Generally, a controllable and reproduced surface roughness for surface-enhanced Raman scattering (SERS) studies can be generated through control of the electrochemical oxidation-reduction cycles (ORC) procedure. In this work, we propose a new sonoelectrochemical approach to prepare SERS-active substrates with two domain-Ag nanostructures. The method is based on a strategy of deposition-dissolution cycles (DDCs) by using a cathodic overpotential and an anodic overpotential from open circuit potential (OCP) in turn under sonication. The prepared SERS-active substrate demonstrates large Raman scattering enhancement for adsorbed Rhodamine 6G (R6G) with an enhancement factor of 2.3×10 8 and a limit of detection of 2×10 -13M. The improved SERS performances can be successfully explained from the viewpoints of electromagnetic (EM) and chemical (CHEM) enhancements.
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