CN114232086B - Growth method for MPCVD single crystal diamond containing crack seed crystal - Google Patents
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- 239000013078 crystal Substances 0.000 title claims abstract description 144
- 239000010432 diamond Substances 0.000 title claims abstract description 63
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 title claims abstract 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000003698 laser cutting Methods 0.000 claims abstract description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 210000002381 plasma Anatomy 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 206010016165 failure to thrive Diseases 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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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
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
-
- 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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
- C30B25/205—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer the substrate being of insulating material
-
- 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
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The invention relates to a growth method of an MPCVD single crystal diamond containing crack seed crystals, which aims to solve the problem that the crack seed crystals are easy to crack in the MPCVD single crystal diamond homoepitaxial growth method. The growth method comprises the following steps: 1. the crack influence area of the single crystal diamond seed crystal is black under orthogonal polarized light; 2. removing the crack influence area by laser cutting to form a rectangular notch; 3. cleaning seed crystals; 4. putting the cleaned seed crystal into a tube furnace for annealing treatment; 5. placing the annealed seed crystal in MPCVD equipment, controlling the pressure, microwave power and seed crystal temperature in a cabin, introducing methane and nitrogen to transversely grow the single crystal diamond and fill the rectangular notch; 6. vertical epitaxial growth of MPCVD single crystal diamond was performed. The invention can effectively process the side surface of the notch and promote the transverse growth, so that the seed crystal containing the crack can be used for the growth of high-quality single crystal, the waste of the seed crystal is reduced, and the production cost is reduced.
Description
Technical Field
The invention belongs to the field of diamond preparation, and particularly relates to a method for treating crack-containing seed crystals and a method for growing single-crystal diamond on the crack-containing seed crystals by Microwave Plasma Chemical Vapor Deposition (MPCVD).
Background
Single crystal diamond is an ancient crystalline material that is commonly used to polish diamonds as an ornamental article or to grind cut material. However, with the advance of technology, many excellent material properties (such as high thermal conductivity, wide electromagnetic wave transmission frequency domain, high carrier mobility, etc.) of single crystal diamond are gradually developed, making it a promising material in the fields of power device heat dissipation, laser window, wide bandgap semiconductor, etc. The Microwave Plasma Chemical Vapor Deposition (MPCVD) technology is a currently accepted approach for artificially preparing large-size and high-quality single crystal diamond, and the growth process thereof is divided into homoepitaxial growth and heteroepitaxial growth according to different selected substrates. Homoepitaxial growth is a method for epitaxial growth by using single crystal diamond seed crystals as a growth substrate, and is an effective way for growing large-thickness and high-quality single crystal diamond due to high lattice matching degree and few defects. High quality single crystal diamond seeds in the homoepitaxial process are generally separated from the grown product (laser cutting) and polished for reuse after the growth is completed due to their expensive price. However, cracks may be generated in the seed crystal during the growth process, the laser cutting process and the polishing process, and the crack-containing seed crystal has crack propagation and even explosion due to high temperature environment in the subsequent growth process, so that the yield is reduced. Therefore, a method for growing the MPCVD single crystal diamond containing the crack seed crystal is needed, so that the crack seed crystal can be reused, the yield is improved, and the production cost is reduced.
Disclosure of Invention
The invention aims to solve the problem that crack-containing seed crystals are easy to crack in the MPCVD single crystal diamond homoepitaxial growth method, and provides a growth method for the MPCVD single crystal diamond containing the crack seed crystals.
The growth method for the MPCVD single crystal diamond containing the crack seed crystal is realized according to the following steps:
1. placing the single crystal diamond seed crystal containing the cracks under a polarizing microscope, wherein the crack influence area is black under orthogonal polarized light, and the non-influence area is a light and dark alternative image, so that the crack influence area is determined;
2. removing the crack influence area by laser cutting to form a rectangular notch, wherein the side wall of the notch is vertical to the upper surface and the lower surface of the diamond seed crystal to obtain the seed crystal with the crack influence area removed;
3. soaking the seed crystal with the crack influence area removed in a cleaning solution to obtain a cleaned seed crystal;
4. placing the cleaned seed crystal in a tube furnace, and annealing at the temperature of 300-500 ℃ in the air atmosphere to obtain the annealed seed crystal;
5. placing the annealed seed crystal in MPCVD (microwave plasma chemical vapor deposition) equipment, closing a cabin door, vacuumizing, introducing hydrogen, starting microwaves to ignite plasmas, increasing the pressure and the microwave input power in the cabin until the pressure in the cabin reaches 150-250mbar, the microwave power reaches 2000-3000W, and introducing methane and nitrogen to transversely grow the single crystal diamond and fill a rectangular notch when the temperature of the seed crystal reaches 800-900 ℃, wherein the content of methane (volume fraction) is 7-15%, and the content of nitrogen (volume fraction) is 0.001-0.1%, so as to obtain the seed crystal after filling treatment;
6. and closing nitrogen, reducing the methane content, increasing the seed crystal temperature, and performing vertical epitaxial growth of the MPCVD single crystal diamond to finish the growth of the MPCVD single crystal diamond containing the crack seed crystal.
