CN108251892B - Device and method for preparing single crystal diamond by laser-enhanced plasma CVD - Google Patents
Device and method for preparing single crystal diamond by laser-enhanced plasma CVD Download PDFInfo
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- CN108251892B CN108251892B CN201810159834.5A CN201810159834A CN108251892B CN 108251892 B CN108251892 B CN 108251892B CN 201810159834 A CN201810159834 A CN 201810159834A CN 108251892 B CN108251892 B CN 108251892B
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
- C23C16/483—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using coherent light, UV to IR, e.g. lasers
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
Abstract
The invention discloses a device and a method for preparing single crystal diamond by laser-enhanced plasma CVD, wherein the device comprises plasma CVD equipment and laser equipment; more than 1 laser device is respectively positioned outside the cylindrical cavity of the plasma CVD device, and laser emitted by the laser device can irradiate the substrate table positioned in the cavity of the plasma CVD device; the substrate table is positioned in the middle of the cavity of the plasma CVD equipment, and a cooling water circulating system is arranged at the lower part of the substrate table and comprises a cooling water inlet and a cooling water outlet; and a raw material air inlet and an air extraction opening are formed in the bottom of the cavity of the plasma CVD equipment. The method combines microwave energy (or electric energy) and laser energy, utilizes low-cost high-energy laser to improve the energy of plasma and the gas dissociation rate in the diamond synthesis process, thereby improving the synthesis rate of the diamond, and effectively solves the problem of high-speed batch preparation of the diamond.
Description
Technical Field
The invention belongs to the technical field of diamond processing, and particularly relates to a device and a method for preparing single crystal diamond by laser-enhanced plasma CVD.
Background
The synthesis rate of the single crystal diamond synthesized by the common plasma CVD (chemical vapor deposition) equipment is low, the yield is low, if the rate needs to be improved, a microwave source with higher power is needed to improve, so the cost and the energy consumption are greatly increased, the cost of the equipment is increased, and the high-speed batch preparation of the diamond is also limited.
In the prior art, a microwave (or direct current, hot wire) plasma chemical vapor deposition technology is adopted to synthesize the single crystal diamond, and the single microwave (or electric energy) energy cannot obtain high-density plasma and high gas dissociation rate, so that the growth rate of the single crystal diamond is low, the product efficiency is low, the cost is high, and the large-scale application of the single crystal diamond is hindered.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a device and a method for preparing single crystal diamond by laser-enhanced plasma CVD, the technology combines microwave energy (or electric energy) and laser energy, and utilizes low-cost high-energy laser to improve the energy of plasma and the gas dissociation rate in the diamond synthesis process, thereby improving the synthesis rate of diamond.
Therefore, the invention adopts the following technical scheme:
a device for preparing single crystal diamond by laser enhanced plasma CVD comprises a plasma CVD device and a laser device; more than 1 laser device is respectively positioned outside the cylindrical cavity of the plasma CVD device, and laser emitted by the laser device can irradiate the substrate table positioned in the cavity of the plasma CVD device; the substrate table is positioned in the middle of the cavity of the plasma CVD equipment, and a cooling water circulating system is arranged at the lower part of the substrate table and comprises a cooling water inlet and a cooling water outlet; and a raw material air inlet and an air extraction opening are formed in the bottom of the cavity of the plasma CVD equipment.
Further, the plasma CVD apparatus is one of hot-wire CVD, microwave CVD, direct-current CVD, and the like.
Further, the cavity of the plasma CVD equipment is sealed, and can be vacuumized or aerated.
Furthermore, the raw material air inlets are uniformly distributed around the substrate table, the size is 1-3mm, and the number is more than 12. Thereby ensuring that the gas flows through the substrate sufficiently and ensures uniform deposition.
