Skip to content

Decoration of growth sector boundaries with nitrogen vacancy centers in as-grown single crystal high-pressure high-temperature synthetic diamond

MetadataDetails
Publication Date2020-09-30
JournalPhysical Review Materials
AuthorsP.L. Diggle, U.F.S. D’Haenens-Johansson, B.L. Green, C.M. Welbourn, Thu Nhi Tran Thi
InstitutionsEngineering and Physical Sciences Research Council, Gemological Institute of America
Citations11
AnalysisFull AI Review Included

This study investigates point defect incorporation in ultra-high purity, low-strain High Pressure High Temperature (HPHT) synthetic diamond, focusing on growth sector boundaries.

  • Ultra-High Purity Achieved: The {001} growth sector exhibits exceptional purity, containing less than 1 ppb of substitutional boron and a bulk luminescent defect concentration below 1011 cm-3 (10-3 ppb).
  • Low Strain/Dislocations: The material shows low internal strain, with an average dislocation density below 103 cm-2, making it suitable for quantum applications.
  • NV- Decoration: Negatively charged Nitrogen Vacancy (NV-) centers are found exclusively decorating the boundaries between the {111} and {113} growth sectors, but not in the bulk sectors themselves.
  • Growth Rate Determination: This NV- decoration pattern allows for the calculation of relative growth rates, yielding V113/V111 ≈ 1.13, suggesting stable growth conditions over time.
  • Defect Orientation: The NV- and Silicon Vacancy (SiV-) defects show no preferential orientation, consistent with the rapid thermal reorientation of NV- at typical HPHT growth temperatures (< 1 minute at 1500 °C).
  • Preferential Nickel Orientation: A nickel-related defect (1.40 eV, 884 nm ZPL) found in the bulk {111} sectors is strongly preferentially oriented, aligning its trigonal axis with the <111> growth direction.
ParameterValueUnitContext
Sample Size4.0 x 4.0 x 0.5mmPlate dimensions
Average Substitutional Nitrogen [N0]6.5 ± 1ppbMeasured by EPR (bulk average)
Boron [B] Concentration ({001} sector)< 1ppbLowest impurity sector
Boron [B] Concentration ({111} sector)84 ± 10ppbHighest impurity sector
Luminescent Defect Concentration ({001})< 1011cm-3Detection limit for common defects
Dislocation Density (Average)< 103cm-2Overall material quality
NV- Single Defect Resolution Limit1.76 x 1011cm-3Bulk concentration equivalent
Nickel Defect ZPL884nmZero Phonon Line (1.40 eV defect)
Relative Growth Rate (V113/V111)≈ 1.13N/ACalculated from decorated boundary angle
NV Reorientation Activation Energy (Ea)≈ 4.0eVThermal stability model
NV Reorientation Time (at 1500 °C)< 1minuteTime required to lose preferential alignment
Excitation Wavelengths (PL)488, 532nmConfocal Photoluminescence
Cathodoluminescence Temperature77KLow temperature measurement

The HPHT diamond was synthesized and characterized using advanced techniques to map defect incorporation and orientation:

  1. HPHT Synthesis:

    • Method: Temperature gradient method in the diamond thermodynamic stability region.
    • Solvent/Catalyst: Co-Fe-C system.
    • Purity Control: Proprietary nitrogen getter used to minimize nitrogen incorporation, resulting in Type IIa material.
    • Growth Conditions (Typical): 1350 - 1600 °C, with linear growth rates around 50 ”m/hour.
  2. Structural and Impurity Assessment:

    • X-ray Diffraction (Laue): Confirmed the (001) orientation of the sample plate.
    • X-ray Topography (XRT): Used white beam XRT (400 reflection) to visualize extended defects (stacking faults) and confirm low dislocation density.
    • Electron Paramagnetic Resonance (EPR): Measured the bulk average concentration of neutral substitutional nitrogen [N0].
    • Low Temperature Cathodoluminescence (CL) (77 K): Used the ratio of the boron bound exciton (BE) signal to the free exciton (FE) signal to determine sector-dependent substitutional boron concentrations (detection limit < 1 ppb).
  3. Point Defect Mapping and Spectroscopy:

    • Confocal Photoluminescence (PL) Microscopy: Diffraction-limited scanning used with 488 nm and 532 nm excitation to map the spatial distribution of NV-, SiV-, and 1.40 eV defects across growth sectors and boundaries.
    • Second Order Photon Autocorrelation (g2): Quantified the number of defects in the optical volume to distinguish between single NV- centers and defect ensembles.
    • Optically Detected Magnetic Resonance (ODMR): Applied an external magnetic field to measure the spin states and confirm the lack of preferential orientation for NV- centers.
    • Optical Polarisation Measurements: Rotated the linear excitation polarization to assess the preferential alignment of SiV- and the 1.40 eV nickel defect based on fluorescence intensity modulation.

The synthesis of ultra-high purity, low-strain HPHT diamond with controlled defect incorporation is highly relevant to several advanced technological fields:

  • Quantum Technologies (Quantum Sensing and Computing):
    • The {001} sector’s high purity and low dislocation density provide an ideal environment for creating high-coherence NV centers (via post-growth methods like ion implantation), crucial for room-temperature quantum sensors (magnetic fields, temperature, pressure).
    • The low background impurity concentration minimizes spin decoherence, potentially allowing this HPHT material to outperform “quantum grade” CVD diamond in certain applications.
  • High-Power Optics and Radiation Windows:
    • The large size (> 100 mm3) and low birefringence (due to low strain) make this material suitable for high-energy laser optics and radiation detector windows.
  • Fundamental Defect Engineering:
    • The clear decoration of growth sector boundaries with NV- centers offers a tool for monitoring and optimizing HPHT growth kinetics and impurity uptake mechanisms in real-time.
  • Silicon Vacancy (SiV-) Applications:
    • SiV- centers, observed in the {111} sectors, are promising quantum emitters, particularly for integrated photonic circuits, though further work is needed to control their orientation in HPHT growth.
View Original Abstract

Large (> 100 mm$^3$), relatively pure (type II) and low birefringence single\ncrystal diamond can be produced by high pressure high temperature (HPHT)\nsynthesis. In this study we examine a HPHT sample of good crystalline\nperfection, containing less than 1 ppb (part per billion carbon atoms) of boron\nimpurity atoms in the {001} growth sector and only tens of ppb of nitrogen\nimpurity atoms. It is shown that the boundaries between {111} and {113} growth\nsectors are decorated by negatively charged nitrogen vacancy centres (NV$^-$):\nno decoration is observed at any other type of growth sector interface. This\ndecoration can be used to calculated the relative {111} and {113} growth rates.\nThe bulk (001) sector contains concentrations of luminescent point defects\n(excited with 488 and 532 nm wavelengths) below 10$^{11}$ cm$^{-3}$ (10$^{-3}$\nppb). We observe the negatively charged silicon-vacancy (SiV$^-$) defect in the\nbulk {111} sectors along with a zero phonon line emission associated with a\nnickel defect at 884 nm (1.40 eV). No preferential orientation is seen for\neither NV$^-$ or SiV$^-$ defects, but the nickel related defect is oriented\nwith its trigonal axis along the <111> sector growth direction. Since the\nNV$^-$ defect is expected to readily re-orientate at HPHT diamond growth\ntemperatures, no preferential orientation is expected for this defect but the\nlack of preferential orientation of SiV$^-$ in {111} sectors is not explained.\n

  1. 2015 - Handbook of Crystal Growth
  2. 2015 - Components Packaging Laser System