Electrochemical Surface Oxidation of Copper Studied by in Situ Grazing Incidence X-ray Diffraction

Abstract

Grazing incidence X-ray diffractometry (GIXRD) can deliver integral information on the structure and chemistry of surface near regions, which can be beneficial for functional materials related to interfacial reactions. Here, we present an in situ laboratory GIXRD setup for electrochemical experiments. The method is capable of directly correlating changes of the crystalline surface structure to the electrochemical conditions. It combines cyclovoltametric (CV) and chronoamperometric (CA) curves of crystalline samples, which can be recorded over the entire pH range, with simultaneous GIXRD measurements. The stepwise oxidation of polycrystalline copper in alkaline medium acts as an example to prove the functionality of the setup. In situ GIXRD measurements during CA experiments reveal a stepwise oxidation mechanism of metallic Cu to Cu 2+ involving crystalline cuprite (Cu 2 O) intermediates. The results highlight the importance of conducting in situ experiments under controlled environments in order to track transient states even for a comparable simple oxidation reaction.

Selective CO2 Electroreduction to Ethylene and Multicarbon Alcohols via Electrolyte‐Driven Nanostructuring

“…7 at % of residual CuI. These results also reveal the higher sensitivity of HERFD‐XANES measurements acquired in grazing configuration to Cu 2 O and CuI species as compared to GI‐XRD which only shows metallic Cu peaks after CO 2 RR (Supporting Information, Figure S2) …”

“…These results also reveal the higher sensitivity of HERFD-XANES measurements acquired in grazing configuration to Cu 2 Oa nd CuI species as compared to GI-XRD which only shows metallic Cu peaks after CO 2 RR (Supporting Information, Figure S2). [36,37] Quasi in situ X-ray photoelectron spectroscopy (XPS) measurements were performed to probe the chemical state and composition of the surface of the Cu catalysts during CO 2 RR. Theelectrochemical cell was directly attached to the Figure 3a nd the Supporting Information, Figures S12 and S13.…”

Probing Electronic Properties of CVD Monolayer Hexagonal Boron Nitride by an Atomic Force Microscope

“…Before the oxidation in air, the presence of only one sharp Cu (111) peak at ∼ 43.3°in the XRD pattern (black line in Figure 4A) confirmed the high crystallinity of the Cu foil. After the copper oxidation, a tiny XRD peak located at ∼ 38.7°appeals (blue line in Figure 4A), revealing the formation of CuO (111) on the top of the copper foil (Scherzer et al, 2019;Chen et al, 2020). A zoomin XRD spectrum as displayed in Figure 4B further confirms the presence of the CuO (111).…”

Chemische Batterien mit CO2

“…10 Monolagen abgeschätzt. [103] Die elektrochemische Oxidation von Kupfer führt zu einer Passivschicht, [104] die aus einem Gemisch von CuO und Cu 2 O besteht und ebenfalls sehr dünn ist.…”