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Observation of Graphite-Like and Diamond-Like Nanostructures in the Raman Spectra of Natural and Synthesized MoS2 Crystals with Small Carbon Additives

MetadataDetails
Publication Date2020-12-30
JournalPhysics and Chemistry of Solid State
AuthorsN. E. ĐšĐŸrnienko, A. P. Naumenko, L.M. Kulikov
InstitutionsNational Academy of Sciences of Ukraine, Frantsevich Institute for Problems in Materials Science
AnalysisFull AI Review Included

Technical Documentation & Analysis: Diamond Nanostructures in TMD Composites

Section titled “Technical Documentation & Analysis: Diamond Nanostructures in TMD Composites”

This research successfully demonstrates the spontaneous formation and detailed characterization of ultra-small diamond-like (sp3) and graphite-like (sp2) carbon nanostructures (CNs) within a 2H-MoS$_{2}$ host matrix using low concentrations of carbon additives (0.5-1.0 wt.%).

  • Novel Synthesis: Diamond-like nanostructures (ND) were formed within the layered Transition Metal Dichalcogenide (TMD) structure without requiring explicit high-pressure or high-temperature synthesis methods.
  • Record Low Frequencies: Raman Spectroscopy (RS) confirmed the existence of diamond-like structures characterized by record low D-band frequencies (1284, 1295 - 1312 cm-1), indicating extremely small sizes, estimated to be less than 1 nm.
  • Structural Control: Increasing carbon content (from 0.5 wt.% to 1.0 wt.%) led to a significant strengthening and ordering of the diamond-like nanostructures, evidenced by a reduction in the D-band Full Width at Half Maximum (FWHM) by approximately 50%.
  • Resonant Activation: Resonant laser excitation (632.8 nm) was shown to activate structural transformation (MoS${2}$ $\rightarrow$ $\alpha$-MoO${3}$ oxidation) and enhance the formation and ordering of the internal carbon nanostructures through strong vibrational-electronic interaction (VEI).
  • Advanced Analysis: A novel two-stage numerical decomposition method was employed to reliably separate highly overlapping D and G(k) spectral components, confirming the fine structure and disorder of the CNs.

The following hard data points were extracted from the analysis of natural and synthesized MoS$_{2}$ crystals and nanocrystallites (NCs) with carbon additives.

ParameterValueUnitContext
Carbon Additive Concentration0.5 and 1.0wt.%Synthesized MoS$_{2}$(C) Nanocrystallites (NCs)
Laser Excitation Wavelength ($\lambda_{L}$)632.8 and 488nmRaman Spectroscopy (Resonant and Near Electron Absorption Edge)
Record Low D-Band Frequencies1284, 1295 - 1312cm-1Diamond-like nanostructures (ND)
High G(k) Band Frequencies1387 and 1402cm-1Graphite-like nanostructures
Estimated Nanostructure Size< 1nmDiamond-like and Graphite-like structures
MoS$_{2}$(C) NC Size ([013] direction)3.9(2)nmX-ray studies (0.5 wt.% and 1.0 wt.% C)
MoS$_{2}$(C) NC Size ([110] direction)9.1(6) to 9.4(6)nmX-ray studies (0.5 wt.% and 1.0 wt.% C)
D-Band FWHM Reduction (0.5% $\rightarrow$ 1.0% C)129 $\rightarrow$ 62cm-1Indicates increased ordering/size of diamond-like structure
MoO$_{3}$ Characteristic Lines818 and 991cm-1Observed under 632.8 nm resonant excitation

The experimental approach focused on controlled synthesis and high-resolution vibrational characterization to identify and analyze the internal carbon nanostructures.

  1. Synthesis of MoS$_{2}$(C) Nanocrystallites: Materials were synthesized using low-temperature Chemical Vapor Deposition (CVD) combined with self-oscillating temperatures, allowing for the controlled incorporation of carbon atoms (0.5 wt.% and 1.0 wt.%) into the 2H-MoS$_{2}$ lattice.
  2. Structural Analysis: High-precision X-ray investigations (full-profile method) were used to determine crystallographic data, unit cell parameters, and average nanocrystallite sizes.
  3. Raman Spectroscopy (RS): Measurements were performed using two distinct laser excitation wavelengths:
    • $\lambda_{L}$ = 488 nm (Ar$^{+}$ laser, near the electron absorption edge).
    • $\lambda_{L}$ = 632.8 nm (He-Ne laser, resonant with exciton states of 2H-MoS$_{2}$).
  4. Spectral Decomposition: A two-stage numerical analysis was applied to the complex, overlapping D and G bands. This involved decomposing the bands into individual spectral components (Lorentz or Gaussian forms) to resolve the fine structure.
  5. Validation of Decomposition: The accuracy of the numerical decomposition was rigorously checked by comparing the calculated spectra against the 2-nd derivatives (d$^{2}$I/d$\nu^{2}$) of the experimentally observed vibrational bands.

