CN104878447A - Seed crystal-substrate in-situ connection method for homoepitaxial-growth monocrystalline diamond - Google Patents
Seed crystal-substrate in-situ connection method for homoepitaxial-growth monocrystalline diamond Download PDFInfo
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- CN104878447A CN104878447A CN201510304886.3A CN201510304886A CN104878447A CN 104878447 A CN104878447 A CN 104878447A CN 201510304886 A CN201510304886 A CN 201510304886A CN 104878447 A CN104878447 A CN 104878447A
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Abstract
A seed crystal-substrate in-situ connection method for a homoepitaxial-growth monocrystalline diamond, the invention relates to the seed crystal-substrate in-situ connection method for the homoepitaxial-growth monocrystalline diamond. The seed crystal-substrate in-situ connection method is used for solving the problems of the existing MWCVD growth system that seed crystals are prone to being deviated from the best position due to airflow blowing, the heat conduction between the seed crystals and a metal molybdenum substrate is difficult, and due to vacuum brazing, the surface quality of the seed crystals is lowered and observation is difficult. The method comprises the steps: (1) cleaning; (2) selecting gold foil; (3) placing samples; (4) carrying out in-situ connection; (5) carrying out diamond growth, thereby completing the seed crystal-substrate in-situ connection method for the homoepitaxial-growth monocrystalline diamond. The invention is applied to the seed crystal-substrate in-situ connection method for the homoepitaxial-growth monocrystalline 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 accurate single-crystal diamond because its high hardness, the highest thermal conductivity, extremely wide electromagnetism are through frequency range, excellent Radiation hardness and corrosion resistance nature, based on the high-tech areas such as precision sizing, high frequency communications, space flight aerospace, sophisticated technology day by day become, crucial even unique material solution.Traditional artificial single crystal's diamond adopts High Temperature High Pressure (HPHT) method, the diamond that the method is prepared is impure more, defect concentration is higher, quality is relatively poor, and size is less, differs greatly compared with the demand of related application, cause the HPHT diamond scope of application narrower, be in downstream in the industry, profit is low, and competitive power is not strong.
Compared to HPHT method, microwave plasma enhanced chemical vapor deposition (MWCVD) method be generally acknowledge at present prepare one of adamantine best approach of large size single crystal, single-crystal diamond prepared by the method has that impurity concentration is low, low through wide waveband, defect concentration, size is comparatively large and the advantage such as growth velocity is controlled, is considered to promise to be the following method producing man-made diamond in enormous quantities most.
During the method epitaxy single-crystal diamond, diamond seed directly contacts with axiolitic plasma body, the concentration of the temperature and plasma body that therefore control seed crystal face is very crucial factor: the too high meeting of temperature causes diamond surface generation greying, and the too low meeting of temperature causes declining to a great extent of seeded growth quality; Meanwhile, the concentration of plasma body and homogeneity also have very large impact to the growth quality of seed crystal and speed.Therefore seed crystal needs to place in place, and under being in suitable temperature field and uniform plasma density, the high quality of guarantee seed crystal grows fast.
In reaction process, diamond seed is positioned over metal molybdenum substrate usually, and metal molybdenum substrate is positioned on the base of MWCVD instrument.Because the quality of diamond seed itself is very little, only have tens milligrams, when instrument vacuumizes and pass into reactant gases, seed crystal is very easily blown by air-flow, cause off-target position, seed crystal position, cause the significantly change of temperature and plasma density, have a strong impact on the growth quality of seed crystal.So in traditional monocrystalline growing process, vacuum brazing furnace is usually adopted diamond seed and substrate to be linked together, to ensure the fixing of seed crystal.But because the vacuum tightness of vacuum brazing furnace is lower, in high temperature brazing process, remaining air very easily makes diamond seed surface greying occur, the growth quality of extreme influence single crystalline layer.And brazing process carries out completely in stove, cannot Real Time Observation be carried out, only after soldering terminates to take out sample, just can learn welding result.
In addition, because the surface of seed crystal and metal molybdenum cannot ensure that degree is smooth absolutely, makes thermal contact conductance face therebetween very little, and have gas blanket to exist, cause forming very large thermal resistance between seed crystal and metal molybdenum, temperature is too high because heat concentrates to make seed crystal face, and growth quality is subject to extreme influence.So be in stable when growing for controlling diamond seed and under the processing parameter of optimum, realize the quick growth of large size high-quality single-crystal diamond, must find can fixed diamond seed crystal, and strengthens the method for heat conduction between seed crystal and substrate.
