WO2024210130A1 - 合成単結晶ダイヤモンド、合成単結晶ダイヤモンドの製造方法およびダイヤモンド基板 - Google Patents

合成単結晶ダイヤモンド、合成単結晶ダイヤモンドの製造方法およびダイヤモンド基板 Download PDF

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WO2024210130A1
WO2024210130A1 PCT/JP2024/013624 JP2024013624W WO2024210130A1 WO 2024210130 A1 WO2024210130 A1 WO 2024210130A1 JP 2024013624 W JP2024013624 W JP 2024013624W WO 2024210130 A1 WO2024210130 A1 WO 2024210130A1
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Prior art keywords
single crystal
diamond
synthetic single
ppm
crystal diamond
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English (en)
French (fr)
Japanese (ja)
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均 角谷
亦康 左
三記 寺本
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Priority to EP24784914.4A priority Critical patent/EP4692428A1/en
Priority to CN202480022293.5A priority patent/CN121002232A/zh
Priority to JP2025513147A priority patent/JPWO2024210130A1/ja
Publication of WO2024210130A1 publication Critical patent/WO2024210130A1/ja
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond

Definitions

  • This disclosure relates to synthetic single crystal diamond, a method for producing synthetic single crystal diamond, and a diamond substrate.
  • This application claims priority to Japanese Patent Application No. 2023-060359, filed on April 3, 2023. All contents of said Japanese Patent Application are incorporated herein by reference.
  • Single crystal diamond is used as the material for the substrate used in producing semiconducting diamond.
  • a substrate made of single crystal diamond will also be referred to as a "diamond substrate.”
  • a diamond substrate used in producing semiconducting diamond a high-purity, highly crystalline diamond substrate with few structural defects such as distortion and dislocations is suitable.
  • Patent Document 1 JP Patent Publication No. 2004-3314466
  • high-purity, highly crystalline type IIa diamond synthesized under high temperature and pressure is used as a substrate for producing semiconducting single crystal diamond.
  • the synthetic single crystal diamond of the present disclosure is A synthetic single crystal diamond having a nitrogen content of 10 ppm or less based on the atomic number of atoms and a boron content of 0.001 ppm or more and 3 ppm or less based on the atomic number of atoms,
  • the synthetic single crystal diamond has an insulation resistance of 1 M ⁇ or more.
  • FIG. 1 is a schematic cross-sectional view showing an example of a sample chamber configuration for use in producing synthetic single crystal diamond according to one embodiment of the present disclosure.
  • FIG. 2 is a diagram showing an example of an infrared absorption spectrum showing that there is no absorption peak in the wave number range of 2790 cm ⁇ 1 or more and 2810 cm ⁇ 1 or less.
  • the present disclosure therefore aims to provide a synthetic single crystal diamond that has high insulation resistance.
  • the synthetic single crystal diamond of the present disclosure is A synthetic single crystal diamond having a nitrogen content of 10 ppm or less based on the atomic number of atoms and a boron content of 0.001 ppm or more and 3 ppm or less based on the atomic number of atoms,
  • the synthetic single crystal diamond has an insulation resistance of 1 M ⁇ or more.
  • This disclosure makes it possible to provide synthetic single crystal diamond with high insulation resistance.
  • the boron content of the synthetic single crystal diamond based on the atomic number may be 0.01 ppm or more and 3 ppm or less. This makes it possible to synthesize a single crystal diamond with a low nitrogen content and few inclusions containing nitrogen getters, thereby making it possible to obtain a high-quality synthetic single crystal diamond.
  • the synthetic single crystal diamond may have no absorption peak in the wave number range of 2790 cm ⁇ 1 to 2810 cm ⁇ 1 in an infrared absorption spectrum measured by Fourier transform infrared spectroscopy, thereby further increasing the insulation resistance of the synthetic single crystal diamond.
  • the method for producing a synthetic single crystal diamond of the present disclosure is a method for producing a synthetic single crystal diamond according to any one of (1) to (3) above, A first step of synthesizing a diamond single crystal having a nitrogen content of 10 ppm or less based on the atomic number and a boron content of 0.001 ppm or more and 3 ppm or less based on the atomic number by a temperature difference method using a solvent metal; A second step of irradiating the diamond single crystal with one or both of an electron beam and a particle beam having an energy of 1 MGy or more and less than 10 MGy to obtain the synthetic single crystal diamond.
  • the diamond single crystal may be irradiated with the electron beam under conditions of an energy of 1.0 MeV to 10 MeV and a dose of 1.0 x 10 e/ m2 to 1.0 x 10 e/ m2 , thereby providing the diamond single crystal with energy of 1 MGy to less than 10 MGy.
  • the diamond substrate of the present disclosure is a diamond substrate made of a synthetic single crystal diamond as described in any one of (1) to (3) above.
  • the diamond substrate of the present disclosure is suitable as a substrate for producing semiconductor diamond.
