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We report for the first time fabrication of self-aligned hexagonally closed-packed titania nanotube arrays of over 1000 μm in length and aspect ratio ≈10 000 by potentiostatic anodization of titanium. We describe a process by which such thick nanotube array films can be transformed into self-standing, flat or cylindrical, mechanically robust, polycrystalline TiO2 membranes of precisely controlled nanoscale porosity. The self-standing membranes are characterized using Brunauer−Emmett−Teller surface area measurements, glancing angle X-ray diffraction, and transmission electron microscopy. In initial application, such membranes are used to control the diffusion of phenol red.