Reactivity of radiolytically and photochemically generated tertiary amine radicals towards a CO2 reduction catalyst

Carr, Cody R.; Vrionides, Michael A.; Grills, David C.

doi:10.1063/5.0180065

Title: Reactivity of radiolytically and photochemically generated tertiary amine radicals towards a CO₂ reduction catalyst

Journal Article · 26 December 2023 · Journal of Chemical Physics

DOI: https://doi.org/10.1063/5.0180065 · OSTI ID:2222380

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^[1]

Brookhaven National Laboratory (BNL), Upton, NY (United States)

Homogeneous solar fuels photocatalytic systems often require several additives in solution with the catalyst to operate, such as a photosensitizer (PS), Brønsted acid/base, and a sacrificial electron donor (SED). Tertiary amines, in particular triethylamine (TEA) and triethanolamine (TEOA), are ubiquitously deployed in photocatalysis applications as SEDs and are capable of reductively quenching the PS’s excited state. Upon oxidation, TEA and TEOA form TEA^•+ and TEOA^•+ radical cations, respectively, which decay by proton transfer to generate redox non-innocent transient radicals, TEA^• and TEOA^•, respectively, with redox potentials that allow them to participate in an additional electron transfer step, thus resulting in net one-photon/two-electron donation. However, the properties of the TEA^• and TEOA^• radicals are not well understood, including their reducing powers and kinetics of electron transfer to catalysts. Herein, we have used both pulse radiolysis and laser flash photolysis to generate TEA^• and TEOA^• radicals in CH₃CN, and combined with UV/Vis transient absorption and time-resolved mid-infrared spectroscopies, we have probed the kinetics of reduction of the well-established CO₂ reduction photocatalyst, fac-ReCl(bpy)(CO)₃ (bpy = 2,2'-bipyridine), by these radicals [k_TEA• = (4.4 ± 0.3) × 10⁹ M^–1 s^–1 and k_TEOA• = (9.3 ± 0.6) × 10⁷ M^–1 s^–1]. The ~50× smaller rate constant for TEOA^• indicates, that in contrast to a previous assumption, TEA^• is a more potent reductant than TEOA^• (by ~0.2 V, as estimated using the Marcus cross relation). This knowledge will aid in the design of photocatalytic systems involving SEDs. Furthermore, we also show that TEA can be a useful radiolytic solvent radical scavenger for pulse radiolysis experiments in CH₃CN, effectively converting unwanted oxidizing radicals into useful reducing equivalents in the form of TEA^• radicals.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB)

Grant/Contract Number:: SC0012704

OSTI ID:: 2222380

Report Number(s):: BNL--225008-2023-JAAM

Journal Information:: Journal of Chemical Physics, Journal Name: Journal of Chemical Physics Journal Issue: 24 Vol. 159; ISSN 0021-9606

Publisher:: American Institute of Physics (AIP)Copyright Statement

Country of Publication:: United States

Language:: English

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