Summary of the invention
The present invention will solve seed crystal in existing MWCVD growing system and easily be blown off-target position by air-flow, and heat conduction difficulty between seed crystal and metal molybdenum substrate, use vacuum brazing to cause seed crystal face Quality Down and the problem of not easily observing, and a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond is provided.
A Seed crystal substrate original position method of attachment for isoepitaxial growth single-crystal diamond, specifically carry out according to following steps:
One, clean: diamond seed and metal molybdenum substrate disk are cleaned, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning;
Two, goldleaf is selected: selection thickness is the smooth goldleaf of 20 μm ~ 100 μm, smooth goldleaf is cut into the square piece of 0.5mm ~ 1.5mm all larger than diamond seed length and width, obtains welding medium;
Described smooth goldleaf purity is 18K ~ 24K;
Three, sample is placed:
Four metal molybdenum filaments are put into " well " font, obtain metal molybdenum filament base, metal molybdenum filament base is positioned in microwave plasma enhanced chemical vapor deposition instrument trays, then the diamond seed after the metal molybdenum substrate disk after cleaning, welding medium and cleaning is placed on metal molybdenum filament base successively, makes the diamond seed surface level after cleaning and be in metal molybdenum filament base center;
Described metal molybdenum filament length is 5mm ~ 20mm, and diameter is 0.3mm ~ 2mm;
Four, original position connects:
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, cabin body is vacuumized, makes cabin body vacuum tightness reach 3.0 × 10
-6mbar ~ 5.0 × 10
-6mbar;
2., opening program, setting hydrogen flowing quantity is 100sccm ~ 200sccm, and cabin body air pressure is 10mbar ~ 30mbar, start microwave generator, activate plasma;
3., be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure with speed, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 90mbar ~ 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 2800W ~ 3700W, diamond seed surface temperature reaches 1100 DEG C ~ 1300 DEG C, continue with speed to be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure, when rapid drawdown 50 DEG C ~ 150 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again redness is become again, welded in place completes,
4., with speed be that 1mbar/s ~ 3mbar/s reduces air pressure, make air pressure be down to 5mbar ~ 10mbar, power is down to 1680W ~ 1750W, and temperature is reduced to room temperature;
5., to cabin body vacuumize, make vacuum tightness in the body of cabin reach 2.0 × 10
-6mbar ~ 8.0 × 10
-6mbar;
6., exit, after making cabin body internal gas pressure arrive 1atm, open the cabin, obtain the sample welded, namely complete the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
The invention has the beneficial effects as follows: 1, the present invention is by the method for original position connection in cabin, make to form mortise between diamond sample and metal molybdenum substrate, prevent the problem of because air-flow is excessive, seed crystal being blown off-target position when vacuumizing and pass into gas, under ensure that diamond seed all-the-time stable in process of growth is in best temperature field and plasma density, ensure that the stable of growth technique.
2, original position interconnection technique eliminates step sample put into vacuum brazing furnace and carry out connecting, and greatly simplifies the operation, has saved time and cost.Operate under hydrogen plasma atmosphere simultaneously in MWCVD instrument compartment body, effectively prevent the graphited problem on diamond seed surface under high temperature, seed crystal face is grown with best in quality.
3, the original position connection procedure in MWCVD instrument can be monitored in real time by the view port of instrument, and the suitable adjustment of processing parameter can be carried out according to different situations, avoid the problem causing connection failure when operating in vacuum brazing furnace because cannot technological process be observed.
4, due to the fabulous ductility of goldleaf and thermal conductivity, ensure that and form good thermal contact conductance between diamond print and metal molybdenum substrate, the heat on diamond sample surface is prevented to concentrate, greatly reduce surface temperature too high and occur graphited may, also, under making diamond sample be in best growthing process parameter, growth result is better simultaneously.