  • a ⁇ B means the upper and lower limits of a range (i.e., greater than or equal to A and less than or equal to B). If no unit is stated for A and only a unit is stated for B, the units of A and B are the same.
  • any one numerical value listed as the lower limit and any one numerical value listed as the upper limit is also considered to be disclosed.
  • a1 or more, b1 or more, and c1 or more are listed as the lower limit and a2 or less, b2 or less, and c2 or less are listed as the upper limit, a1 or more and a2 or less, a1 or more and b2 or less, a1 or more and c2 or less, b1 or more and a2 or less, b1 or more and b2 or less, b1 or more and c2 or less, c1 or more and a2 or less, c1 or more and b2 or less, and c1 or more and c2 or less are considered to be disclosed.
  • a synthetic single crystal diamond according to one embodiment of the present disclosure (hereinafter also referred to as “embodiment 1”) is A synthetic single crystal diamond having a nitrogen content based on the number of atoms (hereinafter also referred to as “nitrogen content”) of 10 ppm or less and a boron content based on the number of atoms (hereinafter also referred to as "boron content”) of 0.001 ppm or more and 3 ppm or less,
  • the synthetic single crystal diamond has an insulation resistance of 1 M ⁇ or more.
  • the synthetic single crystal diamond of embodiment 1 can have high insulation resistance. Furthermore, the synthetic single crystal diamond of embodiment 1 has a nitrogen content based on atomic number of 10 ppm or less and a boron content based on atomic number of 0.001 ppm or more and 3 ppm or less, has few structural defects such as distortion and dislocation, and is high purity and highly crystalline. In this disclosure, high purity means that the nitrogen content based on atomic number is 10 ppm or less and the boron content based on atomic number is 0.001 ppm or more and 3 ppm or less. Therefore, the synthetic single crystal diamond of embodiment 1 is suitable for use as a substrate material or heat sink used in producing semiconductor diamond.
  • the nitrogen content of the synthetic single crystal diamond of embodiment 1 is 10 ppm or less. According to this, synthetic single crystal diamond has few structural defects such as distortion and dislocation, and is likely to be high purity and high crystallinity. It also tends to have high insulation resistance.
  • the upper limit of the nitrogen content of synthetic single crystal diamond is 10 ppm or less, may be 5 ppm or less, 1 ppm or less, 0.8 ppm or less, 0.05 ppm or less, 0.04 ppm or less, 0.03 ppm or less, or 0.02 ppm or less.
  • the lower limit of the nitrogen content of synthetic single crystal diamond is not particularly limited, and may be 0 ppm or more, or 0.008 ppm or more.
  • the nitrogen content of the synthetic single crystal diamond may be 0 ppm or more and 10 ppm or less, 0.008 ppm or more and 10 ppm or less, 0 ppm or more and 0.8 ppm or less, or 0.008 ppm or more and 0.8 ppm or less.
  • the nitrogen content of the synthetic single crystal diamond is measured by secondary ion mass spectrometry (SIMS) using a CAMECA "IMS-7f" (trademark) measuring device and 15.0 keV Cs + ions as the primary ion beam.
  • SIMS secondary ion mass spectrometry
  • the boron content of the synthetic single crystal diamond of embodiment 1 based on the atomic number is 0.001 ppm or more and 3 ppm or less. According to this, synthetic single crystal diamond has few structural defects such as distortion and dislocation, and tends to be high purity and high crystallinity. It also tends to have high insulation resistance.
  • the upper limit of the boron content of synthetic single crystal diamond is 3 ppm or less, may be 2.3 ppm or less, may be 1.5 ppm or less, may be 0.5 ppm or less, may be 0.21 ppm or less, may be 0.19 ppm or less, or may be 0.11 ppm or less.
  • the lower limit of the boron content of synthetic single crystal diamond is 0.001 ppm or more, may be 0.01 ppm or more, or may be 0.05 ppm or more.
  • the boron content of the synthetic single crystal diamond is from 0.001 ppm to 3 ppm, optionally from 0.001 ppm to 2.3 ppm, optionally from 0.001 ppm to 1.5 ppm, optionally from 0.01 ppm to 3 ppm, optionally from 0.01 ppm to 2.3 ppm.
  • the boron content of synthetic single crystal diamond is measured by secondary ion mass spectrometry (SIMS).
  • SIMS secondary ion mass spectrometry
  • the synthetic single crystal diamond of embodiment 1 may contain impurities other than nitrogen and boron.
  • impurities include hydrogen.
  • the total content of impurities other than nitrogen and boron in the synthetic single crystal diamond of embodiment 1 based on the atomic number may be 10 ppm or less.
  • the insulation resistance of the synthetic single crystal diamond of embodiment 1 is 1 M ⁇ or more.
  • a synthetic single crystal diamond having an insulation resistance of 1 M ⁇ or more means that the synthetic single crystal diamond has high insulation resistance.
  • the insulation resistance of synthetic single crystal diamond is measured by the two-terminal measurement method, for example, using a Sanwa Electric Instruments analog insulation resistance meter PDM509S.
  • the size of the measurement sample can be set appropriately depending on the size of the synthetic single crystal diamond.
