A Free-Standing Boron-Doped Diamond Grid Electrode for Fundamental Spectroelectrochemistry

Patenaude, Hannah K.; Damjanovic, Nastasija; Rakos, Jason; Weber, Dustyn C.; Jacobs, Aaron I.; Bryan, Samuel A.; Lines, Amanda M.; Heineman, William R.; Branch, Shirmir D.; Rusinek, Cory A.

doi:10.1021/acs.analchem.4c00906

Title: A Free-Standing Boron-Doped Diamond Grid Electrode for Fundamental Spectroelectrochemistry

Journal Article · Wed Nov 13 00:00:00 UTC 2024 · Analytical Chemistry

DOI: https://doi.org/10.1021/acs.analchem.4c00906 · OSTI ID:2552921

^[1]; Damjanovic, Nastasija ^[2]; Rakos, Jason ^[3]; Weber, Dustyn C. ^[4];

^[5];

^[6]; Lines, Amanda M. ^[6]; Heineman, William R. ^[7]; Branch, Shirmir D. ^[6];

^[4]

University of Nevada, Las Vegas, NV (United States); Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)
University of Nevada, Las Vegas, NV (United States)
University of Nevada, Las Vegas, NV (United States); Miami University, Oxford, OH (United States); Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
University of Nevada, Las Vegas, NV (United States); Miami University, Oxford, OH (United States)
Michigan State University, East Lansing, MI (United States)
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
University of Cincinnati, OH (United States)

Spectroelectrochemistry (SEC) is a powerful technique that enables a variety of redox properties to be studied, including formal potential (E^o), thermodynamic values (ΔG, ΔH, ΔS), diffusion coefficient (D), electron transfer stoichiometry (n), and others. SEC requires an electrode which light can pass through while maintaining sufficient electrical conductivity. This has been traditionally composed of metal or metal oxide films atop transparent substrates like glass, quartz, or metallic mesh. Robust electrode materials like boron-doped diamond (BDD) could help expand the environments in which SEC can be performed, but most designs are limited to thin films (~100–200 nm) on transparent substrates less resilient than free-standing BDD. Here, this work presents a free-standing BDD grid electrode (G-BDD) for fundamental SEC measurements, using the well-characterized Fe(CN)₆^3–/4– redox couple as proof-of-concept. With a combination of cyclic voltammetry (CV), thin-layer SEC, and chronoabsorptometry, several of the redox properties mentioned above were calculated and compared. For E^o', n, and D, similar results were obtained when comparing the CV [E^o' = +0.279 (±0.002) V vs Ag/AgCl; n = 0.97; D = 4.1 × 10^–6 cm²·s^–1] and SEC [E^o' = +0.278 (±0.001) V vs Ag/AgCl; n = 0.91; D = 5.2 × 10^–6 cm²·s^–1] techniques. Both values align with what has been previously reported. To calculate D from the SEC data, modification of the classical equation used in chronoabsorptometry was required to accommodate the G-BDD electrode geometry. Overall, this work expands on the applicability of SEC techniques and BDD as a versatile electrode material.

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Research Organization:: Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE Office of Nuclear Energy (NE), Nuclear Energy University Program (NEUP)

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 2552921

Report Number(s):: PNNL-SA--194619

Journal Information:: Analytical Chemistry, Journal Name: Analytical Chemistry Journal Issue: 47 Vol. 96; ISSN 0003-2700

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
boron-doped diamond electrode
spectroelectrocemistry

Title: A Free-Standing Boron-Doped Diamond Grid Electrode for Fundamental Spectroelectrochemistry

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