CN109518272A - A kind of preparation method of large size single crystal diamond - Google Patents
A kind of preparation method of large size single crystal diamond Download PDFInfo
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- CN109518272A CN109518272A CN201811342144.XA CN201811342144A CN109518272A CN 109518272 A CN109518272 A CN 109518272A CN 201811342144 A CN201811342144 A CN 201811342144A CN 109518272 A CN109518272 A CN 109518272A
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- crystal diamond
- substrate
- preparation
- large size
- single crystal
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- 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
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention proposes a kind of preparation methods of large size single crystal diamond, single-crystal diamond substrate is placed on the chip bench of microwave cavity in method of the invention, it is ionized the mixed reaction gas such as methane and hydrogen before entering microwave cavity laser dissociation is intracavitary, laser dissociation chamber can make laser in intracavitary formation resonances, light intensity is improved 10 times or more, the power of laser can be effectively reduced；Gas largely absorbs energy and is sufficiently dissociated into after plasma under electric field action into microwave resonance is intracavitary and grown, under the action of microwave energy, unionized gas molecule is ionized again, so that hydrocarbon active group concentration increases, to realize the purpose for accelerating single-crystal diamond fast-growth, and growing large-size single-crystal diamond can be used to, the single-crystal diamond size prepared can reach 300mm.
Description
Technical field
The present invention relates to technical field of film preparation more particularly to a kind of preparation methods of large size single crystal diamond.
Background technique
Diamond is a kind of semiconductor material with wide forbidden band, band gap width 5.5eV.It has extremely excellent physical
Matter, such as high carrier mobility high heat conductance (22Wcm-1K-1), high breakdown electric field (10MVcm-1), high carrier are full
(electronic carrier saturation rate is 1.5 × 107~2.7 × 107cms-1, and holoe carrier saturation rate is 0.85 with rate
× 107~1.2 × 107cms-1) and low-k (5.7) etc..Based on these excellent performance parameters, diamond is recognized
To be to prepare next-generation high power, high frequency, high temperature and the most promising material of low-power consumption electronic device.
The preparation method of diamond mainly includes high temperature and pressure (HTHP) method and chemical vapor deposition (CVD) method.High temperature is high
The diamond of platen press preparation typically contains certain impurity, influences the quality of diamond, and expensive, technical requirements are severe
It carves.Tool grade diamond is mainly prepared at present, is used for tool coating.The diamond of the available high quality of CVD method, without impurity
Incorporation, it is substantially colorless transparent.CVD method mainly include HFCVD method, microwave plasma CVD (MPCVD) method, etc. from
CVD method, hot cathode plasma CVD method and laser induced plasma CVD method etc. are sprayed in daughter.Wherein HFCVD method, MPCVD
Method and plasma jet CVD method are current main technologies of preparing.And MPCVD method can produce due to using electrodeless discharge
Pure plasma becomes preparation high-quality Buddha's warrior attendant to avoid polluting as caused by electrode use in other growing methods
The prefered method of stone film.
Summary of the invention
The main purpose of the present invention is to provide a kind of preparation methods of large size single crystal diamond, it is desirable to provide one kind is adopted
The method for preparing large size single crystal diamond with MPCVD method.
To achieve the above object, the preparation method of a kind of large size single crystal diamond provided by the invention, the method packet
Include following steps:
Step 10, substrate is pre-processed using predetermined manner；
Step 20, diamond substrate is pre-processed；
Step 30, pretreated diamond substrate will be carried out and substrate is installed to predeterminated position；
Step 40, gas washing processing is carried out to chamber, and carries out vacuumize process after gas washing；
Step 50, the gas containing carbon source is passed through into laser dissociation chamber to be ionized；
Step 60, apply electric field between chip bench and spray head；
Step 70, the gas after ionization is then passed through progress microwave plasma chemical gas phase in the microwave cavity
Deposition, grows single-crystal diamond on substrate.
Preferably, pretreated step is carried out to substrate using predetermined manner in the step 10 are as follows: throw to substrate
Light processing makes substrate surface flat.
It preferably, is that polishing pretreatment is carried out to diamond substrate in the step 20, so that diamond surface planarizes.
Preferably, the pressure after being vacuumized by step 40 is 5.6 × 10-4~6.4 × 10-4。
Preferably, the carbon source in the step 50 is CH4.
Preferably, the pulsewidth that the intracavitary laser of the laser dissociation is injected in the step 50 is 50~100fs
Preferably, the intensity of the electric field applied between the chip bench and the spray head in the step 60 is
300~500V/m.
