CN114318529B - Diamond and synthesis process thereof - Google Patents
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- CN114318529B CN114318529B CN202111423495.5A CN202111423495A CN114318529B CN 114318529 B CN114318529 B CN 114318529B CN 202111423495 A CN202111423495 A CN 202111423495A CN 114318529 B CN114318529 B CN 114318529B
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- 238000000034 method Methods 0.000 title claims abstract description 70
- 239000010432 diamond Substances 0.000 title claims abstract description 63
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 63
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 70
- 238000005530 etching Methods 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- 238000005498 polishing Methods 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 241000252506 Characiformes Species 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 230000003746 surface roughness Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 description 19
- 239000002184 metal Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000010437 gem Substances 0.000 description 5
- 229910001751 gemstone Inorganic materials 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004050 hot filament vapor deposition Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention relates to a diamond and a synthesis process thereof, comprising the following steps: s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the growth surface is a (100) surface, and polishing the growth surface. S2, cleaning seed crystals, and then placing the seed crystals into a cavity of microwave plasma chemical vapor deposition equipment; s3, introducing H into the cavity 2 ，H 2 Etching the seed crystal with the flow rate of 100-1000 standard milliliters per minute; s4, after etching is finished, introducing a carbon source, the carbon source and H into the cavity 2 And (3) performing stable growth with the volume ratio of 1-12%, wherein the concentration of the carbon source is reduced by 0.1-0.5% every 50-199 hours, and other process parameters are kept unchanged until the target thickness is reached. The method for controlling the concentration of the carbon source in a staged manner maintains the equipment to stably operate for a long time, can grow to the target thickness at one time, and can ensure that the grown diamond product reaches low defect density and uniform and consistent optical performance.
Description
Technical Field
The invention belongs to the technical field of diamond synthesis, and particularly relates to diamond and a synthesis process thereof.
Background
Diamond has been attracting attention as a third generation semiconductor material with its remarkable advantages of high thermal conductivity, high carrier mobility, wide forbidden bandwidth, and the like. However, high quality natural diamond has a limited reserves and is extremely expensive to develop, so various synthetic diamond methods have been developed, such as high temperature High Pressure (HPHT), hot wire chemical vapor deposition (HJCVD), microwave Plasma Chemical Vapor Deposition (MPCVD). Among them, the MPCVD method for synthesizing diamond is the most potential method for synthesizing high-quality, large-area electronic grade diamond material because of no introduction of impurities.
The quality of MPCVD diamond synthesis is dependent on a number of factors including carbon source concentration, gas flow, temperature, substrate table height, microwave power, synthesis temperature, plasma species and density distribution, temperature uniformity, etc. However, in the process of synthesizing diamond products of precious stone grade, long-time stable operation growth is required due to the characteristics of low growth speed, large growth thickness, long growth period and the like. However, during long growth, the technician is faced with the following problems: as the growth time increases, the growth thickness of the single crystal diamond accumulates, and the quality of the resulting diamond growth layer product gradually decreases. This is manifested in the optical properties of the product. Therefore, after a long period of stable operation for several hundred hours, the resulting product cannot be sold as a gemstone-grade diamond product, which is a problem to be solved.
The Washington Kaneki institute geophysical laboratory group Mao Heguang applied MPCVD method at a power of 3-5kw and a power density of 50-100w/cm 3 The cavity pressure is 100-200torr, the growth temperature is 1100-1300 ℃, the proportion of CH4/H2 is 8-22%, the growth rate of the monocrystalline diamond substrate is 9x9mm, the process method is 50-100um/H, meanwhile, the process method is adopted to grow for many times, the growth layer and impurities in the cavity are taken out after a period of growth, and finally, the monocrystalline diamond sample with the thickness of more than 5mm is prepared. The key point of the method is that the method is used for multiple growth, and the grown defects are removed manually in time, so that the high-quality jewel grade diamond blank product is finally synthesized. However, in the actual operation, the method is carried out for a plurality of times, and the processing procedures of laser cutting and polishing are increased, so that a great amount of time is consumed in the processing procedure, and the defects of microcracks, scratches and the like introduced in the cutting and polishing procedures are increased.
Element six a high quality single crystal diamond sample was synthesized by MPCVD. The quality of the gas is monitored in real time by using a GC (gas chromatography) method, the impurity content of the doped gas is accurately controlled and regulated, the doping amount is controlled at ppb level, the selected crystal orientation of the seed crystal is controlled within 5 DEG from the (001) plane and cannot exceed 10 DEG at maximum, the etching temperature before growth is 600-1100 ℃, the optimal temperature is 800 ℃, ar is introduced in the growth process, the synthesis temperature is 750-900 ℃, the thickness of the synthesized product is more than 2mm, the N content is lower than 300ppb, and the diamond can be used as diamond at the precious stone level for growth. According to the method, the impurity content of the gas is accurately controlled, and Ar gas is introduced, so that the diamond growth process is stable. However, the method has extremely high requirements on equipment hardware, and meanwhile, the problem of aging and replacement of spare parts after long-time growth operation of the equipment is difficult to ensure the gas leakage rate with high precision, so that the implementation of the process method is influenced.
