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

Abstract

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, CO 2 reduction experiments were carried out onmore » a plasmonic nanostructured silver photocathode and showed different product distributions under dark and illuminated conditions.« less

Authors:
ORCiD logo [1]; ORCiD logo [1];  [2]; ORCiD logo [2];  [2];  [1]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Univ. of California, Berkeley, CA (United States)
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1530357
Alternate Identifier(s):
OSTI ID: 1437678
Grant/Contract Number:  
AC02-05CH11231; SC0004993
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 89; Journal Issue: 5; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 47 OTHER INSTRUMENTATION

Citation Formats

Corson, Elizabeth R., Creel, Erin B., Kim, Youngsang, Urban, Jeffrey J., Kostecki, Robert, and McCloskey, Bryan D. A temperature-controlled photoelectrochemical cell for quantitative product analysis. United States: N. p., 2018. Web. doi:10.1063/1.5024802.
Corson, Elizabeth R., Creel, Erin B., Kim, Youngsang, Urban, Jeffrey J., Kostecki, Robert, & McCloskey, Bryan D. A temperature-controlled photoelectrochemical cell for quantitative product analysis. United States. doi:10.1063/1.5024802.
Corson, Elizabeth R., Creel, Erin B., Kim, Youngsang, Urban, Jeffrey J., Kostecki, Robert, and McCloskey, Bryan D. Fri . "A temperature-controlled photoelectrochemical cell for quantitative product analysis". United States. doi:10.1063/1.5024802. https://www.osti.gov/servlets/purl/1530357.
@article{osti_1530357,
title = {A temperature-controlled photoelectrochemical cell for quantitative product analysis},
author = {Corson, Elizabeth R. and Creel, Erin B. and Kim, Youngsang and Urban, Jeffrey J. and Kostecki, Robert and McCloskey, Bryan D.},
abstractNote = {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.},
doi = {10.1063/1.5024802},
journal = {Review of Scientific Instruments},
number = 5,
volume = 89,
place = {United States},
year = {2018},
month = {5}
}

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Figures / Tables:

Fig. 1 Fig. 1: Schematic of the photoelectrochemical (PEC) cell. The copper and aluminum heat sink (not shown) is secured against the aluminum back plate (1) that transfers heat from the Peltier element (2). The working photoelectrode (3) is in close proximity to the reference electrode (4) and thermistor (8) and ismore » separated from the counter electrode (10) by a membrane (7). Gas enters through the glass frit at the bottom (5) and flows through tubing at the top (6) to the GC for product analysis. A hole in the front plate (11) allows light to shine through the quartz window (9) onto the photoelectrode (3). The total volume of the electrolyte used in the working electrode chamber is 2.3 ml, and the electrode surface areas are 1 cm2 (1.1 cm diameter).« less

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