CN108977880A - A method of intersecting splicing growing large-area single-crystal diamond - Google Patents

A method of intersecting splicing growing large-area single-crystal diamond Download PDF

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Publication number
CN108977880A
CN108977880A CN201810993970.4A CN201810993970A CN108977880A CN 108977880 A CN108977880 A CN 108977880A CN 201810993970 A CN201810993970 A CN 201810993970A CN 108977880 A CN108977880 A CN 108977880A
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China
Prior art keywords
crystal diamond
splicing
diamond
generated
long face
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Pending
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CN201810993970.4A
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Chinese (zh)
Inventor
王宏兴
王艳丰
常晓慧
王若铮
刘璋成
赵丹
魏孔庭
邵国庆
张景文
卜忍安
侯洵
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Xi'an Te Te Semiconductor Technology Co ltd
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Xian Jiaotong University
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Priority to CN201810993970.4A priority Critical patent/CN108977880A/en
Publication of CN108977880A publication Critical patent/CN108977880A/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/04Diamond
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02Epitaxial-layer growth
    • C30B25/18Epitaxial-layer growth characterised by the substrate
    • C30B25/186Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02Epitaxial-layer growth
    • C30B25/18Epitaxial-layer growth characterised by the substrate
    • C30B25/20Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer

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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 for intersecting splicing growing large-area single-crystal diamond, n single-crystal diamond splicing, and n is the positive integer more than or equal to 2;Wherein, the long face to be generated of adjacent single crystalline diamond is not parallel two-by-two, and forms crosspoint in adjacent long face to be generated;Grow complete large single crystal diamond simultaneously in the long face to be generated of n single-crystal diamond.Two pieces of diamond single crystal microstructures of growth connection since crosspoint, then entire splicing inclined-plane is gradually extended to, it realizes the secured connection of two blocks of diamonds and forms monocrystalline on splicing inclined-plane, grow complete large area single-crystal diamond for splicing and provide a kind of new method.

Description

A method of intersecting splicing growing large-area single-crystal diamond
[technical field]
The invention belongs to Material growth technical fields, and in particular to a kind of to intersect splicing growing large-area single-crystal diamond Method.
[background technique]
Single-crystal diamond has the performances such as excellent heat, electricity, sound, light, Biostatic as a kind of wide bandgap semiconductor. Such as: thermal conductivity is high, small, especially at high temperature the heat dissipation of hot melt is more significant, and forbidden bandwidth is wide, electrons and holes migrate Rate is big, critical breakdown electric field is big, most hard natural materials, all has high transmitance to infrared entire wave band diamond from ultraviolet (in addition to about 3~5 μm of positions just other than small absorption peak), chemical stability, the non-oxidizing acid being resistant at various temperature, nothing Poison.This makes diamond have broad application prospects and huge economic potential in related fields.Since successfully preparing people Since work diamond synthesis, the preparation of diamond just becomes very burning hot.However, the diamond size prepared at present all compares It is smaller, limit the related application of diamond.In order to play the application potential of diamond, prepare large-sized single-crystal diamond at For inevitable problem.Therefore, necessary for the research of large area single crystal diamond film.
Splicing and hetero-epitaxial process are the main methods of current growing large-size single-crystal diamond.Although different at present The maximum gauge of matter epitaxial diamond reaches 92 millimeters, however, this method still has many problems, such as: substrate preparation Complex process, substrate uniformity be poor, heat power transmission and stress distribution are uneven in growth course, during causing hetero-epitaxy Diamond nucleation is difficult, diamond is easily detached from substrate material or even bursts, and the quality of hetero-epitaxy single-crystal diamond is universal It is not high.Splicing growth is that the small single-crystal diamond of muti-piece is stitched together, and is put into microwave plasma chemical depositing system, is led to Epitaxial growth is crossed, connecting cracks are sticked together using the single-crystal diamond newly grown, then proceed to epitaxial growth, is obtained complete Large single crystal diamond.The splicing growing large-area diamond problems faced hetero-epitaxy that is far from is more, it is only necessary to solve splicing Complete monocrystalline is securely spliced and formed to seam in the process, can accomplish the not only quick but also growing large-area single crystal diamond of high quality Stone.But during splicing, due to can not be completely the same in stitching portion atomic arrangement, existing very big may be two Block diamond can not form complete monocrystalline at all, and respective extension is respective, and splicing is caused to fail.
[summary of the invention]
The object of the present invention is to provide a kind of methods for intersecting splicing growing large-area single-crystal diamond, to solve existing skill Art is during splicing, due to the problem of stitching portion atomic arrangement can not be completely the same, and splicing is easy to cause to fail.
The invention adopts the following technical scheme: a kind of method for intersecting splicing growing large-area single-crystal diamond, n monocrystalline Diamond is connected together, and n is the positive integer more than or equal to 2;Wherein, the long face to be generated of adjacent single crystalline diamond is uneven two-by-two Row, and two adjacent long faces to be generated intersect to form crosspoint;Covering institute is grown in the long face to be generated of n single-crystal diamond State the complete large single crystal diamond on n single-crystal diamond surface.
Further, the inclination angle of long face to be generated with respect to the horizontal plane is acute angle.
Further, before splicing, single-crystal diamond is cleaned and is dried up.
Further, it is grown on the single-crystal diamond being stitched together using plasma chemical deposition technology at n Cover the complete large single crystal diamond on the n single-crystal diamond surface.
Compared with prior art, the present invention at least has the advantages that of the invention in diamond growth process, from Crosspoint starts growth two pieces of diamond single crystal microstructures of connection, then gradually extends to entire splicing inclined-plane, realizes two pieces The secured connection of diamond simultaneously forms monocrystalline on splicing inclined-plane, grows complete large area single-crystal diamond for splicing and provides one kind New method.
[Detailed description of the invention]
Fig. 1 is the obtained sample structure schematic diagram of the embodiment of the present invention;
Fig. 2-1 to Fig. 2-3 is the method flow diagram of the embodiment of the present invention.
Wherein, 1. single-crystal diamond a, 2. single-crystal diamond b, 3. splicing inclined-plane a, 4. splice inclined-plane b, 5. crosspoints.
[specific embodiment]
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
The present invention provides it is a kind of intersect splicing growing large-area single-crystal diamond method, specifically: be to n monocrystalline Diamond is spliced, and n is the positive integer more than or equal to 2;Wherein, the long face to be generated of adjacent single crystalline diamond is not parallel two-by-two, And crosspoint is intersected to form in two adjacent long faces to be generated;Using plasma chemical deposition technology in n single-crystal diamond Long face to be generated on grow covering n single-crystal diamond surface complete large single crystal diamond, as shown in Figure 1.
Long face to be generated is located at phase the same side of each single-crystal diamond, and long face to be generated can be in each single-crystal diamond Top surface, front or behind etc. surface are cut or the inclined-plane that is ground, adjacent long face to be generated must in long face to be generated shape At crosspoint, and crosspoint cannot be formed on the extended line of long face to be generated.
When n is 2, a method of intersecting splicing growing large-area single-crystal diamond specifically: to single-crystal diamond a1 It is cleaned, and is dried up with single-crystal diamond b2;Single-crystal diamond a1 is ground again to obtain splicing inclined-plane a3, by single-crystal diamond B2 grinds to obtain splicing inclined-plane b4;Single-crystal diamond a1 and single-crystal diamond b2 is spliced again, so that splicing inclined-plane a3 and and spelling It is not parallel to meet inclined-plane b4, and forms crosspoint 5 on splicing inclined-plane;Using plasma chemical deposition technology in single-crystal diamond Complete large single crystal diamond is grown on the splicing inclined-plane b4 of the splicing inclined-plane a3 and single-crystal diamond b2 of a1 simultaneously.
Embodiment
1) substrate of single-crystal diamond a1 and single-crystal diamond b2 select 3 х 0.5mm of (100) 3 х3Single-crystal diamond makes The substrate of single-crystal diamond a1 and single-crystal diamond b2 are cleaned with the sour alkali washing process of standard, remove the on-monocrystalline on surface Diamond phase, as shown in Fig. 2-1.
2) the splicing inclined-plane b4 of the splicing inclined-plane a3 and single-crystal diamond b2 of single-crystal diamond a1 is prepared using grinder, slightly Rugosity is less than 5nm, and gradient is 5 °, as shown in Fig. 2-2.
3) the splicing inclined-plane b4 of the splicing inclined-plane a3 of single-crystal diamond a1 and single-crystal diamond b2 is spliced manually, and ensured Splice inclined-plane a3 and splicing inclined-plane b4 be not parallel and two sample sides on there is splicing crosspoint 5, as Figure 2-3;
5) extension is carried out to the substrate spliced using microwave plasma body technique, forms complete large single crystal diamond 6. The growth conditions of microwave plasma chemical deposition technique are as follows: power 600W, chamber pressure be 50Torr, total gas flow rate 500sccm, As shown in Figure 1.
The present invention is artificially to provide a tie point, shape between adjacent two blocks of diamonds in diamond growth process At the starting point of perfect monocrystalline, completes securely to connect and formed perfect microcosmic monocrystalline first in the tie point, then gradually extend To entire splicing inclined-plane, complete large area single-crystal diamond is grown for the splicing of small area monocrystalline and provides a kind of new method.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention Protection scope within.

