CN111074345A - Preparation device and preparation method of large-particle diamond - Google Patents
Preparation device and preparation method of large-particle diamond Download PDFInfo
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- CN111074345A CN111074345A CN202010033316.6A CN202010033316A CN111074345A CN 111074345 A CN111074345 A CN 111074345A CN 202010033316 A CN202010033316 A CN 202010033316A CN 111074345 A CN111074345 A CN 111074345A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 74
- 239000010432 diamond Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002245 particle Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 52
- 239000013078 crystal Substances 0.000 claims description 44
- 238000001816 cooling Methods 0.000 claims description 17
- 239000002826 coolant Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000008602 contraction Effects 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 240000002836 Ipomoea tricolor Species 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000001276 controlling effect Effects 0.000 description 18
- 230000001105 regulatory effect Effects 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Classifications
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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
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/10—Heating of the reaction chamber or the substrate
- C30B25/105—Heating of the reaction chamber or the substrate by irradiation or electric discharge
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/12—Substrate holders or susceptors
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of diamond preparation, in particular to a preparation device of large-particle diamond and a preparation method thereof, the preparation device of the large-particle diamond comprises a growth chamber, a sample holder and a microwave unit, wherein the sample holder is arranged in the growth chamber, the microwave unit is connected with the growth chamber, the preparation device also comprises a process gas unit and a rotation adjusting unit, the process gas unit is communicated with the growth chamber, the rotation adjusting unit is connected with the sample holder, the sample holder is provided with a groove for placing a diamond sample, and the inner side of the groove is in an arc surface shape; the preparation method has the advantages of simple process and high preparation efficiency, and the prepared large-particle diamond has good quality and meets the requirement of industrialized production.
Description
Technical Field
The invention relates to the technical field of diamond preparation, in particular to a preparation device and a preparation method of large-particle diamond.
Background
The single crystal diamond has excellent physical and chemical properties, has important application value in the fields of machinery, electronics, jewelry and the like, and needs to be prepared into large-particle diamond in order to expand the application.
Among various diamond preparation methods, the microwave plasma chemical vapor deposition method is the preferred method for preparing high-quality diamond due to the characteristics of high plasma power density, no electrode discharge pollution, stable performance and the like, in the process of producing large-particle monocrystalline diamond by the current method, the diamond seed crystal is generally fixed on a deposition table, the temperature of the seed crystal is controlled by cooling the deposition table, unidirectional growth is carried out on the side of the seed crystal facing to plasma, polycrystalline or amorphous carbonization is often caused at the edge due to the difference of growth environments of the side edge and the center of the crystal, dislocation is more and more spread to the growth surface, the growth surface of the single crystal is smaller and smaller, the crystal needs to be repeatedly cleaned and cut and then grows again or grows in a splicing manner, and the production efficiency and the product quality are seriously influenced.
In view of the above technical problems, there is a need for a new diamond manufacturing apparatus and a new diamond manufacturing method to better solve the above technical problems.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation device and a preparation method of large-particle diamond, and the preparation device provided by the invention has the advantages of simple structure, reasonable design and convenience for preparing large-particle diamond; the preparation method provided by the invention has simple process, can effectively control the temperature in the growth process of the diamond seed crystal, and the prepared diamond product has high quality.
The technical scheme adopted by the invention is as follows:
the utility model provides a preparation facilities of large granule diamond, holds in the palm and the microwave unit including growth cavity, sample, and the sample holds in the palm the dress and locates in the growth cavity, and the microwave unit is connected with the growth cavity, still includes process gas unit and rotation regulation unit, and process gas unit and growth cavity intercommunication, rotation regulation unit hold in the palm with the sample and are connected.
Further, the sample support is provided with a groove for placing a diamond sample, and the inner side of the groove is designed into an arc surface shape.
Further, the device also comprises a cooling device, wherein the cooling device is positioned below the sample support and is cooled by introducing a cooling medium, and the cooling device is provided with a cooling medium inlet and a cooling medium outlet.
Further, the device also comprises a heating device, and the heating device is connected with the sample holder.
Furthermore, the inner side of the groove is of a hemispherical cambered surface type.
Furthermore, the inner side of the groove is designed into a flying saucer-shaped cambered surface type.
Furthermore, the edge of the groove is inwards shrunk to form a limiting table.
Furthermore, the growth chamber is provided with a gas inlet for introducing process gas and a gas outlet for introducing the process gas, and the gas inlet is connected with the process gas unit.
