In situ electrochemical regeneration of nanogap hotspots for continuously reusable ultrathin SERS sensors

Sarah May Sibug-Torres, David-Benjamin Grys, Gyeongwon Kang, Marika Niihori, Elle Wyatt, Nicolas Spiesshofer, Ashleigh Ruane, Bart Nijs and Jeremy J. Baumberg ()
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Sarah May Sibug-Torres: University of Cambridge
David-Benjamin Grys: University of Cambridge
Gyeongwon Kang: University of Cambridge
Marika Niihori: University of Cambridge
Elle Wyatt: University of Cambridge
Nicolas Spiesshofer: University of Cambridge
Ashleigh Ruane: University of Cambridge
Bart Nijs: University of Cambridge
Jeremy J. Baumberg: University of Cambridge

Nature Communications, 2024, vol. 15, issue 1, 1-13

Abstract: Abstract Surface-enhanced Raman spectroscopy (SERS) harnesses the confinement of light into metallic nanoscale hotspots to achieve highly sensitive label-free molecular detection that can be applied for a broad range of sensing applications. However, challenges related to irreversible analyte binding, substrate reproducibility, fouling, and degradation hinder its widespread adoption. Here we show how in-situ electrochemical regeneration can rapidly and precisely reform the nanogap hotspots to enable the continuous reuse of gold nanoparticle monolayers for SERS. Applying an oxidising potential of +1.5 V (vs Ag/AgCl) for 10 s strips a broad range of adsorbates from the nanogaps and forms a metastable oxide layer of few-monolayer thickness. Subsequent application of a reducing potential of −0.80 V for 5 s in the presence of a nanogap-stabilising molecular scaffold, cucurbit[5]uril, reproducibly regenerates the optimal plasmonic properties with SERS enhancement factors ≈106. The regeneration of the nanogap hotspots allows these SERS substrates to be reused over multiple cycles, demonstrating ≈5% relative standard deviation over at least 30 cycles of analyte detection and regeneration. Such continuous and reliable SERS-based flow analysis accesses diverse applications from environmental monitoring to medical diagnostics.

Date: 2024
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DOI: 10.1038/s41467-024-46097-y

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