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Title: A Versatile Electrochemical Cell for Operando XAS

Journal Article · · ChemCatChem

In situ and operando X–ray absorption spectroscopy (XAS) provides fundamental insight into the working principles of electrocatalysts and is an important tool for future catalyst development. However, the design of an operando XAS electrocatalytic cell is not facile, and researchers designing cells, whether new cells or modifications to previous cells, often spend many hours on cell design before obtaining high–quality XAS data. Here, we describe the design, with engineering drawings, and operation of a versatile XAS cell with options for gas flow, electrolyte flow, pH monitoring, temperature monitoring, and the ability to handle many catalyst forms (any catalyst that can be deposited onto a conductive X–ray transparent substrate). We benchmarked XAS spectra collected using the new experimental cell to a previous cell design showing its ability to produce quality XAS data. We demonstrate the viability of this cell by providing insight into electrocatalysts by studying cation effects and show the tetrabutylammonium cation prevents bulk oxidation of copper. Finally, we hope the availability of this cell allows researchers to convert time typically spent on cell design to time spent on breakthroughs in electrocatalysis.

Research Organization:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Office of Workforce Development for Teachers & Scientists (WDTS); USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB)
Grant/Contract Number:
AC02-76SF00515
OSTI ID:
2407199
Journal Information:
ChemCatChem, Journal Name: ChemCatChem Journal Issue: 15 Vol. 16; ISSN 1867-3880
Publisher:
ChemPubSoc EuropeCopyright Statement
Country of Publication:
United States
Language:
English

References (25)

Operando X-ray absorption spectroscopy: A powerful tool toward water splitting catalyst development journal October 2017
Recent advances in platinum monolayer electrocatalysts for oxygen reduction reaction: Scale-up synthesis, structure and activity of Pt shells on Pd cores journal March 2010
In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy journal November 2017
Carbon-supported Pt during aqueous phenol hydrogenation with and without applied electrical potential: X-ray absorption and theoretical studies of structure and adsorbates journal December 2018
In Situ / Operando Electrocatalyst Characterization by X-ray Absorption Spectroscopy journal September 2020
Well-Defined Nanoparticle Electrocatalysts for the Refinement of Theory journal October 2019
Identifying the Local Atomic Environment of the “Cu3+” State in Alkaline Electrochemical Systems journal May 2023
Cation Incorporation into Copper Oxide Lattice at Highly Oxidizing Potentials journal September 2023
Fe Coordination Environment, Fe-Incorporated Ni(OH)2 Phase, and Metallic Core Are Key Structural Components to Active and Stable Nanoparticle Catalysts for the Oxygen Evolution Reaction journal January 2022
An Operando Investigation of (Ni–Fe–Co–Ce)O x System as Highly Efficient Electrocatalyst for Oxygen Evolution Reaction journal January 2017
Revealing the Active Phase of Copper during the Electroreduction of CO 2 in Aqueous Electrolyte by Correlating In Situ X-ray Spectroscopy and In Situ Electron Microscopy journal May 2020
Chemical Structure of Fe–Ni Nanoparticles for Efficient Oxygen Evolution Reaction Electrocatalysis journal October 2019
The Role of the Copper Oxidation State in the Electrocatalytic Reduction of CO 2 into Valuable Hydrocarbons journal November 2018
In Situ Electrochemical X-ray Absorption Spectroscopy of Oxygen Reduction Electrocatalysis with High Oxygen Flux journal December 2011
Operando Insight into the Correlation between the Structure and Composition of CuZn Nanoparticles and Their Selectivity for the Electrochemical CO 2 Reduction journal November 2019
Highly selective plasma-activated copper catalysts for carbon dioxide reduction to ethylene journal June 2016
Simultaneous detection of electronic structure changes from two elements of a bifunctional catalyst using wavelength-dispersive X-ray emission spectroscopy and in situ electrochemistry journal January 2015
Effects of temperature and gas–liquid mass transfer on the operation of small electrochemical cells for the quantitative evaluation of CO 2 reduction electrocatalysts journal January 2016
Controlling the 3-D morphology of Ni–Fe-based nanocatalysts for the oxygen evolution reaction journal January 2019
The chemical identity, state and structure of catalytically active centers during the electrochemical CO 2 reduction on porous Fe–nitrogen–carbon (Fe–N–C) materials journal January 2018
Linking the evolution of catalytic properties and structural changes in copper–zinc nanocatalysts using operando EXAFS and neural-networks journal January 2020
How cations affect the electric double layer and the rates and selectivity of electrocatalytic processes journal October 2019
ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT journal June 2005
Combining theory and experiment in electrocatalysis: Insights into materials design journal January 2017
Electrochemical Flow-Cell Setup for In Situ X-ray Investigations: I. Cell for SAXS and XAS at Synchrotron Facilities journal January 2016