The method for preparing the large-particle diamond by adopting the preparation device of the large-particle diamond comprises the following steps:
the method comprises the following steps: placing the spherical diamond seed crystals in the grooves, and adjusting the sample holder to rotate at variable speed through the rotation adjusting unit to enable the spherical diamond seed crystals to roll along with the sample holder in three dimensions in the grooves;
step two: coating the plasma generated by the microwave unit above the diamond seed crystal;
step three: controlling the growth temperature and pressure of the crystal to obtain the large-particle diamond.
Further, in the third step, the growth temperature of the crystal is controlled by controlling the power of the microwave unit and by controlling the temperature of the gas inlet of the process gas unit, and the cavity pressure in the growth chamber is adjusted by controlling the gas inlet and outlet of the process gas unit.
The invention has the following beneficial effects:
1. the invention comprises a growth chamber, a sample holder and a microwave unit, wherein the sample holder is arranged in the growth chamber, the microwave unit is connected with the growth chamber, the invention also comprises a process gas unit and a rotation regulating unit, the process gas unit is communicated with the growth chamber, the rotation regulating unit is connected with the sample holder, the invention has simple structure and reasonable design, the rotation regulating unit is used for regulating the variable-speed rotation of the sample holder, the spherical diamond seed crystal is driven by the rotation regulating unit to roll in a groove of the sample holder in a controlled manner, the growth temperature of the crystal is controlled by controlling the power of the microwave unit and controlling the temperature of the gas inlet of the process gas unit, the cavity pressure in the growth chamber is regulated by controlling the gas inlet and outlet of the process gas unit, so that the diamond seed crystal can obtain equal growth opportunities and growth conditions in all directions, and the diamond crystal can grow uniformly in three-dimensional directions, thereby reducing the internal stress, avoiding the crack caused by the stress in the growth process, continuously growing for a long time and preparing the high-quality large-particle diamond.
2. The preparation method has simple process, meets the industrial production requirement, simultaneously controls the growth temperature of the diamond seed crystal accurately in the preparation process, and has high preparation efficiency and good quality of the prepared large-particle diamond.
Drawings
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention;
description of reference numerals: 1. the device comprises a spherical diamond seed crystal, 2. a sample holder, 3. a rotary adjusting unit, 4. a growth chamber, 5. a cooling medium inlet, 6. a cooling medium outlet, 7. a microwave unit, 8. an air inlet and 9. an air outlet.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, the device for preparing large-particle diamond of this embodiment includes a growth chamber 4, a sample holder 2 and a microwave unit 7, the sample holder 2 is installed in the growth chamber 4, the microwave unit 7 is connected with the growth chamber 4, the device further includes a process gas unit and a rotation adjusting unit 3, the process gas unit is communicated with the growth chamber 4, the rotation adjusting unit 3 is connected with the sample holder 2, the invention has simple structure and reasonable design, the rotation adjusting unit 3 adjusts the variable-speed rotation of the sample holder 2, the spherical diamond seed crystal 1 is controlled to roll in the sample holder 2 under the driving of the rotation adjusting unit 3, the growth temperature of the crystal is controlled by controlling the power of the microwave unit 7 and the temperature of the inlet gas of the process gas unit, the cavity pressure in the growth chamber 4 is adjusted by controlling the inlet gas amount and the outlet gas amount of the process gas unit, the invention can continuously grow for a long time to prepare high-quality large-particle diamond, as a preferred embodiment, on the basis of the embodiment, a groove for placing a diamond sample can be arranged on a sample holder 2, and the inner side of the groove is designed into a cambered surface type, so that the arrangement is more beneficial to the controlled rolling of the spherical diamond seed crystal, thereby further ensuring that each point on the surface of the diamond spherical seed crystal has equal chance of facing the plasma, and reducing the growth environment difference between the growth surface of the diamond crystal and the side edge, and preparing the high-quality diamond.
In some embodiments, the diamond crystal growth device further comprises a cooling device, the cooling device is located below the sample holder 2, the cooling device is provided with a cooling medium inlet 5 and a cooling medium outlet 6, specifically, the cooling device in this embodiment is located at the bottom of the sample holder 2, in this embodiment, the sample holder 2 can be subjected to cooling control by controlling the entering amount of the cooling medium of the cooling device and the temperature of the cooling medium, and the temperature of the growth chamber 4 is controlled by matching with the microwave unit 7 and the process gas unit, so that more accurate temperature control can be realized, thereby effectively ensuring the balance of the growth conditions of the diamond crystal of the invention and preparing the high-quality large-particle diamond.
