Abstract
Synchrotron-based scanning photoelectron microscopy (SPEM) has opened unique opportunities for exploiting processes occurring at surfaces and interfaces, which control the properties of materials for electrochemical devices, where issues of chemical and morphological complexity at microscopic length scales should be faced and understood. The present article aims to demonstrate the present capabilities of SPEM to explore the surface composition of micro- and nano-structured materials, focusing on cases relevant to electrochemical technologies. We report and discuss a selection of recent results about three different systems, targeting hot topics in the fields of electrochemical energy storage and electrochemical fabrication: (i) an in-depth analysis of Ag-In electrodeposited alloys exhibiting dynamic pattern formation, (ii) the analysis of electrochemical processes at the electrodes of a self-driven solid oxide fuel cell and (iii) an operando characterization of a single-chamber solid oxide fuel cell. The last example has been performed at near-ambient pressure conditions using a unique specially designed setup which extends the traditional capabilities of scanning photoemission microscopes in the ultra-high and high-vacuum regimes to operating conditions that are closer to realistic ones, contributing to overcome the so-called “pressure gap”.
Highlights
The ubiquitous and enabling role of electrochemical technologies in many different fields of technology [1], but especially in energy storage [2], cannot be overemphasized
A characteristic aspect of electrodeposited alloy patterns is that these structures can be imaged very precisely by visible-light microscopy, but exhibit a strikingly poor contrast in SEM, owing to their extreme surface-confinement
As proved in ref. [26,36], scanning photoelectron microscopy (SPEM), owing to its high chemical-state sensitivity combined with surface sensitivity and lateral resolution, is the method of choice for unravelling the morphochemical details of electrodeposited alloy patterns
Summary
The ubiquitous and enabling role of electrochemical technologies in many different fields of technology [1], but especially in energy storage [2], cannot be overemphasized. APXPS) to the characterization of electrochemical systems, largely diffused [14,15,16], it is worthwhile to mention a couple of developments adaptable to electrochemistry: (i) the implementation of hard X-rays XPS, which allows spectroscopy investigation of deeper layers [17] such as buried interfaces and (ii) the “dip and tip” method to study solid-liquid interfaces [18,19], available at few synchrotron beamlines In spite of their innovation all these approaches fail in combining APXPS with submicron spatial resolution; this technological problem started to be solved as recently as in the last decade thanks to the efforts of the team of the Escamicroscopy beamline at Elettra which allowed the development and implementation of innovative technical solutions for SPEM, capable of performing near-ambient pressure photoemission spectromicroscopy while keeping the typical SPEM performance [20,21]. Fuel cell (SC-SOFC) at near-ambient pressure conditions, using a newly developed cell
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