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氧化鋅空心球和納米纖維的制備

發(fā)布時間:2018-02-27 03:34

  本文關(guān)鍵詞: 氧化鋅 氫氧化鋅 空心球 納米纖維 出處:《上海交通大學(xué)》2015年碩士論文 論文類型:學(xué)位論文


【摘要】:在眾多Zn O納米材料中,空心球和一維的納米纖維因其結(jié)構(gòu)的獨特性,分別在微型反應(yīng)器、藥物緩釋、化學(xué)存儲和大規(guī)模集成電路、微型精密儀器等領(lǐng)域有著良好的應(yīng)用前景。采用可控的方法合成不同結(jié)構(gòu)的氧化鋅材料有著十分重要的意義。本文第一部分選用醋酸鋅(二水)的乙醇胺溶液,利用溶劑熱法,在無催化劑和模板的條件下一步合成了直徑1.5μm~4.5μm的氧化鋅空心微米球。通過改變反應(yīng)時間、水含量和Zn2+的濃度等反應(yīng)條件,推測出在該反應(yīng)體系中氧化鋅空心微米球的形成機(jī)理:晶核生長為氧化鋅納米棒,納米棒形成小的錐形聚集體,小聚集體堆積成球并經(jīng)過Ostwald熟化形成空心結(jié)構(gòu)。隨后考察了換用正丁胺、異丁胺、乙二胺和向體系中引入聚乙烯吡咯烷酮、精對苯二甲酸、十六烷基三甲基溴化銨對晶體形貌的影響。第二部分在常溫常壓的條件下大量的制得了超長的氧化鋅納米纖維。首先利用正辛胺和醋酸鋅(二水)的三甘醇溶液合成了長100~200nm,寬25~50nm的氧化鋅納米棒。將該納米棒分散在堿(如異丁胺、吡啶、異戊胺)和溶劑(如水、DMF、乙酸乙酯、環(huán)己烷等)的混合溶液中。滴加400μl該體系在蓋玻片上自然揮發(fā),觀察到氧化鋅的溶解以及溶解反應(yīng)產(chǎn)物結(jié)晶出超長的納米纖維并組成網(wǎng)絡(luò)結(jié)構(gòu)。實驗發(fā)現(xiàn)當(dāng)所用堿的堿性較強、溶劑的揮發(fā)性和環(huán)境濕度較高時對反應(yīng)有利。其次選擇ZnO濃度為1.0mg/ml的異丁胺:乙酸乙酯=1:15(V:V)分散體系,在開口的樣品瓶中進(jìn)行揮發(fā)實驗,對產(chǎn)物采用SEM、TEM、XRD、紅外光譜、熱重分析、元素分析等手段進(jìn)行表征,推測反應(yīng)過程機(jī)理:揮發(fā)過程中空氣中的水進(jìn)入體系中,異丁胺與水反應(yīng)生成氫氧根,ZnO在堿性環(huán)境下溶解,最終生成Zn(OH)2。在這個過程中的關(guān)鍵因素是氧化鋅晶體周圍堿性的強弱,決定了反應(yīng)能否發(fā)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.

【學(xué)位授予單位】:上海交通大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ132.41;TQ343.5

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 鄧文雅;趙宗彬;沈琳;邱介山;;氧化鋅空心球的制備及光致發(fā)光特征[J];功能材料;2007年09期

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本文編號:1540969

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