Single-crystal diamond substrate, is placed on microwave resonance by the growing method of efficient large size single crystal diamond of the invention
On the chip bench of chamber, fill the mixed reaction gas such as methane and hydrogen before entering microwave cavity laser dissociation is intracavitary
Divide ionization, laser dissociation chamber can make laser in intracavitary formation resonances, and light intensity is improved 10 times or more, can be effectively reduced sharp
The power of light device；Gas largely absorb energy be sufficiently dissociated into after plasma under electric field action enter microwave resonance it is intracavitary into
Row growth, under the action of microwave energy, unionized gas molecule is ionized again, so that hydrocarbon active group concentration increases
Add, to realize the purpose for accelerating single-crystal diamond fast-growth, and growing large-size single-crystal diamond, preparation can be used to
Single-crystal diamond size out can reach 300mm.
Specific embodiment
The technical issues of embodiment of the present invention is solved combined with specific embodiments below, used technical solution and reality
Existing technical effect carries out clear, complete description.Obviously, described embodiment is only that a part of the application is implemented
Example, is not whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not making the creative labor
Under the premise of, all other equivalent or obvious variant embodiment obtained is fallen within the scope of protection of the present invention.This hair
Bright embodiment can be embodied according to the multitude of different ways being defined and covered by claim.
It should be noted that in the following description, understanding for convenience, giving many details.But it is very bright
Aobvious, realization of the invention can be without these details.
It should be noted that in the absence of clear limitations or conflicts, each embodiment in the present invention and its
In technical characteristic can be combined with each other and form technical solution.
In the present embodiment, described method includes following steps:
Step 10, substrate is pre-processed using predetermined manner；
Step 20, diamond substrate is pre-processed；
Step 30, pretreated diamond substrate will be carried out and substrate is installed to predeterminated position；
Step 40, gas washing processing is carried out to chamber, and carries out vacuumize process after gas washing；
Step 50, the gas containing carbon source is passed through into laser dissociation chamber to be ionized；
Step 60, apply electric field between chip bench and spray head；
Step 70, the gas after ionization is then passed through progress microwave plasma chemical gas phase in the microwave cavity
Deposition, grows single-crystal diamond on substrate.
Efficient large size single crystal diamond growth device includes vapor deposition portion, laser dissociation portion, electric field applying unit), with
And gas supply part.
Vapor deposition portion is MPCVD equipment, it includes microwave cavity, chip bench and microwave generator.
Microwave cavity is used for diamond epitaxial growth, and in the present embodiment, the internal diameter of microwave cavity is 360mm.Microwave
Resonant cavity side lower is equipped with exhaust outlet, and exhaust outlet is controlled to a vacuum pump by bellows；Gas is being passed through to microwave resonance is intracavitary
Before body, cavity pressure can be controlled in 0.1Pa or higher by vacuum pump；Microwave cavity is equipped with thermocouple on side
Sensor.
Chip bench is erected in microwave cavity, and upper surface is for placing diamond epitaxial substrate.When work, above substrate
It will form plasma sphere.
Microwave generator includes Mode-transducing antenna, waveguide and microwave source；Mode-transducing antenna setting is humorous in microwave
Shake 21 top of chamber, and lower end connects microwave cavity；The front-end and back-end of waveguide respectively with Mode-transducing antenna and microwave source phase
Even.
Laser dissociation portion includes laser dissociation chamber, spray head, laser and connecting tube.
Laser dissociation chamber is connected with microwave cavity, it includes laser dissociation cavity, preceding mirror and rear mirror.
Embodiment 1: monocrystalline is grown using the method that laser dissociation chamber is combined with microwave plasma CVD
Diamond before deposition first polishes seeded growth face, supersound washing in pickling and deionized water, and is blown with hot wind
It is put on chip bench after dry.Intracavitary air pressure is evacuated to 5.6 × 10 using vacuum pump-4Pa is passed through the H2 of 100sccm to entire microwave
It is replaced in resonant cavity.Microwave generator is opened, microwave power and air pressure are separately positioned on 8kW and 18kPa, deposition temperature
Degree control opens gas supply part and is passed through reaction gas after 980 DEG C, stabilization to be achieved, CH4:H2=1.5% (V/ in reaction gas
V), total gas flow rate control is in 400sccm.Laser is opened, selects central wavelength for the femtosecond laser of 1061nm, pulsewidth
50fs, laser light incident peak power 2 × 1012W/cm2.Rear mirror on laser dissociation chamber is 100% to incident light reflectivity, electric field
The external electronic field that applying unit provides is 400V/m, after sedimentation time 20h, closes laser, microwave generator, electric field and applies
Portion and gas supply part further take out sample, and the growth rate that single-crystal diamond is obtained after measurement is 30 μm/h.
