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Title: A temperature-controlled photoelectrochemical cell for quantitative product analysis

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.5024802· OSTI ID:1530357

In this study, we describe the design and operation of a temperature-controlled photoelectrochemical cell for analysis of gaseous and liquid products formed at an illuminated working electrode. This cell is specifically designed to quantitatively analyze photoelectrochemical processes that yield multiple gas and liquid products at low current densities and exhibit limiting reactant concentrations that prevent these processes from being studied in traditional single chamber electrolytic cells. The geometry of the cell presented in this paper enables front-illumination of the photoelectrode and maximizes the electrode surface area to electrolyte volume ratio to increase liquid product concentration and hence enhances ex situ spectroscopic sensitivity toward them. Gas is bubbled through the electrolyte in the working electrode chamber during operation to maintain a saturated reactant concentration and to continuously mix the electrolyte. Gaseous products are detected by an in-line gas chromatograph, and liquid products are analyzed ex situ by nuclear magnetic resonance. Cell performance was validated by examining carbon dioxide reduction on a silver foil electrode, showing comparable results both to those reported in the literature and identical experiments performed in a standard parallel-electrode electrochemical cell. Furthermore, to demonstrate a photoelectrochemical application of the cell, CO2 reduction experiments were carried out on a plasmonic nanostructured silver photocathode and showed different product distributions under dark and illuminated conditions.

Research Organization:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-05CH11231; SC0004993
OSTI ID:
1530357
Alternate ID(s):
OSTI ID: 1437678
Journal Information:
Review of Scientific Instruments, Vol. 89, Issue 5; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 10 works
Citation information provided by
Web of Science

References (20)

Effect of Temperature on Electrochemical Reduction of High-Pressure CO 2 with In, Sn, and Pb Electrodes journal September 1995
Plasmonic Properties of Copper Nanoparticles Fabricated by Nanosphere Lithography journal July 2007
Effect of the surface roughness on the spectral distribution of photoemission current at the silver/solution contact journal May 1995
Electrochemical Reduction of High Pressure CO[sub 2] on Ni Electrodes journal January 1993
Photocatalytic Conversion of CO 2 to Hydrocarbon Fuels via Plasmon-Enhanced Absorption and Metallic Interband Transitions journal July 2011
Theoretical predictions for hot-carrier generation from surface plasmon decay journal December 2014
Plasmon-Enhanced Photocatalytic CO 2 Conversion within Metal–Organic Frameworks under Visible Light journal December 2016
PRODUCTION OF CO AND CH 4 IN ELECTROCHEMICAL REDUCTION OF CO 2 AT METAL ELECTRODES IN AQUEOUS HYDROGENCARBONATE SOLUTION journal November 1985
Hot-Electron-Induced Dissociation of H 2 on Gold Nanoparticles Supported on SiO 2 journal December 2013
Product selectivity in plasmonic photocatalysis for carbon dioxide hydrogenation journal February 2017
Nano-photocatalytic Materials: Possibilities and Challenges journal October 2011
Photocatalytic Reduction of CO2 into Methanol over Ag/TiO2 Nanocomposites Enhanced by Surface Plasmon Resonance journal July 2013
Production of Methane and Ethylene in Electrochemical Reduction of Carbon Dioxide at Copper Electrode in Aqueous Hydrogencarbonate Solution journal June 1986
Photogeneration of hot plasmonic electrons with metal nanocrystals: Quantum description and potential applications journal February 2014
New insights into the electrochemical reduction of carbon dioxide on metallic copper surfaces journal January 2012
Mechanism of the electrochemical reduction of carbon dioxide at inert electrodes in media of low proton availability journal January 1996
Electrochemical Reduction of Carbon Dioxide on Various Metal Electrodes in Low-Temperature Aqueous KHCO3 Media journal January 1990
Electrochemical reduction of CO2 on Au in KOH + methanol at low temperature journal January 1998
Electrochemical reduction of CO2 at an Ag electrode in KOH-methanol at low temperature journal September 1998
Plasmonic-metal nanostructures for efficient conversion of solar to chemical energy journal November 2011

Figures / Tables (6)