This paper presents a clean electrodeposition strategy to fabricate a gold hierarchically micro/nanostructured pore array based on a polystyrene sphere colloidal monolayer. The electrodeposition is carried out in an additive-free HAuCl4 electrolyte to assure a gold structure without surface adsorption of surfactants. By controlling the electrodeposition time, the nano-building blocks in the array can be controlled from quasi spherical nanoparticles to quasi rod-shaped nanostructures. Importantly, the gold quasi rod-shaped nanoparticle-built hierarchically micro/nanostructured pore array shows structurally enhanced surface-enhanced Raman scattering (SERS) performance: high activity, nice uniformity and good stability. Such an array as a SERS active substrate may find important applications in analytical chemistry, electrochemistry, sensors, and so on.
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