A method for preparing single crystal diamond by laser-enhanced plasma CVD comprises the following steps:
step one, cleaning and drying seed crystals;
step two, putting the seed crystal into a cavity of a plasma CVD device, and then vacuumizing the background to 1 x 10-4Within Pa, opening a cooling water circulation system, then introducing 1-1000sccm hydrogen and maintaining the gas intakeBalancing air extraction, keeping the air pressure constant, inputting energy, generating discharge, adjusting the temperature of the seed crystal to a certain temperature, and treating for a certain time;
step three, introducing carbon-containing gas for growth, turning on a power supply of laser equipment, adjusting a laser beam to irradiate the surface of the substrate, controlling the temperature of the seed crystal at a certain temperature, and growing for a certain time;
and step four, taking out the diamond sheet after the growth is finished, and carrying out post-treatment to obtain the single crystal diamond sheet.
Further, in the step one, volatile liquid such as acetone and alcohol is adopted to clean impurities such as organic matters on the surface of the seed crystal, and the drying temperature is 60 ℃.
Further, the plasma CVD equipment in the second step includes hot filament CVD, microwave CVD, direct current CVD, etc., and the energy includes hot filament, microwave, direct current, etc.; the seed crystal temperature is adjusted to be 600-800 ℃, and the treatment time is 1-120 minutes.
Further, in the third step, the carbon-containing gas comprises methane, acetone, carbon dioxide and the like, the seed crystal is controlled at the temperature of 800-1000 ℃, and the growth time is 10-100 hours.
Further, the post-processing in the fourth step comprises the steps of processing by laser cutting, cutting polycrystalline on the periphery of the diamond, longitudinally cutting, stripping the single crystal substrate to separate the single crystal substrate from the growth layer, and finally polishing the two sides.
Compared with the prior art, the invention has the beneficial effects that:
(1) the laser reinforcing method can improve the density of the excited plasma and the dissociation rate of the gas, thereby accelerating the growth efficiency.
(2) The laser irradiates the surface of the substrate to increase the surface temperature of the substrate, thereby improving the surface activity of the particles and improving the growth quality.
(3) The laser-assisted microwave (or electric energy) can effectively reduce energy consumption, the energy consumption can reach 10kW by adopting common microwave energy, and the same effect can be achieved by adopting a 5kW microwave source and 2 1kW laser sources for growing the single crystal diamond by adopting laser assistance, so that the cost is greatly saved.
(4) The raw material gas is uniformly introduced into the edge of the substrate, and the gas is extracted from the outside of the substrate, so that the uniformity of gas molecules passing through the surface of the substrate is increased, the gas molecules can be fully dissociated, and the difference between the edge and the central area is reduced;
(5) the invention adopts a mode of integrating the water path and the air path, can effectively solve the problem of uneven air flow distribution of a common air inlet due to pressure difference generated by heat, can maintain the temperature of the air inlet and ensure the flow rate of the air by adopting a method of wrapping the air path by the water path, and further ensures the growth uniformity of plasma and a substrate.
Drawings
FIG. 1 is a structural diagram of a device for preparing single crystal diamond by laser-enhanced plasma CVD.
Description of reference numerals: 1. a plasma CVD apparatus; 2. a laser device; 3. a substrate stage; 4. a cooling water inlet; 5. a cooling water outlet; 6. a raw material inlet; 7. an air exhaust port.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments, which are provided for illustration only and are not to be construed as limiting the invention.
As shown in figure 1, the invention discloses a device for preparing single crystal diamond by laser-enhanced plasma CVD, which comprises a plasma CVD device 1 and a laser device 2; the number of the laser devices 2 is more than 1, the laser devices are respectively positioned outside the cylindrical cavity of the plasma CVD device 1, and laser emitted by the laser devices 2 can irradiate the substrate table 3 positioned in the cavity of the plasma CVD device 1; the substrate table 3 is positioned in the middle of the cavity of the plasma CVD equipment 1, and the lower part of the substrate table 3 is provided with a cooling water circulating system which comprises a cooling water inlet 4 and a cooling water outlet 5; the bottom of the cavity of the plasma CVD equipment 1 is provided with a raw material air inlet 6 and an air exhaust opening 7.
