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Title: Electrochemical Roughening of Thin-Film Platinum for Neural Probe Arrays and Biosensing Applications

In this work, we report a method for electrochemical roughening of thin-film platinum (Pt) electrodes that increases active surface area, decreases electrode impedance, increases charge injection capacity, increases sensitivity of biosensors and improves adhesion of electrochemically deposited films. First, a well-established technique for electrochemical roughening of thick Pt electrodes (wires and foils) by oxidation-reduction pulses was modified for use on thin-film Pt. Optimal roughening of thin-film Pt electrodes with this established protocol in a sulfuric acid solution was found to occur at about four times lower frequency than that typically used for thick Pt. This modification in established procedure created a 21x surface area increase but showed nanoscale cracks from inter-grain Pt dissolution that compromised film integrity. A crack free surface with Pt nanocrystal re-deposition (20–30 nm in size) and higher enhancement in surface area (44x) was obtained when the electrolyte was switched to a non-adsorbing perchloric acid solution. These electrochemically roughened electrodes have charge injection limits comparable to titanium nitride and just below carbon nanotube-based materials. Roughened microelectrodes showed a 2.8x increase in sensitivity to hydrogen peroxide detection, indicative of improved enzymatic biosensor performance. Platinum iridium and iridium oxide coatings on these roughened surfaces showed an improvement in adhesion.
Authors:
 [1] ; ORCiD logo [1] ; ORCiD logo [1] ;  [2] ;  [3] ;  [1] ;  [1] ;  [1] ;  [1]
  1. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Engineering Directorate
  2. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Physical and Life Science Directorate
  3. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Engineering Directorate; Neuralink Corp., San Francisco, CA (United States)
Publication Date:
Report Number(s):
LLNL-JRNL-746398
Journal ID: ISSN 0013-4651; 900205
Grant/Contract Number:
AC52-07NA27344; 16-ERD-035
Type:
Published Article
Journal Name:
Journal of the Electrochemical Society
Additional Journal Information:
Journal Volume: 165; Journal Issue: 12; Journal ID: ISSN 0013-4651
Publisher:
The Electrochemical Society
Research Org:
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sponsoring Org:
USDOE National Nuclear Security Administration (NNSA); USDOE Laboratory Directed Research and Development (LDRD) Program
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; 42 ENGINEERING; 77 NANOSCIENCE AND NANOTECHNOLOGY; 59 BASIC BIOLOGICAL SCIENCES; Electrochemical roughening; microelectrode; neuromodulation
OSTI Identifier:
1464289
Alternate Identifier(s):
OSTI ID: 1467810

Ivanovskaya, Anna N., Belle, Anna M., Yorita, Allison M., Qian, Fang, Chen, Supin, Tooker, Angela, Lozada, Rose García, Dahlquist, Dylan, and Tolosa, Vanessa. Electrochemical Roughening of Thin-Film Platinum for Neural Probe Arrays and Biosensing Applications. United States: N. p., Web. doi:10.1149/2.0171812jes.
Ivanovskaya, Anna N., Belle, Anna M., Yorita, Allison M., Qian, Fang, Chen, Supin, Tooker, Angela, Lozada, Rose García, Dahlquist, Dylan, & Tolosa, Vanessa. Electrochemical Roughening of Thin-Film Platinum for Neural Probe Arrays and Biosensing Applications. United States. doi:10.1149/2.0171812jes.
Ivanovskaya, Anna N., Belle, Anna M., Yorita, Allison M., Qian, Fang, Chen, Supin, Tooker, Angela, Lozada, Rose García, Dahlquist, Dylan, and Tolosa, Vanessa. 2018. "Electrochemical Roughening of Thin-Film Platinum for Neural Probe Arrays and Biosensing Applications". United States. doi:10.1149/2.0171812jes.
@article{osti_1464289,
title = {Electrochemical Roughening of Thin-Film Platinum for Neural Probe Arrays and Biosensing Applications},
author = {Ivanovskaya, Anna N. and Belle, Anna M. and Yorita, Allison M. and Qian, Fang and Chen, Supin and Tooker, Angela and Lozada, Rose García and Dahlquist, Dylan and Tolosa, Vanessa},
abstractNote = {In this work, we report a method for electrochemical roughening of thin-film platinum (Pt) electrodes that increases active surface area, decreases electrode impedance, increases charge injection capacity, increases sensitivity of biosensors and improves adhesion of electrochemically deposited films. First, a well-established technique for electrochemical roughening of thick Pt electrodes (wires and foils) by oxidation-reduction pulses was modified for use on thin-film Pt. Optimal roughening of thin-film Pt electrodes with this established protocol in a sulfuric acid solution was found to occur at about four times lower frequency than that typically used for thick Pt. This modification in established procedure created a 21x surface area increase but showed nanoscale cracks from inter-grain Pt dissolution that compromised film integrity. A crack free surface with Pt nanocrystal re-deposition (20–30 nm in size) and higher enhancement in surface area (44x) was obtained when the electrolyte was switched to a non-adsorbing perchloric acid solution. These electrochemically roughened electrodes have charge injection limits comparable to titanium nitride and just below carbon nanotube-based materials. Roughened microelectrodes showed a 2.8x increase in sensitivity to hydrogen peroxide detection, indicative of improved enzymatic biosensor performance. Platinum iridium and iridium oxide coatings on these roughened surfaces showed an improvement in adhesion.},
doi = {10.1149/2.0171812jes},
journal = {Journal of the Electrochemical Society},
number = 12,
volume = 165,
place = {United States},
year = {2018},
month = {8}
}

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