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The research has been conducted on various classes of catalysts, with recent work focusing specifically on catalyst surfaces for proton exchange membrane (PEM) fuel cells. We investigate the performance of multilayer, ultra-thin catalyst surfaces fabricated directly on gas diffusion layers (GDL) under ultra-high vacuum (UHV) conditions. The activity and durability of Pt-supported alloy thin-film surfaces—synthesized either as sequential multilayers or via co-sputtering—are prepared using two different magnetron sputtering systems in our laboratory and subsequently characterized through electrochemical measurements and fuel cell testing. Furthermore, an analysis chamber integrated with the one of the magnetron sputtering system enables in-situ and ex-situ surface characterization via X- ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), scanning tunneling microscopy (STM), Auger electron spectroscopy (AES), low-energy electron diffraction (LEED), and quadrupole mass spectrometry (QMS), allowing comparison of catalyst surfaces before and after electrochemical testing.