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Diamond membrane production : the critical role of radicals in the non-contact electrochemical etching of sp2 carbon

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Tully, Joshua J., Braxton, Emily, Cobb, Samuel J., Breeze, Ben, Markham, Matthew, Newton, Mark E., Rodriguez, Paramaconi and Macpherson, Julie V. (2021) Diamond membrane production : the critical role of radicals in the non-contact electrochemical etching of sp2 carbon. Carbon, 185 . pp. 717-726. doi:10.1016/j.carbon.2021.09.054 ISSN 0008-6223.

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Official URL: http://dx.doi.org/10.1016/j.carbon.2021.09.054

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Abstract

Sub-micrometre single crystal diamond membranes are of huge importance for next generation optical, quantum and electronic device applications. Electrochemical etching has proven a critical step in the production of such membranes. Etching is used to selectively remove a very thin layer of sub-surface sp2 carbon, prepared by ion implantation in bulk diamond, releasing the diamond membrane. Due to the nanosized dimensions, etching is typically carried out using non-contact electrochemistry in low conductivity solutions (bipolar arrangement) which whilst effective, results in extremely slow etch rates. In this work, a new method of non-contact electrochemical etching is presented which uses high conductivity, high concentration, fully dissociated aqueous electrolytes. Careful choice of the electrolyte anion results in significant improvements in the sp2 carbon etch rate. In particular, we show both chloride and sulfate electrolytes increase etch rates significantly (up to × 40 for sulfate) compared to our measurements using the current state-of-the-art solutions and methodologies. Electron paramagnetic resonance experiments, recorded after the electrode potential has been switched off, reveal sizeable hydroxyl radical concentrations at timescales > 107 longer than their lifetime (≤μs). These measurements highlight the importance of electrochemically initiated, solution chemistry radical generation and regeneration pathways in high concentration sulfate and chloride solutions for nano-etching applications.

Item Type: Journal Article
Subjects: T Technology > TP Chemical technology
Divisions: Faculty of Science, Engineering and Medicine > Science > Chemistry
Faculty of Science, Engineering and Medicine > Science > Physics
Library of Congress Subject Headings (LCSH): Diamonds, Artificial -- Research, Diamonds -- Electric properties, Semiconductors -- Etching, Electrochemical analysis, Carbon, Diamond thin films
Journal or Publication Title: Carbon
Publisher: Elsevier Ltd
ISSN: 0008-6223
Official Date: 15 November 2021
Dates:
DateEvent
15 November 2021Published
29 September 2021Available
22 September 2021Accepted
Volume: 185
Page Range: pp. 717-726
DOI: 10.1016/j.carbon.2021.09.054
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Restricted or Subscription Access
Date of first compliant deposit: 4 November 2021
Date of first compliant Open Access: 29 September 2022
RIOXX Funder/Project Grant:
Project/Grant IDRIOXX Funder NameFunder ID
EP/M013243/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
EP/L015307/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
INF/PHD/180016[RS] Royal Societyhttp://dx.doi.org/10.13039/501100000288
EP/L015315/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266

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