CN108754600A - A method of splicing growing large-area single-crystal diamond - Google Patents
A method of splicing growing large-area single-crystal diamond Download PDFInfo
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- CN108754600A CN108754600A CN201810671783.4A CN201810671783A CN108754600A CN 108754600 A CN108754600 A CN 108754600A CN 201810671783 A CN201810671783 A CN 201810671783A CN 108754600 A CN108754600 A CN 108754600A
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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
- 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
- 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 discloses a kind of methods of splicing growing large-area single-crystal diamond, in the same direction by two pieces of single-crystal diamond Mosaic faces, it is chamfer from two single-crystal diamond upper surfaces to single-crystal diamond lower surface, cutting forms two splicing inclined-planes being mutually parallel, then by two splicing inclined-plane splicings, finally complete large area single-crystal diamond is grown in single-crystal diamond upper surface.Solves the problem of stitching portion slight crack occurred during splicing diamond in the prior art is big, leads to splicing failure.
Description
【Technical field】
The invention belongs to Material growth technical fields, and in particular to a kind of side of splicing growing large-area single-crystal diamond
Method.
【Background technology】
Single-crystal diamond has the performances such as excellent heat, electricity, power, light, Biostatic as a kind of wide bandgap semiconductor.
In calorifics field, the thermal conductivity of diamond is high, small, especially at high temperature the heat dissipation of hot melt is more notable, therefore can be with
As fabulous heat sink material；In electricity field, diamond has wide energy gap, high electrons and holes mobility, big
The excellent properties such as critical breakdown electric field, therefore it is huge in the high-power field application potential of high voltagehigh frequency；In mechanics field, gold
Hard rock is known most hard natural materials, therefore can be used under the deposition material and vacuum condition of cutting tool, grinding tool needing
Dry friction material；In optical field, diamond in addition to about 3~5 μm of positions just other than small absorption peak, from ultraviolet to infrared
Entire wave band diamond all has high transmitance, therefore can use it for radar protection cover；In biological field, diamond tool
There is good chemical stability, the non-oxidizing acid being resistant at various temperature, and because the ingredient of diamond is carbon, it is nontoxic, it is right
Human body containing a large amount of carbon does not play rejection, and therefore, diamond is ideal medico's object implantation material, such as heart again
Valve.And these applications all be unable to do without the preparation of high-quality large-size monocrystal diamond, therefore single-crystal diamond is given birth to
Long research is necessary.
Currently, the method for growth single-crystal diamond has very much, such as Microwave plasma CVD, DC glow
The methods of electric discharge, high temperature and pressure.Using it is more be MPCVD method, the benefit of this method growth
It is plasma and cavity separation, to reduce corrasion of the plasma to cavity, reduces the pollution of impurity, improves
The single-crystal diamond quality of epitaxial growth.The microwave source generally used is 2.45GHz, and growth technique is：Operating pressure 50-
100Torr (support), temperature 800-1000 DEG C (degree Celsius), power 500-800W (watt).By the way that methane, hydrogen, nitrogen, oxygen is added
Gas etc. provides predecessor for diamond growth, close by adjusting gas component, reaction temperature, chamber pressure, plasma power
The conditions such as degree realize the growth of single-crystal diamond.
Large-sized single-crystal diamond in order to obtain, splicing are used.This method is by two pieces of small single crystal diamonds
Stone is stitched together, and is put into microwave plasma chemical depositing system, by epitaxial growth, uses the single-crystal diamond newly grown
Splicing slight crack is sticked together, epitaxial growth is then proceeded to, obtains complete large area single-crystal diamond.But in splicing
In the process, the slight crack of stitching portion may be very big, this plays the process that slight crack is bonded to the single-crystal diamond newly grown below very
Big inhibition, or even two pieces of small single-crystal diamonds can not be stitched together, cause splicing to fail.Stitching portion is caused to split
The big possible factor of trace has very much, such as：Early growth period leads to two pieces small of single-crystal diamond relative position due to mechanical oscillation
It shifts；Early growth period leads to relative position movement etc. of the flow perturbation to small diamond due to the addition of hydrogen, methane.
【Invention content】
The object of the present invention is to provide a kind of methods of splicing growing large-area single-crystal diamond, to solve in the prior art
It is big to splice the stitching portion slight crack occurred during diamond, the problem of causing to splice failure.
