Single-phase CuInSe2 nanowire (NW) arrays were prepared at various pH values in a heated electrolyte by using pulse electrodeposition techniques and an anodized aluminum oxide template. X-ray diffraction showed that the CuInSe2 NW nucleation mechanism received H+ constraints when the NWs were deposited at pH 1.7 with a (112) orientation and annealed at 550 °C. The CuInSe2 NW band gap was determined to be approximately 1 eV through optical measurements. Transmission electron microscopy showed that at the pH value of 1.7, small particles of the single-phase CuInSe2 NWs aligned along the crystallographic direction are nucleated to form large particles. Scanning electron microscopy revealed that the NW diameter and the length were 80 nm and 2.3 μm, respectively. From Mott–Schottky and Ohmic contact plots, the CuInSe2 NWs were found to be p-type semiconductors, and their work function was estimated to be approximately 4.69 eV.
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