  • the measurement sample can be prepared by processing synthetic single crystal diamond into a plate of 5 mm square and 1 mm thick. Measurements are performed at room temperature (20°C ⁇ 2°C).
  • the absorption peak in the wave number range of 2790 cm -1 to 2810 cm -1 is derived from isolated substitutional boron atoms having a positive (+) charge.
  • the synthetic single crystal diamond having a positive (+) charge becomes a P-type semiconductor and generates electrical conductivity.
  • the synthetic single crystal diamond having no absorption peak in the wave number range of 2790 cm -1 to 2810 cm -1 does not generate electrical conductivity derived from isolated substitutional boron atoms having a positive (+) charge, so that the insulation resistance is further increased.
  • the absence of an absorption peak in the wave number range of 2790 cm -1 to 2810 cm -1 in the infrared absorption spectrum means that no absorption other than the inherent absorption spectrum of diamond is observed in the spectrum in the wave number range. This means that no maximum value is present in the infrared absorption spectrum in the wave number range of 2790 cm -1 to 2810 cm -1 in the macroscopic view.
  • the inherent absorption spectrum of diamond in the wave number range of 2790 cm -1 to 2810 cm -1 corresponds to the infrared absorption spectrum shown in FIG. 2, for example.
  • the horizontal axis indicates the wave number (cm -1 )
  • the vertical axis indicates the intensity.
  • the infrared absorption spectrum of synthetic single crystal diamond is obtained by measurement using Fourier transform infrared spectroscopy at a temperature of 23°C ⁇ 2°C.
  • the measurement procedure is as follows.
  • the synthetic single crystal diamond sample to be measured is processed into a plate with a thickness of approximately 1 mm, and the two light-transmitting surfaces are polished with a metal-bonded grinding wheel so that the surface roughness Ra is 20 nm or less.
  • the polished surfaces are irradiated with infrared light to create an infrared absorption spectrum.
  • the measurement is performed at a temperature of 23°C ⁇ 2°C (21°C or higher and 25°C or lower).
  • the temperature change of the measuring equipment and sample during the measurement is kept to within ⁇ 1°C.
  • Embodiment 2 Method for producing synthetic single crystal diamond
  • a method for producing a synthetic single crystal diamond according to one embodiment of the present disclosure (hereinafter also referred to as "embodiment 2") is the method for producing a synthetic single crystal diamond according to embodiment 1, A first step of synthesizing a diamond single crystal having a nitrogen content of 10 ppm or less based on the atomic number and a boron content of 0.001 ppm or more and 3 ppm or less based on the atomic number by a temperature difference method using a solvent metal; A second step of irradiating the diamond single crystal with one or both of an electron beam and a particle beam having an energy of 1 MGy or more and less than 10 MGy to obtain a synthetic single crystal diamond.
  • a diamond single crystal is synthesized by a temperature difference method using a solvent metal, the nitrogen content based on the atomic number being 10 ppm or less, and the boron content based on the atomic number being 0.001 ppm or more and 3 ppm or less.
  • a diamond single crystal can be produced by the temperature difference method using a sample chamber having the configuration shown in Figure 1.
  • a sample chamber 10 used for manufacturing a diamond single crystal 1 an insulator 2, a carbon source 3, a solvent metal 4, and a seed crystal 5 are arranged in a space surrounded by a graphite heater 7, and a pressure medium 6 is arranged outside the graphite heater 7.
  • the temperature difference method is a synthesis method in which a vertical temperature gradient is provided inside the sample chamber 10, a carbon source 3 is arranged in a high temperature section (T high ), a diamond seed crystal 5 is arranged in a low temperature section (T low ), a solvent metal 4 is arranged between the carbon source 3 and the seed crystal 5, and the diamond single crystal 1 is grown on the seed crystal 5 under conditions maintained at a temperature at which the solvent metal 4 melts and at a pressure at which diamond becomes thermally stable.
  • the pressure in the sample chamber is controlled to 5.0 to 6.0 GPa
  • the temperature of the high temperature section of the solvent metal is controlled to 1400°C to 1500°C
  • the temperature of the low temperature section is controlled to 1360°C to 1380°C, and maintained for 50 to 200 hours to grow a diamond single crystal on the seed crystal.
  • diamond powder As the solvent metal 4, one or more metals selected from iron (Fe), cobalt (Co), nickel (Ni), manganese (Mn), etc., or an alloy containing these metals can be used.
  • the carbon source 3 may contain boron (B) as an impurity.
  • Affordable and easily available carbon sources (diamond powder) contain more than several tens of ppm of boron as an impurity.
