CN102230216B - Preparation method of laminar flow plasma of single crystal diamond - Google Patents
Preparation method of laminar flow plasma of single crystal diamond Download PDFInfo
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- CN102230216B CN102230216B CN 201110164532 CN201110164532A CN102230216B CN 102230216 B CN102230216 B CN 102230216B CN 201110164532 CN201110164532 CN 201110164532 CN 201110164532 A CN201110164532 A CN 201110164532A CN 102230216 B CN102230216 B CN 102230216B
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- crystal diamond
- seed crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 71
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 41
- 239000010432 diamond Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000008021 deposition Effects 0.000 claims abstract description 12
- 230000033001 locomotion Effects 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 238000005219 brazing Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000003870 refractory metal Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009304 pastoral farming Methods 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 230000005281 excited state Effects 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- 239000012530 fluid Substances 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 10
- 238000001237 Raman spectrum Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000000149 penetrating effect Effects 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 101100202502 Caenorhabditis elegans scd-2 gene Proteins 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- AEDMQUAPBVOJNN-UHFFFAOYSA-N [3-[2-[4-[2-(trifluoromethyl)phenoxy]piperidin-1-yl]-1,3-thiazol-5-yl]-1,2,4-oxadiazol-5-yl]methanol Chemical compound O1C(CO)=NC(C=2SC(=NC=2)N2CCC(CC2)OC=2C(=CC=CC=2)C(F)(F)F)=N1 AEDMQUAPBVOJNN-UHFFFAOYSA-N 0.000 description 2
- 241000212346 Spermolepis Species 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- VYMDGNCVAMGZFE-UHFFFAOYSA-N phenylbutazonum Chemical compound O=C1C(CCCC)C(=O)N(C=2C=CC=CC=2)N1C1=CC=CC=C1 VYMDGNCVAMGZFE-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of laminar plasma of single crystal diamond, and belongs to the technical field of single crystal diamond preparation. In the preparation method, by regulating and controlling fluid characteristics of the plasma, a stable laminar plasma boundary layer is constructed so that the single crystal diamond can grow stably on a large-sized substrate, which avoids problems such as poly-crystallization and small-sized substrate of the current single crystal diamond prepared through direct current plasma deposition. The preparation method has the advantages that a way to stably prepare the single crystal diamond by utilizing large-sized seed crystal is provided so that size of a stable growing region of the single crystal diamond reaches 7cm along the direction of a motion axis of the plasma, and meanwhile poly-crystallization on the single crystal growing surface is effectively inhibited.
Description
Technical field:
The invention belongs to the single-crystal diamond preparing technical field, a kind of preparation method of laminar flow plasma of single-crystal diamond particularly is provided; The laminar boundary layer environment of penetrating direct-current plasma is plunderred in utilization, the preparation single-crystal diamond.
Technical background:
Chemical vapour deposition (CVD) large size single crystal diamond is (C.Yan etc. after being reported in 2002; Proc.Nat.Acad.Sci.99 (2002) R25-27); Research and development have worldwide been obtained paying close attention to widely and following up; Wherein strengthen chemical vapour deposition technique (Q.Liang, etc., Diamond & Related Materials 18 (2009) 698-703) and direct-current plasma enhancing chemical vapour deposition technique (G.C.Chen with microwave plasma; Deng, Diamond &Related Materials 19 (2010) 1078-1084) actual application value arranged most.Current; The single-crystal diamond of microwave plasma deposition techniques can reach 50～150 microns/hour deposition velocity (Y.Mokuno; Deng, Diamond& Related Materials 15 (2006) 455-459), and full-size can surpass the single-crystal diamond dish (H.Yamada of 1 inch diameter; Deng, Diamond & Related Materials 20 (2011) 616-619).But this technology complicated operation can not be realized the continuous growth (Y.Mokuno, etc., Diamond &Related Materials 14 (2005) 1743-1746) of single-crystal diamond; In addition, this technological core frock is mainly the U.S., Japan, Britain and has that (Russell J He Mulei is etc., CN101198544; Good number is sincere, etc., CN101053075; HP dagger-axe Freed, etc., CN200380101681.0), China this technical elements still be in the starting stage (Li Hongdong, etc., CN101311339).Direct-current plasma deposition single-crystal diamond technology is the original technology (Chen Guangchao of China; Deng; CN200510086580.1 and CN200710064728.0), can reach 30 microns/hour deposition velocity at present, and realize the continuous growth (G.C.Chen of single-crystal diamond; Deng, Diamond & Related Materials19 (2010) 1078-1084).The deposition velocity that should be noted that 30 microns/hour is the deposition velocity of intrinsic single-crystal diamond of nitrogen of undoping, and the speed (50 microns/hour) of this and microwave plasma deposition techniques intrinsic single-crystal diamond is close.