In some embodiments, the apparatus further comprises a heating device, the heating device is connected with the sample holder 2, specifically, the heating device in this embodiment is arranged at the bottom of the sample holder 2, the heating device in this embodiment can control the heating of the sample holder 2, and the temperature of the growth chamber 4 can be controlled by cooperating with the microwave unit 7, the process gas unit and the cooling device, so as to realize more precise temperature control, thereby effectively ensuring the balance of the growth conditions of the diamond crystal of the present invention, and preparing high-quality large-particle diamond, specifically, for the heating device in this embodiment, the cooling device can be arranged at the middle position of the bottom of the sample holder 2 in cooperation with the arrangement of the cooling device in the above embodiments, and the heating device is arranged at the periphery of the sample holder 2, so as to be more beneficial to cooling the region with relatively more heated middle of the sample holder 2, the place where the edge of the sample support 2 is heated less is heated by the heating device to supplement heat, thereby further reducing the difference of the growth environment of the growth surface and the side edge of the diamond crystal and preparing the high-quality diamond.
In some optional embodiments, the inner side of the groove is a hemispherical cambered surface or a flying saucer-shaped cambered surface, and a limiting table is formed at the edge of the groove by inward contraction, in this embodiment, the inner side of the groove is a hemispherical or flying saucer-shaped groove, which is mainly used for facilitating the rolling of the spherical diamond seed crystal, and the belt is formed by inward contraction at the edge of the groove and is mainly used for preventing the spherical diamond seed crystal 1 from flying away from the sample holder 2 when the rotating speed is too high.
In other specific examples, the growth chamber 4 is provided with a gas inlet 8 for introducing the process gas and a gas outlet 9 for introducing the process gas, and the process gas unit is connected with the gas inlet 8, specifically, in the present embodiment, flowmeters may be respectively disposed at the gas inlet 8 and the gas outlet 9 to adjust and control the gas amount.
The method for preparing the large-particle diamond by using the preparation device comprises the following steps:
the method comprises the following steps: placing the spherical diamond seed crystal 1 in the groove, and adjusting the sample holder 2 to rotate at variable speed through the rotation adjusting unit 3, so that the spherical diamond seed crystal 1 rolls along with the sample holder 2 in three dimensions in the groove;
step two: the plasma generated by the microwave unit 7 is coated above the diamond seed crystal;
step three: controlling the growth temperature and pressure of the crystal to obtain the large-particle diamond.
In the third step, the growth temperature of the crystal is controlled by controlling the power of the microwave unit 7 and by controlling the temperature of the gas inlet of the process gas unit, and the cavity pressure in the growth chamber 4 is adjusted by controlling the gas inlet and outlet of the process gas unit.
The preparation method of the invention has simple process, meets the requirement of industrialized preparation production, and in the process of preparing the large-particle diamond, the sample holder 2 is adjusted to rotate at variable speed by the rotation adjusting unit 3, the spherical diamond seed crystal 1 is driven by the rotation adjusting unit 3, controlled rolling in the groove of the sample holder 2, and controlling the growth temperature of the crystal by controlling the power of the microwave unit 7 and by controlling the inlet gas temperature of the process gas unit, the cavity pressure in the growth chamber 4 is adjusted by controlling the gas input and output of the process gas unit, so that the diamond seed crystal can obtain equal growth opportunities and growth conditions in all directions, the diamond crystal can grow in three-dimensional direction in a balanced way, thereby reducing the internal stress, avoiding the crack caused by the stress in the growth process, continuously growing for a long time and preparing the high-quality large-particle diamond.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The utility model provides a preparation facilities of large granule diamond, holds in the palm and the microwave unit including growth cavity, sample, and the sample holds in the palm the dress and locates in the growth cavity, and the microwave unit is connected with the growth cavity, its characterized in that still includes process gas unit and rotation regulation unit, and process gas unit and growth cavity intercommunication, rotation regulation unit hold in the palm with the sample and are connected.
2. The apparatus for preparing a large granular diamond according to claim 1, wherein the sample holder is provided with a groove for placing a diamond sample, and the inner side of the groove is formed in a cambered surface shape.
