CN108103570A - A kind of method and system for splicing growth single-crystal diamond - Google Patents
A kind of method and system for splicing growth single-crystal diamond Download PDFInfo
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- CN108103570A CN108103570A CN201711310411.0A CN201711310411A CN108103570A CN 108103570 A CN108103570 A CN 108103570A CN 201711310411 A CN201711310411 A CN 201711310411A CN 108103570 A CN108103570 A CN 108103570A
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- crystal
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- crystal 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
- 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
-
- 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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- 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 belongs to technical field of diamond preparation, disclose a kind of method and system for splicing growth single-crystal diamond, seed crystal is placed into plasma CVD apparatus cavity, then base vacuum is taken out, then passes to hydrogen, input energy, electric discharge is generated, adjusts seed temperature；Methane (or the carbonaceous gas such as acetone, carbon dioxide) gas is passed through to be grown, seed temperature at 800 DEG C~1000 DEG C, carry out growth 1 it is small when~100 it is small when etc..The present invention is using CVD method splicing growth single-crystal diamond, achieve the purpose that large area deposition single-crystal diamond, the growth of existing single-crystal diamond can only carry out longitudinal expansion on original seed crystal, so the size of seed crystal directly determines the size of synthesis, this is clearly identical using two sizes, and splicing is fixed in the close single crystal diamond flag of thickness, then grows simultaneously, large size single crystal diamond is obtained, solves bottleneck problem.
Description
Technical field
The invention belongs to technical field of diamond preparation more particularly to a kind of method for splicing growth single-crystal diamond and it is
System.
Background technology
Single-crystal diamond synthesis at present is restricted by size, typically using single natural diamond or artificial synthesized
Single-crystal diamond thin slice is grown, since large size single crystal diamond is rare and price as seed crystal in its original size
Costliness, so as to which the diamond synthesized is limited be subject to seed size, since seed crystal edges defect is more and not easy to control easy
Grow polycrystalline diamond so that the size for obtaining product is not more than the size of original seed crystal, therefore can not obtain large scale
Single-crystal diamond.
In conclusion problem existing in the prior art is：
Existing process is single seed crystal face cross growth, but this method difficulty is larger (needs accurately control growth ginseng
Number, surge area very little), (depositing device using high configuration is needed to realize) of high cost, and actual effect is not obvious and (expands
Size is no more than 1mm, and seed crystal corner can not be grown since orientation limits).Particular problem is as follows：First；Due to seed crystal edges
" edge effect " can be generated and cause marginal discharge, so as at seed crystal edges trigger active group aggregation, this atomic hydrogen without
Method induces the generation of non-diamond impurity and polycrystalline structure in the environment of fully etching, cause the expansion of polycrystalline diamond, finally
Further reduce single-crystal diamond size；Second, since cross growth rate is slower, the generally longitudinally half of growth rate,
Thus horizontal area can with longitudinal area increase and increase, the product grown is not complete block materials, but under it is narrow
Upper wide trapezoidal product, can not obtain large area product after cutting and polishing；3rd, it is single due to the limitation of crystal orientation
Diamond growth can be along 100 directions, and the direction of seed crystal corner is 111 orientations, only can be along 100 directions in growth course
It grows up, and 111 four angular direction do not grow monocrystalline but impurity defect, are not whole growths.In conclusion the prior art without
Method solves the root problem of growing large-size single-crystal diamond.
The content of the invention
In view of the problems of the existing technology, grow the method for single-crystal diamond the present invention provides a kind of splicing and be
System.The effect of the present invention is exactly to provide thinking to obtain large size single crystal diamond product, and obtains certain technology and dash forward
It is broken.
The present invention is achieved in that a kind of method for splicing growth single-crystal diamond, the splicing growth single crystal diamond
The method of stone is fixed using the identical single crystal diamond flag of two sizes, thickness, is then grown simultaneously, obtains large scale list
Diamond.
