High pressure high temperature synthesis of highly boron doped diamond microparticles and porous electrodes for electrochemical applications

Wood, Georgia; Zvoriste-Walters, Carmen E.; Munday, Mark; Newton, Mark E.; Shkirskiy, Viacheslav; Unwin, Patrick R.; Macpherson, Julie V.

doi:10.1016/j.carbon.2020.09.038

Cited by 35 publications

(31 citation statements)

References 56 publications

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“…47,48 While interrogation of the single-crystal surface is extremely useful for fundamental studies, the vast majority of researchers employ polycrystalline BDD, both in the thick film, i.e., freestanding and polished, and in the thin film (still attached to growth wafer) and as-grown state. 1 Nearly all SECM and SECCM studies have been carried out on the freestanding polished surface, 1,[21][22][23][26][27][28][29][30]39 with limited SECM success on the as-grown material, 24 due to the lack of topographical control. Prior to this data, no SECCM measurements had been made on the as-grown BDD.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Electrochemical imaging techniques are important tools for the high-resolution imaging of electrochemical surfaces. Scanning electrochemical microscopy (SECM) − and scanning electrochemical cell microscopy (SECCM) − have been used to characterize the crystal facet-dependent electrochemical reactivity of CVD-grown O-terminated polycrystalline BDD electrodes. Here the material was grown thick (hundreds of μm) and then mechanically polished, resulting in a dominant (110) textured surface, , such that the resulting crystal faces were large enough with an ∼ nm surface roughness, for electrochemical interrogation and correlation with complementary imaging techniques such as Raman microscopy, conducting atomic force microscopy (c-AFM), and scanning electron microscopy (SEM) .…”

mentioning

confidence: 99%

“…Here the material was grown thick (hundreds of μm) and then mechanically polished, resulting in a dominant (110) textured surface, , such that the resulting crystal faces were large enough with an ∼ nm surface roughness, for electrochemical interrogation and correlation with complementary imaging techniques such as Raman microscopy, conducting atomic force microscopy (c-AFM), and scanning electron microscopy (SEM) . SECCM has also been used to map the electrochemical activity and porosity of compacted HPHT BDD particulate electrodes and selectively electrochemically pattern H-terminated polycrystalline surfaces with O-termination …”

mentioning

confidence: 99%

“…Here the material was grown thick (hundreds of μm) and then mechanically polished, resulting in a dominant (110) textured surface, 27,32 such that the resulting crystal faces were large enough with an ∼ nm surface roughness, for electrochemical interrogation and correlation with complementary imaging techniques such as Raman microscopy, conducting atomic force microscopy (c-AFM), and scanning electron microscopy (SEM). 23 SECCM has also been used to map the electrochemical activity and porosity of compacted HPHT BDD particulate electrodes 26 and selectively electrochemically pattern H-terminated polycrystalline surfaces with O-termination. 31 For fast electron-transfer redox couples ("outer sphere"), [Ru(NH 3 ) 6 ] 3+/2+ and FcTMA + , the studies revealed a correlation between boron dopant density (density of states) and electron-transfer rate constant, with the latter values determined to be at least 2 orders of magnitude lower than those at metal electrodes.…”

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confidence: 99%

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Nanoscale Reactivity Mapping of a Single-Crystal Boron-Doped Diamond Particle

et al. 2021

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Boron-doped diamond (BDD) is most often grown by chemical vapor deposition (CVD) in polycrystalline form, where the electrochemical response is averaged over the whole surface. Deconvoluting the impact of crystal orientation, surface termination, and boron-doped concentration on the electrochemical response is extremely challenging. To tackle this problem, we use CVD to grow isolated single-crystal microparticles of BDD with the crystal facets (100, square-shaped) and (111, triangle-shaped) exposed and combine with hopping mode scanning electrochemical cell microscopy (HM-SECCM) for electrochemical interrogation of the individual crystal faces (planar and nonplanar). Measurements are made on both hydrogen- (H-) and oxygen (O-)-terminated single-crystal facets with two different redox mediators, [Ru(NH3)6]3+/2+ and Fe(CN)6 4–/3–. Extraction of the half-wave potential from linear sweep and cyclic voltammetric experiments at all measurement (pixel) points shows unequivocally that electron transfer is faster at the H-terminated (111) surface than at the H-terminated (100) face, attributed to boron dopant differences. The most dramatic differences were seen for [Ru(NH3)6]3+/2+ when comparing the O-terminated (100) surface to the H-terminated (100) face. Removal of the H-surface conductivity layer and a potential-dependent density of states were thought to be responsible for the behavior observed. Finally, a bimodal distribution in the electrochemical activity on the as-grown H-terminated polycrystalline BDD electrode is attributed to the dominance of differently doped (100) and (111) facets in the material.