3. The apparatus according to claim 1, further comprising a cooling device disposed below the sample holder, wherein the cooling device is cooled by introducing a cooling medium, and the cooling device is provided with a cooling medium inlet and a cooling medium outlet.
4. The apparatus of claim 1, further comprising a heating device, wherein the heating device is connected to the sample holder.
5. The apparatus for preparing a large granular diamond according to claim 1, wherein the inside of the groove is formed in a hemispherical curved shape.
6. The apparatus for preparing a large granular diamond according to claim 1, wherein the inner side of the groove is formed in a shape of a flying saucer arc.
7. The apparatus of claim 1, wherein a stopper is formed at the edge of the groove by inward contraction.
8. The apparatus of claim 1, wherein the growth chamber is provided with a gas inlet for introducing a process gas and a gas outlet for introducing the process gas, and the gas inlet is connected to the process gas unit.
9. The method for preparing a large granular diamond according to any one of claims 1 to 8, comprising the steps of:
the method comprises the following steps: placing the spherical diamond seed crystals in the grooves, and adjusting the sample holder to rotate at variable speed through the rotation adjusting unit to enable the spherical diamond seed crystals to roll along with the sample holder in three dimensions in the grooves;
step two: coating the plasma generated by the microwave unit above the diamond seed crystal;
step three: controlling the growth temperature and pressure of the crystal to obtain the large-particle diamond.
10. The method for preparing a large granular diamond according to claim 9, wherein in the third step, the growth temperature of the crystal is controlled by controlling the power of the microwave unit and by controlling the temperature of the gas introduced into the process gas unit, and the chamber pressure in the growth chamber is adjusted by controlling the amount of the gas introduced into and discharged from the process gas unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010033316.6A CN111074345A (en) | 2020-01-13 | 2020-01-13 | Preparation device and preparation method of large-particle diamond |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010033316.6A CN111074345A (en) | 2020-01-13 | 2020-01-13 | Preparation device and preparation method of large-particle diamond |
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| CN111074345A true CN111074345A (en) | 2020-04-28 |
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| CN202010033316.6A Pending CN111074345A (en) | 2020-01-13 | 2020-01-13 | Preparation device and preparation method of large-particle diamond |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114059159A (en) * | 2021-11-18 | 2022-02-18 | 北京大学东莞光电研究院 | Diamond growth method |
| CN114318521A (en) * | 2021-12-28 | 2022-04-12 | 北京大学东莞光电研究院 | Diamond growth method |
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| US20090004093A1 (en) * | 2006-02-07 | 2009-01-01 | Nee Han H | Materials and methods for the manufacture of large crystal diamonds |
| CN207552442U (en) * | 2017-11-28 | 2018-06-29 | 中国科学院金属研究所 | A kind of large area HF CVD diamond film growth device |
| CN108531986A (en) * | 2017-03-06 | 2018-09-14 | 上海启发电子科技有限公司 | A kind of preparation method of bulky diamond |
| CN109735828A (en) * | 2019-03-15 | 2019-05-10 | 张家港市微纳新材料科技有限公司 | A kind of boron mixes the preparation system and method for cvd diamond single crystal grain |
| CN212128339U (en) * | 2020-01-13 | 2020-12-11 | 北京大学东莞光电研究院 | Preparation facilities of large granule diamond |
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2020
- 2020-01-13 CN CN202010033316.6A patent/CN111074345A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090004093A1 (en) * | 2006-02-07 | 2009-01-01 | Nee Han H | Materials and methods for the manufacture of large crystal diamonds |
| CN108531986A (en) * | 2017-03-06 | 2018-09-14 | 上海启发电子科技有限公司 | A kind of preparation method of bulky diamond |
| CN207552442U (en) * | 2017-11-28 | 2018-06-29 | 中国科学院金属研究所 | A kind of large area HF CVD diamond film growth device |
| CN109735828A (en) * | 2019-03-15 | 2019-05-10 | 张家港市微纳新材料科技有限公司 | A kind of boron mixes the preparation system and method for cvd diamond single crystal grain |
| CN212128339U (en) * | 2020-01-13 | 2020-12-11 | 北京大学东莞光电研究院 | Preparation facilities of large granule diamond |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114059159A (en) * | 2021-11-18 | 2022-02-18 | 北京大学东莞光电研究院 | Diamond growth method |
| CN114318521A (en) * | 2021-12-28 | 2022-04-12 | 北京大学东莞光电研究院 | Diamond growth method |
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