Design, fabrication and characterization of well-aligned porous nanofibers with large electroactive surface areas were performed. Highly ordered nickel-iron alloy nanofiber arrays were fabricated within porous anodic aluminum oxide (AAO) templates via electrodeposition. In order to further increase the electroactive surface area, dealloying was performed to extract the less noble metallic element, iron, from the nickel alloy to form porous structures. Electrocatalytic properties of the nanoarchitectured porous Ni nanofiber arrays were characterized by cyclic voltammetry (CV). Comparative studies on the electrochemical activities of the nanoarchitectured porous Ni fiber electrode in pure methanol and methanol sulfuric mixture solution were performed. The potential for methanol oxidation is about 0.4 V. It is found that sulfuric acid facilitates the oxidation of methanol. Preliminary studies on the electrocatalytic behavior of the nanoporous nickel in several other solutions containing sugar, orange juice, soy beam juice, tomato sauce were also performed. The stress state of the nanofiber in the AAO templates was derived as well.

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