Disclosure of Invention
The invention provides a diamond and a synthesis process thereof, which maintain the long-time stable operation of equipment by a method of controlling the concentration of a carbon source in a staged way, can grow to a target thickness at one time, can ensure that the grown diamond product has the characteristics of low defect density and uniform and consistent optical performance, and can be used as a precious stone grade diamond product.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the growth surface is a (100) surface, and polishing the growth surface;
s2, cleaning seed crystals, and then placing the seed crystals into a cavity of microwave plasma chemical vapor deposition equipment;
s3, introducing H into the cavity 2 ，H 2 Etching seed crystal with flow rate of 100-1000 standard ml/min (100-1000 SSCM, SSCM is the unit of volume flow rate, standard ml is the ml under index condition, standard condition is that temperature is 0deg.C, air pressure is 101325Pa (760 mmHg)), etching seed crystal;
s4, after etching is finished, maintaining the introduced H 2 The flow is unchanged, a carbon source and H are introduced into the cavity 2 The volume ratio is 1-12%, stable growth is carried out, the concentration of the carbon source is reduced by 0.1-0.5% every 50-199 hours of stable growth (based on the carbon source at the time)Concentration is reduced) and other process parameters remain unchanged until the target thickness is reached.
Further, in the step S1, the surface roughness Ra of the growth surface after the polishing treatment is less than 50nm, preferably controlled within 10 nm.
Further, in the step S2, the cleaning process of the seed crystal is performed as follows: washing the surface of the seed crystal by acetone or absolute ethyl alcohol, washing off organic matters on the surface of the seed crystal, carrying out acid washing treatment by using a piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, and carrying out drying treatment.
Further, in the step S3, the etching operation is: hold H 2 The flow is 100-1000 standard milliliters per minute, and under the pressure of 2-20mabr, 300-1500 watts is ignited to generate plasma, then the pressure and power are gradually increased, so that the seed crystal is stabilized at the temperature of 700-1000 ℃, and then O is introduced 2 ，O 2 And H is 2 Etching the substrate with the volume ratio of less than 10%;
further, in the step S3, the etching time is 15-60min.
Further, in the step S4, O is introduced during the growth process 2 ，O 2 /H 2 The proportion of (2) is 0-8%.
Further, in the step S4, ar and Ar/H are also introduced in the growth process 2 The proportion of (C) is 0-30%.
Further, in the step S4, the carbon source concentration is reduced by 0.1% (based on the current carbon source concentration) every 50-100 hours of stable growth.
Further, in the step S4, the carbon source includes CH 4 、CO 2 Any of CO or ethanol gas.
The invention also provides a diamond prepared by the synthesis method of the diamond.
Compared with the prior art, the method for controlling the carbon source concentration in a staged manner maintains the equipment to stably run for a long time, can grow to the target thickness at one time, and can ensure that the grown diamond product reaches low defect density and uniform and consistent optical performance.
As the growth process proceeds, carbon-related species are deposited on the inner walls of the chamber, and during this process, the carbon source in the plasma will be of two sources: (1) continuously introducing carbon source gas, and ionizing in plasma to form different particles; (2) carbon-related impurities deposited on the inner wall of the cavity and carbon-related impurities deposited on the surface of the substrate table, wherein the impurities are mainly deposited in the form of graphite in the cavity. The carbon-related impurities in the inner wall are ionized again under the bombardment of the plasma, so that the density and concentration of the carbon-related particles in the plasma are uniformly changed, and the tendency of gradual increase is caused. This is also an important cause of deterioration of growth quality as the growth time is longer. Therefore, the invention ensures that the internal environment of the whole growth process is uniform and controllable by strictly controlling the concentration of the introduced carbon source gas, thereby realizing the preparation of the precious stone-grade diamond with low defect density and uniform and consistent optical performance.
Drawings
FIG. 1 is a FTIR chart of a diamond product synthesized in example 4 of the present invention;
FIG. 2 is a FTIR chart of a diamond product synthesized in comparative example 1 of the present invention;
FIG. 3 is a Raman diagram of a diamond product synthesized in example 4 of the present invention;
fig. 4 is a Raman diagram of a diamond product synthesized in comparative example 1 of the present invention.
Detailed Description
The following examples are provided to further illustrate the invention but are not to be construed as limiting the invention in any way.
