In situ soft X-ray dynamic microscopy of electrochemical processes

In situ soft X-ray absorption spectroscopy investigation of electrochemical corrosion of copper in aqueous NaHCO3 solution

“…The large absorption cross-section of most gases and liquids in this energy range requires the use of UHV instrumentation. However by using ultrathin membranes to separate the samples from the UHV environment, soft x-rays can be used for studies under real conditions, such as high-pressure gas and liquid environments [14][15][16][17][18][19][20][21].…”

“…However, due to the lack of potential control, these studies were limited to "static" electrochemical conditions [19]. In situ electrochemical reactions have also been studied by scanning transmission x-ray microscopy, where liquid cells without the capability of flowing the electrolyte solution were used [20,21]. These setups suffered from the formation of gas bubbles during electrochemical reactions and the difficult exchange of electrolytes [17,20].…”

Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

“…In particular, as a simple demostrative test case, with no claim of specific materials-science interest, we studied Au corrosion in an RTIL electrolyte and we recorded images of mesoscopic features of Au corrosion product organisation. configuration described in [4][5][6][7], since the sealing method is not impacted by the new electrode system. The potential applications are stability of materials for fuel-cells and sensors.…”

“…Of course, the stringent sample requirements of techniques based on transmission of soft X-rays impose severe constraints to in situ operation. As far as electrochemical cells are concerned, two types of concepts have been described so far in the literature: the pioneering two electrode system with polymeric electrolyte proposed in the seminal paper [3] and the Si 3 N 4 -supported, cells with lithographed square electrodes employed by the authors in [4][5][6][7][8][9]. The latter system has allowed in situ dynamic work both with sealed, aqueous electrolytes [4][5][6][7] and with open, room-temperature ionic-liquids (RTIL) [8,9]; nevertheless, the poor current density (c.d.)…”

Spatiotemporal Mapping of Diffusion Layers Using Synchrotron Infrared Radiation

“…The recognition that spatiotemporal mapping of active catalysts provides new information on heterogeneous surfaces has sparked increasing interest in using spectroscopy techniques to follow reaction kinetics with spatial resolution exceeding the length scale of the active catalyst [15]. For example, synchrotron sourced soft x-ray imaging and spectromicroscopy techniques have been used to follow temporal changes during metal deposition [16,17], reactions within electrodeposited polymers [18,19] and mass-transport phenomena in fuel-cells [20,21]. Recently, vibrational imaging of heterogeneous catalysts such as zeolites [22,23] and even microreactors under operating conditions [24] have been reported demonstrating that synchrotron infrared radiation is a powerful tool for mapping the spatiotemporal dependence of chemical reactions.…”