This research highlights the critical role of high-quality carbon materials, particularly nanodiamonds, in creating novel nanocomposites with unique electronic and vibrational properties. 6CCVD is uniquely positioned to supply the foundational diamond materials and advanced processing required to replicate and scale this research into functional devices.

Research Requirement / Challenge6CCVD Solution & CapabilityTechnical Advantage
High-Purity Diamond Reference Material (For sp$^{3}$ structure comparison and quantum applications)Optical Grade Single Crystal Diamond (SCD): Available in thicknesses from 0.1 ”m up to 500 ”m, with ultra-low nitrogen and defect concentrations.Provides the highest quality, controlled sp$^{3}$ matrix, essential for engineering quantum defects (e.g., NV centers) relevant to the observed VEI phenomena.
Scaling Nanocomposite Substrates (Need for large-area integration)Polycrystalline Diamond (PCD) Wafers: Custom dimensions available up to 125 mm diameter, with substrate thicknesses up to 10 mm.Enables industrial scaling of hybrid TMD/diamond nanocomposites for thermal management, high-power electronics, and large-area sensor arrays.
Controlling Electronic States & Conductivity (To replicate VEI and resonant effects)Boron-Doped Diamond (BDD): Available in both SCD and PCD formats, offering precise control over conductivity and electrochemical properties.Allows researchers to tune the semiconductor properties of the diamond component, critical for optimizing the strong vibrational-electronic interaction observed under resonant excitation.
Device Integration and Interfacing (Need for electrical contacts on diamond surfaces)Custom Metalization Services: Internal capability for depositing Au, Pt, Pd, Ti, W, and Cu contacts.Facilitates the fabrication of complex heterostructures and devices, ensuring robust, low-resistance interfaces between the diamond layer and other materials (like MoS${2}$ or MoO${3}$).
Surface Quality for High-Resolution Analysis (Minimizing background noise in RS)Precision Polishing Services: SCD surfaces polished to Ra < 1 nm; Inch-size PCD polished to Ra < 5 nm.Guarantees atomically smooth surfaces, crucial for minimizing scattering and maximizing signal-to-noise ratio in advanced optical and Raman studies.
Global Supply ChainGlobal Shipping (DDU default, DDP available): Reliable, secure delivery worldwide.Ensures prompt access to specialized CVD diamond materials for international research teams replicating this work.

Engineering Support: 6CCVD’s in-house PhD team specializes in the growth and characterization of MPCVD diamond, including advanced Raman analysis of defect structures and doping profiles. We offer consultation services to assist researchers in selecting the optimal diamond material (SCD, PCD, or BDD) and specifications needed to replicate or extend projects focused on nanodiamond synthesis, TMD heterostructures, or vibrational-electronic coupling.

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View Original Abstract

A comparative study of Raman spectra excited by laser radiation λL = 632.8 nm and 488 nm of natural crystals of 2H-MoS2 and nanocrystallites MoS2 (C) containing 0.5 and 1.0 wt.% Carbon additives. A detailed numerical analysis of the shape of observed D and G bands was performed. The complication of the spectra of graphite-like and diamond-like structures with the appearance of additional spectral components at 1440-1500 cm-1 and 1230-1270 cm-1 as a result of doubling the size of the corresponding elementary quasi-cells are analyzed. It is shown that the frequencies of D-bands of diamond-like nanostructures 1297 Ă· 1302 cm-1 don’t depend on λL in contrast to the change in the frequencies of the G (k)-bands. A significant effect of 632.8 nm resonant radiation on the electronic states and properties of MoS2 (C) NC was established. The strengthening of the D bands of the diamond-like structure and the ordering of the graphite structure with increasing carbon content in MoS2 (C) nanocrystals have been established. The change of spectral positions of D, G, and G (k) bands at strengthening the degree of disordering of a diamond- and graphite-like structures is considered. The influence of laser radiation on carbon structures is discussed.