Specifically, the plasma CVD apparatus 1 is one of hot-wire CVD, microwave CVD, direct-current CVD, and the like.
The chamber of the plasma CVD apparatus 1 is sealed, and may be evacuated or filled with gas.
The raw material air inlets 6 are uniformly distributed around the substrate table 3, the size is 1-3mm, and the number is more than 12. Thereby ensuring that the gas flows through the substrate sufficiently and ensures uniform deposition.
Examples
The method for preparing the single crystal diamond by adopting the device for preparing the single crystal diamond by the laser-enhanced plasma CVD provided by the invention comprises the following steps:
(1) cleaning seed crystals, namely cleaning impurities such as organic matters on the surfaces of the seed crystals by using volatile liquid such as acetone and alcohol; then drying at 60 ℃;
(2) placing seed crystal into the cavity of plasma CVD equipment (hot filament CVD, microwave CVD, direct current CVD, etc.), and vacuumizing to 1 x 10-4Within Pa, opening a cooling water circulation system, then introducing 1-1000sccm hydrogen and maintaining the balance of air intake and air exhaust to ensure a certain air pressure, inputting energy (including hot wires, microwaves, direct current and the like) to generate discharge, adjusting the temperature of the seed crystal to 600-800 ℃, and treating for 1-120 minutes;
(3) introducing carbon-containing gas such as methane, acetone, carbon dioxide and the like for growth, turning on a laser power supply, adjusting a laser beam to irradiate the surface of the substrate, controlling the temperature of the seed crystal at 800-;
(4) and after the growth is finished, taking out the diamond wafer, processing by adopting laser cutting, cutting off polycrystal around the diamond, then longitudinally cutting, stripping the single crystal substrate to separate from the growth layer, and then polishing the two sides to obtain the high-quality single crystal diamond wafer.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and scope of the present invention should be included in the present invention.
Claims (8)
1. A method for preparing single crystal diamond by laser enhanced plasma CVD comprises a plasma CVD device and a laser device, and is characterized in that: more than 1 laser device is respectively positioned outside the cylindrical cavity of the plasma CVD device, and laser emitted by the laser device can irradiate the substrate table positioned in the cavity of the plasma CVD device; the substrate table is positioned in the middle of the cavity of the plasma CVD equipment, and a cooling water circulating system is arranged at the lower part of the substrate table and comprises a cooling water inlet and a cooling water outlet; the bottom of the cavity of the plasma CVD equipment is provided with a raw material air inlet and an air exhaust opening, the distance between the raw material air inlet and the substrate table is less than the distance between the raw material air exhaust opening and the substrate table, an air outlet of the raw material air inlet pipeline is higher than an air inlet of the air exhaust pipeline, and a cooling water inlet and a cooling water outlet are positioned on the inner side of the raw material air inlet; the method comprises the following steps:
step one, cleaning and drying seed crystals;
step two, putting the seed crystal into a cavity of a plasma CVD device, and then vacuumizing the background to 1 x 10-4Within Pa, opening a cooling water circulation system, then introducing 1-1000sccm hydrogen, maintaining the balance of air intake and air exhaust, keeping the air pressure constant, inputting energy to generate discharge, adjusting the temperature of the seed crystal to 600-800 ℃, and treating for 1-120 minutes;
step three, introducing carbon-containing gas for growth, turning on a power supply of laser equipment, adjusting a laser beam to irradiate the surface of the substrate, controlling the temperature of the seed crystal to be 800-1000 ℃, and growing for 10-100 hours;
and step four, taking out the diamond sheet after the growth is finished, and carrying out post-treatment to obtain the single crystal diamond sheet.
2. A method of laser-enhanced plasma CVD of single crystal diamond according to claim 1, wherein: the plasma CVD apparatus is one of hot filament CVD and microwave CVD.
