CN108315818A - Single-crystal diamond synthesizer and method - Google Patents
Single-crystal diamond synthesizer and method Download PDFInfo
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- CN108315818A CN108315818A CN201810408768.0A CN201810408768A CN108315818A CN 108315818 A CN108315818 A CN 108315818A CN 201810408768 A CN201810408768 A CN 201810408768A CN 108315818 A CN108315818 A CN 108315818A
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- 239000010432 diamond Substances 0.000 title claims abstract description 64
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 64
- 239000013078 crystal Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title description 13
- 238000010168 coupling process Methods 0.000 claims abstract description 52
- 238000005859 coupling reaction Methods 0.000 claims abstract description 52
- 230000008878 coupling Effects 0.000 claims abstract description 51
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 238000010189 synthetic method Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 22
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 150000002500 ions Chemical class 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000011733 molybdenum Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 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
- 230000005284 excitation Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 2
- 238000012545 processing Methods 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
- 241000196324 Embryophyta Species 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000233855 Orchidaceae Species 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000005484 gravity 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
- 238000009434 installation Methods 0.000 description 1
- 239000008141 laxative Substances 0.000 description 1
- 230000002475 laxative effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 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
- 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
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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
This application discloses a kind of single-crystal diamond synthesizers, including microwave source, plasmon coupling device and resonance device, the resonance device includes a resonant cavity, there is a diamond growth face, plasmon coupling device can excite to form plasma in the lower section in diamond growth face by the microwave from the microwave source in the resonant cavity.Disclosed herein as well is a kind of single-crystal diamond synthetic methods.The present invention with the impurity in effective solution diamond production process by that in substrate lower surface depositing diamond film, can be polluted.
Description
Technical field
This application involves chemical vapor depsotition equipments, more particularly to a kind of single-crystal diamond synthesizer and method.
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.
It is single that Chinese Patent No. 201720707933.3 discloses a kind of MPCVD method growth
The deposition table of diamond, plasma are happened at top, and workbench is in lower part.Due to by gravity and its cavity flow field
It influences, the impurity of polycrystalline and its C that growth course generates can pollute monocrystalline, so as to cause having impurity in the diamond produced.
Invention content
The purpose of the present invention is to provide a kind of single-crystal diamond synthesizer and method, with overcome it is in the prior art not
Foot.
To achieve the above object, the present invention provides the following technical solutions：
The embodiment of the present application discloses a kind of single-crystal diamond synthesizer, including microwave source, plasmon coupling device and
Resonance device,
The resonance device includes a resonant cavity, in the resonant cavity on be provided with pedestal, the lower surface of the pedestal to
Substrate is supported,
Plasmon coupling device is located at the lower section of the pedestal, and can be by the microwave from the microwave source in base
The coupling of seat lower section forms plasma.
Preferably, in above-mentioned single-crystal diamond synthesizer, the plasmon coupling device is coupled using antenna
Formula.
Preferably, in above-mentioned single-crystal diamond synthesizer, the plasmon coupling device includes waveguide, mould
Formula converting antenna, coupling conversion chamber and medium window,
The waveguide is connected between the microwave source and coupling conversion chamber；
The top of the Mode-transducing antenna extends to the coupling conversion intracavitary；
The coupling conversion chamber is set to the lower section of the resonant cavity, and the medium window is located at the resonant cavity and coupling
Between conversion chamber.
Preferably, in above-mentioned single-crystal diamond synthesizer, the waveguide includes first wave conduit and the second wave
Conduit,
The first wave conduit is rectangular waveguide；
The coupling converts chamber as circular waveguide, and the second waveguide pipe is connected to the first wave conduit and coupling turns
It changes between the bottom end of chamber, the second waveguide pipe is vertically arranged with first wave conduit；
The bottom end of the Mode-transducing antenna extends in the second waveguide pipe.
