CN104878447B - A kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond - Google Patents
A kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond Download PDFInfo
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Abstract
A kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond, the present invention relates to the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.The invention solves the problems that seed crystal is easily blown off-target position by air-flow in existing MWCVD growing system, and between seed crystal and metal molybdenum substrate, heat conduction is difficult, causes seed crystal face Quality Down and the problem being difficult to observe using vacuum brazing.Method：First, clean；2nd, select native gold；3rd, place sample；4th, connect in situ；5th, diamond film, that is, complete the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.The present invention is used for a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
Description
Technical field
The present invention relates to the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
Background technology
In recent years, large size single crystal diamond and quasi- single-crystal diamond are due to its high hardness, highest thermal conductivity, pole
Wide electromagnetism passes through frequency range, excellent Radiation hardness and decay resistance, in Precision Machining, high frequency communications, space flight aerospace, point
Based on the high-tech areas such as end technology day by day become, crucial or even unique material solution.Traditional artificial single crystal's Buddha's warrior attendant
Stone is using High Temperature High Pressure (HPHT) method, and the diamond that the method is prepared is impure more, and defect concentration is higher, and quality is relatively
Poor, and size is less, differs greatly compared with the demand of related application, leads to the HPHT diamond scope of application narrower, is expert at
It is in downstream, profit is low, and competitiveness is not strong in industry.
Compared to HPHT method, microwave plasma enhanced chemical vapor deposition (MWCVD) method is that preparing of generally acknowledging at present is big
One of best approach of size single crystal diamond, the method preparation single-crystal diamond have impurity concentration low, through wide waveband,
The advantages of defect concentration is low, size is larger and growth rate is controlled is it is considered to be promise to be following production in enormous quantities people most
The method making diamond.
During the method epitaxial growth single-crystal diamond, diamond seed and axiolitic plasma directly contact, therefore
The concentration of the temperature of control seed crystal face and plasma is the factor of non-the normally off key：Temperature is too high to lead to diamond surface
There is graphitization, temperature is too low to lead to declining to a great extent of seeded growth quality；Meanwhile, the concentration of plasma and uniformity
Growth quality on seed crystal and speed have very big impact.Therefore seed crystal needs to place in place, and is in suitably
Under temperature field and uniform plasma density, the high-quality fast-growth of guarantee seed crystal.
During the course of the reaction, diamond seed is typically placed in metal molybdenum substrate, and metal molybdenum substrate is positioned over MWCVD
On the base of instrument.Due to the quality very little of diamond seed itself, only tens milligrams, in instrument evacuation and be passed through reaction
During gas, seed crystal is easily blown by air-flow, leads to seed crystal position deviation optimum position, causes the big of temperature and plasma density
Amplitude variation, has a strong impact on the growth quality of seed crystal.So in traditional monocrystalline growing process, generally will using vacuum brazing furnace
Diamond seed and substrate link together, to ensure the fixation of seed crystal.But because the vacuum of vacuum brazing furnace is relatively low, in height
In warm brazing process, remaining air easily makes diamond seed surface that graphitization, the growth of extreme influence single crystalline layer occur
Quality.And brazing process carries out it is impossible to carry out Real Time Observation completely in stove, only could obtain after soldering terminates to take out sample
Know welding result.
Further, since the surface of seed crystal and metal molybdenum cannot ensure to spend absolutely smooth so that thermal contact conductance face therebetween
Very little, and with the presence of gas blanket, lead between seed crystal and metal molybdenum, form very big thermal resistance so that seed crystal face is because heat concentrates
Temperature is too high, and growth quality is subject to extreme influence.So, for controlling diamond seed to be in stable and optimum work in growth
Under skill parameter, realize the fast-growth of large scale high-quality single-crystal diamond it is necessary to find can fixed diamond seed crystal, and strengthen
The method of heat conduction between seed crystal and substrate.
Content of the invention
The invention solves the problems that in existing MWCVD growing system, seed crystal is easily blown off-target position by air-flow, and seed
Brilliant heat conduction difficulty and metal molybdenum substrate between, causes seed crystal face Quality Down using vacuum brazing and is difficult the problem observed,
And a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond is provided.
A kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond, specifically enters according to following steps
Row：
First, clean：Diamond seed and metal molybdenum substrate disk are carried out, the diamond seed after being cleaned and
Metal molybdenum substrate disk after cleaning；
2nd, select native gold：The smooth native gold selecting thickness to be 20 μm～100 μm, smooth native gold is cut into and compares diamond
The square piece of all big 0.5mm～1.5mm of seed crystal length and width, obtains welding medium；
Described smooth native gold purity is 18K～24K；
3rd, place sample：
Four metal molybdenum filaments are put into " well " font, obtains metal molybdenum filament base, metal molybdenum filament base is positioned over micro-
In ripple plasma auxiliary chemical vapor deposition instrument trays, then by cleaning after metal molybdenum substrate disk, welding medium and
Diamond seed after cleaning is sequentially placed on metal molybdenum filament base, makes the diamond seed surface level after cleaning and is in gold
Belong to molybdenum filament base center；
Described metal molybdenum filament length is 5mm～20mm, a diameter of 0.3mm～2mm；
4th, connect in situ：
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, evacuation is carried out to nacelle, makes nacelle true
Reciprocal of duty cycle reaches 3.0 × 10-6Mbar～5.0 × 10-6mbar；
2., opening program, sets hydrogen flowing quantity as 100sccm～200sccm, and nacelle air pressure is 10mbar～30mbar,
Start microwave generator, activate plasma；
3., with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, real-time monitoring diamond seed surface temperature,
With the rising of nacelle air pressure, diamond seed surface temperature raises, when nacelle air pressure is increased to 90mbar～120mbar
When, now the power of microwave plasma enhanced chemical vapor deposition instrument is 2800W～3700W, diamond seed surface temperature
Degree reach 1100 DEG C～1300 DEG C, continue with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, work as diamond seed
50 DEG C～150 DEG C of rapid drawdown in surface temperature, and diamond seed brightness deterioration, again becomes redness again, welded in place completes；
4., with speed as 1mbar/s～3mbar/s reduce air pressure, make air pressure be down to 5mbar～10mbar, power is down to
1680W～1750W, temperature is reduced to room temperature；
5., to nacelle evacuation, vacuum in nacelle is made to reach 2.0 × 10-6Mbar～8.0 × 10-6mbar；
6., exit, after making nacelle internal gas pressure reach 1atm, open the cabin, obtain the sample being welded, that is, complete homoepitaxy life
The Seed crystal substrate original position method of attachment of long single-crystal diamond.
The invention has the beneficial effects as follows：1st, the present invention passes through the method connecting in situ in cabin, makes diamond sample and metal
Form strong bonded it is therefore prevented that seed crystal is blown deviation in evacuation with when being passed through gas because air-flow is excessive between molybdenum substrate
The problem of best placement is it is ensured that diamond seed all-the-time stable in growth course is in optimal temperature field and plasma is dense
Degree lower it is ensured that the stablizing of growth technique.
2nd, original position interconnection technique eliminates and for sample to put into the step that vacuum brazing furnace is attached, and greatly simplifies behaviour
Make, saved time and cost.Operate under the hydrogen plasma atmosphere in MWCVD instrument room body simultaneously, effectively prevent height
The graphited problem on the lower diamond seed surface of temperature, makes seed crystal face be grown with best in quality.
3rd, the original position connection procedure in MWCVD instrument can carry out monitor in real time by the watch window of instrument, and can
Carry out the suitable adjustment of technological parameter according to different situations, it is to avoid because work cannot be observed when being operated in vacuum brazing furnace
Skill process and lead to the problem of connection failure.
4th, because the fabulous ductility of native gold and heat conductivity are it is ensured that form good between diamond print and metal molybdenum substrate
Good thermal contact conductance, it is therefore prevented that the heat on diamond sample surface is concentrated, greatly reduces surface temperature too high and stone occurs
The possibility of inkization, also makes diamond sample be under optimal growthing process parameter, growth result is more preferable simultaneously.
