Jump to main content
Jump to site search
SCHEDULED MAINTENANCE Close the message box

Maintenance work is planned for Monday 16 August 2021 from 07:00 to 23:59 (BST).

Website performance may be temporarily affected and you may not be able to access some PDFs or images. If this does happen, refreshing your web browser should resolve the issue. We apologise for any inconvenience this might cause and thank you for your patience.


Issue 17, 2020

Copper and silver gas diffusion electrodes performing CO2 reduction studied through operando X-ray absorption spectroscopy

Author affiliations

Abstract

X-ray absorption spectroscopy (XAS) offers the unique possibility to study metal electrocatalysts such as silver and copper while they are performing electrochemical carbon dioxide (CO2) reduction. In this work, we present an approach to perform operando XAS experiments on an electrochemical cell performing CO2 reduction with a gas diffusion electrode (GDE) as cathode. The experimental set-up, advantages and drawbacks, XAS data analysis, and XAS theory are discussed. Results on copper and silver GDEs obtained through the presented procedures are then presented and discussed. Structural and compositional catalyst data acquired under operando conditions can help further density functional theory calculations, and catalytic, and systems studies on CO2 reduction. Structural and compositional data including crystallite size were obtained while performing high current density (up to 200 mA cm−2) CO2 reduction. On the silver catalysts at higher than 100 mA cm−2 applied current density, a Ag–X contribution was found and is ascribed to Ag–O. For both silver and copper, the XAS experiments revealed that the crystallite size of the ex situ samples is smaller than the samples during CO2 reduction. Furthermore, metal particle size polydispersity was found in the silver catalysts by comparing the obtained coordination numbers with theoretical values. The operando EXAFS data was of such high quality (k: 3–14 Å−1) that four shells could be fitted. The value of combining ex situ material characterisation and electrocatalyst performance data with operando XAS experiments is discussed and found to be of great importance to further CO2 reduction research.

Graphical abstract: Copper and silver gas diffusion electrodes performing CO2 reduction studied through operando X-ray absorption spectroscopy

Supplementary files

Article information


Submitted
24 Jun 2020
Accepted
28 Jul 2020
First published
29 Jul 2020

Catal. Sci. Technol., 2020,10, 5870-5885
Article type
Paper

Copper and silver gas diffusion electrodes performing CO2 reduction studied through operando X-ray absorption spectroscopy

N. J. Firet, T. Burdyny, N. T. Nesbitt, S. Chandrashekar, A. Longo and W. A. Smith, Catal. Sci. Technol., 2020, 10, 5870 DOI: 10.1039/D0CY01267J

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.


Social activity

Search articles by author

Spotlight

Advertisements