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Interactions of Nitrogen‐Vacancy Centers in Diamond with Electron Beams - Implications for Quantum Sensing and Photoluminescence Stability

MetadataDetails
Publication Date2025-10-26
JournalAdvanced Optical Materials
AuthorsBradley T. Flinn, William J. Cull, Ian Cardillo‐Zallo, James Kerfoot, Benjamin L. Weare
InstitutionsUniversity of Nottingham
AnalysisFull AI Review Included

Technical Documentation & Analysis: Interactions of Nitrogen-Vacancy Centers in Diamond with Electron Beams

Section titled “Technical Documentation & Analysis: Interactions of Nitrogen-Vacancy Centers in Diamond with Electron Beams”

This research provides critical insights into the stability and controlled manipulation of Nitrogen-Vacancy (NV) centers in diamond under electron beam irradiation, directly supporting the development of robust nanoscale quantum sensing and nanofabrication techniques.

  • Core Mechanism Identified: Electron beam damage to NV photoluminescence (PL) and sensing contrast (ODMR/MM) is dominated by a complex interplay of ionization and Direct Knock-On (DKO) effects, leading to vacancy migration away from the nitrogen atom.
  • Optimal Non-Invasive Conditions: For Correlative Light-Electron Microscopy (CLEM) applications requiring maximum NV retention, the optimal parameters are identified as 200 keV beam energy at a low electron fluence (< 10⁵ e⁻nm⁻²).
  • Controlled Deactivation: High fluence irradiation (e.g., 9.0 x 10⁶ e⁻nm⁻² at 200 keV) successfully quenches PL and sensing contrast to near-zero levels (4% residual PL), enabling controlled, top-down spatial patterning of diamond PL.
  • Material Sensitivity: Damage mechanisms occur well below the displacement energy thresholds for pristine bulk diamond, indicating high sensitivity in NV-rich nanodiamonds (FNDs) due to ionization-assisted DKO.
  • 6CCVD Value Proposition: 6CCVD offers the high-purity Single Crystal Diamond (SCD) and large-area Polycrystalline Diamond (PCD) substrates necessary to replicate and scale this patterning methodology for integrated quantum devices.

The following hard data points were extracted from the analysis of NV center stability under varying electron beam conditions:

ParameterValueUnitContext
Optimal E-Beam Energy (Non-Invasive)200keVRecommended for CLEM (Fluence < 10⁵ e⁻nm⁻²)
Optimal Electron Fluence (Non-Invasive)< 10⁵e⁻nm⁻²Retains > 90% PL and sensing contrast
Maximum Fluence Tested9.0 x 10⁶e⁻nm⁻²Highest damage condition
Residual PL (Max Damage)4 ± 1%200 keV, 9.0 x 10⁶ e⁻nm⁻²
Residual ODMR Contrast (Max Damage)5 ± 3%200 keV, 9.0 x 10⁶ e⁻nm⁻²
Carbon Displacement Energy ($E_{d}$) (Pristine Lattice)30 - 80eVLiterature range (requires 145-330 keV beam)
Carbon Displacement Energy ($E_{d}$) (Adjacent to Vacancy)2.3 - 13.0eVRange used for DKO cross-section calculation
Maximum Transferable Energy ($E_{Tmax}$)43.7eVAchieved by 200 keV beam
Displacement Cross Section ($\sigma_{d}$) ($E_{d}$ = 2.3 eV)329barn200 keV beam energy
Ionization Cross Section ($\sigma_{i}$) (C L shell)1.2Mbarn200 keV beam energy

Note: 1 barn = 10⁻²⁸ m².

The experimental approach combined high-resolution electron microscopy with quantum sensing techniques to precisely monitor NV center properties during irradiation.

  1. Material Preparation: Commercially available NV-rich Fluorescent Nanodiamonds (FNDs, ≈100 nm diameter, HPHT synthesis) were drop-cast onto Au holey carbon TEM finder grids.
  2. Irradiation Source: Transmission Electron Microscopy (TEM, JEOL 2100+) was used at four distinct accelerating voltages: 20, 80, 100, and 200 keV.
  3. Fluence Control: Electron fluence was systematically varied across seven orders of magnitude (≈10³ to 10⁷ e⁻nm⁻²) using a custom electron microscope script for precise exposure timing.
  4. Quantum Sensing (ODMR/MM): NV sensing contrast was monitored via Optically Detected Magnetic Resonance (ODMR) and Magnetic Modulation (MM) of Photoluminescence (PL) using a custom PCB with a Cu wire for microwave delivery (2.77-2.97 GHz) and an external electromagnet (0-40 mT).
  5. Optical Characterization: PL intensity and NV charge-state ratios (NV⁻ ZPL at 637 nm and NV⁰ ZPL at 575 nm) were mapped using a confocal Raman microscope before and after irradiation.
  6. Simulation & Analysis: Monte Carlo CASINO simulations were performed to model electron trajectories and interaction volumes in diamond, supporting calculations of atomic displacement ($\sigma_{d}$) and ionization ($\sigma_{i}$) cross-sections.

