CN117552097A - Substrate for single crystal diamond growth and method for producing single crystal diamond - Google Patents
Substrate for single crystal diamond growth and method for producing single crystal diamond Download PDFInfo
- Publication number
- CN117552097A CN117552097A CN202311638119.7A CN202311638119A CN117552097A CN 117552097 A CN117552097 A CN 117552097A CN 202311638119 A CN202311638119 A CN 202311638119A CN 117552097 A CN117552097 A CN 117552097A
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- CN
- China
- Prior art keywords
- substrate
- single crystal
- crystal diamond
- growth chamber
- nonmetallic
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- 239000000758 substrate Substances 0.000 title claims abstract description 59
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 55
- 239000010432 diamond Substances 0.000 title claims abstract description 55
- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000012495 reaction gas Substances 0.000 claims abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 230000006835 compression Effects 0.000 claims description 12
- 238000007906 compression Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002210 silicon-based material Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 238000011109 contamination Methods 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009643 growth defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- 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)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the field of diamond manufacturing, in particular to a manufacturing method of single crystal diamond, which comprises the following steps: selecting a proper nonmetallic substrate, placing the nonmetallic substrate in a growth chamber, heating and pressurizing to form a reaction system on the substrate; placing a limit frame on the top of the nonmetallic substrate; and (3) introducing a reaction gas into the growth chamber, and reacting the reaction gas under a high-temperature and high-pressure environment to generate graphite which becomes monocrystalline diamond through high temperature and high pressure. According to the invention, through the use of the nonmetallic substrate, residual pollutants in growth are less, and the limiting frame is used for limiting the growth of polycrystal; the pressure is precisely controlled through the pressure detection mechanism in the artificial synthesis process, and the reasonable application range of the air pressure is controlled, so that the quality of the diamond is ensured.
Description
Technical Field
The invention relates to the technical field of diamond manufacturing, in particular to a substrate for single crystal diamond growth and a manufacturing method of single crystal diamond.
Background
The diamond has excellent mechanical, thermal, electrical, optical, acoustical and chemical properties, so that the diamond has wide application prospects in a plurality of high and new technical fields, such as heat sinks, optical windows, photoconductive detectors and the like. However, natural diamond often contains nitrogen impurities and growth defects, which results in degradation of diamond quality, and has problems of thin number, high price, small size, etc., which are far from meeting the demands of people, so that it is desired to prepare high-quality inch-grade diamond films by a synthetic method.
Currently, there are two main methods of synthesizing diamond crystals: high Pressure High Temperature (HPHT) and Chemical Vapor Deposition (CVD). For HPHT methods, it is difficult to grow large-sized single crystal diamond, which is typically less than 10X 10mm in crystal size 2 Often, the requirements cannot be met; while the CVD method is a viable method for producing large-sized diamond films, the CVD method mainly uses metal as a growth substrate, and there are problems such as residual contamination in the transfer process. In addition, the diamond needs to accurately control the pressure in the artificial synthesis process, and the reasonable application range of the air pressure is controlled, so that the quality problem of the diamond is guaranteed.
Accordingly, a substrate for single crystal diamond growth and a method for manufacturing single crystal diamond are provided by those skilled in the art to solve the problems set forth in the background art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for manufacturing single crystal diamond, which comprises the following steps:
step S1: screening nonmetallic substrates with proper sizes according to requirements, placing the nonmetallic substrates in a growth chamber, increasing the temperature in the growth chamber through heating equipment, and performing high-temperature treatment on the substrates to form a reaction system on the substrates;
step S2: placing a limit frame on the top of the nonmetallic substrate;
step S3: and introducing a pressurizing pipeline into the growth chamber to increase the pressure in the growth chamber, introducing a reaction gas, and reacting the reaction gas under a high-temperature and high-pressure environment to generate graphite to become monocrystalline diamond.
Preferably: in the step S2, the limiting frame is disposed at the top peripheral edge of the single crystal diamond, and the limiting frame is used for preventing polycrystalline growth on the single crystal diamond.
Preferably: the limiting frame is made of diamond material or silicon material.
Preferably: and an air inlet and an air outlet are arranged on two sides of the growth chamber and are used for guiding and discharging reaction gas.