No matter current chemical vapour deposition (CVD) single-crystal diamond technology is microwave plasma body technique or direct current plasma body technique, all exists deposit to be prone to the problem of polycrystallization.With regard to the direct current plasma body technique, the reason of polycrystallization is that direct-current plasma is prone to Turbulence Flow.Because the appearance of turbulent flow has increased the unsteadiness in the deposition process, has strengthened the tendency of deposit polycrystallization.Except the polycrystallization problem, also there is another problem in the direct current plasma body technique, and the method for promptly present direct-current plasma deposition single-crystal diamond can not utilize large-sized substrate to carry out single crystal preparation.This is because in the present direct current plasma body technique; Plasma is to flow with the impact jet flow mode with respect to substrate; Formed a plurality of flow field regions of different nature in the service area, i.e. free jet district, stagnation region and along the wall fluerics, between each zone and each intra-zone all have temperature gradient and the excessive problem of velocity gradient; Therefore cause the uniform flow field zone little, cause the depositional environment that is unfavorable for that large-sized substrate is used.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of laminar flow plasma of single-crystal diamond; Fluid behaviour through the regulation and control plasma; Construct stable laminar flow plasma boundary layer, make the single-crystal diamond can be in the method for the enterprising line stabilization of large-sized substrate growth.Thereby avoid the polycrystallization of current direct-current plasma deposition single-crystal diamond and the problem of small size substrate.
Single-crystal diamond is plunderred to penetrate in the laminar flow depositing system at plasma and is carried out.Wherein contain excitation state carbon atom, hydrocarbon molecules and hydrogen atom in the composition of direct-current plasma, the electron temperature 0.3～0.5eV of plasma.The spout geometry of plasma is circle or rectangle, and wherein the rectangular jet area is 10～15 centimetres
2, 7～18 centimetres of circular areas of injection orifice
2The axis of movement of plasma is parallel to horizontal direction, and Reynolds number 20～800, plasma become 80 °～100 ° angle to plunder with axis of movement to penetrate seed crystal face with the seed crystal normal.Seed crystal is a single-crystal diamond; It exposes crystal face to the open air can be perhaps (111) crystal face of (100) crystal face; Mode with cast setting or vacuum brazing is fixed on the refractory metal seed crystal carriage with water-cooled function; The size of seed crystal is 0.1～6 centimetre at the plasma motion axis direction, and seed crystal is 0.5～1.5 centimetre apart from the distance of plasma spout, and seed temperature is between 650 ℃～1300 ℃.Reaction chamber pressure is between 6000～18000Pa.
Advantage of the present invention and good effect:
This method provides an approach that is fit to adopt large scale seed crystal, stable preparation single-crystal diamond, makes single-crystal diamond stable growth district size reach 7 centimetres at the plasma motion axis direction, and has effectively suppressed the polycrystallization on crystal growth surface.
Description of drawings
Fig. 1 is that laminar flow plasma is plunderred the sketch map of penetrating depositing system.Wherein, plasma spout 1, water-cooled seed crystal carriage 2, outlet pipe 3, seed crystal 4, water inlet pipe 5, plasma 6, reaction chamber 7, vacuum pump 8.
Fig. 2 be the composition of plasma with plunderring the situation of change of penetrating distance, the h value representation is apart from the height of seed crystal face among the figure.
Fig. 3 is the electron microscopic result of gained single-crystal surface, the growing surface of SCD-1 monocrystal in the table 1.
Fig. 4 is the electron microscopic result of gained single-crystal surface, the growing surface of SCD-2 monocrystal in the table 1.
Fig. 5 is the electron microscopic result of gained single-crystal surface, the growing surface of SCD-3 monocrystal in the table 1.
Fig. 6 is the Raman spectrum result of gained single-crystal surface, the Raman spectrum result of the growing surface of SCD-1 monocrystal in the table 1.
Fig. 7 is the Raman spectrum result of gained single-crystal surface, the Raman spectrum result of the growing surface of SCD-2 monocrystal in the table 1.
Fig. 8 is the Raman spectrum result of gained single-crystal surface, the Raman spectrum result of the growing surface of SCD-3 monocrystal in the table 1.
Embodiment
Plunder at laminar flow plasma shown in Figure 1 and to penetrate in the depositing system, utilize composition that light emission spectrum tested plasma, obtained the result of Fig. 2 with plunderring the situation of change of penetrating distance.The result of Fig. 2 shows that the stable growth district of monocrystalline reaches 7 centimetres in the plasma motion axial line distance.With (100) and (111) crystal face is that the single-crystal diamond that exposes crystal face to the open air is a substrate, carries out the single-crystal diamond deposition, and technological parameter is seen table 1, and the electron microscopic result of each gained single-crystal surface and surperficial Raman (Raman) spectrum result see Fig. 3～8 respectively.
The deposition parameter of table 1 single-crystal diamond.
The deposition parameter of table 1 single-crystal diamond.
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110164532 CN102230216B (en) | 2011-06-19 | 2011-06-19 | Preparation method of laminar flow plasma of single crystal diamond |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110164532 CN102230216B (en) | 2011-06-19 | 2011-06-19 | Preparation method of laminar flow plasma of single crystal diamond |
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| CN102230216A CN102230216A (en) | 2011-11-02 |
| CN102230216B true CN102230216B (en) | 2012-11-14 |
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| CN 201110164532 Expired - Fee Related CN102230216B (en) | 2011-06-19 | 2011-06-19 | Preparation method of laminar flow plasma of single crystal diamond |
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| CN104878447B (en) * | 2015-06-04 | 2017-03-01 | 哈尔滨工业大学 | A kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH03150341A (en) * | 1989-11-07 | 1991-06-26 | Onoda Cement Co Ltd | Conjugate torch type plasma generator and plasma generating method using the same |
| US5704976A (en) * | 1990-07-06 | 1998-01-06 | The United States Of America As Represented By The Secretary Of The Navy | High temperature, high rate, epitaxial synthesis of diamond in a laminar plasma |
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