Example 1
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 30 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow rate is 100 standard milliliters/min, and under the pressure of 2mabr, 1500W is ignited to generate plasma, then the pressure and the power are gradually increased to make the seed crystal stable at 700 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 10%, and etching is carried out for 15min;
s4, closing O after etching 2 CO is introduced into 2 Performing stable growth process, and initiating CO 2 And H is 2 The CO concentration was reduced by 0.5% every 199 hours of stable growth, and the other process parameters remained unchanged until the target thickness was reached.
Example 2
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 10 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow is 1000 standard milliliters/min, and under the pressure of 10mabr, 1000W is ignited to generate plasma, then the pressure and the power are gradually increased to make the seed crystal stable at 900 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 8%, and etching is carried out for 30min;
s4, closing O after etching 2 Introducing CO to perform stable growth process, and initializing CO and H 2 The volume ratio of (2) is 10%, the CO concentration is reduced by 0.2% every 100 hours of stable growth, and other process parameters are kept unchangedAnd changing until the target thickness is grown.
Example 3
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 30 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow rate is 500 standard milliliters/min, and the plasma is generated by ignition of 300W under 15mabr pressure, then the pressure and the power are gradually increased, so that the seed crystal is stabilized at 1000 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 8%, and etching is carried out for 60min;
s4, closing O after etching 2 Introducing CH 4 Performing stable growth process, initial and H 2 Is 10% by volume, and is grown for 50 hours every time, CH is added 4 The concentration is reduced by 0.1%, and other process parameters remain unchanged until the target thickness is reached.
Example 4
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 8 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, firstly, etching for a certain time before growthEtching, introducing H into the cavity 2 ，H 2 The flow rate is 800 standard milliliters/min, and under the pressure of 20mabr, 800W is ignited to generate plasma, then the pressure and the power are gradually increased, so that the seed crystal is stabilized at 850 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 8%, etching is carried out for 40min;
s4, closing O after etching 2 Introducing CH 4 Performing stable growth process, initial CH 4 And H is 2 Is 10% by volume, and after 50 hours of stable growth, CH is added 4 The concentration is reduced by 0.1 percent, and after the stable growth is carried out for 70 hours, CH is added 4 The concentration is reduced by 0.1%, and CH is added every 120 hours after the subsequent stable growth 4 The concentration is reduced by 0.2%, and other process parameters remain unchanged until the target thickness is reached.
Example 5
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 8 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow is 300 standard milliliters/min, and under the pressure of 20mabr, 800W is ignited to generate plasma, then the pressure and the power are gradually increased, so that the seed crystal is stabilized at the temperature of 700-1000 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 7%, etching is carried out for 40min;
s4, keeping the O in 2 ，O 2 /H 2 Is 6% by volume, and is introduced with CH 4 Performing stable growth process, initial CH 4 And H is 2 Is 10% by volume, and after 50 hours of stable growth, CH is added 4 The concentration is reduced by 0.1 percent,after a further 70 hours of stable growth, CH 4 The concentration is reduced by 0.1%, and CH is added every 120 hours after the subsequent stable growth 4 The concentration is reduced by 0.2%, and other process parameters remain unchanged until the target thickness is reached.
Example 6
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 20 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow rate is 600 standard milliliters/min, and under the pressure of 20mabr, 800W is ignited to generate plasma, then the pressure and the power are gradually increased, so that the seed crystal is stabilized at 950 ℃ and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 6%, etching is carried out for 40min;
s4, introducing Ar, ar/H 2 Is 20% by volume, and is introduced with CH 4 And ethanol, and initial carbon source (CH 4 Mixed gas with ethanol) and H 2 After 50 hours of stable growth, the carbon source concentration is reduced by 0.1 percent, after 100 hours of stable growth, the carbon source concentration is reduced by 0.2 percent, and after 180 hours of stable growth, the carbon source concentration is reduced by 0.4 percent, and other process parameters are kept unchanged until the target thickness is reached.
Comparative example 1
A diamond synthesis process, comprising the steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the upper and lower growth surfaces are (100) surfaces, polishing the growth surfaces, and the surface roughness Ra of the growth surfaces after polishing is about 8 nm.
S2, cleaning the surface of the seed crystal by using acetone, carrying out acid washing treatment by using the prepared piranha solution, removing metal impurities on the surface of the seed crystal, washing off acid liquor by using deionized water, carrying out drying treatment, and then putting the seed crystal into a cavity of MPCVD equipment for preparation for growth;
s3, etching for a certain time before growth, and introducing H into the cavity 2 ，H 2 The flow rate is 800 standard milliliters/min, and under the pressure of 20mabr, 800W is ignited to generate plasma, then the pressure and the power are gradually increased, so that the seed crystal is stabilized at 850 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is 8%, etching is carried out for 40min;
s4, closing O after etching 2 Introducing CH 4 Performing stable growth process, maintaining CH 4 And H is 2 The volume ratio of (2) is 10%, and other technological parameters are kept unchanged until the target thickness is reached.
