CN108360065A - A kind of method and growth structure of growth single-crystal diamond - Google Patents
A kind of method and growth structure of growth single-crystal diamond Download PDFInfo
- Publication number
- CN108360065A CN108360065A CN201810327256.1A CN201810327256A CN108360065A CN 108360065 A CN108360065 A CN 108360065A CN 201810327256 A CN201810327256 A CN 201810327256A CN 108360065 A CN108360065 A CN 108360065A
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- growth
- crystal diamond
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- preferred orientation
- substrate
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 120
- 239000010432 diamond Substances 0.000 title claims abstract description 120
- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000758 substrate Substances 0.000 claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011435 rock Substances 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000001657 homoepitaxy Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching 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
- C30B25/20—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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
Abstract
The invention discloses a kind of methods and growth structure of growth single-crystal diamond.Wherein, a method of growth single-crystal diamond includes the following steps：Step 1 grows one layer with preferred orientation polycrystalline diamond layer in the substrate surface cleaned；Step 2, the continued growth single-crystal diamond on preferred orientation polycrystalline diamond layer, obtain single-crystal diamond.Solves the problem that diamond growth size is small, and growth gained single-crystal diamond internal stress is big.
Description
【Technical field】
The invention belongs to Material growth technical fields, and in particular to a kind of method and grown junction of growth single-crystal diamond
Structure.
【Background technology】
Diamond is a kind of excellent semi-conducting material, all has superior performance in heat, electricity, sound, light etc..It is big
Energy gap, thermal coefficient, critical breakdown strength, hole and electron mobility so that diamond be very suitable for preparing high temperature,
High frequency, high pressure, high power electronic electrical device；Its superpower capability of resistance to radiation so that the power electronics device prepared by diamond
The devices such as part, MEMS can work in very harsh environment；Its big light transmission and thermal conductivity so that diamond can be with
As the output window of high power laser and electromagnetic wave, can use in optics and electromagnetic transmission field.Therefore, Buddha's warrior attendant stone material
Material is with very high use potentiality.
Into 20 years, Microwave plasma CVD technique made as the main technique for preparing single-crystal diamond
With 2.45GHz (girz) microwave source.Single crystal diamond film technique is generally：Operating pressure 50-300Torr (support), temperature
700-1300 DEG C (degree Celsius), power 500-5000W (watt).Reaction gas is mainly methane, hydrogen and nitrogen.By adjusting temperature
The conditions such as degree, gas component and plasma power density realize the life of preferred orientation polycrystalline diamond and single-crystal diamond
It is long.
Currently, preparing single-crystal diamond using Microwave plasma CVD system is divided into homoepitaxy and heterogeneous
Two kinds of extension.In homoepitaxy, using diamond as substrate, diamond quality prepared by this method is high, and defect is few, but
It is, the disadvantage is that diamond size prepared by this method is small, cannot meet the needs of super large-scale integration；In hetero-epitaxy,
Metal iridium is generally used, transversal epitaxial growth is patterned, diamond size prepared by this method is big, still, the disadvantage is that
Diamond quality prepared by this method is poor, cannot be satisfied its application in heat, electricity, sound, light etc..Therefore need one kind can be with
Go out the method for high quality single crystal diamond in unlike material Grown.
【Invention content】
The object of the present invention is to provide a kind of methods and growth structure of growth single-crystal diamond, to solve diamond growth
Size is small, and the problem that growth gained single-crystal diamond internal stress is big.
The technical solution used in the present invention is：A method of growth single-crystal diamond includes the following steps：
Step 1 grows one layer with preferred orientation polycrystalline diamond layer in the substrate surface cleaned；
Step 2, the continued growth single-crystal diamond on preferred orientation polycrystalline diamond layer, obtain single-crystal diamond.
Further, the preferred orientation of preferred orientation polycrystalline diamond layer is<100>Or<110>Or<111>.
Further, the thickness of preferred orientation polycrystalline diamond layer is more than 1nm.
Further, it in step 1, using Microwave plasma CVD method, is preferentially taken in substrate surface growth
It is to the condition of polycrystalline diamond layer：Total gas flow rate 500sccm, methane flow 0-200sccm, chamber pressure are 50Torr, power
600W, 600-1300 DEG C of temperature.
Further, in step 2, using Microwave plasma CVD method, in preferred orientation polycrystalline diamond
The condition of growth single-crystal diamond is on layer：Total gas flow rate 500sccm, methane flow 0-200sccm, chamber pressure are 50Torr,
Power 600W, 600-1300 DEG C of temperature.
Further, substrate surface for roughness is less than 100 μm.