Embodiment 2: monocrystalline is grown using the method that laser dissociation chamber is combined with microwave plasma CVD
Diamond before deposition first polishes seeded growth face, supersound washing in pickling and deionized water, and is blown with hot wind
It is put on chip bench after dry.Intracavitary air pressure is evacuated to 5.6 × 10 using vacuum pump-4Pa is passed through the H2 of 100sccm to entire microwave
It is replaced in resonant cavity.Microwave generator is opened, microwave power and air pressure are separately positioned on 8kW and 18kPa, deposition temperature
Degree control opens gas supply part and is passed through reaction gas after 980 DEG C, stabilization to be achieved, CH4:H2=2.5% (V/ in reaction gas
V), total gas flow rate control is in 400sccm.Laser is opened, selects central wavelength for the femtosecond laser of 1061nm, pulsewidth
80fs, laser light incident peak power 2 × 1012W/cm2.Rear mirror on laser dissociation chamber is 100% to incident light reflectivity, electric field
The external electronic field that applying unit provides is 400V/m, after sedimentation time 20h, closes laser, microwave generator, electric field and applies
Portion and gas supply part further take out sample, and the growth rate that single-crystal diamond is obtained after measurement is 35 μm/h.
Embodiment 3: monocrystalline is grown using the method that laser dissociation chamber is combined with microwave plasma CVD
Diamond before deposition first polishes seeded growth face, supersound washing in pickling and deionized water, and is blown with hot wind
It is put on chip bench after dry.Intracavitary air pressure is evacuated to 5.6 × 10 using vacuum pump-4Pa is passed through the H2 of 100sccm to entire microwave
It is replaced in resonant cavity.Microwave generator is opened, microwave power and air pressure are separately positioned on 8kW and 18kPa, deposition temperature
Degree control opens gas supply part and is passed through reaction gas after 980 DEG C, stabilization to be achieved, CH4:H2=3.5% (V/ in reaction gas
V), total gas flow rate control is in 400sccm.Laser is opened, selects central wavelength for the femtosecond laser of 1061nm, pulsewidth
100fs, laser light incident peak power 2 × 1012W/cm2.Rear mirror on laser dissociation chamber is 100% to incident light reflectivity, electricity
The external electronic field that applying unit provides is 400V/m, after sedimentation time 20h, closes laser, microwave generator, electric field and applies
Portion and gas supply part further take out sample, and the growth rate that single-crystal diamond is obtained after measurement is 40 μm/h.
Single-crystal diamond substrate, is placed on microwave resonance by the growing method of efficient large size single crystal diamond of the invention
On the chip bench of chamber, fill the mixed reaction gas such as methane and hydrogen before entering microwave cavity laser dissociation is intracavitary
Divide ionization, laser dissociation chamber can make laser in intracavitary formation resonances, and light intensity is improved 10 times or more, can be effectively reduced sharp
The power of light device；Gas largely absorb energy be sufficiently dissociated into after plasma under electric field action enter microwave resonance it is intracavitary into
Row growth, under the action of microwave energy, unionized gas molecule is ionized again, so that hydrocarbon active group concentration increases
Add, to realize the purpose for accelerating single-crystal diamond fast-growth, and growing large-size single-crystal diamond, preparation can be used to
Single-crystal diamond size out can reach 300mm.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of large size single crystal diamond, which is characterized in that described method includes following steps:
Step 10, substrate is pre-processed using predetermined manner；
Step 20, diamond substrate is pre-processed；
Step 30, pretreated diamond substrate will be carried out and substrate is installed to predeterminated position；
Step 40, gas washing processing is carried out to chamber, and carries out vacuumize process after gas washing；
Step 50, the gas containing carbon source is passed through into laser dissociation chamber to be ionized；
Step 60, apply electric field between chip bench and spray head；
Step 70, the gas after ionization is then passed through progress microwave plasma chemical gas phase in the microwave cavity to sink
Product, grows single-crystal diamond on substrate.
2. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that adopted in the step 10
Pretreated step is carried out to substrate with predetermined manner are as follows: be processed by shot blasting to make substrate surface flat to substrate.
3. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that be in the step 20
Polishing pretreatment is carried out to diamond substrate, so that diamond surface planarizes.
4. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that carried out by step 40
Pressure after vacuumizing is 5.6 × 10-4~6.4×10-4。
5. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that in the step 50
Carbon source is CH4.
6. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that penetrated in the step 50
The pulsewidth for entering the intracavitary laser of the laser dissociation is 50~100fs.
7. the preparation method of large size single crystal diamond according to claim 1, which is characterized in that in the step 60
The intensity of the electric field applied between the chip bench and the spray head is 300~500V/m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811342144.XA CN109518272A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of large size single crystal diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811342144.XA CN109518272A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of large size single crystal diamond |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109518272A true CN109518272A (en) | 2019-03-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811342144.XA Withdrawn CN109518272A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of large size single crystal diamond |
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| CN (1) | CN109518272A (en) |
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2018
- 2018-11-12 CN CN201811342144.XA patent/CN109518272A/en not_active Withdrawn
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Application publication date: 20190326 |
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