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Section: ■ Results and Discussionmentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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confidence: 99%

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Nanoscale Reactivity Mapping of a Single-Crystal Boron-Doped Diamond Particle

et al. 2021

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“…Beyond this, future studies will also likely become more application‐driven, expanding the capability of SECCM towards new electrolytes (e.g., ionic liquids, [ 64 ] non‐aqueous solvents, [ 65 ] gel electrolytes, [ 66 ] etc.) and more complex electrode materials [e.g., conductive polymer blends, [ 18 ] composite electrodes, [ 67 ] (nano)porous materials, [ 68 ] etc.]. In any case, SECCM has firmly cemented itself as a premier tool for microscopic structure−function studies, which will no doubt play an important role in the guided discovery, design, and engineering of novel electrode materials, moving forward.…”

Section: Discussionmentioning

confidence: 99%

Scanning electrochemical cell microscopy for the study of (nano)particle electrochemistry: From the sub‐particle to ensemble level

Bentley

2021

Electrochemical Science Adv

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Scanning electrochemical cell microscopy (SECCM) is a scanning‐droplet‐based technique that allows electrochemical fluxes and/or interfacial reactivity to be measured and visualized with high spatiotemporal resolution. This minireview spotlights the use of SECCM for studying the electrochemistry of (nano)particles, highlighting recent works spanning multiple timescales (i.e., microseconds to seconds) and lengthscales (i.e., nanometers to micrometers) to probe physicochemical phenomena at the sub‐particle, single particle, and/or (micro)ensemble levels. In SECCM, single (nano)particles (or small particle ensembles) are electrochemically interrogated—directly from colloidal solution (i.e., by investigating electrochemical nanoimpacts with a substrate electrode) or supported on an electrochemically inert support electrode—with a pipette probe that is operated in either a stationary (point measurement) or dynamic scanning/imaging mode. Nanoscale‐resolved electrochemical information (e.g., local rates of electron‐ or ion‐transfer, catalytic activity, corrosion resistance, etc.) from SECCM is readily related to (nano)particle structure and properties, collected at a commensurate scale with complementary, co‐located microscopy/spectroscopy techniques, allowing structure and function to be resolved directly and unambiguously down to the sub‐particle level. Understanding structure−function on this scale enables macroscopic “particle‐on‐support” electrode behavior to be rationalized and further predicted, guiding the discovery, design, and engineering of novel electromaterials with enhanced function, which is a “holy grail” in materials science.

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Electrocatalysis for Green(er) Chemistry: Limitations and Opportunities with Traditional and Emerging Characterization Methods for Tangible Societal Impact

Sherrell,

Iesalnieks,

Ehrnst

et al. 2024

Adv Energy and Sustain Res

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The world is facing grand challenges in energy security, environmental pollution, and sustainable use (and re‐use) of resources. Electrochemical processes, incorporating electrosynthesis, electrochemical catalysis, and electrochemical energy storage devices, provide pathways to address these challenges via green chemistry. However, the applicability of electrochemical processes for these systems is limited by the required energy input, the “electrons” in electrochemistry. Electrocatalysis as a subset of electrochemistry is set to underpin many of the United Nations Sustainable Development Goals, including “Affordable and Clean Energy” through the production of future fuels and abatement of carbon emissions; “Responsible Consumption and Production” through recycling and degradation of waste; and “Climate Action” through CO2 (and other greenhouse gas) remediation. The rise of green photovoltaic power has lowered the carbon cost of these electrons, making electrocatalysis an even more viable, green(er), chemical conversion pathway. This perspective highlights the need for comprehensive understanding of catalyst structure via in situ and operando analysis to complement device design considerations. The challenges faced by the field of electrocatalysis in data reporting, elimination of electrochemical artifacts, catalyst stability, and scaling to industrial relevance, along with opportunities, emerging tools, are discussed with a view to achieve the maximum ‘potential’ of electrocatalysis.

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High pressure high temperature synthesis of highly boron doped diamond microparticles and porous electrodes for electrochemical applications

Abstract: High pressure high temperature (HPHT) synthesis of crystallographically well-defined boron doped diamond (BDD) microparticles, suitable for electrochemical applications and using the lowest P and T (5.5 GPa and

Cited by 35 publications

References 56 publications

Nanoscale Reactivity Mapping of a Single-Crystal Boron-Doped Diamond Particle

Nanoscale Reactivity Mapping of a Single-Crystal Boron-Doped Diamond Particle

Scanning electrochemical cell microscopy for the study of (nano)particle electrochemistry: From the sub‐particle to ensemble level

Electrocatalysis for Green(er) Chemistry: Limitations and Opportunities with Traditional and Emerging Characterization Methods for Tangible Societal Impact

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