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ODMR active bright sintered detonation nanodiamonds obtained without irradiation

MetadataDetails
Publication Date2023-01-01
JournalФизика и техника полупроводников
AuthorsK. V. Likhachev, M. V. Uchaev, I. D. Breev, A. V. Ankudinov, R. A. Babunts
InstitutionsIoffe Institute, ITMO University
AnalysisFull AI Review Included

Technical Documentation & Analysis: ODMR Active Sintered Nanodiamonds

Section titled “Technical Documentation & Analysis: ODMR Active Sintered Nanodiamonds”

This document analyzes the research concerning the synthesis of high-quality, low-stress diamond microcrystals containing bright Nitrogen-Vacancy (NV) centers via HPHT sintering of detonation nanodiamonds (DND). This material is highly relevant to 6CCVD’s core mission of supplying advanced MPCVD diamond materials for quantum technologies and sensing applications.


The research successfully demonstrates a novel method for creating high-quality, optically active diamond microcrystals suitable for quantum sensing applications.

  • Core Achievement: Synthesis of single-crystal microdiamonds (0.1-15 µm) containing bright, optically active Nitrogen-Vacancy (NV) centers directly through High-Pressure High-Temperature (HPHT) sintering of 4-5 nm Detonation Nanodiamonds (DND).
  • Elimination of Post-Processing: The method eliminates the need for high-energy particle irradiation and subsequent annealing typically required to create NV centers in synthetic diamond.
  • Superior Crystalline Quality: ODMR analysis shows that the resulting Sintered DND (SDND) exhibits significantly lower internal stress (2E = 12.2 ± 0.2 MHz) compared to traditional HPHT synthetic diamonds (2E = 16.2 ± 0.3 MHz).
  • Quality Benchmark: The crystalline perfection of the SDND approaches that of high-quality natural diamond, making it a strong candidate for quantum magnetometry.
  • Application Proof-of-Concept: The SDND particles were successfully integrated onto a commercial AFM probe tip, demonstrating their immediate utility as robust, nanoscale magnetic sensors.
  • 6CCVD Relevance: This work highlights the critical demand for low-stress, high-purity diamond materials, a requirement perfectly met by 6CCVD’s Optical Grade Single Crystal Diamond (SCD) wafers.

The following hard data points were extracted from the experimental results and synthesis parameters:

ParameterValueUnitContext
Initial DND Particle Size4-5nmPrecursor material for sintering
Resulting SDND Crystal Size0.1-15µmSize range of synthesized single crystals
HPHT Sintering Pressure (P)~7GPaSynthesis condition
HPHT Sintering Temperature (T)1300-1700°CSynthesis condition
Raman Shift (Diamond Peak)1333cm⁻¹Confirms high crystalline quality
PL Excitation Wavelength532nmUsed for spectroscopy
NV⁻ Zero Field Splitting (D)2.87GHzTriplet ground state (at 25 °C)
SDND NV⁻ Splitting (2E)12.2 ± 0.2MHzIndicates low internal stress
Natural Diamond NV⁻ Splitting (2E)8.8 ± 0.1MHzReference for minimal internal stress
AN HPHT Diamond NV⁻ Splitting (2E)16.2 ± 0.3MHzReference for high internal stress (traditional synthesis)
ODMR Measurement Temperature300KRoom temperature (RT)
AFM Probe Stiffness (k)4N/mUsed for force calculation

The experiment relied on a combination of high-pressure synthesis and advanced optical characterization techniques:

  1. Precursor Preparation: Detonation Nanodiamond (DND) particles (4-5 nm) were prepared, often mixed with hydrocarbons (e.g., hexane), to serve as the carbon source.
  2. HPHT Sintering: The DND was subjected to extreme conditions (P ~ 7 GPa, T ~ 1300-1700 °C) for very short durations (8-15 s) to induce oriented attachment and growth of microcrystalline single diamonds.
  3. Structural Characterization (Raman): Confocal Raman spectroscopy (532 nm excitation, 0.7 cm⁻¹ resolution) was used to confirm the formation of high-quality diamond crystals via the characteristic 1333 cm⁻¹ peak.
  4. Optical Defect Characterization (PL): Photoluminescence spectroscopy (532 nm excitation, 0.7 nm resolution) confirmed the presence of NV centers, specifically the null-phonon lines for NV⁰ (575 nm) and NV⁻ (638 nm).
  5. Spin Property Measurement (ODMR): Optically Detected Magnetic Resonance was performed at 300 K in the 2.8-2.95 GHz range to measure the zero-field splitting (2E), which serves as a direct measure of internal stress and crystalline perfection.
  6. Nanosensor Integration: SDND particles were fixed onto a commercial silicon AFM probe tip using a UV50 urethane acrylic adhesive, demonstrating a simple, scalable method for creating quantum sensing probes.