The present invention uses following technical scheme：A method of splicing growing large-area single-crystal diamond, by two pieces of small lists
Diamond Mosaic face is chamfer in the same direction, from two single-crystal diamond upper surfaces to single-crystal diamond lower surface, and cutting is formed
Two splicing inclined-planes being mutually parallel, then by two splicing inclined-plane splicings, finally in single-crystal diamond upper surface, growth is complete
The large area single-crystal diamond without splicing seams.
Further, it is specifically implemented according to the following steps：
1), single-crystal diamond A and single-crystal diamond B are cleaned, and dried up；
2) single-crystal diamond A Mosaic faces, are beveled to the lower surfaces single-crystal diamond A from the upper surfaces single-crystal diamond A, are formed
Single-crystal diamond A splices inclined-plane；Single-crystal diamond B Mosaic faces are beveled to list from the upper surfaces single-crystal diamond B in the same direction
The lower surfaces diamond B form single-crystal diamond B and splice inclined-plane；
3), the splicing inclined-planes single-crystal diamond A and single-crystal diamond B splicings inclined-plane are spliced；
4), using plasma chemical deposition technology the upper surfaces single-crystal diamond A and the upper surfaces single-crystal diamond B simultaneously
Grow complete large area single-crystal diamond.
Further, the splicing inclined-plane of single-crystal diamond A is parallel with the splicing inclined-plane of single-crystal diamond B, and roughness exists
Between 1nm and 100 μm.
Further, the angle that single-crystal diamond A splices inclined-plane and the upper surfaces single-crystal diamond A is acute angle, and range is more than
0 ° and be less than 90 °.
Further, the angle that single-crystal diamond B splices inclined-plane and the lower surfaces single-crystal diamond B is acute angle, and range is more than
0 ° and be less than 90 °.
Second of technical solution that the present invention uses is a kind of large area single-crystal diamond of splicing growth, including splicing
The splicing of the single-crystal diamond A and single-crystal diamond B of growth and shaping, single-crystal diamond A and single-crystal diamond B use claim
The method of any one in 1-5 is realized.
Compared with prior art, the present invention at least has the advantages that：Invention increases the contact surfaces of Mosaic face
Product so that single-crystal diamond is splicing in epitaxial process, and splicing gap keeps very little, is easy to lattice amendment, is formed single
Crystalline substance interconnection provides a kind of new method for splicing growing large-area single-crystal diamond.
【Description of the drawings】
Fig. 1 is a kind of obtained sample overall diagram of method of splicing growing large-area single-crystal diamond of the present invention；
Fig. 2-1 to Fig. 2-3 is a kind of method flow diagram of splicing growing large-area single-crystal diamond of the present invention；
Fig. 3 is the optical photograph of the large area single-crystal diamond grown using the present invention.
Wherein：1. the lower surfaces single-crystal diamond A；2. the upper surfaces single-crystal diamond A；3. single-crystal diamond A Mosaic faces；4. single
The upper surfaces diamond B；5. the lower surfaces single-crystal diamond B；6. single-crystal diamond B Mosaic faces；7. single-crystal diamond B splicings are oblique
Face；8. single-crystal diamond A splices inclined-plane；9. large area single-crystal diamond.
【Specific implementation mode】
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
The present invention provides a kind of methods of splicing growing large-area single-crystal diamond will as shown in Fig. 2-1 and Fig. 2-2
Two pieces of single-crystal diamond Mosaic faces are chamfer in the same direction, from two single-crystal diamond upper surfaces to single-crystal diamond lower surface, are cut
It cuts to form two splicing inclined-planes being mutually parallel, then by two splicing inclined-plane splicings, finally look unfamiliar in single-crystal diamond upper table
The long completely large area single-crystal diamond without splicing seams, shown in figure Fig. 1.Fig. 3 is uses the large area list that is grown of the present invention
The optical photograph of diamond, due in microscope opposite side polishing, it is possible to see original splicing inclined-plane.The figure illustrates
Two diamond splicings can be grown to serve as complete, not splicing seams large area by the method spliced using inclined-plane
Single-crystal diamond.
The present invention is specifically implemented according to the following steps：
1), single-crystal diamond A and single-crystal diamond B are cleaned, and dried up, as shown in Fig. 2-1；
2), as shown in Fig. 2-2, single-crystal diamond A Mosaic faces are beveled to single-crystal diamond from the upper surfaces single-crystal diamond A
The lower surfaces A form single-crystal diamond A and splice inclined-plane；In the same direction by single-crystal diamond B Mosaic faces from single-crystal diamond B
Surface is beveled to the lower surfaces single-crystal diamond B, forms single-crystal diamond B and splices inclined-plane；
3), the splicing inclined-planes 8 single-crystal diamond A and single-crystal diamond B splicings inclined-plane 7 are spliced, as Figure 2-3；
4), same in the upper surfaces single-crystal diamond A 2 and the upper surfaces single-crystal diamond B 4 using plasma chemical deposition technology
The complete large area single-crystal diamonds 9 of Shi Shengchang, as shown in Figure 1.
