CN108588820A - The synthetic method of microwave plasma CVD device and diamond - Google Patents
The synthetic method of microwave plasma CVD device and diamond Download PDFInfo
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- CN108588820A CN108588820A CN201810408710.6A CN201810408710A CN108588820A CN 108588820 A CN108588820 A CN 108588820A CN 201810408710 A CN201810408710 A CN 201810408710A CN 108588820 A CN108588820 A CN 108588820A
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- 238000005268 plasma chemical vapour deposition Methods 0.000 title claims abstract description 34
- 239000010432 diamond Substances 0.000 title claims abstract description 26
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 26
- 238000010189 synthetic method Methods 0.000 title claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 230000008878 coupling Effects 0.000 claims description 27
- 238000010168 coupling process Methods 0.000 claims description 27
- 238000005859 coupling reaction Methods 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 230000007704 transition Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000000151 deposition Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000000644 propagated effect Effects 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Substances OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 230000035899 viability Effects 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/276—Diamond only using plasma jets
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Plasma & Fusion (AREA)
- Physics & Mathematics (AREA)
- Chemical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
This application discloses a kind of microwave plasma CVD devices, and using plasma antenna is as coupled antenna.Disclosed herein as well is a kind of synthetic method of diamond, using plasma antenna passes through microwave plasma CVD method diamond synthesis as coupled antenna.Disclosed herein as well is application of the microwave plasma CVD device in single-crystal diamond synthesis.The microwave plasma CVD device of the present invention, using plasma antenna are coupled, and the efficiency of antenna can be greatly improved.
Description
Technical field
This application involves single-crystal diamond synthesis technical fields, heavy more particularly to a kind of microwave plasma chemical gas phase
The synthetic method of product device and diamond.
Background technology
The microwave waveguide transmissions that microwave plasma CVD (MPCVD) generates microwave generator are to anti-
Device is answered, and is passed through CH into reactor4With H2Mixed gas, high intensity microwave energy excitation decompose substrate above carbon containing gas
The Viability carbon-containing group of the bodily form and atom state hydrogen, and plasma is formed, to obtain diamond thin in deposition on substrate.
Difference lies in the differences of plasma-reaction-chamber form for different types of MPCVD devices.From vacuum deposition chamber
Form is divided, and has quartz tube type, quartz clock bell-type and a metal cavity formula with microwave window.From the coupling of microwave and plasma
Mode point, there is surface wave manifold type, direct coupling type and antenna manifold type.
In the prior art, in antenna coupling system, generally use metal antenna is coupled, but metal antenna has effect
The low problem of rate.
Invention content
The purpose of the present invention is to provide a kind of synthesis sides of microwave plasma CVD device and diamond
Method, to overcome deficiency in the prior art.
To achieve the above object, the present invention provides the following technical solutions：
The embodiment of the present application discloses a kind of microwave plasma CVD device, using plasma antenna conduct
Coupled antenna.
Preferably, in above-mentioned microwave plasma CVD device, the plasma antenna includes being situated between
Matter pipe, inert gas and electrode, in the medium tube, the electrode is set to the inert gas for the inert gas seal
Both ends.
Preferably, in above-mentioned microwave plasma CVD device, the medium tube is quartz glass tube.
Preferably, in above-mentioned microwave plasma CVD device, device includes that waveguide and coupling turn
Chamber is changed, one end of coupled antenna extends the coupling conversion intracavitary.
Preferably, in above-mentioned microwave plasma CVD device, the waveguide includes first wave guide
Pipe and second waveguide pipe, second waveguide pipe are connected between the first wave conduit and coupling conversion chamber, the second waveguide pipe
It is vertically arranged with first wave conduit；Coupled antenna is coaxially disposed with second waveguide pipe.
Preferably, in above-mentioned microwave plasma CVD device, the first wave conduit is rectangular wave
Conduit, coupling convert chamber as circular waveguide.
Disclosed herein as well is a kind of synthetic method of diamond, using plasma antenna passes through as coupled antenna
Microwave plasma CVD method diamond synthesis.
Preferably, in the synthetic method of above-mentioned diamond, in microwave plasma CVD method, excitation
The shape of the plasma of generation is spherical shape.
Preferably, in the synthetic method of above-mentioned diamond, in microwave plasma CVD method, technique
Gas is passed through resonant cavity using vortex intake method.