Preferably, it in above-mentioned single-crystal diamond synthesizer, is provided between the first wave conduit and microwave source
Tuner, the tuner is adjusting the waveform of the microwave transmitted in first wave conduit.
Preferably, in above-mentioned single-crystal diamond synthesizer, the side wall of the coupling conversion chamber is provided with water cooling dress
It sets.
Preferably, in above-mentioned single-crystal diamond synthesizer, the resonance device includes upper shell and lower housing, institute
It states upper shell to be close to or far from the lower housing, to seal or open the resonant cavity.
Preferably, in above-mentioned single-crystal diamond synthesizer, guiding is provided between the upper shell and lower housing
Bar, the upper shell are slided up and down along the guide rod.
Preferably, further include water-cooling shaft in above-mentioned single-crystal diamond synthesizer, the bottom end of the water-cooling shaft passes through institute
It states upper shell and is connected to the pedestal, water-cooling shaft controls the temperature of pedestal by water-cooling pattern.
Preferably, in above-mentioned single-crystal diamond synthesizer, the water-cooling shaft convexedly stretches in outside the upper shell
Part is arranged with expansion corrugated pipe, and a closed cavity is formed between the expansion corrugated pipe and water-cooling shaft, upper shell.
Preferably, in above-mentioned single-crystal diamond synthesizer, the position that substrate is corresponded on the resonant cavity is provided with
An at least form.
Preferably, in above-mentioned single-crystal diamond synthesizer, the position that substrate is corresponded on the resonant cavity is provided with
Double-colored sensor.
Preferably, in above-mentioned single-crystal diamond synthesizer, the side wall of the resonant cavity is provided with circulating water
Device.
Correspondingly, disclosed herein as well is a kind of single-crystal diamond synthetic method, plasma is formed in the lower section of substrate,
And in the lower surface depositing monocrystalline diamond of substrate.
Preferably, in above-mentioned single-crystal diamond synthetic method, the substrate is seed crystal.
Preferably, in above-mentioned single-crystal diamond synthetic method, the plasma is formed using antenna coupling system.
Compared with the prior art, the advantages of the present invention are as follows：The present invention by substrate lower surface depositing diamond film,
It can be polluted with the impurity in effective solution diamond production process.
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 single-crystal diamond synthesizer in the specific embodiment of the invention；
Fig. 2 show the mounting structure schematic diagram of pedestal and substrate 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, the present embodiment provides a kind of single-crystal diamond synthesizers, including microwave source 10, plasma
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-
It can be 915MHz-2.45GHz that the power of wave, which can be 6-75kW, frequency,.
In the present embodiment, microwave source 10 generate microwave power be 6-10kW, frequency 2.45GHz.
In conjunction with shown in Fig. 2, resonance device 30 includes a resonant cavity 31, in resonant cavity 31 on be provided with pedestal 32, the pedestal
32 lower surface is supporting substrate 33.Plasmon coupling device 20 is located at the lower section of pedestal 32, and can will come from micro-
The microwave of wave source 10 excites below pedestal 32 and forms plasma.
Substrate 33 is to provide the coated surface of a depositing diamond film, and material is preferably diamond seed, at other
In embodiment, alumina substrate etc. can also be used.
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.
In the technical solution, by that in substrate lower surface depositing diamond film, can be produced with effective solution diamond
Impurity pollution in the process.
In a preferred embodiment, plasmon coupling device 20 uses antenna manifold type.
Specifically, plasmon coupling device 20 includes waveguide, Mode-transducing antenna 21, coupling conversion chamber 22 and medium
Window 23.
Wherein, waveguide is connected between microwave source 10 and coupling conversion chamber 22；The top of Mode-transducing antenna 21 extends
To coupling conversion chamber 22；Coupling conversion chamber 22 is set to the lower section of resonant cavity 31, and medium window 23 is located at resonant cavity 31 and coupling
It closes between converting chamber 22.
Substrate 33 is used for deposition film, such as diamond thin, is fixed on 32 lower section of pedestal, and substrate 33 should be corresponded to and be set
It sets in the surface of medium window 23, and plated film placed face down.
