Controllable Electrochemical Synthesis of Ag Hierarchical Micro/Nanostructures with High SERS-Activity

We report a one-step electrochemical deposition technique to prepare three-dimensional (3D) Ag hierarchical micro/nanostructured film consisting of well-crystallized Ag nanosheets grown on an indium tin oxide (ITO) conductive substrate. The Ag hierarchical micro/nanostructures were fabricated in the mixed solution of AgNO 3 and sodium citrate in a constant current system at room temperature. Through reduction of Ag[Formula: see text] electrodeposited on the surface of ITO substrate, nanoparticles were grown to form nanosheets which further combined into 3D sphere-like microstructures. The 3D Ag micro/nanostructures have many sharp edges and nanoscale gaps which can give rise to good Raman-enhanced effect. Due to localized surface plasmon resonance (LSPR) effects, these special Ag micro/nanostructures exhibited good Raman-enhanced performance. Using Rhodamine 6G (R6G) molecules as probe molecule, we studied the influence of excitation wavelength on Raman enhancement. The results showed that the 532[Formula: see text]nm excitation wavelength is the best to obtain the strongest Raman signal and to reduce the influence of other impurity peaks. Using the as-synthesized Ag hierarchical micro/nanostructures, we can detect the 10[Formula: see text][Formula: see text]mol/L R6G aqueous solution, exhibiting great Raman-enhanced effect.