In situ soft x-ray fluorescence and absorption microspectroscopy: A study of Mn-Co/polypyrrole electrodeposition

This paper reports the development and application of a novel thin-layer electrochemical microcell for in situ soft x-ray fluorescence and absorption microspectroscopy. The microcell, fabricated using ultraviolet lithography, is an improved version of concepts previously developed in our group, featuring a wide optical window that allows the extension of the range of accessible in situ microspectroscopy and imaging methods, including those requiring small emission take-off angles. The three-electrode design implemented in the cell enables optimal electrochemical control. The first in situ experiment employing this new cell explores the electrochemical growth of a novel Mn-Co/polypyrrole composite that is a prospective electrocatalyst for Pt replacement in air cathodes. Morphological, compositional, and chemical-state distributions of Mn and Co codeposited with polypyrrole are subsequently performed in situ as a function of time and position, yielding otherwise unachievable information regarding the electrodeposition process.