Benchtop Fabricated Nano‐Roughened Microstructured Electrodes for Electrochemical and Surface‐Enhanced Raman Scattering Sensing

Abstract Tailoring a material's surface with hierarchical structures from the micro‐ to the nanoscale is key for fabricating highly sensitive detection platforms. To achieve this, the fabrication method should be simple, inexpensive, and yield materials with a high density of surface features. Here, using benchtop fabrication techniques, gold surfaces with hierarchically structured roughness are generated for sensing applications. Hierarchical gold electrodes are prepared on pre‐stressed polystyrene substrates via electroless deposition and amperometric pulsing. Electrodes fabricated using 1 m m HAuCl₄ and roughened with 80 pulses revealed the highest electroactive surface area. These electrodes are used for enzyme‐free detection of glucose in the presence of bovine serum albumin and achieved a limit of detection of 0.36 m m , below glucose concentrations in human blood. The surfaces nanoroughened with 100 pulses also showed excellent surface‐enhanced Raman scattering (SERS) response for the detection of rhodamine 6G, with an enhancement factor of ≈2 × 10 6 compared to detection in solution, and for the detection of a self‐assembled monolayer of thiophenol, with an enhancement factor of ≈30 compared to the response from microstructured gold surfaces. It is envisioned that the simplicity and low fabrication cost of these gold‐roughened structures will expedite the development of electrochemical and SERS sensing devices.