The method for growing the MPCVD single crystal diamond containing the crack seed crystal comprises the steps of firstly determining a crack influence area through a polarization microscope, wherein due to the characteristics of a single crystal diamond crystal structure, cracks are formed along a (111) dissociation plane, and due to the existence of a crack interface under the polarization microscope, polarized light cannot be transmitted and is displayed as black; completely removing the affected area through laser cutting after determining the crack affected area so as to prevent the affected area from extending and expanding due to high temperature in the subsequent growth process to cause growth failure; simultaneously, impurities and ablation areas introduced in the side face of the notch in the machining process are eliminated by adopting a mixed solution of concentrated sulfuric acid and hydrogen peroxide and annealing in a tube furnace, conditions are provided for subsequent transverse growth, and the growth quality is improved; and finally, promoting the rapid transverse growth connection of the side surface of the notch by adopting the growth conditions of low temperature, high methane content and high nitrogen content, and further realizing the high-quality growth of the MPCVD single crystal diamond on the seed crystal.
The method for growing the MPCVD single crystal diamond containing the crack seed crystal has the following beneficial effects:
1. the crack influence area can be rapidly determined and completely removed, and crack extension expansion and cracking are prevented in the subsequent growth process;
2. the side surface of the notch can be effectively treated and the transverse growth is promoted, so that the seed crystal containing the crack can be used for the growth of high-quality single crystal, the waste of the seed crystal is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a flow chart of a MPCVD single crystal diamond growth method for use with a crack seed in an example;
FIG. 2 is a photograph of a single crystal diamond seed crystal containing a crack according to an example;
FIG. 3 is a photograph of a seed crystal for removing a crack-affected zone in step two of the example;
FIG. 4 is a photograph of a seed crystal after the filling treatment of step five in the example;
FIG. 5 is a photograph showing crack extension and fracture of a diamond seed crystal containing cracks during high temperature growth and cooling.
Detailed Description
The first specific implementation way is as follows: the growth method of the MPCVD single crystal diamond containing the crack seed crystal is implemented according to the following steps:
1. placing the single crystal diamond seed crystal containing the cracks under a polarizing microscope, wherein the crack influence area is black under orthogonal polarized light, and the non-influence area is a light and dark alternate image, so that the crack influence area is determined;
2. removing the crack influence area by laser cutting to form a rectangular notch, wherein the side wall of the notch is vertical to the upper surface and the lower surface of the diamond seed crystal to obtain the seed crystal with the crack influence area removed;
3. soaking the seed crystal with the crack influence area removed in a cleaning solution to obtain a cleaned seed crystal;
4. placing the cleaned seed crystal in a tube furnace, and annealing at the temperature of 300-500 ℃ in the air atmosphere to obtain the annealed seed crystal;
5. placing the annealed seed crystal in MPCVD (microwave plasma chemical vapor deposition) equipment, closing a cabin door, vacuumizing, introducing hydrogen, starting microwaves to ignite plasmas, increasing the air pressure and microwave input power in the cabin until the air pressure in the cabin reaches 150-250mbar, the microwave power reaches 2000-3000W, introducing methane and nitrogen to enable the single crystal diamond to transversely grow and fill a rectangular notch when the temperature of the seed crystal reaches 800-900 ℃, wherein the content of methane (volume fraction) is 7-15%, and the content of nitrogen (volume fraction) is 0.001-0.1%, and obtaining the seed crystal after filling treatment;
6. and closing nitrogen, reducing the methane content, increasing the seed crystal temperature, and performing vertical epitaxial growth of the MPCVD single crystal diamond to finish the growth of the MPCVD single crystal diamond containing the crack seed crystal.
