pH Micro-Sensor from IrO_x SECM Microelectrode for Local pH Measurement While Chromium Electrodeposition

摘要

In this work, it will be presented the chromium electrodeposition mechanisms with the use of a Scanning ElectroChemical Microscopy (SECM) micro-electrode. Among several factors, the pH is key to achieve even a metallic deposit. pH buffers and complexing agents are often used for this purpose but in the vicinity of the electrode, at the electrode/electrolyte interface, strong variations are highly likely to occur. To this respect, since pH is a key parameter, a pH micro-electrode is intended to be developed to scan the pH gradient upon the electrodeposition of chromium. The first part of this work is so devoted to the pH micro-electrode realization from microelectrode on which iridium oxide is deposited. Iridium oxide has been reported to be suitable for local pH sensing. Different parameters have been studied such as IrO_x thickness and thermal treatment. The addition of Nafion has been assessed as well to achieve a tradeoff between fast response time, good selectivity and good stability. An optimized IrO_x micro-electrode has been obtained and used as SECM micro-electrode to get the evolution of the pH at the electrode/electrolyte interface upon electrodeposition. Different micro-electrode diameters have been used to improve the resolution. These results are promising and will allow going further to the development of chromium electrodeposition electrolyte helping to select the different complexing agents.