe; microsphere; hydrothermal method; photocatalysis