Further, in step 1, the substrate is selected<100>Single-crystal diamond, using the sour alkali washing process of standard to lining
Bottom is cleaned, and is removed the non-diamond phase on surface, is then cleaned to substrate using alcohol, acetone, deionized water, finally
Substrate is dried up using nitrogen.
Second of technical solution that the present invention uses is a kind of single crystal diamond film structure, using arbitrary in above-mentioned 1-7
A kind of method of growth single-crystal diamond described in one is made, and growth structure is the substrate being cascading, preferentially takes
To polycrystalline diamond layer and single-crystal diamond.
Further, the preferred orientation of preferred orientation polycrystalline diamond layer is<100>Or<110>Or<111>.
Further, the thickness of preferred orientation polycrystalline diamond layer is more than 1nm.
The invention has the advantages that：Preferred orientation polycrystalline diamond layer is grown on substrate, it is then more at this
Single-crystal diamond is grown on diamond layer.This allows single-crystal diamond to be grown on different size substrates, and this
The single-crystal diamond quality that kind of method obtains is higher than the obtained single-crystal diamond quality of direct extension, internal stress it is small and
It is evenly distributed, a kind of new method is provided for the preparation of single-crystal diamond.
【Description of the drawings】
Fig. 1 is substrat structure schematic diagram in a kind of method of growth single-crystal diamond of the present invention；
Fig. 2 is to grow preferred orientation polycrystalline diamond on substrate in a kind of method of growth single-crystal diamond of the present invention
The schematic diagram of layer；
Fig. 3 is to grow preferred orientation polycrystalline diamond on substrate in a kind of method of growth single-crystal diamond of the present invention
The schematic diagram of layer and single-crystal diamond.
Wherein, 1. substrate；2. preferred orientation polycrystalline diamond layer；3. single-crystal diamond.
【Specific implementation mode】
The structural principle and operation principle of the present invention are described further below in conjunction with the accompanying drawings.
The present invention provides a kind of methods of growth single-crystal diamond to be carried out successively according to the following steps such as Fig. 1-Fig. 3：
Step 1 grows one layer with preferred orientation polycrystalline diamond layer 2 on 1 surface of substrate cleaned；
Step 2, the continued growth single-crystal diamond 3 on preferred orientation polycrystalline diamond layer 2, obtain single-crystal diamond.
Wherein, the preferred orientation of preferred orientation polycrystalline diamond layer 2 is<100>Or<110>Or<111>.Preferred orientation is more
The thickness of diamond layer 2 is more than 1nm.
In step 1, on 1 surface of substrate, the method for growth preferred orientation polycrystalline diamond layer 2 can utilize microwave plasma
Body CVD method, growth condition can be：Total gas flow rate 500sccm, methane flow 0-200sccm, chamber pressure are
50Torr, power 600W, 600-1300 DEG C of temperature.
In step 2, growth single-crystal diamond 3 can utilize microwave plasma on preferred orientation polycrystalline diamond layer 2
CVD method, growth condition can be：Total gas flow rate 500sccm, methane flow 0-200sccm, chamber pressure are
50Torr, power 600W, 600-1300 DEG C of temperature.
Substrate 1 can be selected<100>Single-crystal diamond or other arbitrary materials, using the sour alkali washing process of standard to substrate
1 is cleaned, and the non-diamond phase on surface is removed, and is then cleaned to substrate 1 using alcohol, acetone, deionized water, finally
Substrate 1 is dried up using nitrogen.1 surface roughness of substrate is less than 100 μm.
The present invention provides a kind of single crystal diamond film structures, using a kind of above-mentioned method system of growth single-crystal diamond
, growth structure is the substrate 1, preferred orientation polycrystalline diamond layer 2 and single-crystal diamond 3 being cascading.Wherein, it selects
It is excellent be orientated polycrystalline diamond layer 2 preferred orientation be<100>Or<110>Or<111>, the thickness of preferred orientation polycrystalline diamond layer
More than 1nm.
Embodiment
It is a kind of growth single-crystal diamond method comprise the following steps：
1) substrate 1 is selected<100>Single-crystal diamond cleans substrate 1 using the sour alkali washing process of standard, removes table
Then the non-diamond phase in face cleans substrate 1 using alcohol, acetone, deionized water, dry up substrate 1 using nitrogen, such as
Shown in Fig. 1.
2) one layer of 200nm thickness is grown on substrate 1 using microwave plasma CVD technology, preferred orientation is
<100>Polycrystalline diamond layer 2, as shown in Figure 2.Growth conditions is：Total gas flow rate 500sccm, methane flow 0-
200sccm, chamber pressure are 50Torr, power 600W, 600-1300 DEG C of temperature.