The diamond products synthesized in the example 4 and the comparative example 1 are detected, and the obtained results are shown in the attached figures 1-4, so that the product prepared by adopting the scheme of regulating the carbon source according to the invention can be seen that the optical transmittance of the product is close to 70% at most and reaches the theoretical limit value of the optical transmittance of the diamond; the optical transmittance of the product prepared in comparative example 1 without using the carbon source regulation scheme is 49% at the highest, which is far lower than that of the product of example 4.
As can be seen from Raman detection, the product prepared in the example 4 has no impurity and high purity, while the Raman chart of the product prepared in the comparative example 1 has obvious impurity peaks, which proves that the product contains impurities; as can be seen from the comparison, the diamond product prepared by stepwise regulating and controlling the concentration of the carbon source can reach high purity and has excellent optical performance, the method can grow high-quality diamond products at one time, and the color of the precious stone sample prepared by processing the diamond products can reach more than H color.
Claims (9)
1. The synthesis process of the diamond is characterized by comprising the following steps of:
s1, selecting single crystal diamond with a flat surface as seed crystal, wherein the growth surface is a (100) surface, and polishing the growth surface;
s2, cleaning seed crystals, and then placing the seed crystals into a cavity of microwave plasma chemical vapor deposition equipment;
s3, introducing H into the cavity 2 ，H 2 Etching the seed crystal with the flow rate of 100-1000 standard milliliters per minute;
s4, after etching is finished, maintaining the introduced H 2 The flow is unchanged, a carbon source and H are introduced into the cavity 2 And (3) performing stable growth with the volume ratio of 1-12%, wherein the concentration of the carbon source is reduced by 0.1-0.5% every 50-199 hours, and other process parameters are kept unchanged until the target thickness is reached.
2. A process for synthesizing diamond according to claim 1, wherein in step S1, the surface roughness Ra of the growth surface after the polishing treatment is less than 50nm.
3. A process for synthesizing diamond according to claim 1, wherein in step S2, the cleaning treatment of the seed crystal is performed as follows: and cleaning the surface of the seed crystal by using acetone or absolute ethyl alcohol, then carrying out acid cleaning treatment by using a piranha solution, washing acid liquor by using deionized water, and then carrying out drying treatment.
4. A process for synthesizing diamond according to claim 1, wherein in step S3, the etching operation is: hold H 2 The flow is 100-1000 standard milliliters per minute, and under the pressure of 2-20mabr, 300-1500 watts is ignited to generate plasma, then the pressure and power are gradually increased, so that the seed crystal is stabilized at the temperature of 700-1000 ℃, and then O is introduced 2 ，O 2 And H is 2 The volume ratio of (2) is within 10%, etching is carried out, and after the etching is finished, the introduction of O is stopped 2 。
5. The process according to claim 1, wherein the etching time in step S3 is 15-60min.
6. The process according to claim 1, wherein in step S4, O is introduced during the growth process 2 ，O 2 /H 2 The volume ratio of (2) is 0-8%.
7. The process according to claim 1, wherein Ar, ar/H is introduced during the growth in step S4 2 The volume ratio of (2) is 0-30%.
8. A process for synthesizing diamond according to claim 1, wherein in step S4, the concentration of the carbon source is reduced by 0.1% every 50 to 100 hours of stable growth.
9. A process for synthesizing diamond according to claim 1, wherein in step S4, the carbon source comprises CH 4 、CO 2 At least one of CO or ethanol gas.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10316491A (en) * | 1997-05-13 | 1998-12-02 | Sharp Corp | Synthesis of highly pure diamond |
| US6162412A (en) * | 1990-08-03 | 2000-12-19 | Sumitomo Electric Industries, Ltd. | Chemical vapor deposition method of high quality diamond |
| CN107740184A (en) * | 2017-09-30 | 2018-02-27 | 湖北碳六科技有限公司 | A kind of gradient single-crystal diamond and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SG157973A1 (en) * | 2008-06-18 | 2010-01-29 | Indian Inst Technology Bombay | Method for growing monocrystalline diamonds |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6162412A (en) * | 1990-08-03 | 2000-12-19 | Sumitomo Electric Industries, Ltd. | Chemical vapor deposition method of high quality diamond |
| JPH10316491A (en) * | 1997-05-13 | 1998-12-02 | Sharp Corp | Synthesis of highly pure diamond |
| CN107740184A (en) * | 2017-09-30 | 2018-02-27 | 湖北碳六科技有限公司 | A kind of gradient single-crystal diamond and preparation method thereof |
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