The research demonstrates the critical need for diamond materials with exceptionally low internal stress and high crystalline perfection for advanced quantum applications. 6CCVD’s MPCVD capabilities are ideally suited to meet and exceed these requirements, offering scalable, high-purity alternatives to sintered DND.

To replicate or extend this research into scalable quantum devices, 6CCVD recommends the following materials:

MaterialDescriptionApplication Relevance
Optical Grade Single Crystal Diamond (SCD)High-purity, low-birefringence SCD with controlled nitrogen incorporation.Direct Replacement: Provides the lowest internal stress (highest crystalline perfection) necessary for long NV coherence times, surpassing the quality achieved by the SDND sintering method. Ideal for integrated quantum circuits and high-sensitivity magnetometers.
High-Purity Polycrystalline Diamond (PCD)Wafers up to 125 mm in diameter, polished to Ra < 5 nm.Bulk Sensing & Heat Management: Suitable for large-area sensor arrays or applications requiring high thermal conductivity and mechanical robustness where single-crystal coherence is not strictly required.
Boron-Doped Diamond (BDD)Custom doping levels available.Integrated Electrodes: Essential for creating integrated diamond devices where electrical control (e.g., charge state manipulation of NV⁻ centers) is required alongside optical sensing.

The integration of diamond particles onto AFM probes highlights the need for precise material handling and custom dimensions. 6CCVD offers comprehensive engineering services to support device fabrication:

  • Custom Dimensions: We supply SCD and PCD plates/wafers up to 125 mm. We can provide custom laser cutting and etching services to produce specific geometries, micro-pillars, or micro-crystals tailored for integration into AFM or other micro-electromechanical systems (MEMS).
  • Precision Polishing: Our SCD is polished to an industry-leading surface roughness of Ra < 1 nm, crucial for minimizing surface defects that can degrade NV center coherence near the surface.
  • Advanced Metalization: The paper’s application requires robust adhesion. 6CCVD offers in-house metalization capabilities, including Au, Pt, Pd, Ti, W, and Cu, allowing researchers to specify custom adhesion layers or electrical contacts for integrated diamond sensors.
  • Thickness Control: We offer precise thickness control for SCD and PCD layers ranging from 0.1 µm to 500 µm, enabling the fabrication of thin-film devices or robust substrates (up to 10 mm).

6CCVD’s in-house PhD team specializes in optimizing diamond growth parameters for quantum applications. We can assist researchers in:

  • Material Selection: Determining the optimal nitrogen concentration and growth orientation for maximizing NV⁻ center yield and coherence time for similar Quantum Magnetometry and Nanosensor projects.
  • Defect Engineering: Utilizing MPCVD to create highly controlled defect ensembles, offering a superior alternative to the stochastic nature of DND sintering.
  • Global Logistics: We provide reliable global shipping (DDU default, DDP available) to ensure materials reach your lab quickly and securely.

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

View Original Abstract

We present the results of study the structure and composition of microcrystalline diamonds obtained by high-pressure high temperature sintering of detonation nanodiamond particles. Using optical detected magnetic resonance method, photoluminescence spectroscopy and Raman spectroscopy we found sintering of detonation nanodiamond significantly differ from initial detonation nanodiamonds and can be compared to high quality diamonds. Monocrystals of diamonds obtained by the method of oriented attachment have dimensions of up to tens of microns, possess the habitus of high-quality diamonds, and do not contain metal catalysts in the lattice structure. In those crystals, the presence of optically active nitrogen impurities in the crystal lattice is observed. In particular, there is a bright nitrogen-vacancy defects. They are characterized by optical detected magnetic resonance method, which shows that spin properties of the obtained single crystals correspond to high-quality natural diamonds and surpass synthetic diamonds obtained from graphite in the presence of metal catalysts, followed by irradiation and annealing to obtain nitrogen-vacancy defects optical defects in the diamond lattice. The presence of nitrogen-vacancy defects defects and the high-quality of the crystal structure of sintering of detonation nanodiamond allows us to consider them as potential candidates in quantum magnetometry. For this purpose, the possibility of a simple way to improve the AFM probe by fixing a microcrystalline sintering of detonation nanodiamond particle on its tip is demonstrated. Keywords: detonation nanodiamond, HPHT sintering, ODMR, single crystalline, photoluminescence, defects.