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Visible-Light Activation of Photocatalytic for Reduction of Nitrogen to Ammonia by Introducing Impurity Defect Levels into Nanocrystalline Diamond

MetadataDetails
Publication Date2020-10-14
JournalMaterials
AuthorsRui Su, Zhangcheng Liu, Haris Naeem Abbasi, Jinjia Wei, Hongxing Wang
InstitutionsXi’an Jiaotong University
Citations5
AnalysisFull AI Review Included

Technical Documentation & Analysis: Visible-Light Activated Photocatalytic Diamond

Section titled “Technical Documentation & Analysis: Visible-Light Activated Photocatalytic Diamond”

This document analyzes the research paper “Visible-Light Activation of Photocatalytic for Reduction of Nitrogen to Ammonia by Introducing Impurity Defect Levels into Nanocrystalline Diamond” and outlines how 6CCVD’s advanced MPCVD diamond capabilities can support and extend this critical research in sustainable ammonia synthesis.


The research successfully demonstrates a high-efficiency, visible-light-activated photocatalytic system for converting nitrogen (N2) to ammonia (NH3) using nitrogen-doped nanocrystalline diamond (NDD).

  • Core Achievement: NDD films, synthesized via MPCVD, achieved an ammonia production rate of 6.27 ± 1.48 nmol/cm2·h, significantly surpassing undoped polycrystalline diamond (PD) and single crystal diamond (SCD).
  • Mechanism: Nitrogen doping introduces intermediate energy levels (specifically the Nitrogen Vacancy, NV- and NV0 centers) within the diamond’s forbidden bandgap.
  • Key Advantage: These defect levels enable efficient internal photoemission, allowing the photocatalytic reaction to proceed under sub-band gap (visible) light ($\lambda$ > 225 nm), overcoming the high energy barrier of intrinsic diamond (5.45 eV).
  • Material Requirement: The superior performance relies on precise control over nitrogen incorporation and the formation of a high-surface-area nanocrystalline structure (grains > 10 nm).
  • 6CCVD Value Proposition: 6CCVD specializes in custom MPCVD diamond materials, offering the precise doping control, thickness uniformity (down to 0.1 ”m), and large-area PCD substrates necessary to scale and optimize this energy-efficient ammonia synthesis technology.

The following hard data points were extracted from the research paper, highlighting the material properties and performance metrics of the tested diamond films.

ParameterValueUnitContext
NDD Ammonia Synthesis Rate6.27 ± 1.48nmol/cm2·hHighest rate achieved under 200-800 nm illumination
SCD Ammonia Synthesis Rate2.53 ± 0.16nmol/cm2·hUndoped single crystal diamond film performance
Diamond Bandgap Energy5.45eVIntrinsic excitation threshold ($\lambda$ < 225 nm)
NV- Zero Phonon Line (ZPL)1.945 (637)eV (nm)Negatively charged nitrogen vacancy state
NV0 Zero Phonon Line (ZPL)2.156 (575)eV (nm)Neutral nitrogen vacancy state
NDD Film Thickness (Active Layer)200nmNitrogen-doped nanocrystalline layer
NDD Average Grain Diameter> 10nmNanocrystalline structure
Photocatalysis Wavelength Range200-800nmUsed 450 W high-pressure Hg/Xe lamp

The experiment relied on precise MPCVD growth parameters to achieve the desired nanocrystalline structure and nitrogen doping levels.

StepParameterValueContext
SubstrateMaterial2-inch SiUsed for polycrystalline growth
Nucleation MethodSeedingNanodiamond particles (5-8 nm)Sonication in ethanol for 15 min
MPCVD SystemEquipmentModified AsTex systemUsed for all diamond deposition
Growth TemperatureTgrowth1000°C
Total Gas Flow RateFlow500sccm
Polycrystal Layer ThicknessThickness3”m
NDD Layer ThicknessThickness200nm
NDD Doping Gas RatioN2/H2 Ratio1%Introduced during the final 200 nm growth step
Polycrystal Gas RatioCH4/H2 Ratio4%Used for the 3 ”m base layer
Microwave Power (NDD/PD)PMW2000W

The successful replication and scaling of this high-efficiency photocatalytic process require precise control over material structure, thickness, and impurity doping—all core competencies of 6CCVD.