Wherein, it is parallel with the splicing inclined-plane 7 single-crystal diamond B to splice inclined-plane 8 by single-crystal diamond A, and roughness in 1nm and
Between 100 μm.Splice that inclined-plane is parallel and to keep the benefit of certain roughness be that can increase the contact area in two faces, allows two
A face perfection fitting so that contact seam reduces, and is easy to form atom level interconnection.
The angle of the splicing inclined-planes 8 single-crystal diamond A and the upper surfaces single-crystal diamond A 2 is acute angle, and range is more than 0 ° and small
In 90 °.The angle of the splicing inclined-planes 7 single-crystal diamond B and the lower surfaces single-crystal diamond B 5 is acute angle, and range is more than 0 ° and is less than
90°.The purpose designed using the angle number of degrees is to increase the contact area in two faces, to increase the friction of two diamonds
Power, avoiding diamond in growth course, there is a phenomenon where relative displacements.
Invention increases the contacts area of Mosaic face so that single-crystal diamond is splicing in epitaxial process, spells
It connects gap and keeps very little, be easy to lattice amendment, form monocrystalline interconnection, grow big face for splicing
Product single-crystal diamond provides a kind of new method.
Embodiment
It is a kind of splicing growing large-area single-crystal diamond method comprise the following steps：
1) single-crystal diamond A and B substrates select (100) single-crystal diamond, using the sour alkali washing process of standard to monocrystalline gold
Hard rock A and B substrate is cleaned, and the on-monocrystalline diamond phase on surface is removed, and then uses alcohol, acetone, deionized water to list
Diamond A and B are cleaned, and are dried up using nitrogen, as shown in Fig. 2-1.
2) it uses single crystal diamond stone grinder to grind single-crystal diamond A Mosaic faces 3, it is oblique to obtain single-crystal diamond A splicings
Face 8, roughness are less than 5nm；The inclined-plane runs through the lower surfaces single-crystal diamond A 1 and the upper surfaces single-crystal diamond A 2, and and monocrystalline
The angle of the upper surfaces diamond A 2 is 60 °, as shown in Fig. 2-2.
3) it uses single crystal diamond stone grinder to grind single-crystal diamond B Mosaic faces 6, it is oblique to obtain single-crystal diamond B splicings
Face 7, roughness are less than 5nm；The inclined-plane runs through the upper surfaces single-crystal diamond B 4 and the lower surfaces single-crystal diamond B 5, and and monocrystalline
Diamond A splicings inclined-plane 8 is parallel, as shown in Fig. 2-2.
4) the splicing inclined-planes 7 single-crystal diamond B and single-crystal diamond A splicings inclined-plane 8 are spliced manually, as Figure 2-3；
5) as shown in Figure 1, carrying out extension to the substrate spliced using microwave plasma body technique, complete big face is formed
Product single-crystal diamond 9.Growth condition is：Power 600W, chamber pressure be 50Torr, total gas flow rate 500sccm,
The above content is merely illustrative of the invention's technical idea, and protection scope of the present invention cannot be limited with this, every to press
According to technological thought proposed by the present invention, any change done on the basis of technical solution each falls within claims of the present invention
Protection domain within.
Claims (6)
1. a kind of method of splicing growing large-area single-crystal diamond, which is characterized in that by two pieces of single-crystal diamond Mosaic face edges
Same direction is chamfer from two single-crystal diamond upper surfaces to single-crystal diamond lower surface, and cutting forms two spellings being mutually parallel
Inclined-plane is connect, then by two splicing inclined-plane splicings, finally grows the completely big face without splicing seams in single-crystal diamond upper surface
Product single-crystal diamond.
2. a kind of method of splicing growing large-area single-crystal diamond as described in claim 1, which is characterized in that specifically according to
Following steps are implemented：
1), single-crystal diamond A and single-crystal diamond B are cleaned, and dried up；
2) single-crystal diamond A Mosaic faces (3), are beveled to the lower surfaces single-crystal diamond A from the upper surfaces single-crystal diamond A (2)
(1), single-crystal diamond A splicings inclined-plane (8) are formed；In the same direction by single-crystal diamond B Mosaic faces (6) from single-crystal diamond B
Upper surface (4) is beveled to the lower surfaces single-crystal diamond B (5), forms single-crystal diamond B splicings inclined-plane (7)；
3), single-crystal diamond A splicings inclined-plane (8) and single-crystal diamond B splicings inclined-plane (7) are spliced；
4), same in the upper surfaces single-crystal diamond A (2) and the upper surfaces single-crystal diamond B (4) using plasma chemical deposition technology
The complete large area single-crystal diamonds (9) of Shi Shengchang.