The present invention is used for a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
Brief description
Fig. 1 welds with metal molybdenum filament and groined type disposing way schematic diagram for the present invention；
Fig. 2 is the metal molybdenum substrate disk after the diamond seed after present invention cleaning, welding medium, cleaning and metal molybdenum
The lamination sequence chart of silk base；1 is the diamond seed after cleaning；2 is welding medium；3 is the metal molybdenum substrate circle after cleaning
Piece；4 is metal molybdenum filament base；
Fig. 3 is the graph of a relation of surface temperature of the present invention-cabin internal gas pressure specification；
Fig. 4 is the growth morphology figure that the Seed crystal substrate not carrying out connecting in situ grows single-crystal diamond；
Fig. 5 is the growth morphology that embodiment one connects the Seed crystal substrate isoepitaxial growth single-crystal diamond of preparation in situ
Figure.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also include each specific embodiment it
Between combination in any.
Specific embodiment one：Illustrate present embodiment in conjunction with Fig. 1 and Fig. 2, the one kind described in present embodiment is same
The Seed crystal substrate original position method of attachment of matter epitaxial growth single-crystal diamond, specifically follows the steps below：
First, clean：Diamond seed and metal molybdenum substrate disk are carried out, the diamond seed after being cleaned and
Metal molybdenum substrate disk after cleaning；
2nd, select native gold：The smooth native gold selecting thickness to be 20 μm～100 μm, smooth native gold is cut into and compares diamond
The square piece of all big 0.5mm～1.5mm of seed crystal length and width, obtains welding medium；
Described smooth native gold purity is 18K～24K；
3rd, place sample：
Four metal molybdenum filaments are put into " well " font, obtains metal molybdenum filament base, metal molybdenum filament base is positioned over micro-
In ripple plasma auxiliary chemical vapor deposition instrument trays, then by cleaning after metal molybdenum substrate disk, welding medium and
Diamond seed after cleaning is sequentially placed on metal molybdenum filament base, makes the diamond seed surface level after cleaning and is in gold
Belong to molybdenum filament base center；
Described metal molybdenum filament length is 5mm～20mm, a diameter of 0.3mm～2mm；
4th, connect in situ：
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, evacuation is carried out to nacelle, makes nacelle true
Reciprocal of duty cycle reaches 3.0 × 10-6Mbar～5.0 × 10-6mbar；
2., opening program, sets hydrogen flowing quantity as 100sccm～200sccm, and nacelle air pressure is 10mbar～30mbar,
Start microwave generator, activate plasma；
3., with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, real-time monitoring diamond seed surface temperature,
With the rising of nacelle air pressure, diamond seed surface temperature raises, when nacelle air pressure is increased to 90mbar～120mbar
When, now the power of microwave plasma enhanced chemical vapor deposition instrument is 2800W～3700W, diamond seed surface temperature
Degree reach 1100 DEG C～1300 DEG C, continue with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, work as diamond seed
50 DEG C～150 DEG C of rapid drawdown in surface temperature, and diamond seed brightness deterioration, again becomes redness again, welded in place completes；
4., with speed as 1mbar/s～3mbar/s reduce air pressure, make air pressure be down to 5mbar～10mbar, power is down to
1680W～1750W, temperature is reduced to room temperature；
5., to nacelle evacuation, vacuum in nacelle is made to reach 2.0 × 10-6Mbar～8.0 × 10-6mbar；
6., exit, after making nacelle internal gas pressure reach 1atm, open the cabin, obtain the sample being welded, that is, complete homoepitaxy life
The Seed crystal substrate original position method of attachment of long single-crystal diamond.
Fig. 3 is the graph of a relation of surface temperature of the present invention-cabin internal gas pressure specification.
Metal molybdenum filament described in present embodiment step 3 is the special metal molybdenum filament of welding；Mesh using metal molybdenum filament
Be the thermal resistance increasing as far as possible between sample and instrument base, so that heat is concentrated at diamond seed, to be brought rapidly up reaching
Fusing point to native gold.