  • Diamond single crystals synthesized using such carbon sources contain boron as an impurity, and therefore are conductive, and therefore cannot be used as a substrate material used in producing semiconductor diamond. According to the manufacturing method of the second embodiment, by performing the second step described below on the diamond single crystal, even a synthetic single crystal diamond containing boron as an impurity has high insulation resistance and can be used as a substrate material used in producing semiconductor diamond.
  • the solvent metal 4 may further contain one or more elements selected from the group consisting of titanium (Ti), vanadium (V), chromium (Cr), copper (Cu), zirconium (Zr), niobium (Nb), molybdenum (Mo), ruthenium (Ru), rhodium (Rh), hafnium (Hf), tantalum (Ta), tungsten (W), osmium (Os), iridium (Ir) and platinum (Pt).
  • the solvent metal 4 may contain boron (B) as an impurity.
  • the diamond single crystal obtained in the first step is irradiated with either or both of an electron beam and a particle beam imparting an energy of 1 MGy or more and less than 10 MGy to obtain a synthetic single crystal diamond.
  • the inventors have newly discovered that by irradiating the diamond single crystal obtained in the first step with either or both of an electron beam and a particle beam that imparts an energy of 1 MGy or more and less than 10 MGy (hereinafter also referred to as "irradiation with electron beam, etc.”), the resulting synthetic single crystal diamond has high insulation resistance.
  • the amount of energy applied is less than 1 MGy, the formation of the vacancy (V) complex may be insufficient.
  • the amount of energy applied is 10 MGy or more, there is a risk that excess vacancies will be generated, resulting in a decrease in crystallinity. Therefore, an energy amount of 1 MGy or more and less than 10 MGy is preferable.
  • a neutron beam or a proton beam can be used as the particle beam.
  • the irradiation conditions are not particularly limited as long as the diamond single crystal can be given an energy of 1 MGy or more and less than 10 MGy.
  • the irradiation conditions may be conditions that can give the diamond single crystal an energy of 1 MGy or more and 5 MGy or less.
  • the diamond single crystal obtained in the first step may be processed to a thickness of 0.1 mm or more and 10 mm or less, for example, in the case of a 10 mm square size.
  • the electron beam irradiation conditions can be, for example, the electron beam energy of 1.0 MeV or more and 10 MeV or less, and the dose amount of 1.0 x 1019 e/m2 or more and 1.0 x 1021 e/m2 or less.
  • the range irradiated by the electron beam is larger than the surface (area) of the diamond single crystal irradiated by the electron beam.
  • a diamond substrate according to one embodiment of the present disclosure (hereinafter also referred to as “embodiment 3") is a diamond substrate made of the synthetic single crystal diamond described in embodiment 1.
  • the diamond substrate of embodiment 1 has high insulation resistance and is therefore suitable as a substrate for producing semiconducting diamond.
  • the temperature inside the sample chamber was adjusted with a heater so that there was a temperature difference of several tens of degrees between the high-temperature section where the carbon source was placed and the low-temperature section where the seed crystal was placed.
  • the pressure was controlled to 5.5 GPa and the temperature of the low-temperature section was kept in the range of 1370°C ⁇ 10°C (1360°C to 1380°C) for 60 hours, and a diamond single crystal was synthesized on the seed crystal.
  • the obtained diamond single crystal is irradiated with an electron beam that gives an energy of 5 MGy or 1 MGy, and each sample of synthetic single crystal diamond is obtained.
  • the conditions of electron beam irradiation are that when the energy of 5 MGy is given, the energy of electron beam is 2 MeV and the dose is 2 x 1020 e/m2.
  • the energy of 1 MGy is given, the energy of electron beam is 2 MeV and the dose is 4 x 1019 e/ m2 .
  • the size of the diamond single crystal is about 5 mm in the diameter of the inscribed circle of the main surface.
  • Table 1 the sample that is written as "None" in the "electron beam irradiation" column of "second step” is not irradiated with electron beam.
  • the nitrogen content and boron content of the synthetic single crystal diamond of each sample are measured by SIMS.
  • the specific measurement conditions are as described in embodiment 1.
  • the nitrogen content and boron content of the synthetic single crystal diamond are confirmed to be the same as the nitrogen content and boron content of the diamond single crystal described in table 1.
  • the nitrogen and boron content of the synthetic single crystal diamond of each sample are measured by SIMS, and the impurity content other than boron is confirmed to be 10 ppm or less in all samples.
  • Samples 2, 4, 6, 8, 10, 12 to 14, and 16 are examples. Although these synthetic single crystal diamonds have different boron contents, they were all confirmed to have high insulation resistance.
  • Samples 1, 3, 5, 7, 9, 11 and 15 are comparative examples. In these samples, nitrogen and boron are unevenly dispersed in the diamond crystal, and it is presumed that the synthetic single crystal diamond contains areas where the positive (+) charge of isolated substitutional boron atoms is present, resulting in electrical conductivity.

