Nanoporous Au Formation on Au Substrates via High Voltage Electrolysis

• Published in: Chemphyschem 2023-03, Vol.24 (5), p.e202200645-n/a
• Main Authors: Artmann, Evelyn, Forschner, Lukas, Schüttler, Konstantin M., Al‐Shakran, Mohammad, Jacob, Timo, Engstfeld, Albert K.
• Format: Article
• Language: English
• Subjects: Contact Glow Discharge Electrolysis; Electrodes; Electrolysis; Glow discharges; Gold; Gold oxide; High voltages; Hydrogen peroxide; Nanoporous Gold; Oxide coatings; Pore size; Substrates; Surface area; X ray photoelectron spectroscopy
• ISSN: 1439-4235; 1439-7641
• DOI: 10.1002/cphc.202200645

Nanoporous Au (NPG) films have promising properties, making them suitable for various applications in (electro)catalysis or (bio)sensing. Tuning the structural properties, such as the pore size or the surface‐to‐volume ratio, often requires complex starting materials such as alloys, multiple synthesis steps, lengthy preparation procedures or a combination of these factors. Here we present an approach that circumvents these difficulties, enabling for a rapid and controlled preparation of NPG films starting from a bare Au electrode. In a first approach a Au oxide film is prepared by high voltage (HV) electrolysis in a KOH solution, which is then reduced either electrochemically or in the presence of H2O2. The resulting NPG structures and their electrochemically active surface areas strongly depend on the reduction procedure, the concentration and temperature of the H2O2‐containing KOH solution, as well as the applied voltage and temperature during HV electrolysis. Secondly, the NPG film can be prepared directly by applying voltages that result in anodic contact glow discharge electrolysis (aCGDE). By carefully adjusting the corresponding parameters, the surface area of the final NPG film can be specifically controlled. The structural properties of the electrodes are investigated by means of XPS, SEM and electrochemical methods. High voltage electrolysis (100–540 V) in alkaline electrolyte can produce Au oxide films, which can be reduced to nanoporous Au in various ways. By varying the parameters of voltage, temperature, time and the amount of H2O2 to reduce the Au oxide, the subsequent nanoporous structure of the Au electrode can be tailored. The choice of the individual high voltage electrolysis and reduction parameters has a sensitive influence on the final surface structure of the Au electrode.