Preferably: the pressure detection mechanism comprises a control valve, a controller, an emitter, a receiver, a supporting tube and a stress push plate, wherein the control valve is arranged on a pressurizing pipeline, the supporting tube is arranged on one side of the top of the growth chamber, the emitter and the receiver are respectively arranged on two sides of the top of the supporting tube, the stress push plate is arranged in an inverted T shape, a compression spring is arranged between the stress push plate and the top of the growth chamber, when the stress push plate does not generate compression force on the compression spring, the top of the stress push plate is positioned in the supporting tube, after the stress push plate is compressed by stress, the compression spring contracts, the top of the stress push plate is positioned between the emitter and the receiver, so that signals are blocked, the emitter, the receiver and the control valve are connected with the controller, an alarm signal is sent, no pressurizing gas is introduced into the growth chamber, and when the pressure in the growth chamber is overlarge, the stress push plate rises, so that laser signals between the emitter and the receiver are blocked.
The scheme also provides a substrate for growing monocrystalline diamond, wherein the substrate is a nonmetallic substrate, the nonmetallic substrate is heated to 1000 ℃ in inert gas to form a reaction system, and then the nonmetallic substrate is annealed at a high temperature for 2 hours.
Preferably: the nonmetallic substrate is a silicon wafer substrate or a quartz wafer substrate.
Preferably: the inert gas adopts a mixed gas of nitrogen and argon.
Preferably: and filling carbon source and water vapor into the growth chamber, and adopting chemical vapor deposition technology.
Preferably: the non-metallic substrate has a thickness greater than 1.5mm.
The invention has the technical effects and advantages that:
by using a non-metallic substrate, there is less residual contamination from growth, and the confinement frame is used to confine the growth of polycrystalline bodies.
The pressure is precisely controlled through the pressure detection mechanism in the artificial synthesis process, and the reasonable application range of the air pressure is controlled, so that the quality of the diamond is ensured.
Drawings
Fig. 1 is a schematic structural view of a substrate for single crystal diamond growth and a method for manufacturing single crystal diamond according to an embodiment of the present application;
in the figure:
1. the non-metal substrate, 2, a growth chamber, 3, a heating device, 4, a limit frame, 5, monocrystalline diamond, 6, a pressurizing pipeline, 7, an air inlet, 8, an air outlet, 9, a control valve, 10, a controller, 11, a transmitter, 12, a receiver, 13, a support tube, 14 and a stress pushing plate.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description. The embodiments of the invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Example 1
Referring to fig. 1, in this embodiment, a substrate for growing single crystal diamond is provided, wherein the substrate is a non-metal substrate 1, the non-metal substrate 1 is heated to 1000 ℃ in inert gas to form a reaction system, and then annealed at high temperature for 2 hours. Wherein, the nonmetallic substrate 1 is a silicon wafer substrate or a quartz wafer substrate. And the thickness of the nonmetallic substrate 1 is greater than 1.5mm.
In a preferred embodiment, a mixture of nitrogen and argon is used as the inert gas.
In addition, carbon source and water vapor are also filled into the growth chamber 2, and chemical vapor deposition technology is adopted.
The present embodiment also provides a method for manufacturing single crystal diamond 5, comprising the steps of:
step S1: screening nonmetallic substrates 1 with proper sizes according to requirements, placing the nonmetallic substrates 1 into a growth chamber 2, increasing the temperature in the growth chamber 2 through a heating device 3, and performing high-temperature treatment on the substrates to form a reaction system on the substrates;
step S2: placing a limit frame 4 on top of the nonmetallic substrate 1; a spacing frame 4 is placed on the top peripheral edge of the single crystal diamond 5, the spacing frame 4 being used to prevent polycrystalline growth on the single crystal diamond 5; the limit frame 4 is made of diamond material or silicon material;
step S3: the pressurizing pipeline 6 is introduced into the growth chamber 2 to increase the pressure in the growth chamber 2, the reaction gas is introduced, and after the reaction gas reacts in a high-temperature and high-pressure environment, graphite is generated to form the monocrystalline diamond 5 through high temperature and high pressure.
In the preferred embodiment, the growth chamber 2 is provided with an air inlet 7 and an air outlet 8 at both sides for introducing and discharging the reaction gas. And still be equipped with pressure detection mechanism in the growth chamber 2, pressure detection mechanism includes control valve 9, a controller 10, the transmitter 11, the receiver 12, stay tube 13 and atress push pedal 14, control valve 9 is located on the pressure boost pipeline 6, stay tube 13 is seted up in growth chamber 2's top one side, the top both sides of stay tube 13 are equipped with transmitter 11 and receiver 12 respectively, atress push pedal 14 is the setting of reverse T shape, be equipped with compression spring between atress push pedal 14 and growth chamber 2's the top, when atress push pedal 14 does not produce compressive force to compression spring, atress push pedal 14's top is located stay tube 13, after the atress push pedal 14 atress compresses, compression spring shrink, atress push pedal 14's top is located between transmitter 11 and the receiver 12, thereby block the signal, transmitter 11, receiver 12, control valve 9 is connected with controller 10, thereby send alarm signal, no longer let in the pressurized gas to growth chamber 2.