According to the embodiment, the crack-containing seed crystal is pretreated, the crack influence area is eliminated, and the transverse epitaxial growth is carried out to realize the integrity of the growth layer single crystal, so that the crack-containing seed crystal can also carry out high-quality growth, and the production cost is reduced.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the cleaning solution in the third step is a mixed reagent of concentrated sulfuric acid and a hydrogen peroxide solution with a mass concentration of 30%.
The volume ratio of the concentrated sulfuric acid to the hydrogen peroxide solution with the mass concentration of 30% in the embodiment is 0.5-0.8:1.
the third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the soaking time in the third step is 5-12h.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is that the annealing time in the fourth step is 3-6 hours.
The fifth concrete implementation mode: the difference between this embodiment and the first to the fourth embodiment is that the vacuum pumping in the fifth step is performed to 5 × 10 -5 mbar or less.
The sixth specific implementation mode is as follows: the difference between this embodiment and one of the first to fifth embodiments is that the flow rate of hydrogen in step five is 300-500sccm.
The seventh embodiment: the difference between the embodiment mode and one of the first to the sixth embodiment modes is that in the fifth step, methane and nitrogen are introduced to enable the single crystal diamond to grow transversely and fill the rectangular notch until the air pressure in the cabin reaches 200-250mbar, the microwave power reaches 2000-2500W, and the temperature of the seed crystal reaches 800-900 ℃.
The specific implementation mode is eight: the difference between the present embodiment and one of the first to sixth embodiments is that in the fifth step, the methane content is controlled to be 8% -12%, and the nitrogen content is controlled to be 0.01% -0.04%.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is that the lateral growth time in the fifth step is 10-20h.
The detailed implementation mode is ten: the difference between the first embodiment and the ninth embodiment is that in the sixth embodiment, the volume content of the methane is reduced to 5-8%, and the temperature of the seed crystal is increased to 900-1100 ℃.
The embodiment is as follows: the growth method of the present example for MPCVD single crystal diamond with crack seed was carried out according to the following steps:
1. placing the single crystal diamond seed crystal containing the cracks under a polarizing microscope, wherein the crack influence area is black under orthogonal polarized light, and the non-influence area is a light and dark alternative image, so that the crack influence area is determined;
2. removing the crack influence area by laser cutting (cutting through) to form a rectangular notch, wherein the side wall of the notch is vertical to the upper surface and the lower surface of the diamond seed crystal to obtain the seed crystal with the crack influence area removed;
3. placing the seed crystal with the crack influence area removed in a cleaning solution, and soaking for 6 hours, wherein the cleaning solution is a mixed reagent of concentrated sulfuric acid and 30% hydrogen peroxide solution, so as to obtain the cleaned seed crystal;
4. placing the cleaned seed crystal in a tube furnace, and annealing for 2h at 480 ℃ in an air atmosphere to obtain the annealed seed crystal;
5. placing the annealed seed crystal in MPCVD (microwave plasma chemical vapor deposition) equipment, closing a hatch door and vacuumizing to 5 x 10 -5 Introducing 260sccm hydrogen below mbar, starting microwave to ignite plasma, increasing the pressure in the chamber and the input power of the microwave until the pressure in the chamber reaches 210mbar, the microwave power reaches 2400W, and introducing gas when the temperature of the seed crystal reaches 800 deg.CAdding methane and nitrogen to enable the single crystal diamond to grow transversely and fill the rectangular gap, wherein the growth time is 20 hours, the content (volume fraction) of methane is 10%, the content (volume fraction) of nitrogen is 0.01%, and the seed crystal after filling treatment is obtained;
6. and closing the nitrogen, adjusting the methane content to be 8%, increasing the seed crystal temperature to be 1000 ℃, and performing vertical epitaxial growth of the MPCVD single crystal diamond to finish the growth of the MPCVD single crystal diamond containing the crack seed crystal.
The flow chart of the growth method of this example for MPCVD single crystal diamond with a crack seed is shown in fig. 1.
In this embodiment, the crack-affected zone is removed, and then the growth conditions of low temperature, high methane content and high nitrogen content are adopted to promote the rapid lateral growth connection of the side surface of the notch, so that a complete growth layer without obvious cracks and defects can be obtained (as shown in fig. 4). Fig. 5 shows a diamond seed crystal containing cracks, which may not be processed in the present embodiment, and crack extension and fragmentation may occur during the high temperature growth and cooling process, so that a complete diamond growth layer may not be obtained, resulting in growth failure.