Further, the method for the splicing growth single-crystal diamond specifically includes：
Seed crystal is chosen, selects 2~4 length and width, consistency of thickness, the identical single crystal diamond flag of color, crystal orientation is made
For seed crystal, single crystal diamond flag is soldered on the smooth molybdenum sheet in surface using vacuum brazing, is closely connected between seed crystal；
Seed crystal cleaning treatment, using acetone, the organic impurities of alcohol liquid cleaning seed crystal face；Then 60 DEG C of drying；
Seed crystal is placed into plasma CVD apparatus cavity, then takes out base vacuum to 1*10-4Pa is then passed to
1sccm~1000sccm hydrogen, input energy generate electric discharge, adjust seed temperature to 600 DEG C~800 DEG C, and processing 1min~
120min；
It is passed through methane (or the carbonaceous gas such as acetone, carbon dioxide) gas to be grown, seed temperature is 800 DEG C~1000
DEG C, carry out growth 1 it is small when~100 it is small when；
Diamond chip is taken out after growth, is handled using laser cutting, cuts off diamond surrounding polycrystalline, Ran Houjin
The cutting of row longitudinal direction, allows the large size single crystal extended outside piece to be separated with seed crystal, carries out twin polishing afterwards, obtain the list of double size
Diamond epitaxial wafer.
Further, the seed crystal of selection is 100,0 degree~10 degree of orientating deviation；Spacing is 0 micron~100 between adjacent seed crystal
Micron.
Another object of the present invention is to provide a kind of system for splicing growth single-crystal diamond.
Advantages of the present invention and good effect are：
The present invention grows single-crystal diamond using CVD method splicing, achievees the purpose that large area deposition single-crystal diamond, existing
The growth of single-crystal diamond can only carry out longitudinal expansion on original seed crystal, and the size of such seed crystal directly determines synthesis
Size, the present invention is identical using two sizes, and the close single crystal diamond flag of thickness is fixed, and then grows simultaneously, obtains
Large size single crystal diamond, solves bottleneck problem.
Cost reduction of the present invention can be realized using common CVD deposition equipment and the growth of normal single crystal diamond seed crystal piece,
No other inputs；
There is big breakthrough in size of the present invention, can realize expansion at double, by the method for splicing, repetition can be passed through
Splicing growth, can obtain infinitely great product, substantially reduce cost, compare original method, and equipment cost reduces by 50%, and rate carries
It doubles, and fundamentally breaches size bottleneck, obtaining 4 inches of diamond semiconductor chips for next step provides method；
Growth quality of the present invention is higher, and large-size high-quality single crystal diamond flag can be obtained by the way of splicing, intact
It falling into, the method by repeating splicing, the large size single crystal diamond product of high quality can be obtained by gradually removing edge defect impurity,
The single-crystal diamond fringe region diamond Raman peaks that prior art growth obtains have the offsets of 0.1-0.15 wave numbers, this be by
Seed crystal support is had no in the new outer single-crystal diamond extended, results in the generation of internal stress, and the present invention is to utilize original seed crystal
As the new product that support obtains, the generation of internal stress free, therefore obtain the single-crystal diamond of high-quality；
The present invention is disposable, and the large size single crystal diamond for growing completion can be taken off seed crystal using laser cutting, then
It is polished polishing and obtains independent large size single crystal diamond chip.
Description of the drawings
Fig. 1 is the method flow diagram of splicing growth single-crystal diamond provided in an embodiment of the present invention.
Fig. 2 is splicing growth model figure provided in an embodiment of the present invention.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Existing process is single seed crystal face cross growth, but this method difficulty is larger (needs accurately control growth ginseng
Number, surge area very little), (depositing device using high configuration is needed to realize) of high cost, and effect is not obvious and (expands size
No more than 1mm, and seed crystal corner can not be grown since orientation limits), the basic of growing large-size single-crystal diamond can not be solved
Problem.
Below in conjunction with the accompanying drawings and specific embodiment is further described the application principle of the present invention.
As shown in Figure 1, the method for splicing growth single-crystal diamond provided in an embodiment of the present invention, including：
S101:Seed crystal is chosen, selects 2-4 pieces length and width close to (within positive and negative 100 microns), (positive and negative 50 microns of consistency of thickness
Within), color, crystal orientation single crystal diamond flag identical (within orientation 0-10 degree), will using vacuum brazing as seed crystal
Single crystal diamond flag is soldered on the smooth molybdenum sheet in surface, is closely connected between seed crystal, and spacing control is at 0-100 microns, molybdenum sheet
Size is consistent with diamond chip, thickness 0.5-2mm；
S102:Seed crystal cleaning treatment, it is miscellaneous using the organic matter of the volatile liquids such as acetone, alcohol cleaning seed crystal face etc.
