Membrane filters with uniformly sized pores have attracted considerable attention because they are useful for filtering a variety of particulates. Among them, anodic porous alumina, obtained by the anodization of Al in an electrolyte, has been studied as a membrane filter for microfiltration because it can form a nanohole array structure with regularly arranged pores of uniform size. We previously reported that a two-layer anodization method using concentrated sulfuric acid can form highly ordered alumina through-hole membranes with high throughput [1]. Using this method, it was possible to form not only flat membrane filters but also tubular membrane filters [2]. Tubular alumina membrane filters have potential applications in filter modules for space savings and efficient microfiltration. To achieve efficient filtration in filter modules consisting of tubular membrane filters, it is necessary to increase the density of the filter packed in the module, which requires the fabrication of tubular filters with small diameters. However, it is difficult to form tubular alumina membrane filters thinner than 1 cm in diameter using a previously reported method. In this report, we describe the results of a new method based on a two-layer anodization process using concentrated sulfuric acid to form tubular membrane filters with millimeter diameters. Electropolished Al wire was anodized in 0.3 M oxalic acid at 40 V to form anodic porous alumina. The sample was then re-anodized in 12M sulfuric acid at 40V to form a highly soluble alumina layer at the bottom of the previously formed anodic porous alumina. After anodization, the sample was immersed in a mixed solution of chromic acid and phosphoric acid to selectively dissolve the alumina layer formed in concentrated sulfuric acid, thereby exposing the Al substrate at the bottom of the pores. Tubular alumina membrane filters were obtained by selectively dissolving the Al substrate through nanopores in an iodine-methanol solution. In this study, Al wires with diameters ranging from 2 to 5 mm were used as the starting materials, and in all cases, it was possible to form tubular alumina membrane filters without cracks. SEM observations of the obtained samples showed that the tubular alumina membrane filter was uniformly sized through the holes. The tubular alumina membrane filter obtained in this study is expected to be useful in a variety of applications.
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