The medium window 23 of 31 bottom 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 bottom end of coupling conversion chamber 22, the second waveguide pipe 25 is vertical with first wave conduit 24 to be set
It sets；Mode-transducing antenna 21 is coaxially disposed with second waveguide pipe 25.
Convert chamber 22 can be metal sidewall for coupling, and when chamber 22 is converted in setting coupling, Mode-transducing antenna 21 can be by
The microwave of TE10 patterns in first wave conduit 24 is converted to TEM mode, and is sent to coupling conversion chamber through second waveguide pipe 25
After 22, the microwave of TEM mode is converted to TM01 patterns by Mode-transducing antenna 21 again, hence into resonant cavity 31.This setting side
Formula can avoid the microwave by TE10 patterns from being converted directly into the microwaves of the not corresponding TM01 patterns of electric field, to make to be formed by
The energy maximization of TM01 modes microwaves further increases the service efficiency of microwave energy.Also, the microwave of TM01 patterns can
So that 33 lower zone of substrate is formed the electromagnetic field of maximum intensity, and is conducive to excite ellipsoid or spherical plasma, to
The side wall for avoiding resonant cavity 31 generates pollution 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
Mode-transducing antenna 21 matches, and to make the microwave energy of input maximize, such as it can be three spiral shells of this field routine
Follow closely impedance 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.Using the mistake of standard
Cross waveguide WR340to 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, 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.
In another embodiment, plasmon coupling device 20 uses surface wave manifold type, principle to be：Microwave is set to pass through
Circulator and waveguide are crossed, vacuum chamber is entered by coupling aperture under the adjusting of waveguide short piston, when microwave power is sufficiently large
When, compared under low pressure can gas breakdown electric discharge, and short-circuit plunger adjusting under form high-density plasma.
In another embodiment, plasmon coupling device 20 uses direct coupling type, principle to be：Make microwave through wave
Conduit enters through quartz window in the vacuum of sealing, the direct-coupling excitation generation in the case where the short-circuit plunger of waveguide pipe end is adjusted
Plasma, however its exist the adjusting tool of output power-adjustable range small, to formation plasma acquire a certain degree of difficulty, film
The defects of degree of purity and limited depositional area.
In conjunction with shown in Fig. 1, in one embodiment, resonance device 30 includes upper shell 34 and lower housing 35, and upper shell 34 can
Close to or away from lower housing 35, to seal or open resonant cavity 31.
Further, guide rod 36 is provided between upper shell 34 and lower housing 35, upper shell 34 is along about 36 guide rod
Sliding.
It is understood that the bottom end of upper shell 34 and the top of lower housing 35 are respectively arranged with upper flange 341 and laxative remedy
Orchid 351, is provided with sealing ring 37, guide rod 36 is fixed on lower flange between upper flange 341 and the contact surface of lower flange 351.
37 material of sealing ring is improved using circle fluorine material, heat-resisting ability, and o-ring groove all has water cooling tank up and down, is used
In coolant seal circle.
Further, further include water-cooling shaft 37, the bottom end of the water-cooling shaft 37 passes through upper shell 34 and is connected to pedestal 32, water
Cold axis 37 controls the temperature of pedestal 32 by water-cooling pattern.
Further, the part that water-cooling shaft 37 convexedly stretches in outside upper shell 34 is arranged with expansion corrugated pipe 38, this is flexible
A closed cavity is formed between bellows 38 and water-cooling shaft 37, upper shell 34.
In the technical solution, the preferably flexible metal bellows of expansion corrugated pipe can be to maintain water-cooling shaft when flexible
The part outside upper shell 34 is protruded out, is in vacuum cavity always, is avoided contacting with extraneous air and pollute and to humorous
The chamber 31 that shakes has an impact.
