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Combined HF+MW CVD Approach for the Growth of Polycrystalline Diamond Films with Reduced Bow

MetadataDetails
Publication Date2023-02-07
JournalCoatings
AuthorsVadim Sedov, А. Ф. Попович, Stepan Linnik, Artem Martyanov, Junjun Wei
InstitutionsUniversity of Science and Technology Beijing, MIREA - Russian Technological University
Citations5
AnalysisFull AI Review Included

This research presents a novel, combined Chemical Vapor Deposition (CVD) approach—Microwave Plasma CVD (MW CVD) followed by Hot Filament CVD (HF CVD)—to produce high-quality polycrystalline diamond (PCD) films on silicon (Si) substrates, specifically targeting thermal management applications.

  • Thermal Conductivity Enhancement: The combined 110 µm film achieved a Thermal Conductivity (TC) of 210 W/mK, representing a 60% improvement compared to the pure 93 µm HF CVD film (130 W/mK).
  • Bow Reduction: The overall substrate bow was reduced by 57% (from -45 µm to -19 µm) by leveraging the opposite stress trends inherent in the two growth methods (MW CVD is typically compressive; HF CVD is typically tensile).
  • Structural Quality Control: The initial 25 µm high-quality MW CVD layer promoted larger diamond grain growth, which propagated through the subsequent 85 µm HF CVD layer, mitigating the negative TC effects usually associated with the small-grained nucleation layer.
  • Cost Efficiency: The use of cost-effective HF CVD for the majority (85 µm) of the film thickness allows for the production of large-area, high-TC PCD plates, overcoming the size and cost limitations of pure MW CVD.
  • Surface Quality: The combined MW+HF film exhibited the lowest root-mean-squared roughness (Rrms = 1.8 µm) compared to both pure MW CVD (3.2 µm) and pure HF CVD (2.7 µm) films.
ParameterValueUnitContext
Combined Film Thickness110µmMW (25 µm) + HF (85 µm) layers
Thermal Conductivity (MW+HF)210 ± 25W/mKMeasured via Laser Flash Technique (LFT)
Thermal Conductivity (Pure HF)130 ± 15W/mK93 µm thick film (Baseline comparison)
Bow (Delta h) Reduction57%Reduction from pure HF (-45 µm) to MW+HF (-19 µm)
Curvature Radius (MW+HF)-1.9mLowest bow achieved; closer to the HF CVD trend
Surface Roughness (Rrms, MW+HF)1.8µmRoot-mean-squared roughness
MW CVD Growth Rate~1µm/hUsed for the initial layer
HF CVD Growth Rate~1.1µm/hUsed for the bulk layer
Diamond Raman Peak (MW+HF)1334.3cm-1Indicates highly compressive stress
FWHM (MW+HF)7.8cm-1Full Width at Half Maximum of diamond peak
Substrate Size (Final)17 x 17mm2Laser-cut from 19 x 19 mm2 Si (111) plates

The combined MW+HF CVD process was executed in two distinct stages on seeded Si (111) substrates:

  • Reactor Type: Microwave Plasma CVD (MW CVD), ARDIS-100 (2.45 GHz).
  • Power: 4.8 kW (Microwave).
  • Gas Mixture: CH4/H2 (3% CH4 concentration).
  • Total Gas Flow: 500 sccm.
  • Pressure: 55 Torr.
  • Substrate Temperature: 850 ± 25 °C.
  • Purpose: To establish a high-quality, large-grain nucleation layer critical for high TC and to introduce compressive stress.
  • Reactor Type: Laboratory-built Hot Filament (HF) reactor (Tungsten filaments, 0.16 mm diameter).
  • Gas Mixture: H2/CH4 (6 vol.% CH4 concentration).
  • Pressure: 20 ± 1 Torr.
  • Substrate Temperature: 850 ± 20 °C.
  • Filament Parameters: Average current 6 ± 0.1 A; distance 12 ± 1 mm.
  • Purpose: To provide cost-effective, high-rate bulk growth while introducing tensile stress to compensate for the initial MW CVD compressive stress.
  • Structure and Morphology: Scanning Electron Microscopy (SEM) in both Secondary Electrons (SE) and Backscattered Electrons (BSE) modes (BSE clearly revealed the MW→HF interface).
  • Phase Composition and Stress: Micro-Raman Spectroscopy (473 nm laser) to analyze the diamond peak shift and the presence of non-diamond phases (t-PA peak at 1490 cm-1).
  • Bow and Roughness: Optical Profilometer (NewView 5000) used to measure curvature radius (r) and Rrms from the substrate side.
  • Thermal Conductivity (TC): Laser Flash Technique (LFT) applied to freestanding PCD films (Si substrate removed) to determine thermal diffusivity (D) perpendicular to the surface.

The development of high-TC, low-bow, cost-effective PCD films is critical for next-generation thermal management in high-power density electronics.

  • Power Electronics:
    • GaN-on-Diamond Devices: Direct application for creating efficient thermal management layers for Gallium Nitride (GaN) High Electron Mobility Transistors (HEMTs) and other high-frequency communications devices, overcoming GaN’s low intrinsic TC.
    • High-Power RF/Microwave Systems: Used as heat spreaders to manage localized heat flux dissipation in high-performance regimes.
  • Thermal Management:
    • Large-Area Heat Sinks: Enables the production of wider-sized PCD plates (surpassing the 2-inch limit of standard 2.45 GHz MW CVD) for industrial heat sink applications where cost and size are primary constraints.
    • Semiconductor Disk Lasers (SDLs): Heat spreaders for high-power laser systems.
  • Protective Coatings:
    • Cutting Tools: Improving the quality and TC of HF CVD diamond films used for hard or protective coatings, benefiting from the enhanced grain structure initiated by the MW layer.
  • General CVD Diamond Industry:
    • The technique provides a blueprint for tuning intrinsic stress (tensile/compressive) in PCD films by combining different CVD regimes, allowing for precise control over substrate bow for various thin-film applications.
View Original Abstract

A combination of two methods of chemical vapor deposition (CVD) of diamond films, microwave plasma-assisted (MW CVD) and hot filament (HF CVD), was used for the growth of 100 µm-thick polycrystalline diamond (PCD) layers on Si substrates. The bow of HF CVD and MW CVD films showed opposite convex\concave trends; thus, the combined material allowed reducing the overall bow by a factor of 2-3. Using MW CVD for the growth of the initial 25 µm-thick PCD layer allowed achieving much higher thermal conductivity of the combined 110 µm-thick film at 210 W/m·K in comparison to 130 W/m·K for the 93 µm-thick pure HF CVD film.

  1. 2018 - Thermal Conductivity of High Purity Synthetic Single Crystal Diamonds [Crossref]
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