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Rare-earth metal catalysts for high-pressure synthesis of rare diamonds

MetadataDetails
Publication Date2021-04-19
JournalScientific Reports
AuthorsYuri N. Palyanov, Yuri M. Borzdov, Igor N. Kupriyanov, Alexander F. Khohkhryakov, Denis V. Nechaev
InstitutionsV.S. Sobolev Institute of Geology and Mineralogy
Citations9
AnalysisFull AI Review Included
  • Novel Catalytic System: The study successfully established 15 Rare-Earth Metals (REM) as effective solvent-catalysts for High-Pressure High-Temperature (HPHT) diamond synthesis at 7.8 GPa and 1800-2100 °C.
  • Nitrogen Gettering: All synthesized diamonds are confirmed to be nitrogen-free (Type II), demonstrating that REMs inherently function as highly effective nitrogen getters, eliminating the need for traditional getter additives (e.g., Ti, Zr).
  • High Efficiency: Highly effective REMs (Sc, Ce, Tm, Lu) achieved graphite-to-diamond conversion rates up to 100% at 2000 °C, with maximum linear growth rates reaching 800 ”m/h (La-C system).
  • Quantum Doping Success: The REM-C systems provide growth conditions favorable for the incorporation of Group IV elements (Si, Ge, Sn), leading to the formation of high-intensity Silicon-Vacancy (SiV-), Germanium-Vacancy (GeV-), and Tin-Vacancy (SnV-) color centers.
  • Morphological Control: Diamond morphology is strongly dependent on the REM catalyst composition, ranging from simple octahedral habits (light REMs like La, Ce) to complex forms bound by tetragon-trioctahedron and trigon-trioctahedron faces (heavy REMs like Er, Lu).
  • Type IIb Synthesis: Diamonds synthesized using heavy REMs (Tb-Lu) and Sc/Y frequently showed B-related absorption, corresponding to Type IIb semiconducting diamond, with boron concentrations estimated between 0.1 and 1 atomic ppm.
ParameterValueUnitContext
Synthesis Pressure7.8GPaAll experiments
Synthesis Temperature Range1800-2100°CAll experiments
Max Graphite-to-Diamond Conversion (a)100%Sc-C system (2000 °C)
Max Linear Growth Rate (V)800”m/hLa-C system (2000 °C)
Typical Nucleation Density (N)36 to 400cm-2Most REM systems (2000 °C)
Anomalous Nucleation Density (N)10,000cm-2Sm-C system (2000 °C)
Max Single Crystal Size2mmCe-C system
Diamond TypeII (Nitrogen-free)N/AAll synthesized diamonds
Boron Concentration (Type IIb)0.1-1atomic ppmHeavy REMs (Tb-Lu), Sc, Y catalysts
SiV- Zero-Phonon Line (ZPL)737nmDominant center in most samples
GeV- ZPL602nmAchieved via Ge doping (Ce-Ge-C system)
SnV- ZPL620nmAchieved via Sn doping (Ce-Sn-C system)
Starting Graphite Purity99.97%Used for carbon source
Starting REM Purity99.99%Used for solvent-catalyst
  1. Apparatus: Experiments were conducted using a split-sphere multi-anvil high-pressure apparatus.
  2. Pressure/Temperature Control: Pressure was maintained at 7.8 GPa. Temperature was varied between 1800 °C and 2100 °C. Run times were 1 hour for 1900-2100 °C runs, and 3-4 hours for 1800 °C runs.
  3. Starting Materials: Graphite rods (99.97% purity), Rare-Earth Metals (99.99% purity), and synthetic diamond seed crystals (0.5 mm cuboctahedrons) were used.
  4. Cell Assembly: Graphite rods were machined into thick-walled capsules (1.5 mm wall thickness). A piece of REM metal was placed in the center hole (3.9 mm diameter, 3.5 mm height), and four seed crystals were placed at the metal-graphite interface.
  5. Oxidation Prevention: Graphite capsules were enveloped with a 0.1 mm thick Molybdenum (Mo) foil to prevent penetration of high-pressure cell components. The assembled cells were dried in a vacuum oven at 100 °C for 24 hours, followed by argon filling.
  6. Doping Experiments: For Group IV doping, 10 wt% of Ge or Sn was added to the Ce-C and Ho-C systems.
  7. Post-Synthesis Processing: Products were recovered by dissolving the cell components in a hot mixture of nitric and hydrochloric acids. Residual graphite was removed from diamond surfaces using an aqueous solution of K2Cr2O7 and concentrated H2SO4.
  8. Characterization:
    • Morphology: Optical microscopy, Scanning Electron Microscopy (SEM), and goniometric measurements.
    • Surface Microrelief: Differential Interference Contrast (DIC) and Total Interference Contrast (TIC) methods were used to profile stepped combination surfaces.
    • Impurity Analysis: Fourier Transform Infrared (FTIR) spectroscopy (for N and B content).
    • Color Centers: Photoluminescence (PL) spectroscopy (excited at 395 nm, recorded at 80 K).
  • Quantum Technologies: The ability to synthesize diamonds containing high concentrations of specific Group IV vacancy centers (SiV-, GeV-, SnV-) is critical for:
    • Solid-State Quantum Computing: Utilizing the spin properties of these centers as qubits.
    • Quantum Sensing and Metrology: Creating highly sensitive sensors based on diamond defects.
    • Single-Photon Emitters: Developing stable, room-temperature light sources for quantum communication.
  • High-Power Electronics and Optics: The production of large, high-quality, nitrogen-free (Type II) diamond crystals is essential for:
    • Heat Sinks: Diamond’s superior thermal conductivity requires Type II material.
    • High-Frequency/High-Power Devices: Utilizing Type IIb (boron-doped semiconducting) diamond synthesized efficiently using heavy REMs.
    • Optical Windows: Creating robust, low-absorption optical components.
  • Advanced Materials Research: The REM-C system provides a unique, ultra-reducing chemical environment, opening new pathways for synthesizing diamond doped with other elements or creating novel defect structures not achievable with traditional Fe-Ni-Co catalysts.
  1. 1999 - Advances in New Diamond Science and Technology
  2. 1979 - The Properties of Diamond
  3. 1992 - The Properties of Natural and Synthetic Diamond
  4. 2015 - Handbook of Crystal Growth (Chap. 17) [Crossref]