Preferably, in the synthetic method of above-mentioned diamond, the both ends of plasma antenna apply high pressure 1000v~
1200v。
Disclosed herein as well is a kind of microwave plasma CVD device answering in single-crystal diamond synthesis
With.
Compared with the prior art, the advantages of the present invention are as follows：The microwave plasma CVD device of the present invention,
Using plasma antenna is coupled, and the efficiency of antenna can be greatly improved.
Description of the drawings
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments described in application, for those of ordinary skill in the art, without creative efforts,
Other drawings may also be obtained based on these drawings.
Fig. 1 show the structural schematic diagram of microwave plasma CVD device in the specific embodiment of the invention；
Fig. 2 show the structural schematic diagram of coupled antenna in the specific embodiment of the invention.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
The every other embodiment that personnel are obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term "center", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for description purposes only, and is not understood to indicate or imply relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
Can also be electrical connection to be mechanical connection；It can be directly connected, can also indirectly connected through an intermediary, Ke Yishi
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
In conjunction with shown in Fig. 1, microwave plasma CVD device includes microwave source 10, plasmon coupling device
20 and resonance device 30.
Microwave source 10 can be the equipment such as the microwave generator of this field routine for generating microwave, generated micro-
The power of wave can be able to be 915MHz-2.45GHz for 6~75kW, frequency.
In the present embodiment, microwave source 10 generate microwave power be 6~10kW, frequency 2.45GHz.
Resonance device 30 includes a resonant cavity 31 and deposition table 32.
The shell of resonant cavity 31 can be made of metal material or quartz material.Preferably, resonant cavity is by metal material (example
Such as aluminium or copper) it is made, to be conducive to carry out water-cooled process to resonant cavity.
The shape of resonant cavity 31 can be various shapes, such as cylindrical.
Plasmon coupling device 20 preferably uses antenna manifold type.
Specifically, plasmon coupling device 20 includes waveguide, coupled antenna 21, coupling conversion chamber 22 and medium window
23。
Wherein, waveguide is connected between microwave source 10 and coupling conversion chamber 22；The bottom end of coupled antenna 21 extends to coupling
It closes in conversion chamber 22；Coupling conversion chamber 22 is set to the top of resonant cavity 31, and medium window 23 is located at resonant cavity 31 and coupling turns
It changes between chamber 22.
The medium window 23 at 31 top of resonant cavity is the window formed by translucent material (such as quartz or sapphire), energy
Enough make microwave transparent hence into resonant cavity 31, and it also ensures the sealing performance of resonant cavity 31.
In the operating condition, coupling converts the operating pressure of chamber 22 as high vacuum (0.13~1.3 × 10-5Pa), resonant cavity
31 operating pressure is ultrahigh vacuum (operating pressure 1.3 × 10-5Pa~1.3 × 10-10Pa)。
Further, waveguide includes first wave conduit 24 and second waveguide pipe 25.
First wave conduit 24 is rectangular waveguide；Coupling converts chamber 22 as circular waveguide, and second waveguide pipe 25 is connected to
Between the first wave conduit 24 and the top of coupling conversion chamber 22, the second waveguide pipe 25 is vertical with first wave conduit 24 to be set
It sets；Coupled antenna 21 is coaxially disposed with second waveguide pipe 25.
It to be metal sidewall that chamber 22 is converted in coupling, and when setting couples conversion chamber 22, coupled antenna 21 can be by first
The microwave of TE10 patterns in waveguide 24 is converted to TEM mode, and after second waveguide pipe 25 is sent to coupling conversion chamber 22,
The microwave of TEM mode is converted to TM01 patterns by coupled antenna 21 again, hence into resonant cavity 31.This set-up mode can avoid
The microwave of TE10 patterns is converted directly into the microwave of the not corresponding TM01 patterns of electric field, to make to be formed by TM01 mode trickles
The energy maximization of wave further increases the service efficiency of microwave energy.Also, the microwave of TM01 patterns can make deposition table 32
Upper area forms the electromagnetic field of maximum intensity, and is conducive to excite spherical plasma 34, so as to avoid resonant cavity 31
Side wall pollution is generated to the diamond thin of deposition.
In one embodiment, tuner 26 is provided between first wave conduit 24 and microwave source 10, the tuner 26 to
Adjust the waveform of the microwave transmitted in first wave conduit 24.
