氧化锌空心球和纳米纤维的制备

发布时间：2018-02-27 03:34

本文关键词： 氧化锌氢氧化锌空心球纳米纤维　出处：《上海交通大学》2015年硕士论文　论文类型：学位论文

【摘要】：在众多Zn O纳米材料中,空心球和一维的纳米纤维因其结构的独特性,分别在微型反应器、药物缓释、化学存储和大规模集成电路、微型精密仪器等领域有着良好的应用前景。采用可控的方法合成不同结构的氧化锌材料有着十分重要的意义。本文第一部分选用醋酸锌(二水)的乙醇胺溶液,利用溶剂热法,在无催化剂和模板的条件下一步合成了直径1.5μm~4.5μm的氧化锌空心微米球。通过改变反应时间、水含量和Zn2+的浓度等反应条件,推测出在该反应体系中氧化锌空心微米球的形成机理:晶核生长为氧化锌纳米棒,纳米棒形成小的锥形聚集体,小聚集体堆积成球并经过Ostwald熟化形成空心结构。随后考察了换用正丁胺、异丁胺、乙二胺和向体系中引入聚乙烯吡咯烷酮、精对苯二甲酸、十六烷基三甲基溴化铵对晶体形貌的影响。第二部分在常温常压的条件下大量的制得了超长的氧化锌纳米纤维。首先利用正辛胺和醋酸锌(二水)的三甘醇溶液合成了长100~200nm,宽25~50nm的氧化锌纳米棒。将该纳米棒分散在碱(如异丁胺、吡啶、异戊胺)和溶剂(如水、DMF、乙酸乙酯、环己烷等)的混合溶液中。滴加400μl该体系在盖玻片上自然挥发,观察到氧化锌的溶解以及溶解反应产物结晶出超长的纳米纤维并组成网络结构。实验发现当所用碱的碱性较强、溶剂的挥发性和环境湿度较高时对反应有利。其次选择ZnO浓度为1.0mg/ml的异丁胺:乙酸乙酯=1:15(V:V)分散体系,在开口的样品瓶中进行挥发实验,对产物采用SEM、TEM、XRD、红外光谱、热重分析、元素分析等手段进行表征,推测反应过程机理:挥发过程中空气中的水进入体系中,异丁胺与水反应生成氢氧根,ZnO在碱性环境下溶解,最终生成Zn(OH)2。在这个过程中的关键因素是氧化锌晶体周围碱性的强弱,决定了反应能否发生。
[Abstract]:In many Zn O nano materials, hollow spheres and one-dimensional nano fiber because of its unique structure, respectively, in the micro reactor, drug delivery, chemical storage and large scale integrated circuit, the field of micro precision instrument has good application prospects. Has a very important significance by controllable synthesis method with different structure Zinc Oxide material. In the first part of this paper using zinc acetate (two water) ethanolamine solution by solvent thermal method, Zinc Oxide hollow microspheres with diameter of 1.5 mu m~4.5 mu m synthesis without catalyst and template conditions in the next step. By changing the reaction time, the concentration of the reaction conditions such as water content and Zn2+, speculate the formation mechanism in the reaction system of Zinc Oxide hollow microspheres: crystal growth for Zinc Oxide nanorods, nanorod cone formed small aggregates, small aggregates piled into a ball and after Ostwald ripening form empty knot Structure. Then examine the change with n-butylamine, isobutylamine, ethylenediamine and system to introduce polyvinylpyrrolidone, terephthalic acid, sixteen alkyl three methyl bromide on crystal morphology. In the second part of the atmospheric conditions a large number of prepared long Zinc Oxide nanofibers. Firstly using n-octylamine and zinc acetate (two water) three diethylene glycol solution synthesis of 100~200nm long, 25~50nm wide. The Zinc Oxide nanorod nanorods dispersed in alkali (such as isobutylamine, pyridine, isoamyl amine) and solvent (such as water, DMF, ethyl acetate and cyclohexane) mixed solution. Adding 400 l of the the coverslip system in natural evaporation, observed Zinc Oxide's dissolution and the dissolution reaction product crystallization of nano fiber long and formed a network structure. It was found that when used alkali alkaline strong, volatile and high humidity environment when the solvent of the reaction. Select the concentration of ZnO is 1.0mg/ml isobutylamine: ethyl acetate =1:15 (V:V) dispersion system, the volatile experiment in the sample bottle opening, the products by SEM, TEM, XRD, infrared spectroscopy, thermogravimetric analysis, elemental analysis and other means of characterization, the reaction process mechanism: system of water in the air into the evaporation process in isobutylamine react with water to produce hydroxyl, ZnO dissolved in alkaline environment, the generated Zn (OH) 2. key factors in this process is the Zinc Oxide crystal surrounding the strength of the alkaline, determine the reaction can occur.

【学位授予单位】：上海交通大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ132.41;TQ343.5

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