3. A method of laser-enhanced plasma CVD for producing single crystal diamond according to claim 1 or 2, wherein: the chamber of the plasma CVD apparatus is sealed.
4. A method of laser-enhanced plasma CVD for producing single crystal diamond according to claim 1 or 2, wherein: the raw material air inlets are uniformly distributed around the substrate table, the size is 1-3mm, and the number is more than 12.
5. A method of laser-enhanced plasma CVD of single crystal diamond according to claim 1, wherein: in the step one, cleaning treatment of the seed crystal adopts acetone and alcohol to clean organic impurities on the surface of the seed crystal, and the drying temperature is 60 ℃.
6. A method of laser-enhanced plasma CVD of single crystal diamond according to claim 1, wherein: and in the second step, the plasma CVD equipment comprises hot wire CVD, microwave CVD and direct current CVD, and the energy comprises hot wire, microwave and direct current.
7. A method of laser-enhanced plasma CVD of single crystal diamond according to claim 1, wherein: in the third step, the carbon-containing gas comprises methane, acetone and carbon dioxide.
8. A method of laser-enhanced plasma CVD for producing single crystal diamond according to any one of claims 1, 2, 5 to 7, wherein: and the post-treatment in the fourth step comprises the steps of carrying out laser cutting treatment, cutting off polycrystal around the diamond, then longitudinally cutting, stripping the single crystal substrate to separate from the growth layer, and finally carrying out double-sided polishing.
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| CN110983435A (en) * | 2019-12-24 | 2020-04-10 | 长沙新材料产业研究院有限公司 | Separation method of CVD single crystal diamond seed crystal and growth layer |
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| CN112481697B (en) * | 2020-08-19 | 2023-01-06 | 上海征世科技股份有限公司 | Base station for growing single crystal diamond by microwave plasma technology |
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| CN112941625A (en) * | 2021-03-22 | 2021-06-11 | 湖北碳六科技有限公司 | System and method for synthesizing diamond by utilizing methane |
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| US5731046A (en) * | 1994-01-18 | 1998-03-24 | Qqc, Inc. | Fabrication of diamond and diamond-like carbon coatings |
| CN2550376Y (en) * | 2002-06-20 | 2003-05-14 | 复旦大学 | Multifunction device for plasma and laser beam combined treatment material |
| CN1473952A (en) * | 2003-07-24 | 2004-02-11 | 复旦大学 | Method for treating material surface under nornal temperature with microvave plasma and laser |
| CN1271242C (en) * | 2003-08-13 | 2006-08-23 | 复旦大学 | Plasma decomposition method and apparatus for preparing diamond-like film |
| KR20080044206A (en) * | 2005-05-25 | 2008-05-20 | 카네기 인스티튜션 오브 워싱턴 | Colorless single-crystal cvd diamond at rapid growth rate |
| CN101736313B (en) * | 2008-11-26 | 2011-07-06 | 北京有色金属研究总院 | Method for preparing diamond-like film on germanium substrate |
| CN101831626B (en) * | 2010-06-11 | 2012-10-24 | 晏双利 | Chemical vapor diamond deposition device |
| CN103602958A (en) * | 2013-11-25 | 2014-02-26 | 李学耕 | Laser-assisted thin film preparation method and equipment |
| CN103668126A (en) * | 2013-11-29 | 2014-03-26 | 武汉理工大学 | Laser CVD (chemical vapor deposition) device |
| CN103911596B (en) * | 2014-02-27 | 2016-07-06 | 武汉工程大学 | A kind of device preparing diamond film and use the method that this device prepares diamond film |
| CN106012003B (en) * | 2016-06-07 | 2018-06-08 | 武汉工程大学 | The two-dimentional expansion method of CVD single-crystal diamonds |
| CN206109529U (en) * | 2016-09-14 | 2017-04-19 | 中国科学院金属研究所 | High power large tracts of land bias voltage microwave plasma diamond films deposition apparatus |
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