CN111270313A - Method for splicing CVD diamond single crystals - Google Patents

Method for splicing CVD diamond single crystals Download PDF

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Publication number
CN111270313A
CN111270313A CN202010252432.7A CN202010252432A CN111270313A CN 111270313 A CN111270313 A CN 111270313A CN 202010252432 A CN202010252432 A CN 202010252432A CN 111270313 A CN111270313 A CN 111270313A
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CN
China
Prior art keywords
cvd diamond
single crystal
diamond single
seed crystals
crystal seed
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CN202010252432.7A
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Chinese (zh)
Inventor
赵芬霞
刘宏明
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Huzhou Zhongxin Semiconductor Technology Co Ltd
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Huzhou Zhongxin Semiconductor Technology Co Ltd
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Priority to CN202010252432.7A priority Critical patent/CN111270313A/en
Publication of CN111270313A publication Critical patent/CN111270313A/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
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/06Joining of crystals
    • 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
    • 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

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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 relates to the technical field of artificial diamonds and discloses a method for splicing CVD diamond single crystals, which comprises the following steps: preparing tools and raw materials, preparing a proper amount of CVD diamond single crystal seed crystals, and preparing an X-ray diffraction spectrometer, a laser cutting machine, a grinding machine and a CVD diamond growth machine; secondly, accurately determining the internal crystal directions of the plurality of CVD diamond single crystal seed crystals by using an X-ray diffraction spectrometer; step three, according to the internal crystal orientation of the plurality of CVD diamond single crystal seed crystals in the step one, laser cutting is carried out on the plurality of CVD diamond single crystal seed crystals in sequence by using a laser cutting machine; and step four, grinding the cutting surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals in the step three by using a grinder to be smooth. The method for splicing the CVD diamond single crystals solves the problem that large CVD diamond single crystals are difficult to produce by the principle that the CVD diamond can automatically repair lattice defects in the growth process.