This research validates a powerful top-down approach for engineering NV properties, moving beyond FNDs toward macroscopic diamond substrates for integrated quantum technologies. 6CCVD is uniquely positioned to supply the high-quality MPCVD diamond materials and customization services required to scale this methodology.

Applicable Materials for Replication and Extension

Section titled “Applicable Materials for Replication and Extension”

To transition this nanoscale patterning technique to functional, integrated quantum devices, researchers require high-purity, low-strain diamond substrates with controlled nitrogen incorporation.

Research Requirement6CCVD Material SolutionKey Specification
High Coherence/Low StrainOptical Grade Single Crystal Diamond (SCD)SCD wafers with Ra < 1 nm polishing, ideal for high-fidelity quantum sensing applications.
Scalable Patterning SubstratesPolycrystalline Diamond (PCD)Plates/wafers up to 125 mm diameter, suitable for large-area nanofabrication and industrial scaling.
Controlled NV CreationCustom Nitrogen-Doped SCD/PCDPrecise control over nitrogen concentration during MPCVD growth to optimize initial NV density prior to e-beam patterning.
Integrated SensingBoron-Doped Diamond (BDD)Available for applications requiring conductive diamond layers or electrochemical sensing integration.

Customization Potential for Advanced Quantum Devices

Section titled “Customization Potential for Advanced Quantum Devices”

The paper highlights the need for precise control over material dimensions and integration features (e.g., microwave delivery lines). 6CCVD’s in-house capabilities directly address these requirements:

  • Custom Dimensions and Thickness: 6CCVD supplies SCD and PCD plates/wafers in custom dimensions up to 125 mm (PCD). We offer precise thickness control for both SCD (0.1 µm - 500 µm) and PCD (0.1 µm - 500 µm), crucial for controlling the depth and volume of e-beam induced defects.
  • Ultra-Low Surface Roughness: To ensure minimal scattering and optimal optical coupling for PL mapping and ODMR, 6CCVD provides superior polishing: Ra < 1 nm for SCD and Ra < 5 nm for inch-size PCD.
  • Integrated Metalization: The experimental setup relied on external Cu wire for microwave delivery. 6CCVD offers internal metalization services (Au, Pt, Pd, Ti, W, Cu) directly onto diamond substrates, enabling the fabrication of integrated quantum devices with on-chip microwave transmission lines for enhanced ODMR/MM performance.
  • Precision Fabrication: We offer custom laser cutting and shaping services to meet unique geometry requirements for TEM grids, PCB integration, or specific device architectures.

6CCVD’s in-house PhD team specializes in MPCVD diamond growth and defect engineering. We provide authoritative professional support for projects involving:

  • Material selection to optimize initial NV concentration and crystal quality for e-beam patterning.
  • Consultation on surface preparation and polishing requirements for high-resolution CLEM and optical measurements.
  • Guidance on integrating custom metalization schemes for advanced [Quantum Sensing and Nanofabrication] projects.

Call to Action: For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.

View Original Abstract

Abstract Nitrogen‐vacancy (NV) photoluminescence (PL) in diamond is fundamental to its function as a color center, underpinning advances in sensing science and quantum technologies. The work herein provides critical insights into the atomistic mechanisms of electron beams interacting with NV centers, which are crucial for advancing robust quantum sensing at the nanoscale and controlling the functional properties of nanodiamonds. NV PL and sensing stability of NV‐rich fluorescent nanodiamonds (FNDs) under electron beam irradiation is probed, across a range of energies (20, 80, 100, and 200 keV) and fluences (≈10 3 to 10 7 e − nm −2 ). PL intensity, NV charge‐state ratios, and sensing contrast, as monitored via optically detected magnetic resonance (ODMR) and magnetic modulation (MM) of PL, are examined. Results reveal complex mechanisms governing interactions between NV‐centers and fast electrons, dominated by ionization and direct knock‐on (DKO) effects, which allow to establish optimum imaging conditions where FNDs can be imaged with sub‐nanometer resolution while preserving their PL and sensing properties (200 keV, <10 5 e − nm −2 ). This methodology enables controlled, top‐down spatial patterning of diamond PL by selectively deactivating NVs, providing novel routes to patterned NV creation.