Nanoporous anodic aluminium oxide has been widely used for the development of various functional nanostructures. So far these self-organized pore structures could only be prepared within narrow processing conditions. Here we report a new oxalic-acid-based anodization process for long-range ordered alumina membranes. This process is a new generation of the so-called "hard anodization" approach that has been widely used in industry for high-speed fabrication of mechanically robust, very thick (>100 microm) and low-porosity alumina films since the 1960s. This hard anodization approach establishes a new self-ordering regime with interpore distances, (D(int))=200-300 nm, which have not been achieved by mild anodization processes so far. It offers substantial advantages over conventional anodization processes in terms of processing time, allowing 2,500-3,500% faster oxide growth with improved ordering of the nanopores. Perfectly ordered alumina membranes with high aspect ratios (>1,000) of uniform nanopores with periodically modulated diameters have been realized.

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Nanoporous anodic aluminium oxide has traditionally been made in one of two ways: mild anodization or hard anodization. The first method produces self-ordered pore structures, but it is slow and only works for a narrow range of processing conditions; the second method, which is widely used in the aluminium industry, is faster, but it produces films with disordered pore structures. Here we report a novel approach termed "pulse anodization" that combines the advantages of the mild and hard anodization processes. By designing the pulse sequences it is possible to control both the composition and pore structure of the anodic aluminium oxide films while maintaining high throughput. We use pulse anodization to delaminate a single as-prepared anodic film into a stack of well-defined nanoporous alumina membrane sheets, and also to fabricate novel three-dimensional nanostructures.

Large-area high density silicon nanowire (SiNW) arrays were fabricated by metal-assisted chemical etching of silicon, utilizing anodic aluminum oxide (AAO) as a patterning mask of a thin metallic film on a Si (100) substrate. Both the diameter of the pores in the AAO mask and the thickness of the metal film affected the diameter of SiNWs. The diameter of the SiNWs decreased with an increase of thickness of the metal film. Large-area SiNWs with average diameters of 20 nm down to 8 nm and wire densities as high as 10 (10) wires/cm (2) were accomplished. These SiNWs were single crystalline and vertically aligned to the (100) substrate. It was revealed by transmission electron microscopy that the SiNWs were of high crystalline quality and showed a smooth surface.