Step 4 3. in, by color and the brightness of diamond seed in observation window astrodome, when with speed being
When 0.5mbar/s～2mbar/s raises nacelle air pressure, the power of microwave plasma enhanced chemical vapor deposition instrument and Buddha's warrior attendant
Carpolite crystalline substance surface temperature also increases, and when nacelle air pressure rises to 60mbar～80mbar, power rises to 2200W～2600W, gold
Hard rock seed crystal face temperature rises to 800 DEG C～1000 DEG C, diamond seed color by secretly reddening, then when nacelle air pressure is increased to
90mbar～120mbar, diamond seed surface temperature reaches 1100 DEG C～1300 DEG C, and power is 2800W～3700W, Buddha's warrior attendant
Carpolite trichite goes out dazzling yellow light, continues to raise nacelle air pressure and power, have dropped 50 to diamond seed surface temperature
DEG C～150 DEG C, diamond seed brightness deterioration simultaneously, again become redness again, welded in place completes.
Present embodiment step 4 6. in open the cabin, take out sample and simultaneously check welding whether success.If seed crystal is served as a contrast with metal molybdenum
Form firm connection between bottom it was demonstrated that welding successfully, otherwise welded unsuccessfully, needed to re-start welding.
The beneficial effect of present embodiment is：1st, present embodiment passes through the method connecting in situ in cabin, makes diamond-like
Form strong bonded it is therefore prevented that blowing seed crystal in evacuation with when being passed through gas because air-flow is excessive between product and metal molybdenum substrate
The problem of dynamic off-target position is it is ensured that diamond seed all-the-time stable in growth course is in optimal temperature field and waits
It is ensured that the stablizing of growth technique under plasma levels.
2nd, original position interconnection technique eliminates and for sample to put into the step that vacuum brazing furnace is attached, and greatly simplifies behaviour
Make, saved time and cost.Operate under the hydrogen plasma atmosphere in MWCVD instrument room body simultaneously, effectively prevent height
The graphited problem on the lower diamond seed surface of temperature, makes seed crystal face be grown with best in quality.
3rd, the original position connection procedure in MWCVD instrument can carry out monitor in real time by the watch window of instrument, and can
Carry out the suitable adjustment of technological parameter according to different situations, it is to avoid because work cannot be observed when being operated in vacuum brazing furnace
Skill process and lead to the problem of connection failure.
4th, because the fabulous ductility of native gold and heat conductivity are it is ensured that form good between diamond print and metal molybdenum substrate
Good thermal contact conductance, it is therefore prevented that the heat on diamond sample surface is concentrated, greatly reduces surface temperature too high and stone occurs
The possibility of inkization, also makes diamond sample be under optimal growthing process parameter, growth result is more preferable simultaneously.
Specific embodiment two：Present embodiment from unlike specific embodiment one：By Buddha's warrior attendant carpolite in step one
Brilliant and metal molybdenum substrate disk is carried out, and specifically carries out according to the following steps：In the bar for 100W～400W for the ultrasonic power
Under part, diamond seed and metal molybdenum substrate disk are sequentially placed into cleaning 15min～30min in acetone, clear in deionized water
Wash 15min～30min, in dehydrated alcohol, clean 15min～30min, the diamond seed after being cleaned and the gold after cleaning
Belong to molybdenum substrate disk.Other identical with specific embodiment one.
Specific embodiment three：Unlike one of present embodiment and specific embodiment one or two：Institute in step 2
The smooth native gold purity stated is 24K.Other identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Select in step 2
Select the smooth native gold that thickness is 100 μm.Other identical with specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Institute in step 3
The metal molybdenum filament length stated is 1cm, a diameter of 1mm.Other identical with specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Step 4 is 1. right
Nacelle carries out evacuation, makes nacelle vacuum reach 3.0 × 10-6mbar.Other identical with specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Step 4 2. in
Set hydrogen flowing quantity as 200sccm, nacelle air pressure is 10mbar.Other identical with specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Step 4 3. with
Speed raises nacelle air pressure for 0.5mbar/s, and real-time monitoring diamond seed surface temperature, with the rising of nacelle air pressure, gold
Hard rock seed crystal face temperature raises, when nacelle air pressure is increased to 120mbar, now microwave plasma Assisted Chemical Vapor
The power of deposition apparatus is 3200W, and diamond seed surface temperature reaches 1300 DEG C, continues to raise with speed for 0.5mbar/s
Nacelle air pressure, when 100 DEG C of rapid drawdown in diamond seed surface temperature, and diamond seed brightness deterioration, again become again red
Color, welded in place completes.Other identical with specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Step 4 4. with
Speed is that 1mbar/s～3mbar/s reduces air pressure, makes air pressure be down to 8mbar, power is down to 1720W, temperature is reduced to room temperature.