The present invention is used for a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
Accompanying drawing explanation
Fig. 1 is welding metal molybdenum filament of the present invention and groined type disposing way schematic diagram;
Fig. 2 is the lamination sequence chart of metal molybdenum substrate disk after diamond seed after the present invention cleans, welding medium, cleaning and metal molybdenum filament base; 1 is the diamond seed after cleaning; 2 is welding medium; 3 is the metal molybdenum substrate disk after cleaning; 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 adamantine growth morphology figure of Seed crystal substrate growing single-crystal not carrying out original position connection;
Fig. 5 is the growth morphology figure that embodiment one original position connects the Seed crystal substrate isoepitaxial growth single-crystal diamond of preparation.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: composition graphs 1 and Fig. 2 illustrate present embodiment, the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond described in present embodiment, specifically carry out according to following steps:
One, clean: diamond seed and metal molybdenum substrate disk are cleaned, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning;
Two, goldleaf is selected: selection thickness is the smooth goldleaf of 20 μm ~ 100 μm, smooth goldleaf is cut into the square piece of 0.5mm ~ 1.5mm all larger than diamond seed length and width, obtains welding medium;
Described smooth goldleaf purity is 18K ~ 24K;
Three, sample is placed:
Four metal molybdenum filaments are put into " well " font, obtain metal molybdenum filament base, metal molybdenum filament base is positioned in microwave plasma enhanced chemical vapor deposition instrument trays, then the diamond seed after the metal molybdenum substrate disk after cleaning, welding medium and cleaning is placed on metal molybdenum filament base successively, makes the diamond seed surface level after cleaning and be in metal molybdenum filament base center;
Described metal molybdenum filament length is 5mm ~ 20mm, and diameter is 0.3mm ~ 2mm;
Four, original position connects:
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, cabin body is vacuumized, makes cabin body vacuum tightness reach 3.0 × 10
-6mbar ~ 5.0 × 10
-6mbar;
2., opening program, setting hydrogen flowing quantity is 100sccm ~ 200sccm, and cabin body air pressure is 10mbar ~ 30mbar, start microwave generator, activate plasma;
3., be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure with speed, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 90mbar ~ 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 2800W ~ 3700W, diamond seed surface temperature reaches 1100 DEG C ~ 1300 DEG C, continue with speed to be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure, when rapid drawdown 50 DEG C ~ 150 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again redness is become again, welded in place completes,
4., with speed be that 1mbar/s ~ 3mbar/s reduces air pressure, make air pressure be down to 5mbar ~ 10mbar, power is down to 1680W ~ 1750W, and temperature is reduced to room temperature;
5., to cabin body vacuumize, make vacuum tightness in the body of cabin reach 2.0 × 10
-6mbar ~ 8.0 × 10
-6mbar;
6., exit, after making cabin body internal gas pressure arrive 1atm, open the cabin, obtain the sample welded, namely complete the Seed crystal substrate original position method of attachment of isoepitaxial growth 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 weld special metal molybdenum filament; The object adopting metal molybdenum filament is the thermal resistance increased as far as possible between sample and instrument base, makes heat concentrate on diamond seed place, so that rapid temperature increases reaches the fusing point of goldleaf.
Step 4 3. in, by color and the brightness of diamond seed in viewing window observation tank, when taking speed as 0.5mbar/s ~ 2mbar/s rising cabin body air pressure, power and the diamond seed surface temperature of microwave plasma enhanced chemical vapor deposition instrument also increase, when cabin, body air pressure rises to 60mbar ~ 80mbar, power rises to 2200W ~ 2600W, diamond seed surface temperature rises to 800 DEG C ~ 1000 DEG C, diamond seed color is by secretly reddening, then when cabin body air pressure is increased to 90mbar ~ 120mbar, diamond seed surface temperature reaches 1100 DEG C ~ 1300 DEG C, power is 2800W ~ 3700W, diamond seed sends dazzling yellow light, continue to raise cabin body air pressure and power, have dropped 50 DEG C ~ 150 DEG C to diamond seed surface temperature, diamond seed brightness deterioration simultaneously, again redness is become again, welded in place completes.
Present embodiment step 4 6. in open the cabin, take out sample and inspection welding whether success.If formed firm connection between seed crystal with metal molybdenum substrate, prove to weld successfully, otherwise welded unsuccessfully, needed to re-start welding.
The beneficial effect of present embodiment is: 1, present embodiment is by the method for original position connection in cabin, make to form mortise between diamond sample and metal molybdenum substrate, prevent the problem of because air-flow is excessive, seed crystal being blown off-target position when vacuumizing and pass into gas, under ensure that diamond seed all-the-time stable in process of growth is in best temperature field and plasma density, ensure that the stable of growth technique.
2, original position interconnection technique eliminates step sample put into vacuum brazing furnace and carry out connecting, and greatly simplifies the operation, has saved time and cost.Operate under hydrogen plasma atmosphere simultaneously in MWCVD instrument compartment body, effectively prevent the graphited problem on diamond seed surface under high temperature, seed crystal face is grown with best in quality.
3, the original position connection procedure in MWCVD instrument can be monitored in real time by the view port of instrument, and the suitable adjustment of processing parameter can be carried out according to different situations, avoid the problem causing connection failure when operating in vacuum brazing furnace because cannot technological process be observed.
4, due to the fabulous ductility of goldleaf and thermal conductivity, ensure that and form good thermal contact conductance between diamond print and metal molybdenum substrate, the heat on diamond sample surface is prevented to concentrate, greatly reduce surface temperature too high and occur graphited may, also, under making diamond sample be in best growthing process parameter, growth result is better simultaneously.