Matter；Then dry；
S103:Seed crystal is placed into plasma CVD apparatus (HF CVD, microwave CVD, direct current CVD etc.) cavity, so
Base vacuum is taken out afterwards within 1*10-4Pa, then passes to 1-1000sccm hydrogen, input energy is (including heated filament, microwave, direct current
Deng), electric discharge is generated, adjustment seed temperature handles 1-120min to 600-800 DEG C；
S104:Be passed through methane, acetone, carbon dioxide, etc. carbonaceous gas grown, seed temperature control in 800-1000
DEG C, carry out growth 10-100 it is small when；
S105:Diamond chip is taken out after growth, is handled using laser cutting, cuts off diamond surrounding polycrystalline,
Then longitudinal cutting is carried out, the large size single crystal extended outside piece is allowed to be separated with seed crystal, carries out twin polishing afterwards, obtains double ruler
Very little single-crystal diamond epitaxial wafer.
As shown in Fig. 2, splicing growth model figure provided in an embodiment of the present invention, model are using small size single crystal diamond
Masonry is seed crystal, is put into after being spliced together in CVD deposition equipment, and adjustment growth parameter(s) is grown, after length to certain thickness
It is cut, large size single crystal diamond chip is obtained after polishing treatment.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (4)
- A kind of 1. method for splicing growth single-crystal diamond, which is characterized in that the method for the splicing growth single-crystal diamond is adopted It is fixed with the identical single crystal diamond flag of two sizes, thickness, then grown simultaneously, obtain large size single crystal diamond.
- 2. the method for splicing growth single-crystal diamond as described in claim 1, which is characterized in that the splicing growth monocrystalline gold The method of hard rock specifically includes：Seed crystal is chosen, selects 2~4 length and width, consistency of thickness, the identical single crystal diamond flag of color, crystal orientation is as seed Single crystal diamond flag using vacuum brazing is soldered on the smooth molybdenum sheet in surface, is closely connected between seed crystal by crystalline substance；Seed crystal cleaning treatment, using acetone, the organic impurities of alcohol liquid cleaning seed crystal face；Then 60 DEG C of drying；Seed crystal is placed into plasma CVD apparatus cavity, then takes out base vacuum to 1*10-4Pa, then pass to 1sccm~ 1000sccm hydrogen, input energy generate electric discharge, and adjustment seed temperature handles 1min~120min to 600 DEG C~800 DEG C；It is passed through methane or acetone or carbon dioxide is grown, it is small to carry out growth 1 at 800 DEG C~1000 DEG C for seed temperature When~100 it is small when；Diamond chip is taken out after growth, is handled using laser cutting, diamond surrounding polycrystalline is cut off, is then indulged To cutting, the large size single crystal extended outside piece is allowed to be separated with seed crystal, carries out twin polishing afterwards, obtain the monocrystalline gold of double size Hard rock epitaxial wafer.
- 3. the method for splicing growth single-crystal diamond as claimed in claim 2, which is characterized in thatThe crystal orientation of the seed crystal of selection is 100,0 degree~10 degree of orientating deviation；Spacing is 0 micron~100 between adjacent seed crystal Micron.
- 4. a kind of splicing growth single-crystal diamond of the method for splicing growth single-crystal diamond as described in claim 1 is System.