Guide sleeve 41 is additionally provided between water-cooling shaft 37 and upper shell 34, guide sleeve 41 is set in the outside of water-cooling shaft 37.
In the technical solution, when guide sleeve 38 ensures that water-cooling shaft position in vertical direction and water-cooling shaft move up and down
Stability.
In one embodiment, the position that substrate 33 is corresponded on resonant cavity 31 is provided with an at least form 39.
In a preferred embodiment, the surrounding of resonant cavity is provided with 2 forms, and form is symmetrical with symmetrical the two of resonant cavity
Side.By form for observing plasma position and shape.
In one embodiment, the position for substrate 33 being corresponded on resonant cavity 31 is provided with double-colored sensor 310.
Non-contact measurement seed temperature may be used in the double-colored sensor.
In one embodiment, the side wall of resonant cavity 31 is provided with circulating water cooling device.
In conjunction with shown in Fig. 2, pedestal 32 is preferably water cooling molybdenum plate, and fixed seat 321 and pressing plate are provided with below water cooling molybdenum plate
Clamp block 322 and fixed seat 321 are fixed on the lower surface of water cooling molybdenum plate by block 322, titanium alloy bolt 323 successively.
Fixed seat 321 is annular, surrounds a located space with the lower surface of water cooling molybdenum plate, substrate 33 is equipped with fixed in this
In bit space, clamp block 322 is annular, and edge is convexedly stretched in below located space, is supported to the edge to substrate.
In one embodiment, the material of clamp block 322 and fixed seat 321 is pure molybdenum.
In the technical solution, titanium alloy bolt, and design bolt long enough and loosened with preventing bolt high-temerature creep.Base
33 top surface of piece comes into full contact with molybdenum plate, the cooling effect for ensureing substrate.
It is necessary, high-purity process gas inlets 311 are also communicated on resonant cavity 31, gas feed is that surrounding is vortexed into chamber
Body, each aperture are about 0.5~1mm of diameter, and circumferencial direction is uniformly distributed general 8~10.
It is necessary, it is additionally provided on resonant cavity 31 and vacuumizes interface 312, vacuumize interface 312 by pipeline and vacuum pump
Connection.
Vacuumizing setting on interface 312, there are two thin film vacuum gauges 313, one of thin film vacuum gauge 313 to be used for
The end vacuum of cavity measures, measurement of another thin film vacuum gauge 313 for process pressure after equipment operation.Processing procedure pressure
Power meter can be interlocked with ratio, arbitrary steady pressure of the control cavity in range.
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 the conversion of Mode-transducing antenna 21,
It is propagated in second waveguide pipe 25, after entering coupling conversion chamber 22, is converted again through Mode-transducing antenna 21 in a tem mode
For TM01 patterns, enter resonant cavity 31, the activity of methane formation carbon-containing group and atomic state of 33 lower section of substrate through medium window 23
Hydrogen, and spherical plasma 40 is formed, to deposit to obtain the diamond thin of large area in 33 lower surface of substrate.
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 31 is opened, seed crystal is fixed on to the lower surface of pedestal 32；
(8), cavity is closed；
(9), low-voltage vacuum is taken out in first wave conduit 24；
(10), it adjusts water-cooling shaft 37 and arrives suitable position, to control the temperature of seed crystal；
(11), resonant cavity 31 is cleaned with high-purity hydrogen：It is evacuated down to end vacuum, or the pumping of resonant cavity 31 is cleaned multiple times
To 5torr, it is pressurized to 20torr, is recycled 4~5 times；
(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), 900~1400 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 single-crystal diamond synthesizer, which is characterized in that filled including microwave source, plasmon coupling device and resonance
It sets,
The resonance device includes a resonant cavity, has a diamond growth face in the resonant cavity,
Plasmon coupling device can excite the microwave from the microwave source in the lower section in diamond growth face to be formed
Gas ions.
2. single-crystal diamond synthesizer according to claim 1, which is characterized in that the plasmon coupling device is adopted
With antenna manifold type.