Other identical with specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Step 4 is 5. right
Nacelle evacuation, makes vacuum in nacelle reach 3.0 × 10-6mbar.Other identical with specific embodiment one to nine.
Verify beneficial effects of the present invention using following examples：
Embodiment one：
A kind of Seed crystal substrate original position method of attachment of the isoepitaxial growth single-crystal diamond described in the present embodiment, specifically
Follow the steps below：
First, clean：Diamond seed and metal molybdenum substrate disk are carried out, the diamond seed after being cleaned and
Metal molybdenum substrate disk after cleaning；
2nd, select native gold：The smooth native gold selecting thickness to be 100 μm, smooth native gold is cut into longer than diamond seed
The square piece of wide all big 0.5mm, obtains welding medium；
Described smooth native gold purity is 24K；
3rd, place sample：
Four metal molybdenum filaments are put into " well " font, obtains metal molybdenum filament base, metal molybdenum filament base is positioned over micro-
On ripple plasma auxiliary chemical vapor deposition instrument trays, then by the metal molybdenum substrate disk after cleaning, welding medium
And the diamond seed after cleaning is sequentially placed on metal molybdenum filament base, makes the diamond seed surface level after cleaning and be in
Metal molybdenum filament base center；
Described metal molybdenum filament length is 1cm, a diameter of 1mm；
4th, connect in situ：
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, evacuation is carried out to nacelle, makes nacelle true
Reciprocal of duty cycle reaches 3.0 × 10-6mbar；
2., opening program, sets hydrogen flowing quantity as 200sccm, and nacelle air pressure is 10mbar, starts microwave generator, swashs
Plasma alive；
3., nacelle air pressure is raised for 0.5mbar/s with speed, real-time monitoring diamond seed surface temperature, with nacelle
The rising of air pressure, diamond seed surface temperature raises, when nacelle air pressure is increased to 120mbar, now microwave plasma
The power of body assistant chemical vapor deposition instrument is 3200W, and diamond seed surface temperature reaches 1300 DEG C, and continuation with speed is
0.5mbar/s raises nacelle air pressure, and when 100 DEG C of rapid drawdown in diamond seed surface temperature, and diamond seed brightness subtracts
Weak, again become redness again, welded in place completes；
4., air pressure is reduced for 2mbar/s with speed, make air pressure be down to 8mbar, power is down to 1720W, temperature is reduced to room
Temperature；
5., to nacelle evacuation, vacuum in nacelle is made to reach 3.0 × 10-6mbar；
6., exit, after making nacelle internal gas pressure reach 1atm, open the cabin, obtain the sample being welded, that is, complete homoepitaxy life
The Seed crystal substrate original position method of attachment of long single-crystal diamond.
Diamond film is carried out to the sample being welded manufactured in the present embodiment, specifically carries out according to the following steps：
1., take out metal molybdenum filament base, the sample being welded is put into microwave plasma enhanced chemical vapor deposition instrument
In device nacelle, close hatch door；
2., evacuation is carried out to nacelle, reach 3.0 × 10 to nacelle vacuum-6mbar；
3., opening program, sets hydrogen flowing quantity as 200sccm, and nacelle air pressure is 10mbar, starts microwave generator, swashs
Plasma alive；
4., raise nacelle air pressure and power, reach 900 DEG C to the specimen surface temperature being welded, be then 900 in temperature
DEG C and hydrogen plasma atmosphere in, by the sample being welded clean 15min, the sample after being cleaned；
5., be passed through oxygen, set oxygen flow as 5sccm, then temperature be 900 DEG C and hydrogen-oxygen hybrid plasma gas
Under atmosphere, by the sample etching 10min after cleaning, the sample after being etched；
6., close oxygen valve, stop being passed through oxygen；
7., open methane gas valve, be passed through methane gas, adjusting methane gas gas flow is 184sccm and hydrogen
Gas flow is 16sccm, and adjusting air pressure is 260mbar so that the specimen surface temperature after etching reaches 940 DEG C, grows 40h,
Completed the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond；
In step one, diamond seed and metal molybdenum substrate disk are carried out, specifically carry out according to the following steps：
Under conditions of ultrasonic power is for 200W, diamond seed and metal molybdenum substrate disk are sequentially placed into cleaning 15min in acetone,
Clean 10min in deionized water, in dehydrated alcohol, clean 20min, the diamond seed after being cleaned and the metal after cleaning
Molybdenum substrate disk.