To replicate or extend the performance of the Nitrogen-Doped Nanocrystalline Diamond (NDD) used in this study, 6CCVD recommends the following materials:

  • Nitrogen-Doped Polycrystalline Diamond (PCD):
    • Requirement Match: This material directly corresponds to the NDD film synthesized. 6CCVD offers precise control over nitrogen gas flow (N2/H2 ratio) during MPCVD growth to tune the concentration of NV centers, optimizing the visible-light absorption peaks (575 nm and 637 nm).
    • Structure Control: We can tailor the grain size to optimize the active site density, crucial for maximizing the N2 reduction rate (6.27 nmol/cm2·h).
  • Optical Grade Single Crystal Diamond (SCD):
    • Requirement Match: For contrast studies or applications requiring superior thermal management and surface flatness (Ra < 1 nm), 6CCVD provides high-purity SCD substrates and homoepitaxial layers.
  • Custom Boron-Doped Diamond (BDD):
    • Extension Potential: While this paper focused on N-doping, BDD is known for its exceptional electrochemical properties and stability. 6CCVD can provide heavy Boron-Doped PCD or SCD for comparative studies in electrocatalytic NRR, offering a large electrochemical potential window.

The research utilized specific film dimensions (200 nm active layer) and growth on 2-inch substrates. 6CCVD’s manufacturing capabilities are ideally suited to meet and exceed these requirements:

Research Requirement6CCVD CapabilityAdvantage for Replication/Scaling
Substrate SizePlates/wafers up to 125 mm (PCD)Enables scaling from 2-inch lab samples to industrial wafer sizes.
Active Layer ThicknessSCD/PCD thickness control from 0.1 ”m to 500 ”mPerfect control over the critical 200 nm active layer thickness used in the study.
Doping ControlPrecise gas flow management (N2, B)Allows fine-tuning of NV center concentration for maximum photocatalytic efficiency.
Surface FinishPolishing to Ra < 5 nm (Inch-size PCD)Ensures reproducible surface quality for consistent photocatalytic testing.
MetalizationInternal capability (Au, Pt, Pd, Ti, W, Cu)Available for integrating diamond films into complex reactor systems or creating electrode structures for photoelectrochemical NRR extensions.

6CCVD’s in-house team of PhD material scientists and engineers can provide authoritative support for projects focused on Photocatalytic Nitrogen Reduction and Quantum Defect Engineering. We assist researchers in selecting the optimal diamond material (PCD vs. SCD), determining the necessary doping concentration (N-doping for NV centers), and specifying the required surface termination and thickness to maximize visible-light activation and NRR yield.

Global Shipping: We ensure reliable, global delivery of custom diamond materials, with DDU as the default and DDP available upon request.

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

View Original Abstract

Nitrogen impurity has been introduced in diamond film to produce a nitrogen vacancy center (NV center) toward the solvated electron-initiated reduction of N2 to NH3 in liquids, giving rise to extend the wavelength region beyond the diamond’s band. Scanning electron microscopy and X-ray diffraction demonstrate the formation of the nanocrystalline nitrogen-doped diamond with an average diameter of ten nanometers. Raman spectroscopy and PhotoLuminescence (PL) spectrum show characteristics of the NV0 and NV− charge states. Measurements of photocatalytic activity using supraband (λ < 225 nm) gap and sub-band gap (λ > 225 nm) excitation show the nitrogen-doped diamond significantly enhanced the ability to reduce N2 to NH3 compared to the polycrystalline diamond and single crystal diamond (SCD). Our results suggest an important process of internal photoemission, in which electrons are excited from negative charge states into conduction band edges, presenting remarkable photoinitiated electrons under ultraviolet and visible light. Other factors, including transitions between defect levels and processes of reaction, are also discussed. This approach can be especially advantageous to such as N2 and CO2 that bind only weakly to most surfaces and high energy conditions.

  1. 2017 - Unoccupied Surface State Induced by Ozone and Ammonia On H-Terminated Diamond Electrodes for Photocatalytic Ammonia Synthesis [Crossref]
  2. 2003 - Electrochemical and Related Processes at Surface Conductive Diamond-Solution Interfaces [Crossref]
  3. 2008 - Electrochemical Oxidation of Highly Oriented Pyrolytic Graphite During Potential Cycling in Sulfuric Acid Solution [Crossref]
  4. 2019 - Electrochemical Fabrication of Porous Au Film On Ni Foam for Nitrogen Reduction to Ammonia [Crossref]
  5. 2019 - Electrochemical Nitrogen Reduction Reaction on Ruthenium [Crossref]
  6. 2018 - Negative Electron Affinity from Aluminium on the Diamond (100) Surface: A Theoretical Study [Crossref]
  7. 2005 - Direct Observation of Negative Electron Affinity in Hydrogen-Terminated Diamond Surfaces [Crossref]
  8. 1998 - Electron Affinity and Schottky Barrier Height of Metal-Diamond (100), (111), (110) Interfaces [Crossref]
  9. 2019 - Efficient Electrocatalytic N2 Fixation with Mxene Under Ambient Conditions [Crossref]
  10. 2008 - Electrical and Photoelectrical Characterization of Undoped and S-Doped Nanocrystalline Diamond Films [Crossref]