3) after there is preferred orientation polycrystalline diamond layer 2 to grow, change microwave plasma CVD work
Skill starts to grow single-crystal diamond 3, as shown in Figure 3.Growth conditions is：Total gas flow rate 500sccm, methane flow 0-
200sccm, chamber pressure are 50Torr, power 600W, 600-1300 DEG C of temperature.
Think in the prior art, single-crystal diamond epitaxial growth typically on single-crystal diamond comes out, and polycrystalline is golden
Single-crystal diamond can not be grown on hard rock.But pass through the study found that on preferred orientation polycrystalline diamond layer 2, and
Under specific growth conditions, single-crystal diamond 3 can be grown.And by obtained by the method for this growth single-crystal diamond
Single-crystal diamond, quality will be far above through the obtained single-crystal diamond quality of direct extension, and monocrystalline obtained is golden
Stress inside hard rock is small and is evenly distributed, and thus the present invention provides a kind of new method for the preparation of single-crystal diamond.
Claims (10)
1. a kind of method of growth single-crystal diamond, which is characterized in that include the following steps：
Step 1 grows one layer with preferred orientation polycrystalline diamond layer (2) on substrate (1) surface cleaned；
Step 2, the continued growth single-crystal diamond (3) on preferred orientation polycrystalline diamond layer (2), obtain single-crystal diamond.
2. a kind of method of growth single-crystal diamond as described in claim 1, which is characterized in that the preferred orientation polycrystalline
The preferred orientation of diamond layer (2) is<100>Or<110>Or<111>.
3. a kind of method of growth single-crystal diamond as claimed in claim 1 or 2, which is characterized in that the preferred orientation
The thickness of polycrystalline diamond layer (2) is more than 1nm.
4. a kind of method of growth single-crystal diamond as claimed in claim 1 or 2, which is characterized in that in the step 1, profit
With plasma chemical vapor deposition method, it is in the condition of substrate (1) surface growth preferred orientation polycrystalline diamond layer (2)：Gas
Body total flow 500sccm, methane flow 0-200sccm, chamber pressure is 50Torr, power 600W, 600-1300 DEG C of temperature.
5. a kind of method of growth single-crystal diamond as claimed in claim 1 or 2, which is characterized in that in the step 2, profit
With plasma chemical vapor deposition method, the condition of single-crystal diamond (3) is grown on preferred orientation polycrystalline diamond layer (2)
For：Total gas flow rate 500sccm, methane flow 0-200sccm, chamber pressure are 50Torr, power 600W, 600-1300 DEG C of temperature.
6. a kind of method of growth single-crystal diamond as claimed in claim 1 or 2, which is characterized in that described substrate (1) table
Surface roughness is less than 100 μm.
7. a kind of method of growth single-crystal diamond as claimed in claim 6, which is characterized in that in the step 1, the lining
Bottom (1) is selected<100>Single-crystal diamond cleans substrate (1) using the sour alkali washing process of standard, removes the non-gold on surface
Then hard rock phase uses alcohol, acetone, deionized water to clean substrate (1), finally use nitrogen drying substrate (1).
8. a kind of single crystal diamond film structure, which is characterized in that using a kind of growth list described in any one of above-mentioned 1-7
The method of diamond is made, and growth structure is the substrate (1) being cascading, preferred orientation polycrystalline diamond layer (2)
With single-crystal diamond (3).
9. a kind of growth single crystal diamond film structure as claimed in claim 8, which is characterized in that the preferred orientation is more
The preferred orientation of diamond layer (2) is<100>Or<110>Or<111>.
10. a kind of growth single crystal diamond film structure as claimed in claim 8 or 9, which is characterized in that described preferentially takes
It is more than 1nm to the thickness of polycrystalline diamond layer (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810327256.1A CN108360065A (en) | 2018-04-12 | 2018-04-12 | A kind of method and growth structure of growth single-crystal diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810327256.1A CN108360065A (en) | 2018-04-12 | 2018-04-12 | A kind of method and growth structure of growth single-crystal diamond |
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| CN108360065A true CN108360065A (en) | 2018-08-03 |
Family
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| CN201810327256.1A Pending CN108360065A (en) | 2018-04-12 | 2018-04-12 | A kind of method and growth structure of growth single-crystal diamond |
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Cited By (2)
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|---|---|---|---|---|
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN114525582A (en) * | 2022-01-05 | 2022-05-24 | 西安电子科技大学 | Single crystal diamond and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN114525582A (en) * | 2022-01-05 | 2022-05-24 | 西安电子科技大学 | Single crystal diamond and preparation method thereof |
| CN114525582B (en) * | 2022-01-05 | 2023-08-04 | 西安电子科技大学 | Single crystal diamond and preparation method thereof |
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