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

Joshua J. Tully, Emily Braxton, Samuel J. Cobb, Ben G. Breeze, Matthew Markham, Mark E. Newton, Paramaconi Rodriguez, Julie V. Macpherson

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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.
Original languageEnglish
Pages (from-to)717-726
JournalCarbon
Volume185
Early online date29 Sept 2021
DOIs
Publication statusPublished - 15 Nov 2021

Keywords

  • Carbon Etching
  • Diamond Membranes
  • EPR
  • Electrochemical Etching
  • Hydroxyl Radicals
  • Radicals
  • Sulfate Electrolytes

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