Description

Method for splicing CVD diamond single crystals
Technical Field
The invention relates to the technical field of artificial diamonds, in particular to a method for splicing CVD diamond single crystals.
Background
CVD diamond, a mixture of carbon-containing gas and oxygen gas, is activated at high temperature and pressure below normal atmospheric pressure to decompose, form active diamond carbon atoms, and deposit on a substrate to grow polycrystalline diamond (or deposit diamond single crystal or quasi-single crystal under controlled deposition growth conditions), and because CVD diamond does not contain any metal catalyst, its thermal stability is close to that of natural diamond. Like high-temperature and high-pressure artificially synthesized polycrystalline diamond, CVD diamond grains are also in disordered arrangement and have no brittle cleavage plane, so that the CVD diamond grains are isotropic. CVD diamond is now used as one of the tool materials.
At present, the synthesis of the single crystal diamond is limited by the size, a single natural diamond or a synthetic single crystal diamond sheet is usually adopted as a seed crystal to grow on the original size, the large-size single crystal diamond is rare and expensive, so that the synthesized diamond is limited by the size of the seed crystal, and the polycrystalline diamond is easy to grow due to more defects on the edge of the seed crystal and difficult to control, so that the size of the obtained product is not larger than the size of the original seed crystal, and the large-size single crystal diamond cannot be obtained.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for splicing CVD diamond single crystals, which has the advantage of solving the problem that large CVD diamond single crystals are difficult to produce by using the principle that the CVD diamond can automatically repair lattice defects in the growth process, and solves the problems provided by the background technology.
(II) technical scheme
In order to solve the problem that a large CVD diamond single crystal is difficult to produce by the principle that the CVD diamond can automatically repair lattice defects in the growth process, the invention provides the following technical scheme: a method of splicing CVD diamond single crystals comprising the steps of:
preparing tools and raw materials, preparing a proper amount of CVD diamond single crystal seed crystals, and preparing an X-ray diffraction spectrometer, a laser cutting machine, a grinding machine and a CVD diamond growth machine;
secondly, accurately determining the internal crystal directions of the plurality of CVD diamond single crystal seed crystals by using an X-ray diffraction spectrometer;
step three, according to the internal crystal orientation of the plurality of CVD diamond single crystal seed crystals in the step one, laser cutting is carried out on the plurality of CVD diamond single crystal seed crystals in sequence by using a laser cutting machine;
step four, grinding the cutting surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals in the step three by using a grinder to be smooth;
step five, sequentially placing a plurality of the CVD diamond single crystal seed crystals ground in the step four in a CVD diamond growth machine for growth, so as to obtain a large and complete CVD diamond single crystal;
and step six, cutting off the seed crystal part on the outer surface of the large complete CVD diamond single crystal in the step five to obtain a seamless complete CVD diamond single crystal finished product.
Preferably, in the first step, a plurality of CVD diamond single crystal seed crystals are cleaned by acetone and alcohol liquid and dried at the drying temperature of 50 ℃.
Preferably, the contact surface contact degree between a plurality of CVD diamond single crystal seed crystals in the fourth step is 100%.
Preferably, the internal temperature in the diamond growth machine in the step five is 800-.
Preferably, in step five, a plurality of the CVD diamond single crystal seed crystals are closely arranged according to a grid-shaped structure.
Preferably, in the third step, a plurality of CVD diamond single crystal seed crystals are all cut into square arrangement.
(III) advantageous effects
Compared with the prior art, the invention provides a method for splicing CVD diamond single crystals, which has the following beneficial effects:
1. the method for splicing the CVD diamond single crystals comprises the steps of accurately determining the internal crystal orientation of a plurality of CVD diamond single crystal seed crystals through an X-ray diffraction spectrometer, sequentially carrying out laser cutting on the plurality of CVD diamond single crystal seed crystals by using a laser cutting machine, grinding the cutting surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals smoothly by using a grinding machine, sequentially placing the plurality of ground CVD diamond single crystal seed crystals in a CVD diamond growth machine for growth, obtaining a large complete CVD diamond single crystal, cutting off the seed crystal part on the outer surface of the large complete CVD diamond single crystal to obtain a seamless complete CVD diamond single crystal finished product, and solving the problem that the large CVD diamond single crystal is difficult to produce through the principle that the CVD diamond can automatically repair lattice defects in the growth process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method of splicing CVD diamond single crystals comprising the steps of:
preparing tools and raw materials, preparing a proper amount of CVD diamond single crystal seed crystals, and preparing an X-ray diffraction spectrometer, a laser cutting machine, a grinding machine and a CVD diamond growth machine;
accurately determining the internal crystal directions of the plurality of CVD diamond single crystal seed crystals by using an X-ray diffraction spectrometer, so that the automatic growth directions of the plurality of CVD diamond single crystal seed crystals can be conveniently determined, and the plurality of CVD diamond single crystal seed crystals can be conveniently cut;
step three, according to the internal crystal orientation of the plurality of CVD diamond single crystal seed crystals in the step one, laser cutting is carried out on the plurality of CVD diamond single crystal seed crystals in sequence by using a laser cutting machine;
step four, grinding the cutting surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals in the step three by using a grinder to be smooth;
step five, sequentially placing a plurality of the CVD diamond single crystal seed crystals ground in the step four in a CVD diamond growth machine for growth, so as to obtain a large and complete CVD diamond single crystal;
and step six, cutting off the seed crystal part on the outer surface of the large complete CVD diamond single crystal in the step five to obtain a seamless complete CVD diamond single crystal finished product.