Fig. 4 is the growth morphology figure that the Seed crystal substrate not carrying out connecting in situ grows single-crystal diamond；Fig. 5 is embodiment one
Connect the growth morphology figure of the Seed crystal substrate isoepitaxial growth single-crystal diamond of preparation in situ；As seen from the figure, embodiment one is former
Position connects the Seed crystal substrate isoepitaxial growth single-crystal diamond surfacing of preparation, and pattern is good；And do not carry out connecting in situ
Seed crystal substrate growth single-crystal diamond rough surface, and there are a lot of coarse grains and can improve it was demonstrated that implementing to connect in situ
The quality of epitaxial growth single-crystal diamond.
Using Renishaw Raman spectroscopy instrument, the present embodiment is connected in situ with the isoepitaxial growth single crystal diamond of preparation
The Seed crystal substrate of stone carries out Raman spectrum test, table 1 Raman spectrum data.As seen from table, preparation is connected in situ to the present embodiment
Seed crystal substrate isoepitaxial growth single-crystal diamond grow drawing of single-crystal diamond than the Seed crystal substrate not carrying out connecting in situ
Graceful spectral peak peak position is closer to the 1332cm of perfect diamond-1And the halfwidth at peak narrower can improve it was demonstrated that implementing to connect in situ
The quality of epitaxial growth single-crystal diamond.
Table 1 Raman spectrum data
Claims (10)
1. a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond is it is characterised in that a kind of homoepitaxy
The Seed crystal substrate original position method of attachment of growth single-crystal diamond follows the steps below：
First, clean：Diamond seed and metal molybdenum substrate disk are carried out, the diamond seed after being cleaned and cleaning
Metal molybdenum substrate disk afterwards；
2nd, select native gold：The smooth native gold selecting thickness to be 20 μm～100 μm, smooth native gold is cut into and compares diamond seed
The square piece of all big 0.5mm～1.5mm of length and width, obtains welding medium；
Described smooth native gold purity is 18K～24K；
3rd, place sample：
Four metal molybdenum filaments are put into " well " font, obtains metal molybdenum filament base, metal molybdenum filament base is positioned over microwave etc.
In gas ions assistant chemical vapor deposition instrument trays, then by the metal molybdenum substrate disk after cleaning, welding medium and cleaning
Diamond seed afterwards is sequentially placed on metal molybdenum filament base, makes the diamond seed surface level after cleaning and is in metal molybdenum
Silk base center；
Described metal molybdenum filament length is 5mm～20mm, a diameter of 0.3mm～2mm；
4th, connect in situ：
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, evacuation is carried out to nacelle, makes nacelle vacuum
Reach 3.0 × 10-6Mbar～5.0 × 10-6mbar；
2., opening program, sets hydrogen flowing quantity as 100sccm～200sccm, and nacelle air pressure is 10mbar～30mbar, starts
Microwave generator, activates plasma；
3., with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, real-time monitoring diamond seed surface temperature, with
The rising of nacelle air pressure, diamond seed surface temperature raises, when nacelle air pressure is increased to 90mbar～120mbar, this
When microwave plasma enhanced chemical vapor deposition instrument power be 2800W～3700W, diamond seed surface temperature reaches
1100 DEG C～1300 DEG C, continue with speed as 0.5mbar/s～2mbar/s raise nacelle air pressure, when diamond seed surface temperature
50 DEG C～150 DEG C of rapid drawdown in degree, and diamond seed brightness deterioration, again becomes redness again, welded in place completes；
4., with speed as 1mbar/s～3mbar/s reduce air pressure, make air pressure be down to 5mbar～10mbar, power is down to 1680W
～1750W, monitoring diamond seed surface temperature is reduced to room temperature；
5., to nacelle evacuation, vacuum in nacelle is made to reach 2.0 × 10-6Mbar～8.0 × 10-6mbar；
6., exit, after making nacelle internal gas pressure reach 1atm, open the cabin, obtain the sample being welded, that is, complete isoepitaxial growth list
The Seed crystal substrate original position method of attachment of diamond.
2. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by step one being carried out diamond seed and metal molybdenum substrate disk, specifically carry out according to the following steps：
Under conditions of ultrasonic power is for 100W～400W, diamond seed and metal molybdenum substrate disk are sequentially placed into cleaning in acetone
15min～30min, cleans 15min～30min in deionized water, cleans 15min～30min, after being cleaned in dehydrated alcohol
Diamond seed and cleaning after metal molybdenum substrate disk.
3. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by that the smooth native gold purity described in step 2 is 24K.
4. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by step 2, selecting the smooth native gold that thickness is 100 μm.
5. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by that the metal molybdenum filament length described in step 3 is 1cm, a diameter of 1mm.
6. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by that 1. step 4 carries out evacuation to nacelle, make nacelle vacuum reach 3.0 × 10-6mbar.
7. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
Be characterised by step 4 2. the middle hydrogen flowing quantity that sets as 200sccm, nacelle air pressure be 10mbar.
8. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by step 4 3. with speed for 0.5mbar/s rising nacelle air pressure, real-time monitoring diamond seed surface temperature, with
The rising of nacelle air pressure, diamond seed surface temperature raises, when nacelle air pressure is increased to 120mbar, now microwave etc.
The power of gas ions assistant chemical vapor deposition instrument is 3200W, and diamond seed surface temperature reaches 1300 DEG C, continues with speed
Spend and raise nacelle air pressure for 0.5mbar/s, when 100 DEG C of rapid drawdown in diamond seed surface temperature, and diamond seed is bright
Degree weakens, and again becomes redness again, and welded in place completes.
9. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
Be characterised by step 4 4. with speed as 1mbar/s～3mbar/s reduce air pressure, make air pressure be down to 8mbar, power is down to
1720W, temperature is reduced to room temperature.
10. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, its
It is characterised by that step 4,5. to nacelle evacuation, makes vacuum in nacelle reach 3.0 × 10-6mbar.
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| CN105525344B (en) * | 2015-12-23 | 2018-05-01 | 中国科学院深圳先进技术研究院 | Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy |
| CN107419329B (en) * | 2017-05-22 | 2019-08-27 | 北京科技大学 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
| CN107675249B (en) * | 2017-09-08 | 2020-07-07 | 西安电子科技大学 | Diameter expanding growth method of single crystal diamond |
| CN108360064B (en) * | 2018-02-26 | 2020-12-29 | 湖北碳六科技有限公司 | Method for improving stability of single crystal diamond prepared by MPCVD |
| CN109537048A (en) * | 2018-11-27 | 2019-03-29 | 西安碳星半导体科技有限公司 | CVD single-crystal diamond eliminates edge polycrystalline method |
| CN110453279A (en) * | 2019-07-24 | 2019-11-15 | 中国电子科技集团公司第十一研究所 | Molecular beam epitaxy substrate adhering method |
| CN112442735A (en) * | 2019-08-30 | 2021-03-05 | 西安交通大学 | Method for growing large-area single crystal diamond by adsorption splicing |
| CN111584382B (en) * | 2020-04-27 | 2023-02-24 | 哈尔滨工业大学 | Method for in-situ characterization of heterogeneous interface state by using diamond NV color center |
| CN112030228B (en) * | 2020-09-11 | 2021-05-18 | 哈尔滨工业大学 | Bridging temperature control method for co-growth of multiple MPCVD single crystal diamonds |
| CN112111786A (en) * | 2020-09-15 | 2020-12-22 | 郑州大学 | Preparation method of optical-grade diamond wafer |
| CN114016130B (en) * | 2021-11-10 | 2022-09-13 | 哈尔滨工业大学 | Method for welding single crystal diamond seed crystal and sample holder |
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