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PCT/JP2024/013624 2023-04-03 2024-04-02 合成単結晶ダイヤモンド、合成単結晶ダイヤモンドの製造方法およびダイヤモンド基板 Ceased WO2024210130A1 (ja)

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EP24784914.4A EP4692428A1 (en) 2023-04-03 2024-04-02 Synthetic single crystal diamond, method for producing synthetic single crystal diamond, and diamond substrate
CN202480022293.5A CN121002232A (zh) 2023-04-03 2024-04-02 合成单晶金刚石、合成单晶金刚石的制造方法以及金刚石衬底
JP2025513147A JPWO2024210130A1 (https=) 2023-04-03 2024-04-02

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0558786A (ja) * 1991-08-29 1993-03-09 Sumitomo Electric Ind Ltd ダイヤモンドの合成方法
JP2004331446A (ja) 2003-05-07 2004-11-25 Sumitomo Electric Ind Ltd 低抵抗ｎ型半導体ダイヤモンド
WO2022210934A1 (ja) * 2021-03-31 2022-10-06 住友電気工業株式会社 単結晶ダイヤモンド及びその製造方法
WO2022210936A1 (ja) * 2021-03-31 2022-10-06 住友電気工業株式会社 単結晶ダイヤモンド及びその製造方法
JP2023060359A (ja) 2018-03-30 2023-04-27 株式会社タムロン ズームレンズ及び撮像装置

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0558786A (ja) * 1991-08-29 1993-03-09 Sumitomo Electric Ind Ltd ダイヤモンドの合成方法
JP2004331446A (ja) 2003-05-07 2004-11-25 Sumitomo Electric Ind Ltd 低抵抗ｎ型半導体ダイヤモンド
JP2023060359A (ja) 2018-03-30 2023-04-27 株式会社タムロン ズームレンズ及び撮像装置
WO2022210934A1 (ja) * 2021-03-31 2022-10-06 住友電気工業株式会社 単結晶ダイヤモンド及びその製造方法
WO2022210936A1 (ja) * 2021-03-31 2022-10-06 住友電気工業株式会社 単結晶ダイヤモンド及びその製造方法

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