Claims (9)
1. A growth method for MPCVD single crystal diamond containing a crack seed crystal, characterized in that the growth method is carried out according to the following steps:
1. placing the single crystal diamond seed crystal containing the cracks under a polarizing microscope, wherein the crack influence area is black under orthogonal polarized light, and the non-influence area is a light and dark alternate image, so that the crack influence area is determined;
2. removing the crack influence area by laser cutting to form a rectangular notch, wherein the side wall of the notch is vertical to the upper surface and the lower surface of the diamond seed crystal to obtain the seed crystal with the crack influence area removed;
3. soaking the seed crystal with the crack influence area removed in a cleaning solution to obtain a cleaned seed crystal;
4. placing the cleaned seed crystal in a tube furnace, and annealing at the temperature of 300-500 ℃ in the air atmosphere to obtain the annealed seed crystal;
5. placing the annealed seed crystal in MPCVD equipment, closing a cabin door, vacuumizing, introducing hydrogen, starting microwaves to ignite plasma, increasing the air pressure and microwave input power in the cabin until the air pressure in the cabin reaches 150-250mbar, the microwave power reaches 2000-3000W, and introducing methane and nitrogen to enable the single crystal diamond to transversely grow and fill a rectangular notch when the temperature of the seed crystal reaches 800-900 ℃, wherein the content of methane is 8-12%, and the content of nitrogen is 0.01-0.04%, so as to obtain the seed crystal after filling treatment;
6. and closing the nitrogen, reducing the methane content, increasing the seed crystal temperature, and performing vertical epitaxial growth of the MPCVD single crystal diamond to finish the growth of the MPCVD single crystal diamond containing the crack seed crystal.
2. The growth method of an MPCVD single crystal diamond containing a crack seed according to claim 1, wherein the cleaning solution in step three is a mixed reagent of concentrated sulfuric acid and a hydrogen peroxide solution with a mass concentration of 30%.
3. A growth method for an MPCVD single crystal diamond containing a crack seed according to claim 1, characterized in that the soaking time in step three is 5-12h.
4. A growth method for MPCVD single crystal diamond with crack seeds as recited in claim 1, characterized in that the annealing treatment time in step four is 3-6h.
5. A growth method for MPCVD single crystal diamond with crack seed crystals as recited in claim 1, characterized in that in step five vacuum is drawn to 5 x 10 -5 Below mbar.
6. A growth method for an MPCVD single crystal diamond containing a crack seed as set forth in claim 1, wherein the flow rate of hydrogen in the fifth step is 300-500 seem.
7. The growth method of an MPCVD single crystal diamond with a crack seed according to claim 1, wherein in step five, methane and nitrogen are introduced to cause the single crystal diamond to grow transversely and fill the rectangular notch until the pressure in the chamber reaches 200-250mbar, the microwave power reaches 2000-2500W, and the temperature of the seed reaches 800-900 ℃.
8. The growth method of an MPCVD single crystal diamond containing a crack seed according to claim 1, characterized in that the lateral growth time in step five is 10-20h.
9. A growth method for MPCVD single crystal diamond containing a crack seed as claimed in claim 1, characterized in that in step six the methane volume content is reduced to 5% -8%, raising the seed temperature to 900-1100 ℃.
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| US5628824A (en) * | 1995-03-16 | 1997-05-13 | The University Of Alabama At Birmingham Research Foundation | High growth rate homoepitaxial diamond film deposition at high temperatures by microwave plasma-assisted chemical vapor deposition |
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| CN110938864A (en) * | 2019-11-08 | 2020-03-31 | 武汉大学 | Method for efficiently regulating and controlling dislocation density of CVD single crystal diamond local area |
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Patent Citations (7)
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|---|---|---|---|---|
| US5628824A (en) * | 1995-03-16 | 1997-05-13 | The University Of Alabama At Birmingham Research Foundation | High growth rate homoepitaxial diamond film deposition at high temperatures by microwave plasma-assisted chemical vapor deposition |
| CN104651928A (en) * | 2015-01-17 | 2015-05-27 | 王宏兴 | Homogeneous epitaxial lateral growth method for diamond |
| CN110023545A (en) * | 2016-12-01 | 2019-07-16 | 六号元素技术有限公司 | Pass through the synthetic diamonds material of chemical vapor deposition |
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| CN109722713A (en) * | 2019-01-31 | 2019-05-07 | 西安交通大学 | A kind of novel diamond substrat structure, cutting technique and application thereof |
| CN110938864A (en) * | 2019-11-08 | 2020-03-31 | 武汉大学 | Method for efficiently regulating and controlling dislocation density of CVD single crystal diamond local area |
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