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Uniform Growth of Two-inch MPCVD Optical Grade Diamond Film

MetadataDetails
Publication Date2023-01-01
JournalJournal of Inorganic Materials
AuthorsS Y Chan, Juping Tu, Ke Huang, Siwu SHAO, Zhiliang Yang
InstitutionsNorth China University of Technology, University of Science and Technology Beijing
Citations3
AnalysisFull AI Review Included

This research successfully optimized the Microwave Plasma Chemical Vapor Deposition (MPCVD) process for growing large-area, high-quality optical grade diamond films by systematically studying the effect of the deposition platform height ($h$).

  • Core Achievement: Uniform growth of a 2-inch (50.8 mm diameter) polycrystalline optical grade diamond film.
  • Optimization Parameter: COMSOL simulation and experimental validation identified the optimal deposition platform height as $h = 2$ mm.
  • Performance Metrics: The resulting film achieved a maximum thickness of 337 µm with a thickness inhomogeneity of less than 11.0%.
  • Optical Quality: High transmittance was confirmed in both visible (up to 70%) and infrared (70% at 10.6 µm) bands.
  • Crystalline Uniformity: Raman spectroscopy showed excellent quality, with the Full Width at Half Maximum (FWHM) ranging narrowly from 3.27 cm-1 (center) to 3.91 cm-1 (edge).
  • Mechanism Insight: Increasing the platform height significantly improved the uniformity of the electric field on the substrate surface, leading to a flatter plasma shape and more uniform distribution of H atoms and carbon-containing radicals.
ParameterValueUnitContext
Substrate Diameter50.8mmN-type (100) Si wafer
Optimal Platform Height ($h$)2mmBased on E-field and plasma uniformity
Maximum Film Thickness337µmAfter 200 h growth
Thickness Inhomogeneity (Δd/d)<11.0%Across 2-inch wafer
Average Growth Rate1.5µm/hAt optimal conditions
Max Visible Transmittance69-70%In the 480-800 nm range
IR Transmittance70.1%At 10.6 µm wavelength
Raman FWHM (Center)3.27cm-1Indicator of high crystalline quality
Raman FWHM (Edge)3.91cm-1Indicator of quality uniformity
Preferred Orientation (XRD)(220)N/AS(220)/S(111) ratio = 76.62
Temperature Uniformity (ΔT)21°CTemperature difference at $h = 2$ mm
E-Field Inhomogeneity14.1%At optimal height (2 mm)

The study utilized a combination of computational modeling and a 2.45 GHz, 6 kW quartz-plate MPCVD system to achieve uniform deposition.

  • Objective: Simulate the multi-physical fields within the reactor, focusing on the impact of platform height ($h$).
  • Variables Studied: Electric field (E-field) distribution, plasma shape, and substrate surface temperature uniformity.
  • Key Finding: As $h$ increased, the E-field uniformity improved significantly (inhomogeneity dropped from 57.4% at -2 mm to 14.1% at 2 mm), and the plasma sphere flattened, becoming nearly parallel to the substrate surface.
  • Material: 50.8 mm diameter, 4 mm thick N-type (100) silicon wafers.
  • Pre-treatment: Mechanical grinding for 30 min using a mixture of 5, 10, and 20 µm diamond powder, followed by 5 min grinding with 0.5 µm powder to create uniform nucleation sites.
  • Cleaning: Ultrasonic cleaning in acetone and alcohol (15 min each).

3. MPCVD Process Parameters (Optimal $h = 2$ mm)

Section titled “3. MPCVD Process Parameters (Optimal $h = 2$ mm)”
PhasePower (kW)Pressure (kPa)Gas Composition (sccm)Temperature (°C)
Nucleation4.721H2: 500, CH4: 35880
Growth4.7-4.921-22H2: 500, CH4: 25, O2: 5870-880
  • Plasma Diagnostics: Optical Emission Spectroscopy (OES) was used to monitor the relative concentrations of key growth species (C2, CH, Hα, Hβ) and estimate electron temperature (Te).
  • Structural Quality: X-ray Diffraction (XRD) confirmed the preferred (220) orientation, and Raman spectroscopy measured crystalline quality and uniformity (FWHM).
  • Optical Performance: UV-VIS-NIR and Fourier Transform Infrared (FTIR) spectroscopy measured transmittance across the 200 nm to 20 µm range.

The production of large-area, thick, uniform optical grade diamond films enables several high-demand engineering applications, leveraging diamond’s unique combination of optical transparency, high thermal conductivity, and mechanical strength.

  • High-Power Laser Optics:
    • Application: Output windows and beam splitters for high-power CO2 lasers and other industrial/military laser systems.
    • Benefit: Diamond’s high thermal conductivity and low absorption minimize thermal lensing and damage under extreme power loads.
  • Fusion Energy Research (ITER):
    • Application: Microwave windows (e.g., gyrotron windows) for electron cyclotron resonance heating (ECRH).
    • Benefit: Low microwave loss (low tan δ) and high thermal stability are critical for transmitting high-frequency, high-power microwave energy into the plasma confinement vessel.
  • Infrared and Multispectral Windows:
    • Application: Protective windows and domes for aerospace, defense, and harsh industrial environments.
    • Benefit: Broad transparency from visible light through the far infrared (including the 10.6 µm CO2 laser wavelength).
  • High-Frequency/High-Power RF Devices:
    • Application: Heat spreaders and substrates for high-power radio frequency (RF) electronics and microwave components where thermal management is paramount.
View Original Abstract

1,2 ,李成明 1 (1.北京科技大学 新材料技术研究院,北京 100083;2.北京科技大学 顺德研究生院,佛山 528399;3.北方工 业大学 机械与材料工程学院,北京 100144) 摘 要: 大尺寸光学级金刚石膜的均匀生长一直是微波化学气相沉积(Microwave plasma chemical vapor deposition, MPCVD)金刚石研究领域的热点和难点之一,沉积台的结构与位置对于金刚石膜均匀性以及厚膜生长的长期稳定 性至关重要。本研究通过 COMSOL 模拟结合实验研究了沉积台高度对衬底表面电场均匀性、等离子体状态和温度 均匀性的影响规律,优化了光学级金刚石膜均匀生长的工艺参数,在最佳的沉积台(高度 2 mm)下沉积得到的 2 英 寸金刚石膜(最大厚度 337 μm),厚度不均匀性<11%,从膜中心到边缘的拉曼半峰全宽为 3~4 cm -1 ,可见光波段内 最高透过率为 69%~70%,10.6 μm 处红外透过率为 70%。结果表明:金刚石膜的厚度和品质较为均匀,实现了两