AAO微纳米网格模板制备方法研究
发布时间：2018-11-09 09:28
【摘要】：多孔阳极氧化铝模板（Porous Anodic Aluminum Oxide Template）具有制备工艺简单、原材料易得且价格低廉、孔阵列高度有序且孔径在一定范围内可调等优点。 本文主要对微孔径、小孔间距阳极氧化铝模板的制备方法进行了研究，通过大量的实验对影响阳极氧化铝模板孔径、孔间距大小和孔规整度的工艺（预处理工艺、电化学抛光工艺和阳极氧化工艺）和工艺参数（氧电压值、电流密度、电解液类型及浓度、电解液温度等）进行了探究。成功的制备出了孔径在20-90nm，氧化膜厚度在200nm-10μ m的高度有序的阳极氧化铝模板。系统的研究了前处理工艺、氧化过程中参数的调整、后处理工艺等对铝片表面所施加的影响。通过调整不同的试验参数获得最优的参数组合，从而得到最佳的制备工艺。采用不同种类、不同浓度的氧化电解液（硫酸和草酸）条件下，研究了不同电压对孔径、孔间距及规整度等技术指标的影响，，分析了氧化过程中电流密度的变化、温度的变化及对氧化时间的影响。将采集到的氧化过程中的产生的电压、电流的变化实时数据绘成图表进行研究。通过控制阳极氧化铝模板的第一次阳极氧化时间、去除一次氧化膜时间以及第二次阳极氧化时间来控制氧化膜表面的形貌。对所制备的阳极氧化铝模板采用扫描电镜SEM与原子力显微镜AFM进行了表征，获得了精确的测量参数。 实验结果表明：（1）高温退火可以有效的去除铝片内部晶界间的应力，使晶粒变大,有利于孔核的形成与生长。电化学抛光可以有效的去除铝片表面的氧化层和纳米级以上的缺陷，并且对铝片表面起到微观整平作用，从而得到超平表面。高温退火以及电化学抛光等前处理工艺有利于提高模板孔的规整度和出孔面积。（2）孔径的大小主要与氧化电压和氧化电解液类型有关：孔径大小和氧化电压成近似的线性关系，氧化电压越大，所形成的孔径越大。不同类型的氧化电解液所需的最佳氧化电压高低不等，其高低关系为硫酸＜草酸＜磷酸。不同类型氧化电解液条件下所制备的模板有序孔的孔径大小关系为硫酸＜草酸＜磷酸。（3）第一次氧化对第二次氧化具有强大的引导作用，适当的延长一次氧化的时间可以提高模板孔的规整度。二次氧化所用条件应与一次氧化条件完全相同，二次氧化时间长短关系到氧化膜的厚度。（4）氧化过程中模板对于温度特别敏感，氧化过程中保持温度稳定在适当的范围内可以减少缺陷产生，提高制备成功率与模板质量。
[Abstract]:Porous anodic alumina template (Porous Anodic Aluminum Oxide Template) has the advantages of simple preparation process, easy availability and low price of raw materials, highly ordered pore array and adjustable pore size in a certain range. In this paper, the preparation method of anodic alumina template with micropore size and pore spacing was studied. The process of influencing the aperture, pore spacing and pore regularity of anodic alumina template was studied by a large number of experiments. The electrochemical polishing process and anodic oxidation process) and process parameters (oxygen voltage, current density, electrolyte type and concentration, electrolyte temperature, etc.) were investigated. A highly ordered anodic alumina template with a pore size of 20-90 nm and an oxide film thickness of 200nm-10 渭 m was successfully prepared. The effects of pretreatment process, parameters adjustment in oxidation process and post-treatment process on the surface of aluminum sheet were systematically studied. By adjusting different experimental parameters, the optimal combination of parameters is obtained, and the best preparation process is obtained. The effects of different voltages on pore diameter, pore spacing and regularity were studied under the conditions of different kinds and different concentrations of oxidized electrolytes (sulfuric acid and oxalic acid), and the change of current density during oxidation was analyzed. The change of temperature and its influence on oxidation time. The real-time data of the voltage and current generated in the oxidation process are graphed for study. The surface morphology was controlled by controlling the first anodizing time of anodic alumina template, removing the first anodizing film time and the second anodizing time. The anodic alumina template was characterized by scanning electron microscope (SEM) and atomic force microscope (AFM). The experimental results show that: (1) the high temperature annealing can effectively remove the stress between grain boundaries in the aluminum sheet, and make the grain size bigger, which is conducive to the formation and growth of the pore nucleus. Electrochemical polishing can effectively remove the oxide layer and the defects above nanometer level on the aluminum sheet surface, and play a micro-leveling role on the aluminum sheet surface, so that the super-flat surface can be obtained. Pre-treatment processes such as high temperature annealing and electrochemical polishing can improve the regularity and area of the template hole. (2) the pore size is mainly related to the oxidation voltage and the type of oxidation electrolyte: pore size and oxidation voltage. In an approximate linear relationship, The larger the oxidation voltage, the larger the pore size. The optimum oxidation voltage for different kinds of electrolytes is different, and the relationship is sulfuric acid < oxalic acid < phosphoric acid. The pore size of the template prepared under different kinds of oxidizing electrolytes is as follows: sulfuric acid < oxalic acid < phosphoric acid. (3) the first oxidation has a strong guiding effect on the second oxidation. The regularity of the template hole can be improved by prolonging the time of primary oxidation. The conditions of secondary oxidation should be exactly the same as that of primary oxidation. The duration of secondary oxidation is related to the thickness of oxide film. (4) the template is particularly sensitive to temperature during oxidation. Keeping the temperature stable in the oxidation process can reduce the production of defects and improve the success rate of preparation and the quality of template.