In the technical solution, tuner to adjust the waveform of the microwave transmitted in first wave conduit 24 to make its with
Coupled antenna 21 matches, and to make the microwave energy of input maximize, such as it can be that three screws of this field routine hinder
Anti- tuner etc..Three screw impedance tuners can manual tuning or automatic tuning.
In one embodiment, transition waceguide 28 is provided between tuner 26 and first wave conduit 24.It is preferred that the standard of using
Transition waceguide WR340 to 284.
In one embodiment, one end of first wave conduit 24 is provided with bosh, and lower part has low pressure to vacuumize interface.
In one embodiment, coupled antenna 21 is plasma antenna.
In conjunction with shown in Fig. 2, plasma antenna includes quartz glass 211, and quartz glass interior sealing has inert gas 212,
The both ends of inert gas 212 are respectively arranged with high-field electrode 213.
In the technical solution, the inert gas both ends of sealing add high pressure, and excitation plasma is used as antenna, can greatly carry
The efficiency of high antenna.
Further, the both ends of plasma antenna apply voltage 1000v~1200v.
Since different intake methods can change plasma shape, methane, carbon dioxide, oxygen, hydrogen in the present embodiment
The process gas such as gas use vortex intake method, so that plasma maintains stable spherical state.
Specifically, high-purity process gas inlets are also communicated on resonant cavity 31, gas feed is that surrounding is vortexed into cavity,
Each aperture is about 0.5~1mm of diameter, and circumferencial direction is uniformly distributed general 8~10.
In one embodiment, the side wall of coupling conversion chamber 22 is provided with water cooling plant 27.
In the technical solution, the side wall of coupling conversion chamber can be arranged to double-deck sandwich, interlayer space passes through
The liquid for being passed through refrigeration carries out temperature control.The liquid of refrigeration is run in a looping fashion, has water guide water route, prevents from having in interlayer " dead
Water " generates.
It is necessary, high-purity process gas inlets are also communicated on resonant cavity 31, gas feed is that surrounding is vortexed into cavity,
Each aperture is about 0.5~1mm of diameter, and circumferencial direction is uniformly distributed general 8~10.
Gas uses swirling manner, is conducive to the spherical plasma of excitation.
The operation principle and process of above-mentioned microwave plasma CVD equipment be：Resonant cavity 31 is carried out first
It vacuumizes, and is passed through the mixed gas of methane and hydrogen composition into resonant cavity 31, microwave is then generated by microwave source 10, it is micro-
Microwave caused by wave source 10 is propagated in first wave conduit with TE10 patterns, after coupled antenna 21 is converted, second
It is propagated in a tem mode in waveguide 25, after entering coupling conversion chamber 22, coupled antenna 21 is again converted to TM01 moulds
Formula enters resonant cavity 31, the activity of methane formation carbon-containing group and atom state hydrogen of 32 top of deposition table, and shape through medium window 23
Glomeration plasma 34, to deposit to obtain diamond thin in seed crystal upper surface.
Specifically, the present embodiment also provides single-crystal diamond synthetic method, including step：
(1), seed crystal (substrate) surface polishes：The planarizing process such as mechanical lapping are carried out to diamond seed surface；
(2), acid processing：With water-sulfuric acid-hydrogen peroxide mixed solution of heating, (ratio is：1:5:1) temperature is heated to 100
It~130 degree, cleans 10~20 minutes；
(3), seed crystal deionized water is rinsed 10~15 minutes；
(4), it is ultrasonically treated：In organic solvent (such as：Isopropanol) be cleaned by ultrasonic 30 minutes.
(5), deionized water is rinsed 6~10 minutes；
(6), dustless oven temperature be heated to 80 degree toast 10~30 minutes；
(7), resonant cavity is opened, seed crystal is fixed on to the upper surface of deposition table；
(8), cavity is closed；
(9), low-voltage vacuum is taken out in first wave conduit；
(10), water-cooling shaft is adjusted to suitable position, to control the temperature of seed crystal；
(11), resonant cavity is cleaned with high-purity hydrogen, can be cleaned multiple times by several times or once cleaned.As primary cleaning is taken out
Vacuum is to 0.0015Torr；Hydrogenation to 5Torr, then in control chamber body stable gas pressure in 5Torr；
(12), microwave source is opened, three needle tuners are adjusted, excites resonant cavity plasma ignition.General plasma ignition hair
Life is in 5~10torr.
