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Neuronal growth on high-aspect-ratio diamond nanopillar arrays for biosensing applications

MetadataDetails
Publication Date2023-04-11
JournalScientific Reports
AuthorsElena Losero, Somanath Jagannath, Maurizio Pezzoli, Valentin Goblot, Hossein Babashah
InstitutionsÉcole Polytechnique FĂ©dĂ©rale de Lausanne, The University of Sydney
Citations29
AnalysisFull AI Review Included

This research successfully validates a nanostructured single-crystal diamond platform for high-resolution, label-free quantum biosensing of neuronal activity, addressing the challenge of low signal sensitivity in mammalian neurons.

  • Platform Development: Large-scale (up to 2 mm x 2 mm) arrays of high-aspect-ratio (HAR) nanopillars (d: 100-500 nm; h: ~1 ”m; AR > 10:1) were reliably fabricated on single-crystal CVD diamond.
  • Quantum Sensing Enhancement: The nanopillars demonstrated a waveguiding effect, increasing Photoluminescence (PL) collection efficiency by 15% compared to flat surfaces, crucial for boosting the sensitivity of Nitrogen-Vacancy (NV) centers.
  • Biocompatibility Confirmed: Primary mouse hippocampal neurons were successfully grown on the nanostructured arrays, maintaining full viability and functional electrophysiological properties (e.g., typical resting potentials and action potential firing).
  • Optimal Interface Achieved: Scanning Electron Microscopy (SEM) confirmed close physical contact between neurites and the pillar apices, validating the geometry required for near-surface NV centers to detect local electric fields without ionic screening.
  • Neuronal Guidance: The nanopillar grid induced preferential neuronal growth along the array axes, demonstrating a method to tailor network architecture for targeted sensing applications.
  • Functional Milestone: This work establishes a critical milestone toward realizing an NV-based quantum sensing platform capable of wide-field, sub-cellular resolution recording of living neuronal networks.
ParameterValueUnitContext
Substrate MaterialSingle-crystal CVD Diamond (100)-Optical grade, Element6
Substrate Dimensions3 x 3 x 0.25mmChip size
Array Size (Max)2 x 2mm2Uniform coverage area
Nanopillar Diameter (d)100 to 500nmRange tested
Nanopillar Height (h)~1 (up to 2)”mTarget height
Aspect Ratio (h:d)> 10:1-Achieved verticality
Nanopillar Pitch (p)1 to 10”mDistance between pillars
NV Center Concentration1.4ppbUniform density in optical grade diamond
Surface Roughness (RMS)< 2nmAfter non-contact polishing
Diamond Etch Rate (O2 Plasma)100nm/minHighly directional O2-plasma etch
PL Enhancement+15%Compared to flat surface (d=500 nm, p=1 ”m)
Neuronal Resting Potential-63 to -49mVMeasured in functional hippocampal neurons
Action Potential Threshold~30pACurrent injection required to elicit firing
EPSP Time Decay Constant (τ)~25msExcitatory postsynaptic potential fit
EBL Exposure TimeLess than 20minutesFor a 2 mm x 2 mm array

The fabrication of the high-aspect-ratio diamond nanopillar arrays followed a multi-step process utilizing electron beam lithography (EBL) and highly directional dry etching.

  1. Substrate Preparation:
    • Commercial (100) CVD single-crystal diamond was cleaned (acetone, piranha solution: 3:1 H2SO4:H2O2).
    • A preliminary non-contact polishing step (physical bombardment with accelerated inert gas ions) was applied to remove mechanical defects and achieve a root mean square (rms) roughness of less than 2 nm.
  2. Hard Mask Deposition:
    • A 200 nm Titanium (Ti) layer was sputtered onto the diamond surface to serve as the hard mask.
  3. Resist Patterning (EBL):
    • A ~150 nm layer of Hydrogen Silsesquioxane (HSQ XR-1541-006) negative resist was spin-coated.
    • Pillars were patterned using Electron Beam Lithography (EBL), followed by development in Tetramethylammonium hydroxide (TMAH 25%).
  4. Mask Transfer (Ti Etch):
    • The HSQ pattern was transferred to the Ti hard mask using a Cl2-based Reactive Ion Etching (RIE) process (STS Multiplex ICP: 800 W ICP power, 150 W bias power, 10 sccm Cl2, 10 sccm BCl3, 3 mTorr).
  5. Diamond Etch (HAR):
    • A highly directional O2-plasma etch was used to create the nanopillars (STS Multiplex ICP: 400 W ICP power, 200 W bias power, 30 sccm O2, 15 mTorr), achieving vertical sidewalls and high aspect ratios.
  6. Mask Removal:
    • The remaining HSQ and Ti masks were stripped using diluted Hydrofluoric Acid (HF, 1% concentration).
  7. Cell Culture Preparation:
    • Sterile diamond chips were coated sequentially with Poly-L-lysine (1 hour) and Laminin (30 minutes at 37 °C) to facilitate neuronal adhesion and growth.
  8. Neuronal Plating:
    • Primary mouse hippocampal neurons (P0/P1 pups) were plated at a density of 150,000 cells/ml and maintained for 10-14 days in vitro (DIV) before imaging or electrophysiology.

The developed nanostructured diamond platform is highly relevant for advanced biosensing and quantum technology sectors:

  • Quantum Biosensing Platforms: Realization of nanophotonic quantum sensing devices utilizing near-surface NV centers for wide-field, label-free recording of biological signals.
  • Neuroscience Research Tools: Development of high-resolution neural interfaces capable of sub-cellular spatial and sub-millisecond temporal resolution for analyzing neuronal network dynamics and information processing.
  • Biophysics Modeling: Providing high-sensitivity measurements of electric and magnetic fields generated by neuronal activity, enabling better modeling of neuronal biophysics.
  • Neurodegenerative Diagnostics: Potential application in identifying early stages of brain disorders (e.g., Parkinson’s and Alzheimer’s) by sensitively measuring subtle changes in neuronal electric/magnetic fields.
  • Diamond Photonics: The robust, scalable fabrication process for HAR diamond structures is applicable to creating other integrated photonic devices, such as waveguides and single-photon sources, particularly when using electronic grade diamond substrates with shallow NV implantation.
  • Biocompatible Interfaces: Use of nanostructured diamond as a highly biocompatible neural interface for electrodes and microelectrode arrays.