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Fabrication and characterization of novel anodic alumina membranes.

机译:新型阳极氧化铝膜的制备与表征。

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The objective of this work was to develop a novel approach to fabricate model membranes of well-defined and well-characterized morphology. The focus of the project was an electrochemical process involving anodic oxidation of high purity aluminum sheets to form porous aluminum oxide films.; Alumina films were prepared by anodizing high purity (99.0% and 99.999%) aluminum sheets using sulfuric acid and phosphoric acid solutions. Current density, temperature, and electrolyte concentration were selected depending on the nature of each electrolyte. From scanning electron micrographs of film cross-sections, the rate of growth of alumina films was observed to be higher when sulfuric acid was used as the anodizing electrolyte than when phosphoric acid was used.; The growth kinetics of porous anodic alumina films formed in phosphoric acid under galvanostatic conditions were studied. Scanning electron microscopy, Faraday's law and oxide film mass measurements were used to analyze the growth kinetics and to obtain film growth rates, pore density, and porosity.; Relationships between anodization conditions and morphological parameters were developed. The effect of current density and solution temperature on the oxide film growth rate and morphology was examined. The rate of growth of the alumina film was found to increase with an increase in current density and decrease with an increase in temperature. The pore density was found to decrease with an increase in current density and with a decrease in temperature. The porosity and the average cross-sectional pore area of the films were found to increase with anodization time and decrease with an increase of current density and temperature. By assuming a conical pore geometry, other morphological parameters such as the average pore size and the surface area of pores can be determined.; Porous films were formed under controlled conditions of concentration and temperature. Single layer films with straight non-intersecting pores of uniform pore size and multi-layer films of different pore size and pore density in each layer were prepared by changing electrolyte type or current density during anodization. These films were separated as membranes from the oxide barrier layer and the unoxidized aluminum using a voltage reduction scheme that did not affect the integrity of the porous structure. Membranes with pre-determined morphology were fabricated.; Diffusion measurements and water flow measurements were used to characterize the fabricated membranes. These techniques were used to compare the measured diffusive and hydraulic permeabilities of the membrane to that predicted using the morphological parameters which were obtained using the quantitative relationships developed from the analysis of the electrochemical process. Close agreement between experimental and predicted permeabilities was observed.
机译:这项工作的目的是开发一种新颖的方法来制造具有明确定义和良好表征的形态的模型膜。该项目的重点是电化学工艺,该工艺涉及高纯度铝板的阳极氧化以形成多孔氧化铝膜。通过使用硫酸和磷酸溶液对高纯度(99.0%和99.999%)铝板进行阳极氧化来制备氧化铝膜。根据每种电解质的性质选择电流密度,温度和电解质浓度。从膜截面的扫描电子显微镜照片观察到,当使用硫酸作为阳极氧化电解质时,氧化铝膜的生长速率高于使用磷酸时。研究了在恒电流条件下在磷酸中形成的多孔阳极氧化铝薄膜的生长动力学。扫描电子显微镜,法拉第定律和氧化膜质量测量用于分析生长动力学并获得膜生长速率,孔密度和孔隙率。建立了阳极氧化条件与形态参数之间的关系。研究了电流密度和溶液温度对氧化膜生长速率和形态的影响。发现氧化铝膜的生长速率随着电流密度的增加而增加,而随着温度的增加而减少。发现孔密度随着电流密度的增加和温度的降低而降低。发现膜的孔隙率和平均横截面孔面积随阳极氧化时间而增加,并随电流密度和温度的增加而减小。通过假定锥形孔的几何形状,可以确定其他形态参数,例如平均孔径和孔的表面积。在受控的浓度和温度条件下形成多孔膜。通过改变阳极氧化过程中的电解质类型或电流密度,制备出具有均匀孔径的直的不相交的孔的单层膜和每层中具有不同孔径和孔密度的多层膜。使用不影响多孔结构完整性的降压方案,将这些膜作为膜与氧化物阻挡层和未氧化的铝分离。制备具有预定形态的膜。扩散测量和水流量测量用于表征所制造的膜。这些技术用于将膜的测得的扩散和水力渗透率与使用形态学参数预测的值进行比较,形态学参数是使用从电化学过程的分析得出的定量关系获得的。观察到实验渗透率和预测渗透率之间的紧密一致性。

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