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

Abstract

A novel electrochemical setup has been developed for soft x-ray absorption studies of the electronic structure of electrode materials during electrochemical cycling. In this communication we illustrate the operation of the cell with a study of the corrosion behavior of copper in aqueous NaHCO 3 solution via the electrochemically induced changes of its electronic structure. This development opens the 2 way for in situ investigations of electrochemical processes, photovoltaics, batteries, fuel cells, water splitting, corrosion, electrodeposition, and a variety of important biological processes.

RIXS investigations of liquids, solutions, and liquid/solid interfaces

“…The problems associated with the static cell setup can be overcome by using a flow-through design [20][21][22][23][24], like the one shown in Fig. 1(b) [21].…”

“…These investigations are made possible by the development of sophisticated experimental setups that overcome the conflict between the high vapor pressure of the studied liquids and the ultra-high vacuum (UHV) requirements of the experimental station. Two experimental concepts are commonly used: first, a liquid jet [14][15][16] or droplet train [17] injected into the vacuum system and then collected by a nitrogen-cooled target, in conjunction with intensive differential pumping, or, second, the separation of the liquid under study and the UHV environment by a thin membrane [2,6,[18][19][20][21][22][23][24]. While the first setup also allows the use of electron spectroscopies, the studied liquid is not in thermodynamic equilibrium and gaseous contributions to the spectra have to be taken into account.…”

Electrokinetic detection for X-ray spectra of weakly interacting liquids: n-decane and n-nonane

“…This vapor background issue can potentially be addressed through the use of liquid flow cells, which have recently been used in XAS studies of a wide variety of systems. [24][25][26] These flow cells separate the liquid from the high vacuum environment through the use of silicon nitride windows. However, in the soft X-ray region, the windows attenuate the incoming X-ray beam, resulting in a significant reduction in signal, and they severely limit the study of nitrogen-containing compounds.…”

An ultra-high vacuum electrochemical flow cell for in situ/operando soft X-ray spectroscopy study

“…1 With reference to this, a flow liquid cell has been demonstrated previously by Jiang et al 22 to study the electrochemical corrosion of copper surface in a sodium bicarbonate solution. The experiment validated the operando monitoring of changes of copper oxidation state under electrochemical cycling.…”