And in the step one, cleaning and drying the plurality of CVD diamond single crystal seed crystals by adopting acetone and alcohol liquid, wherein the drying temperature is 50 ℃, the organic matters on the surfaces of the plurality of CVD diamond single crystal seed crystals are conveniently cleaned, and the CVD diamond single crystal seed crystals are quickly dried, so that the growth of the CVD diamond single crystal seed crystals is prevented from being influenced.
And in the step four, the contact surface contact degree between the plurality of CVD diamond single crystal seed crystals is 100%, so that two adjacent CVD diamond single crystal seed crystals can be in close contact, and the two adjacent CVD diamond single crystal seed crystals can be conveniently grown into a whole.
And fifthly, the internal temperature in the diamond growth machine is 800-1000 ℃, and gases such as methane, acetone, carbon dioxide and the like are introduced into the diamond growth machine, so that the CVD diamond single crystal seed crystals in the diamond growth machine can grow rapidly.
And in the fifth step, the plurality of CVD diamond single crystal seed crystals are closely arranged according to a grid structure, so that the plurality of CVD diamond single crystal seed crystals can be conveniently grown into a large and complete CVD diamond single crystal seed crystal finished product.
And in the third step, the plurality of diamond single crystal seed crystals are all cut into square arrangement, so that the plurality of CVD diamond single crystal seed crystals can be conveniently and closely spliced.
In conclusion, the method for splicing the CVD diamond single crystals comprises the steps of preparing tools and raw materials, preparing a proper amount of CVD diamond single crystal seed crystals, and preparing an X-ray diffraction spectrometer, a laser cutting machine, a grinding machine and a CVD diamond growing machine; the method comprises the following steps of accurately determining the internal crystal directions of a plurality of CVD diamond single crystal seed crystals by using an X-ray diffraction spectrometer, conveniently determining the automatic growth directions of the plurality of CVD diamond single crystal seed crystals, conveniently cutting the plurality of CVD diamond single crystal seed crystals, and sequentially performing laser cutting on the plurality of CVD diamond single crystal seed crystals by using a laser cutting machine; grinding the cut surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals by using a grinder to be smooth; placing a plurality of ground CVD diamond single crystal seed crystals in a CVD diamond growth machine in sequence for growth, so as to obtain a large and complete CVD diamond single crystal; and cutting off the seed crystal part on the outer surface of the large complete CVD diamond single crystal to obtain a seamless complete CVD diamond single crystal finished product.
It is to be noted that the term "comprises," "comprising," or any other variation thereof is intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. A method of splicing CVD diamond single crystals comprising the steps of:
preparing tools and raw materials, preparing a proper amount of CVD diamond single crystal seed crystals, and preparing an X-ray diffraction spectrometer, a laser cutting machine, a grinding machine and a CVD diamond growth machine;
secondly, accurately determining the internal crystal directions of the plurality of CVD diamond single crystal seed crystals by using an X-ray diffraction spectrometer;
step three, according to the internal crystal orientation of the plurality of CVD diamond single crystal seed crystals in the step one, laser cutting is carried out on the plurality of CVD diamond single crystal seed crystals in sequence by using a laser cutting machine;
step four, grinding the cutting surfaces of the plurality of laser-cut CVD diamond single crystal seed crystals in the step three by using a grinder to be smooth;
step five, sequentially placing a plurality of the CVD diamond single crystal seed crystals ground in the step four in a CVD diamond growth machine for growth, so as to obtain a large and complete CVD diamond single crystal;
and step six, cutting off the seed crystal part on the outer surface of the large complete CVD diamond single crystal in the step five to obtain a seamless complete CVD diamond single crystal finished product.
2. A method of splicing a CVD diamond single crystal according to claim 1, wherein: and in the first step, cleaning a plurality of CVD diamond single crystal seed crystals by adopting acetone and alcohol liquid, and drying at the drying temperature of 50 ℃.
3. A method of splicing a CVD diamond single crystal according to claim 1, wherein: step four, the contact surface contact degree among a plurality of CVD diamond single crystal seed crystals is 100%.
4. A method of splicing a CVD diamond single crystal according to claim 1, wherein: and fifthly, the internal temperature in the diamond growth machine is 800-1000 ℃, and gases such as methane, acetone, carbon dioxide and the like are introduced into the diamond growth machine.
5. A method of splicing a CVD diamond single crystal according to claim 1, wherein: and in the fifth step, a plurality of CVD diamond single crystal seed crystals are closely arranged according to a grid structure.
6. A method of splicing a CVD diamond single crystal according to claim 1, wherein: and in the third step, a plurality of CVD diamond single crystal seed crystals are all cut into square arrangement.
CN202010252432.7A 2020-04-01 2020-04-01 Method for splicing CVD diamond single crystals Pending CN111270313A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113529175A (en) * 2021-07-05 2021-10-22 深圳技术大学 Substrate, substrate splicing method and preparation method of single crystal diamond

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108754600A (en) * 2018-06-26 2018-11-06 西安交通大学 A method of splicing growing large-area single-crystal diamond
CN110230091A (en) * 2019-06-26 2019-09-13 北京科技大学 It is a kind of vertically to splice preparation large scale cvd diamond and cutting method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108754600A (en) * 2018-06-26 2018-11-06 西安交通大学 A method of splicing growing large-area single-crystal diamond
CN110230091A (en) * 2019-06-26 2019-09-13 北京科技大学 It is a kind of vertically to splice preparation large scale cvd diamond and cutting method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YAMADA.H等: ""A 2-in. mosaic wafer made of a single-crystal diamond"", 《APPLIED PHYSICS LETTERS》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113529175A (en) * 2021-07-05 2021-10-22 深圳技术大学 Substrate, substrate splicing method and preparation method of single crystal diamond

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Application publication date: 20200612

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