3. a kind of method of splicing growing large-area single-crystal diamond as claimed in claim 2, which is characterized in that the monocrystalline
The splicing inclined-plane (8) of diamond A is parallel with splicing inclined-plane (7) of single-crystal diamond B, and roughness is between 1nm and 100 μm.
4. a kind of method of splicing growing large-area single-crystal diamond as claimed in claim 2, which is characterized in that the monocrystalline
The angle of diamond A splicings inclined-plane (8) and the upper surfaces single-crystal diamond A (2) is acute angle, and range is more than 0 ° and is less than 90 °.
5. a kind of method of splicing growing large-area single-crystal diamond as claimed in claim 2, which is characterized in that the monocrystalline
The angle of diamond B splicings inclined-plane (7) and the lower surfaces single-crystal diamond B (5) is acute angle, and range is more than 0 ° and is less than 90 °.
6. a kind of large area single-crystal diamond of splicing growth, which is characterized in that the single-crystal diamond A including splicing growth and shaping
With single-crystal diamond B, the splicing of the single-crystal diamond A and single-crystal diamond B are using described in any one in claim 1-5
Method realize.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810671783.4A CN108754600A (en) | 2018-06-26 | 2018-06-26 | A method of splicing growing large-area single-crystal diamond |
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| CN201810671783.4A CN108754600A (en) | 2018-06-26 | 2018-06-26 | A method of splicing growing large-area single-crystal diamond |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110184653A (en) * | 2019-06-04 | 2019-08-30 | 北京科技大学 | A method of improving large size single crystal diamond seam quality |
| 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 |
| CN112391680A (en) * | 2020-11-16 | 2021-02-23 | 物生生物科技(北京)有限公司 | Splicing growth process for large-size single crystal diamond |
| 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 |
| CN112725902A (en) * | 2020-12-23 | 2021-04-30 | 西安交通大学 | Single crystal diamond substrate structure and splicing processing method thereof |
| CN114571079A (en) * | 2022-04-08 | 2022-06-03 | 中南大学 | Ultrafast laser preparation device and preparation method of large-breadth window mirror |
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| WO2004027123A1 (en) * | 2002-09-20 | 2004-04-01 | Element Six Limited | Single crystal diamond |
| CN108103570A (en) * | 2017-12-11 | 2018-06-01 | 湖北碳六科技有限公司 | A kind of method and system for splicing growth single-crystal diamond |
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2018
- 2018-06-26 CN CN201810671783.4A patent/CN108754600A/en active Pending
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| WO2004027123A1 (en) * | 2002-09-20 | 2004-04-01 | Element Six Limited | Single crystal diamond |
| CN108103570A (en) * | 2017-12-11 | 2018-06-01 | 湖北碳六科技有限公司 | A kind of method and system for splicing growth single-crystal diamond |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110184653A (en) * | 2019-06-04 | 2019-08-30 | 北京科技大学 | A method of improving large size single crystal diamond seam quality |
| 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 |
| 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 |
| CN112391680A (en) * | 2020-11-16 | 2021-02-23 | 物生生物科技(北京)有限公司 | Splicing growth process for large-size single crystal diamond |
| CN112725902A (en) * | 2020-12-23 | 2021-04-30 | 西安交通大学 | Single crystal diamond substrate structure and splicing processing method thereof |
| CN112725902B (en) * | 2020-12-23 | 2022-04-19 | 西安交通大学 | Single crystal diamond substrate structure and splicing processing method thereof |
| CN114571079A (en) * | 2022-04-08 | 2022-06-03 | 中南大学 | Ultrafast laser preparation device and preparation method of large-breadth window mirror |
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Effective date of registration: 20211117 Address after: 710000 No. 4169, maker space, 1896, 4th floor, returnees building, No. 18, Gaoxin 1st Road, high tech Zone, Xi'an, Shaanxi Province Applicant after: Xi'an te te Semiconductor Technology Co.,Ltd. Address before: Beilin District Xianning West Road 710049, Shaanxi city of Xi'an province No. 28 Applicant before: XI'AN JIAOTONG University |
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Application publication date: 20181106 |