高分子网络凝胶法制备纳米氧化锌的工艺控制_英文_

· 1782 ·2009年

高分子网络凝胶法制备纳米氧化锌的工艺控制

吴建锋，刘孟，方斌正，张锋意，赵娜，徐晓虹

(武汉理工大学材料科学与工程学院，武汉 430070)

摘要：以乙酸锌[Zn(Ac)2]为原料，丙烯酰胺(AM)为单体，N,N’–亚甲基双丙烯酰胺(MABM)为网络剂，采用高分子网络凝胶法制备了纳米ZnO粉体，研究了其制备过程中反应物浓度、引发剂(NH4)2S2O8含量、溶液的pH值及各反应条件对纳米ZnO晶粒尺寸的影响。X射线衍射分析结果表明：纳米ZnO颗粒的平均晶粒大小随Zn2+起始浓度及引发剂含量的增加而增加，随溶液pH值的增加而减小。确定了用高分子网络凝胶法制备纳米ZnO粉体的最佳工艺参数为：反应温度80℃；反应时间2h；干燥温度100℃；干燥时间4h。

关键词：高分子网络凝胶法；纳米氧化锌；平均晶粒尺寸；制备工艺控制

中图分类号：TB303；TB34 文献标志码：A 文章编号：0454–5648(2009)10–1782–09

PROCESS CONTROL OF ZINC OXIDE NANO-CRYSTALLINE PREPARED BY A

POLYACYLAMIDE-GEL METHOD

WU Jianfeng，LIU Meng，FANG Binzheng, ZHANG Fengyi，ZHAO Na，XU Xiaohong

(School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070, China)

Abstract: Nanosized ZnO powders were synthesized from zinc acetate by a polyacrylamide-gel method. Acrylamide and N,N’– methylenebisacrylamide were used in the synthesis as a monomer, and a network reagent, respectively. The effects of the parameters (such as reactant concentration, content of reaction initiator (NH4)2S2O8, pH value of solvent, etc.) on the properties of the nanosized ZnO powders were investigated. The crystalline characteristics of the powders was determined by X-ray diffraction. The results indi-cate that the nanosized ZnO all belong to a hexagonal structure, and the average crystalline grain size decreases with the decreasing of reactant concentration and the reaction initiator content and increasing pH value. In addition, the synthesis process parameters can be optimized at the reaction temperature of 80℃ for 2h and drying at 100℃ for 4h.

Key words: polyacrylamide-gel method; nanometer zinc oxide; mean crystal size; process control

Nanosized ZnO particles are an inorganic functional material. As known, the nano-sized particles of ZnO have some characteristics such as surface/interface, small size, quantum size and macro-quantum tunneling as well, which can not be provided by the bulk materials. Since the nanosized ZnO particles exhibit semiconducting, piezoelectric, fluorescence and photoelectric multiple properties, they have widely been applied to piezoresis-tance, conducting materials, luminescent materials, pho-toelectron element, gas sensor, photo catalyst and coating materials, etc..[1] The existing methods for the preparation of nanosized ZnO particles include sol–gels method, chemical precipitation, hydro-thermal, microemulsion and fog-spray heat-decomposing method. Any method has its own default as a result of limitation surrounding. Odier firstly used a polyacrylamide-gel method to pre-pare nanosized YBa2Cu3O7–x powders.[2–3] The particles of the powder could not move freely and dispersed uni-formly in the network configuration due to the limitation of gel network. In the process of gel, drying and decom-posing, however, the particles had little chance to contact and reunite, which was propitious to obtain the nanosized powders with small size, high purity and uniform disper-sion. Therefore, the polyacrylamide-gel method has been widely used for preparing various nanosized powders due to the unique merits. Jiang et al.[4] reported that a solid electrolyte nanosized SrCe0.90Y0.10O2.95 powder was syn-thesized by the method, and the crystalline grain size of the powder was in a range of 31 to 50nm. Liu et al.[5] reported that a superfine NiO powder was synthesized by

收稿日期：2008–11–05。修改稿收到日期：2009–04–20。基金项目：国家支撑计划(2008ACB41B00)资助项目。

第一作者：吴建锋(1963—)，男，博士，教授。Received date:2008–11–05. Approved date: 2009–04–20. First author: WU Jianfeng (1963–), male, Ph.D., professor.

E-mail: wujf@

第37卷第10期2009年10月

硅酸盐学报

JOURNAL OF THE CHINESE CERAMIC SOCIETY

Vol. 37，No. 10

October，2009