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铝阳极氧化多孔膜的制备、表征及应用研究

Fabrication, Characterization and Application of Porous Alumina Film

【作者】 朱静

【导师】 王为;

【作者基本信息】 天津大学 , 应用化学, 2005, 硕士

【摘要】 近年来研究制备具有纳米孔结构的氧化铝多孔膜越来越受到人们的关注。这种具有纳米孔结构的三氧化二铝膜具有特殊的性能而被广泛地用于各个领域:超微过滤和催化反应器,电解质的质子交换膜,微电子及电容器件,制备纳米材料的模板。本论文采用阳极氧化方法制备氧化铝多孔膜并对阳极氧化条件对氧化铝膜形成过程及结构的影响及氧化铝多孔膜的性能及应用进行了研究。1.具有纳米孔阵列结构的三氧化二铝多孔膜的制备过程的研究。分别在不含添加剂的草酸体系和含有添加剂的草酸体系,进行恒压直流阳极氧化。采用电化学联机测试系统对氧化膜形成过程进行记录,研究添加剂对氧化铝多孔膜形成过程的影响。并在硫酸和磷酸体系中进行试验,验证上述规律研究证明,加入添加剂降低氧化膜的生长速度和纳米孔阻挡层的形成速度。分别对两种体系生成的氧化膜进行XRD分析,分析结果表明,两种体系中生成的氧化铝多孔膜均为馒头峰,证明加入添加剂对氧化铝多孔膜的晶态结构没有影响; 对两种体系生成的氧化铝薄膜进行扫描电镜SEM分析,结果表明:加入添加剂的体系生成的氧化铝多孔膜的纳米孔孔径较小,孔隙率较高,孔形规整程度较好; 对两种体系生成的氧化铝多孔膜进行红外吸收IR分析,结果表明:两种体系中生成的氧化铝多孔膜的成分不相同,含有添加剂的体系生成的氧化膜阻挡层中有添加剂的官能团存在有利于提高氧化膜的性能。2.研究氧化铝多孔膜的机械性能。采用弯曲断裂法测试冷轧态和退火态铝基材生成的氧化膜的断裂韧性; 含添加剂和不含添加剂两种体系生成的氧化膜的断裂韧性。研究表明,退火态铝基材生成的氧化膜的断裂韧性优于冷轧态铝; 含添加剂体系生成的氧化膜的断裂韧性优于不含添加剂体系。3.氧化铝多孔膜在温差电材料中的应用。研究了沉积电位、氧化铝模板厚度、孔径等对温差电材料电沉积过程的影响; 采用透射电镜TEM对沉积的温差电纳米线进行分析,采用本课题组自行研制的温差电测试系统对纳米线阵列的温差电性能及电阻进行测试。

【Abstract】 In recent years , alumina membranes have attracted increasing amount of attention due to their potential use in several field of technological interest , such as micro and ultrafiltration catalytic reactors and electrolytes for proton exchange, wear-resistance coatings. PAA membranes with straight nanochannels of uniform diameter and length have been widely used to fabricate one-dimensional nanomaterials with controllable orientation, position and size, or two dimensional nanoparticle arrays. 1. Effect of glycerin on the process of anodization. In this experiment, AAO with parallel nanochannels was anodized by anodizing high-purity Al in 3% oxalic acid solution and 3% oxalic acid solution with additive 10g/L. The process of alumina membranes growth were recorded by electrochemical computer test system . The morphology of the samples was examined by scanning electron microscope (SEM) and structure was tested by XRD, composition of the alumina and anodization electrolyte was found by IR transparent spectra method. The density-voltage show that glycerin can decrease the speed of the growth of barrier layer and nanopores, The XRD sprctra show that only amorphous alumina exists in the membranes prepared either in oxalic acid solution or oxalic acid solution with organic additive. According to the measurement , we come to the conclusion that the glycerin doesn’t change the structure of alumina. IR spectra show that the additive had reacted during the anodization process and effect the diameter of the nanopore. 2. Mechanical property of alumina membranes. Mchanical property of AAO was measured by crook break measurement. The result show that first the property of membranes obtained on annealed aluminium is better than cold aluminium. Second, the property of the samples obtained in oxalic acid solution with glycerin is better than that obtained in oxalic acid solution. 3. Fabrication of thermoelectric materials in AAO. In this experiment, AAO was used as a template to electrodepose Bi2Te3 nanowires. The effect of voltage , diameter of nanopore and length of nanopore on the process of deposition were studied by electrochemical working system. Morphology and composition of nanowire were tested by TEM. Thermoelectric properties of the material were measured by thermoelectric test system developed by our team.

  • 【网络出版投稿人】 天津大学
  • 【网络出版年期】2006年 06期
  • 【分类号】O614.31
  • 【被引频次】5
  • 【下载频次】859
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