Depto. de Física Aplicada I, Facultad de Ciencias, Universidad de Málaga, E-29071 Málaga, Spain.
J Colloid Interface Sci. 2012 Jun 15;376(1):40-6. doi: 10.1016/j.jcis.2012.02.066. Epub 2012 Mar 7.
Highly ordered Nanoporous Alumina Membranes (NPAMs) with a precise control of the pore size and different porosity but thickness around 63 μm were fabricated by the two-step anodization process using different acidic aqueous solutions, oxalic (Al-Ox), sulfuric (Al-Sf), and phosphoric (Al-Ph) acids, respectively. The pore size was controlled by properly changing the anodization voltage and the electrochemical bath conditions, obtaining the following average pores diameter values, d(p), as determined by scanning electron micrographic analysis: Al-Ox (d(p)=46±2 nm), Al-Sf (d(p)=27±2 nm), and Al-Ph (d(p)=240±20 nm). A pore increasing of around 5% for samples Al-Ox and Al-Sf was obtained after membranes immersion in 5 wt.% phosphoric acid for a certain etching time. Electrochemical characterization of NPAMs was performed with the samples in contact with NaCl solutions at different electrolyte concentrations. Ionic transport numbers and effective membrane fixed charge were determined from membrane potential measurements, which clearly show the significant influence of the pore diameter on ions transport. Moreover, frictional and electrical effects on mass transfer parameters (salt and ions diffusion coefficients) into the pores of alumina membranes were also evaluated from these results.
采用两步阳极氧化工艺,分别使用草酸(Al-Ox)、硫酸(Al-Sf)和磷酸(Al-Ph)酸性水溶液,制备出具有精确孔径控制和不同孔隙率但厚度约为 63μm 的高度有序纳米多孔氧化铝膜(NPAMs)。通过适当改变阳极氧化电压和电化学浴条件来控制孔径,得到以下通过扫描电子显微镜分析确定的平均孔径值 d(p):Al-Ox(d(p)=46±2nm)、Al-Sf(d(p)=27±2nm)和 Al-Ph(d(p)=240±20nm)。将样品 Al-Ox 和 Al-Sf 浸入 5wt.%磷酸中一定时间进行蚀刻后,孔径增加了约 5%。通过将 NPAMs 样品与不同电解质浓度的 NaCl 溶液接触来进行 NPAMs 的电化学特性测试。通过膜电位测量确定离子迁移数和有效膜固定电荷,这清楚地表明孔径对离子传输有显著影响。此外,还从这些结果评估了摩擦和电效应对氧化铝膜孔中传质参数(盐和离子扩散系数)的影响。