Publication date: 15th December 2025
Alloying and doping are important tools to improve the activity and stability of oxygen reduction reaction (ORR) electrocatalysts. To understand the role that the doping/alloying elements play during the catalysis, revealing their interfacial electrochemical behavior is critical. Here, I will show my group’s recent efforts to obtain such insight using electrochemical X-ray photoelectron spectroscopy (EC-XPS). In EC-XPS, an electrochemical cell capped by a graphene window is used inside the vacuum of the spectroscopy chamber, facilitating in situ XPS measurements that can resolve the concentration and chemical state of the dopants at the catalyst surface. We have used this to study the potential-dependent structure of Pt3Ni, Pt9Au and N-doped graphene ORR catalysts. Our results universally show that the catalyst structure is highly dynamic. For the Pt3Ni and Pt9Au alloys, we find that the elemental distribution within the catalyst nanoparticles reversibly changes with the applied potential (see figure) [1], and that this leads to potential-dependent catalytic properties. For nitrogen-doped graphene oxygen reduction catalysts, we find a similar dynamic response in the structure around the N dopants. These examples highlight the importance of understanding the operando restructuring for multi-element catalyst design, and show how the element and depth-sensitivity of electrochemical XPS can be used to obtain such insight.
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