Claims (4)

1. a kind of method for intersecting splicing growing large-area single-crystal diamond, which is characterized in that n single-crystal diamond connects Together, n is the positive integer more than or equal to 2;Wherein, two-by-two the long face to be generated of adjacent single crystalline diamond it is not parallel and adjacent two A long face to be generated intersects to form crosspoint;The covering n single crystal diamond is grown in the long face to be generated of n single-crystal diamond The complete large single crystal diamond on stone surface.
2. a kind of method for intersecting splicing growing large-area single-crystal diamond as described in claim 1, which is characterized in that described The inclination angle of long face to be generated with respect to the horizontal plane is acute angle.
3. a kind of method for intersecting splicing growing large-area single-crystal diamond as claimed in claim 1 or 2, which is characterized in that Before splicing, single-crystal diamond is cleaned and is dried up.
4. a kind of method for intersecting splicing growing large-area single-crystal diamond as claimed in claim 1 or 2, which is characterized in that It is grown on the single-crystal diamond being stitched together using plasma chemical deposition technology at n and covers the n single crystal diamond The complete large single crystal diamond on stone surface.
CN201810993970.4A 2018-08-29 2018-08-29 A method of intersecting splicing growing large-area single-crystal diamond Pending CN108977880A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112725902A (en) * 2020-12-23 2021-04-30 西安交通大学 Single crystal diamond substrate structure and splicing processing method thereof
CN113584580A (en) * 2021-08-05 2021-11-02 北京大学东莞光电研究院 Radial growth method and device for diamond wafer

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
舒国阳等: "Mosaic拼接法高质量大尺寸单晶金刚石生长研究", 《中国优秀硕士学位论文全文数据库(工程科技I辑)》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN113584580A (en) * 2021-08-05 2021-11-02 北京大学东莞光电研究院 Radial growth method and device for diamond wafer
CN113584580B (en) * 2021-08-05 2022-08-19 北京大学东莞光电研究院 Radial growth method and device for diamond wafer

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