3. single-crystal diamond synthesizer according to claim 2, which is characterized in that the plasmon coupling device packet
Waveguide, Mode-transducing antenna, coupling conversion chamber and medium window are included,
The waveguide is connected between the microwave source and coupling conversion chamber；
The top of the Mode-transducing antenna extends to the coupling conversion intracavitary；
The coupling conversion chamber is set to the lower section of the resonant cavity, and the medium window is located at the resonant cavity and coupling is converted
Between chamber.
4. single-crystal diamond synthesizer according to claim 3, which is characterized in that the waveguide includes first wave guide
Pipe and second waveguide pipe,
The first wave conduit is rectangular waveguide；
The coupling converts chamber as circular waveguide, and the second waveguide pipe is connected to the first wave conduit and coupling conversion chamber
Bottom end between, the second waveguide pipe is vertically arranged with first wave conduit；
The bottom end of the Mode-transducing antenna extends in the second waveguide pipe.
5. single-crystal diamond synthesizer according to claim 4, which is characterized in that the first wave conduit and microwave source
Between be provided with tuner, the tuner is adjusting the waveform of the microwave transmitted in first wave conduit.
6. single-crystal diamond synthesizer according to claim 3, which is characterized in that the side wall of the coupling conversion chamber is set
It is equipped with water cooling plant.
7. single-crystal diamond synthesizer according to claim 1, which is characterized in that the resonance device includes upper shell
And lower housing, the upper shell is close to or far from the lower housing, to seal or open the resonant cavity.
8. single-crystal diamond synthesizer according to claim 7, which is characterized in that between the upper shell and lower housing
It is provided with guide rod, the upper shell is slided up and down along the guide rod.
9. single-crystal diamond synthesizer according to claim 7, which is characterized in that be provided with base in the resonant cavity
Seat, to mounted substrate, single-crystal diamond synthesizer further includes water-cooling shaft for the lower surface of the pedestal, and the bottom end of the water-cooling shaft is worn
It crosses the upper shell and is connected to the pedestal, water-cooling shaft controls the temperature of pedestal by water-cooling pattern.
10. single-crystal diamond synthesizer according to claim 9, which is characterized in that the water-cooling shaft convexedly stretches in described
Part outside upper shell is arranged with expansion corrugated pipe, and a closing chamber is formed between the expansion corrugated pipe and water-cooling shaft, upper shell
Body.
11. single-crystal diamond synthesizer according to claim 1, which is characterized in that correspond to substrate on the resonant cavity
Position be provided with an at least form.
12. single-crystal diamond synthesizer according to claim 1, which is characterized in that correspond to substrate on the resonant cavity
Position be provided with double-colored sensor.
13. single-crystal diamond synthesizer according to claim 1, which is characterized in that the side wall of the resonant cavity is arranged
There is circulating water cooling device.
14. a kind of single-crystal diamond synthetic method, which is characterized in that excite plasma in the lower section of substrate, and in substrate
Lower surface depositing monocrystalline diamond.
15. single-crystal diamond synthetic method according to claim 14, which is characterized in that the substrate is seed crystal.
16. single-crystal diamond synthetic method according to claim 14, which is characterized in that formed using antenna coupling system
The plasma.
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| CN111235634A (en) * | 2020-03-09 | 2020-06-05 | 上海三朗纳米技术有限公司 | Microwave plasma diamond growth equipment and application method thereof |
| 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 |
| CN113058506A (en) * | 2021-03-23 | 2021-07-02 | 湖州中芯半导体科技有限公司 | High-efficiency synthesis process and device for MPCVD diamond |
| CN113265649A (en) * | 2021-06-18 | 2021-08-17 | 长沙新材料产业研究院有限公司 | A flange and MPCVD device for MPCVD cavity is connected |
| CN119571453A (en) * | 2025-02-05 | 2025-03-07 | 浙江晶盛机电股份有限公司 | Diamond crystal growth device |
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