In the production of single crystal diamond 5, the use of nonmetallic substrate 1 results in less residual contamination of growth, and limiting frame 4 is used to limit the growth of polycrystalline body. The pressure is precisely controlled through the pressure detection mechanism in the artificial synthesis process, and the reasonable application range of the air pressure is controlled, so that the quality of the diamond is ensured. When the pressure in the growth chamber 2 is too high, the stressed pushing plate 14 rises, so that the laser signal between the emitter 11 and the receiver 12 is blocked, an alarm function is generated, and the control valve 9 is closed, so that the pressure is not increased.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art and which are included in the embodiments of the present invention without the inventive step, are intended to be within the scope of the present invention. Structures, devices and methods of operation not specifically described and illustrated herein, unless otherwise indicated and limited, are implemented according to conventional means in the art.
Claims (10)
1. A method for producing a single crystal diamond, comprising the steps of:
step S1: screening nonmetallic substrates with proper sizes according to requirements, placing the nonmetallic substrates in a growth chamber, increasing the temperature in the growth chamber through heating equipment, and performing high-temperature treatment on the substrates to form a reaction system on the substrates;
step S2: placing a limit frame on the top of the nonmetallic substrate;
step S3: and introducing a pressurizing pipeline into the growth chamber to increase the pressure in the growth chamber, introducing a reaction gas, and reacting the reaction gas under a high-temperature and high-pressure environment to generate graphite to become monocrystalline diamond.
2. A method of producing single crystal diamond according to claim 1, wherein in step S2, the stopper frame is placed on the top peripheral edge of the single crystal diamond, the stopper frame serving to prevent polycrystalline growth on the single crystal diamond.
3. A method of manufacturing single crystal diamond according to claim 1, wherein the spacing frame is formed of diamond material or silicon material.
4. A method of producing a single crystal diamond according to claim 1, wherein the growth chamber is provided with an air inlet and an air outlet on both sides thereof for introducing and discharging a reaction gas.
5. The method for manufacturing single crystal diamond according to claim 1, wherein the growth chamber is further provided with a pressure detection mechanism, the pressure detection mechanism comprises a control valve, a controller, a transmitter, a receiver, a support tube and a stress pushing plate, the control valve is arranged on the pressurizing pipeline, the support tube is arranged on one side of the top of the growth chamber, the transmitter and the receiver are respectively arranged on two sides of the top of the support tube, the stress pushing plate is arranged in an inverted T shape, a compression spring is arranged between the stress pushing plate and the top of the growth chamber, when the stress pushing plate does not generate compression force on the compression spring, the top of the stress pushing plate is positioned in the support tube, after the stress pushing plate is subjected to stress compression, the compression spring contracts, the top of the stress pushing plate is positioned between the transmitter and the receiver, so that signals are blocked, the transmitter, the receiver, the control valve are connected with the controller, and therefore, an alarm signal is sent, and pressurizing gas is not introduced into the growth chamber any more.
6. A substrate for single crystal diamond is characterized in that the substrate is a nonmetallic substrate, the nonmetallic substrate is heated to 1000 ℃ in inert gas to form a reaction system, and then the nonmetallic substrate is annealed at a high temperature for 2 hours.
7. A substrate for single crystal diamond according to claim 6, wherein the nonmetallic substrate is a silicon wafer substrate or a quartz wafer substrate.
8. A substrate for single crystal diamond according to claim 6, wherein the inert gas is a mixed gas of nitrogen and argon.
9. A substrate for single crystal diamond according to claim 6, wherein the growth chamber is further filled with a carbon source and water vapor by chemical vapor deposition.
10. A substrate for single crystal diamond according to claim 6, wherein the non-metallic substrate has a thickness of greater than 1.5mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311638119.7A CN117552097A (en) | 2023-12-02 | 2023-12-02 | Substrate for single crystal diamond growth and method for producing single crystal diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311638119.7A CN117552097A (en) | 2023-12-02 | 2023-12-02 | Substrate for single crystal diamond growth and method for producing single crystal diamond |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117552097A true CN117552097A (en) | 2024-02-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311638119.7A Pending CN117552097A (en) | 2023-12-02 | 2023-12-02 | Substrate for single crystal diamond growth and method for producing single crystal diamond |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117552097A (en) |
-
2023
- 2023-12-02 CN CN202311638119.7A patent/CN117552097A/en active Pending
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