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Design of a flexible but robust setup for temperature-dependent electrochemistry down to cryogenic temperatures

Title data

Fink, Michael ; Schönfeld, Sophie ; Schreck, Constantin ; Hörner, Gerald ; Weber, Birgit:
Design of a flexible but robust setup for temperature-dependent electrochemistry down to cryogenic temperatures.
In: Electroanalysis. (23 June 2023) . - e202300154.
ISSN 1521-4109

Abstract in another language

Electrochemistry and its analytics are essential in a variety of scientific and technological fields where properties related to reduction-oxidation reactions, so-called redox properties, are to be explored. While methodological standards for experiments are well established at room temperature, this is still untrue at sub-zero/cryogenic temperatures, the conditions required for the survey of (ultra−)rapid processes and their intermediates. Problems due to “hand-waving” temperature regulation/conditioning and common usage of pseudo-reference electrodes renders cryo-electrochemistry a great challenge. Herein, we describe a robust setup for performing reliable cryo-electrochemical experiments down to −80 °C. It combines highly stable but flexible temperature conditioning with gas-tight sealing of the electrochemical cell setup. Modification of a commercial palladium hydride reference electrode (PdH RE) allows for rapid temperature cycling under cryogenic conditions in aprotic organic solvents. Validation of the setup with the well-known Ferrocene|Ferrocenium (Fc|Fc+) redox couple gave good compliance with literature data at room temperature in a range of organic solvent-based electrolytes. Evaluation of temperature-dependent diffusion kinetic parameters, such as diffusion coefficients (D) and diffusional activation energies (Ea,D) from CVs at multiple potential scan-rates and temperature levels emphasize the reliability of the presented cryo-electrochemical setup.

Further data

Item Type: Article in a journal
Refereed: Yes
Institutions of the University: Faculties > Faculty of Biology, Chemistry and Earth Sciences > Department of Chemistry > Chair Inorganic Chemistry IV > Chair Inorganic Chemistry IV - Univ.-Prof. Dr. Birgit Weber
Result of work at the UBT: Yes
DDC Subjects: 500 Science > 540 Chemistry
Date Deposited: 21 Jul 2023 06:17
Last Modified: 21 Jul 2023 06:17