【学位授予单位】：内蒙古科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ133.1;TQ150
本文编号：2320025
[Abstract]:Porous anodic alumina template (Porous Anodic Aluminum Oxide Template) has the advantages of simple preparation process, easy availability and low price of raw materials, highly ordered pore array and adjustable pore size in a certain range. In this paper, the preparation method of anodic alumina template with micropore size and pore spacing was studied. The process of influencing the aperture, pore spacing and pore regularity of anodic alumina template was studied by a large number of experiments. The electrochemical polishing process and anodic oxidation process) and process parameters (oxygen voltage, current density, electrolyte type and concentration, electrolyte temperature, etc.) were investigated. A highly ordered anodic alumina template with a pore size of 20-90 nm and an oxide film thickness of 200nm-10 渭 m was successfully prepared. The effects of pretreatment process, parameters adjustment in oxidation process and post-treatment process on the surface of aluminum sheet were systematically studied. By adjusting different experimental parameters, the optimal combination of parameters is obtained, and the best preparation process is obtained. The effects of different voltages on pore diameter, pore spacing and regularity were studied under the conditions of different kinds and different concentrations of oxidized electrolytes (sulfuric acid and oxalic acid), and the change of current density during oxidation was analyzed. The change of temperature and its influence on oxidation time. The real-time data of the voltage and current generated in the oxidation process are graphed for study. The surface morphology was controlled by controlling the first anodizing time of anodic alumina template, removing the first anodizing film time and the second anodizing time. The anodic alumina template was characterized by scanning electron microscope (SEM) and atomic force microscope (AFM). The experimental results show that: (1) the high temperature annealing can effectively remove the stress between grain boundaries in the aluminum sheet, and make the grain size bigger, which is conducive to the formation and growth of the pore nucleus. Electrochemical polishing can effectively remove the oxide layer and the defects above nanometer level on the aluminum sheet surface, and play a micro-leveling role on the aluminum sheet surface, so that the super-flat surface can be obtained. Pre-treatment processes such as high temperature annealing and electrochemical polishing can improve the regularity and area of the template hole. (2) the pore size is mainly related to the oxidation voltage and the type of oxidation electrolyte: pore size and oxidation voltage. In an approximate linear relationship, The larger the oxidation voltage, the larger the pore size. The optimum oxidation voltage for different kinds of electrolytes is different, and the relationship is sulfuric acid < oxalic acid < phosphoric acid. The pore size of the template prepared under different kinds of oxidizing electrolytes is as follows: sulfuric acid < oxalic acid < phosphoric acid. (3) the first oxidation has a strong guiding effect on the second oxidation. The regularity of the template hole can be improved by prolonging the time of primary oxidation. The conditions of secondary oxidation should be exactly the same as that of primary oxidation. The duration of secondary oxidation is related to the thickness of oxide film. (4) the template is particularly sensitive to temperature during oxidation. Keeping the temperature stable in the oxidation process can reduce the production of defects and improve the success rate of preparation and the quality of template.
【学位授予单位】：内蒙古科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ133.1;TQ150
【参考文献】
相关期刊论文 前2条
1 徐源;G.E.Thompson;G.C.Wood;;多孔型铝阳极氧化膜孔洞形成过程的研究[J];中国腐蚀与防护学报;1989年01期
2 朱绪飞;宋晔;肖迎红;朱晴;高魁;陆路德;;纳米多孔铝阳极氧化膜的形成机理研究[J];真空科学与技术学报;2007年02期
本文编号：2320025
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