Coupled Inductive Annealing‐Electrochemical Setup for Controlled Preparation and Characterization of Alloy Crystal Surface Electrodes

Abstract The present versatile multifunctional electrochemical crystal preparation‐test station features capabilities for controlled thermal annealing of any type of (binary) metallic or oxidic catalyst or support crystal surfaces, in particular single crystals. The setup enables rapid inductive heating of the electrodes to temperatures up to 1900 °C under precise infrared temperature control in controlled gas atmospheres. The constant overpressure inside the cell prevents the ambient atmosphere to permeate and contaminate the process. Finely adjusted sensors afford accurate and instant information on the electrodes' surface temperature. The subsequent cooling process in argon atmosphere proceeds without any treatment in water. After annealing, the crystals inside the chamber can immediately be subjected to any type of electrochemical deposition, modification, or characterization in two distinct three‐electrode chambers, again without any exposure to air. Both chambers feature pump‐controlled supply and withdrawal of liquid electrolyte. A special characteristic is the inert‐gas flow inversion capability to transfer electrodes into separate portable inert‐gas chambers. Design details are presented and their functionality during thermal preparation and electrochemical voltammetry of Ir(111) catalysts for the oxygen evolution reaction are demonstrated. The station provides a crystal handling environment superior to the classic flame annealing approaches, yet to constitute a cost‐effective alternative to vacuum chambers.