(1. 東北大學 材料各向異性與織構教育部重點實驗室，沈陽 110819；
2. 東北大學 材料科學與工程學院，先進陶瓷材料研究中心，沈陽 110819)
摘 要: 本文以綠色、環(huán)境友好的沒食子酸(GA)為還原劑，一步水熱合成制備出納米顆粒自組裝成的ZnSe微米球。同時研究了水熱反應中GA添加量、反應溫度及時間等參量對產(chǎn)物組成與形貌的影響以及ZnSe微球生長機制。利用XRD、SEM、TEM、XPS、UV-Vis DRS、FTIR等手段表征了樣品物相組成、形貌、光譜特征。利用紫外光催化降解羅丹明B(RhB)溶液評價ZnSe微球的光催化性能。結果表明，在GA的還原作用下，Se被有效還原為Se2-，并與Zn2+反應形成閃鋅礦ZnSe。GA添加量和水熱溫度是控制產(chǎn)物組成與形貌的關鍵。ZnSe一次顆粒尺寸隨GA添加量的增加而逐漸減小；只有溫度達到150 ℃及以上時，產(chǎn)物才為單相ZnSe。在15 mmol GA、200 ℃、24 h優(yōu)化條件下制備的ZnSe微球具有優(yōu)異的光催化性能，紫外光照2.5 h后，ZnSe微球?qū)hB的光催化降解率達98.1%。
關鍵字: 沒食子酸；ZnSe；微米球；水熱法；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
