Lead (Pb) nanowire arrays were fabricated with anodic aluminum oxide (AAO) templates of 30, 100 and 300 nm in pore diameters. Through vacuum injection molding process, Pb/AAO composite was obtained, and lead sulfide (PbS) could further be synthesized after exposing to sulfur gas. AAO templates with different pore sizes were fabricated by using pure aluminum in a two-step anodization. Three types of solutions, which are 10 vol% sulfuric acid, 3 wt% oxalic acid and 1 vol% phosphoric acid, were adopted to achieve AAO of various pore sizes. Different sulfurization temperatures and time spans were applied for studying on the formation mechanism of PbS. Finally, the morphology, composition, structure and elements distribution of the as-prepared Pb and PbS nanowires were confirmed through the use of scanning electron microscopy, energy dispersive x-ray spectroscopy, element-mapping, x-ray diffraction and transmission electron microscopy analysis. The results indicated that Pb nanowires were successfully obtained after applying vacuum injection molding process with 50 kgf cm−2 hydraulic pressure, and PbS nano arrays can be formed by sulfurization at 500 °C for 5 h. Furthermore, an optical property, ultraviolet–visible (UV–Vis) absorption, was also measured. The measurement of the PbS nanowires showed that a significant quantum confinement effect made the energy gap produce a blue shift from 0.41 eV to 1.65 eV or 1.72 eV.
In this study, we have developed a swift and well-ordered growth of the Anodic Aluminum Oxide (AAO) nanoporous structure by two-step high temperature anodization of pure Aluminum substrate. The pre-anodization surface treatment of the aluminum substrate assists in the formation of well-organized nanoporous structures. The two-step anodization process was performed in 0.3 M of oxalic acid at 20 °C for 40 V and 45 V to obtain tunable pore diameters. The high temperature of the electrolyte solution helps in the rapid growth of the AAO nanoporous structure. The top surface image of AAO shows a well-ordered nanoporous structure with an average pore diameter of 70 nm at 40 V and 100 nm at 45 V. The SEM cross sectional view also illustrates the well-ordered nano channel and the elemental mapping elaborates the presence of aluminum and oxygen. The thickness of the AAO nanoporous structure was determined by using SEM for three anodization time spans (20, 24 and 28 hours), in which an increasing trend was observed. The fabricated AAO has a higher thickness and a well-ordered nanoporous structure that shows it can be used as a template for fabricating nanostructured materials.
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