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| CN201711310411.0A CN108103570A (en) | 2017-12-11 | 2017-12-11 | A kind of method and system for splicing growth single-crystal diamond |
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| CN201711310411.0A CN108103570A (en) | 2017-12-11 | 2017-12-11 | A kind of method and system for splicing growth single-crystal diamond |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108677246A (en) * | 2018-06-26 | 2018-10-19 | 西安交通大学 | A method of splicing growing large-area single-crystal diamond of laterally putting up a bridge |
| CN108754600A (en) * | 2018-06-26 | 2018-11-06 | 西安交通大学 | A method of splicing growing large-area single-crystal diamond |
| CN108977880A (en) * | 2018-08-29 | 2018-12-11 | 西安交通大学 | A method of intersecting splicing growing large-area single-crystal diamond |
| CN109161964A (en) * | 2018-09-30 | 2019-01-08 | 济南中乌新材料有限公司 | A kind of preparation method of large scale cvd diamond crystal |
| CN109989111A (en) * | 2019-03-13 | 2019-07-09 | 电子科技大学 | Preparation method, monocrystal thin films and the resonator of spliced small size monocrystal thin films |
| CN110079860A (en) * | 2019-03-29 | 2019-08-02 | 郑州磨料磨具磨削研究所有限公司 | A kind of splicing growing method of large size single crystal diamond epitaxial wafer |
| CN110857467A (en) * | 2018-08-23 | 2020-03-03 | 中国科学院宁波材料技术与工程研究所 | Diamond compact and preparation method thereof |
| 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 |
| CN111270313A (en) * | 2020-04-01 | 2020-06-12 | 湖州中芯半导体科技有限公司 | Method for splicing CVD diamond single crystals |
| CN112064111A (en) * | 2020-08-18 | 2020-12-11 | 北京大学东莞光电研究院 | Preparation device and preparation method of large-diameter diamond sheet |
| CN112442735A (en) * | 2019-08-30 | 2021-03-05 | 西安交通大学 | Method for growing large-area single crystal diamond by adsorption splicing |
| CN114150376A (en) * | 2021-10-14 | 2022-03-08 | 吉林大学 | Large-size single crystal diamond splicing growth method |
-
2017
- 2017-12-11 CN CN201711310411.0A patent/CN108103570A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754600A (en) * | 2018-06-26 | 2018-11-06 | 西安交通大学 | A method of splicing growing large-area single-crystal diamond |
| CN108677246A (en) * | 2018-06-26 | 2018-10-19 | 西安交通大学 | A method of splicing growing large-area single-crystal diamond of laterally putting up a bridge |
| CN110857467A (en) * | 2018-08-23 | 2020-03-03 | 中国科学院宁波材料技术与工程研究所 | Diamond compact and preparation method thereof |
| CN108977880A (en) * | 2018-08-29 | 2018-12-11 | 西安交通大学 | A method of intersecting splicing growing large-area single-crystal diamond |
| CN109161964A (en) * | 2018-09-30 | 2019-01-08 | 济南中乌新材料有限公司 | A kind of preparation method of large scale cvd diamond crystal |
| CN109989111A (en) * | 2019-03-13 | 2019-07-09 | 电子科技大学 | Preparation method, monocrystal thin films and the resonator of spliced small size monocrystal thin films |
| CN110079860A (en) * | 2019-03-29 | 2019-08-02 | 郑州磨料磨具磨削研究所有限公司 | A kind of splicing growing method of large size single crystal diamond epitaxial wafer |
| CN110079860B (en) * | 2019-03-29 | 2020-10-02 | 郑州磨料磨具磨削研究所有限公司 | Splicing growth method of large-size single crystal diamond epitaxial wafer |
| CN112442735A (en) * | 2019-08-30 | 2021-03-05 | 西安交通大学 | Method for growing large-area single crystal diamond by adsorption splicing |
| 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 |
| CN111270313A (en) * | 2020-04-01 | 2020-06-12 | 湖州中芯半导体科技有限公司 | Method for splicing CVD diamond single crystals |
| CN112064111A (en) * | 2020-08-18 | 2020-12-11 | 北京大学东莞光电研究院 | Preparation device and preparation method of large-diameter diamond sheet |
| CN112064111B (en) * | 2020-08-18 | 2021-09-07 | 北京大学东莞光电研究院 | Preparation device and preparation method of large-diameter diamond sheet |
| CN114150376A (en) * | 2021-10-14 | 2022-03-08 | 吉林大学 | Large-size single crystal diamond splicing growth method |
| CN114150376B (en) * | 2021-10-14 | 2023-10-24 | 吉林大学 | Large-size single crystal diamond splicing growth method |
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Application publication date: 20180601 |