(13), increase power according to the following table 1, adjust air pressure, coupled and adjusted by power air pressure, it is ensured that plasma is not
It can loss.
Table 1
| Plasma power | 600w | 1000w | 1500w | 2000w | 2500w | 3000w | 3500w~8000w |
| Air pressure | 10torr | 20torr | 50torr | 100torr | 120torr | 150torr | 150torr |
(14), the position for finely tuning microwave power and water-cooling shaft controls seed temperature by double-colored sensor.
(15), with hydrogen etched seed surface 15min.
(16), 800~1400 degree of seed temperature is controlled.
(17), process gas 50scmm methane, 500sccm hydrogen, diamond continued propagation are passed through.
(18), resonant cavity is opened after completing growth.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (16)
1. a kind of microwave plasma CVD device, using plasma antenna is as coupled antenna.
2. microwave plasma CVD device according to claim 1, it is characterised in that：The plasma
Antenna includes medium tube, inert gas and electrode, and in the medium tube, the electrode is set to institute for the inert gas seal
State the both ends of inert gas.
3. microwave plasma CVD device according to claim 2, it is characterised in that：The medium tube is
Quartz glass tube.
4. microwave plasma CVD device according to claim 1, it is characterised in that：Device includes waveguide
One end of pipe and coupling conversion chamber, coupled antenna extends the coupling conversion intracavitary.
5. microwave plasma CVD device according to claim 4, it is characterised in that：The waveguide packet
First wave conduit and second waveguide pipe are included, second waveguide pipe is connected between the first wave conduit and coupling conversion chamber, described
Second waveguide pipe is vertically arranged with first wave conduit；Coupled antenna is coaxially disposed with second waveguide pipe.
6. microwave plasma CVD device according to claim 5, it is characterised in that：The first wave guide
Pipe is rectangular waveguide, and coupling converts chamber as circular waveguide.
7. microwave plasma CVD device according to claim 5, it is characterised in that：It further include microwave
The power in source, microwave caused by microwave source is 6~75kW, and frequency is 915MHz~2.45GHz.
8. microwave plasma CVD device according to claim 7, it is characterised in that：First wave conduit and
Tuner is provided between microwave source.
9. microwave plasma CVD device according to claim 8, it is characterised in that：Tuner uses three
Screw impedance tuner.
10. microwave plasma CVD device according to claim 8, it is characterised in that：Tuner and
It is provided with transition waceguide between one waveguide.
11. microwave plasma CVD device according to claim 10, it is characterised in that：Transition waceguide is adopted
With WR340 to 284.
12. a kind of synthetic method of diamond, which is characterized in that using plasma antenna passes through microwave as coupled antenna
Plasma activated chemical vapour deposition method diamond synthesis.
13. the synthetic method of diamond according to claim 12, which is characterized in that microwave plasma chemical gas phase is heavy
In product method, it is spherical shape to excite the shape of the plasma of generation.
14. the synthetic method of diamond according to claim 13, which is characterized in that microwave plasma chemical gas phase is heavy
In product method, process gas is passed through resonant cavity using vortex intake method.
15. the synthetic method of diamond according to claim 12, which is characterized in that the both ends of plasma antenna apply
Voltage 1000v~1200v.
16. any microwave plasma CVD device of claim 1 to 11 is in single-crystal diamond synthesis
Application.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US201862661807P | 2018-04-24 | 2018-04-24 | |
| US62/661,807 | 2018-04-24 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108588820A true CN108588820A (en) | 2018-09-28 |
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ID=63619481
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| CN201810408710.6A Pending CN108588820A (en) | 2018-04-24 | 2018-05-02 | The synthetic method of microwave plasma CVD device and diamond |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373651A (en) * | 2019-09-04 | 2019-10-25 | 成都道启弘环境科技有限公司 | A kind of equipment of microwave plating nano-diamond film |
| CN111826634A (en) * | 2020-07-27 | 2020-10-27 | 中国科学院半导体研究所 | A kind of high uniformity semiconductor film growth device and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710748A (en) * | 2013-12-12 | 2014-04-09 | 王宏兴 | Growth method of high-quality high-speed monocrystal diamond film |
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