Embodiment two: present embodiment and embodiment one unlike: in step one, diamond seed and metal molybdenum substrate disk are cleaned, specifically carry out according to the following steps: be under the condition of 100W ~ 400W at ultrasonic power, diamond seed and metal molybdenum substrate disk are placed in acetone successively and clean 15min ~ 30min, 15min ~ 30min is cleaned in deionized water, clean 15min ~ 30min in dehydrated alcohol, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two unlike: the smooth goldleaf purity described in step 2 is 24K.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: select thickness to be the smooth goldleaf of 100 μm in step 2.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the metal molybdenum filament length described in step 3 is 1cm, and diameter is 1mm.Other is identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: 1. step 4 vacuumizes cabin body, makes cabin body vacuum tightness reach 3.0 × 10
-6mbar.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: step 4 2. in setting hydrogen flowing quantity be 200sccm, cabin body air pressure is 10mbar.Other is identical with embodiment one to six.
Embodiment eight: 3. one of present embodiment and embodiment one to seven are that 0.5mbar/s raises cabin body air pressure with speed unlike: step 4, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 3200W, diamond seed surface temperature reaches 1300 DEG C, continue with speed to be that 0.5mbar/s raises cabin body air pressure, when rapid drawdown 100 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again redness is become again, welded in place completes.Other is identical with embodiment one to seven.
Embodiment nine: 4. one of present embodiment and embodiment one to eight are that 1mbar/s ~ 3mbar/s reduces air pressure with speed unlike: step 4, and make air pressure be down to 8mbar, power is down to 1720W, and temperature is reduced to room temperature.Other is identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: 5. step 4 vacuumizes cabin body, makes vacuum tightness in the body of cabin reach 3.0 × 10
-6mbar.Other is identical with embodiment one to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond described in the present embodiment, specifically carry out according to following steps:
One, clean: diamond seed and metal molybdenum substrate disk are cleaned, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning;
Two, goldleaf is selected: selection thickness is the smooth goldleaf of 100 μm, smooth goldleaf is cut into the square piece of 0.5mm all larger than diamond seed length and width, obtains welding medium;
Described smooth goldleaf purity is 24K;
Three, sample is placed:
Four metal molybdenum filaments are put into " well " font, obtain metal molybdenum filament base, metal molybdenum filament base is positioned on microwave plasma enhanced chemical vapor deposition instrument trays, then the diamond seed after the metal molybdenum substrate disk after cleaning, welding medium and cleaning is placed on metal molybdenum filament base successively, makes the diamond seed surface level after cleaning and be in metal molybdenum filament base center;
Described metal molybdenum filament length is 1cm, and diameter is 1mm;
Four, original position connects:
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, cabin body is vacuumized, makes cabin body vacuum tightness reach 3.0 × 10
-6mbar;
2., opening program, setting hydrogen flowing quantity is 200sccm, and cabin body air pressure is 10mbar, start microwave generator, activate plasma;
3. be, that 0.5mbar/s raises cabin body air pressure with speed, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 3200W, diamond seed surface temperature reaches 1300 DEG C, continue with speed to be that 0.5mbar/s raises cabin body air pressure, when rapid drawdown 100 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again become redness again, welded in place completes;
4., with speed be that 2mbar/s reduces air pressure, make air pressure be down to 8mbar, power is down to 1720W, and temperature is reduced to room temperature;
5., to cabin body vacuumize, make vacuum tightness in the body of cabin reach 3.0 × 10
-6mbar;
6., exit, after making cabin body internal gas pressure arrive 1atm, open the cabin, obtain the sample welded, namely complete the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
The sample that the welding prepared the present embodiment is good carries out diamond film, specifically carries out according to the following steps:
1., take out metal molybdenum filament base, the sample welded is put into microwave plasma enhanced chemical vapor deposition instrument compartment body, close hatch door;
2., to cabin body vacuumize, reach 3.0 × 10 to cabin body vacuum tightness
-6mbar;
3., opening program, setting hydrogen flowing quantity is 200sccm, and cabin body air pressure is 10mbar, start microwave generator, activate plasma;
4., raise cabin body air pressure and power, reach 900 DEG C to the specimen surface temperature of weld, then in temperature is 900 DEG C and hydrogen plasma atmosphere, the sample welded is cleaned 15min, obtains the sample after cleaning;
5., pass into oxygen, setting oxygen flow is 5sccm, then under temperature is 900 DEG C and hydrogen-oxygen hybrid plasma atmosphere, by the sample etching 10min after cleaning, obtains the sample after etching;
6., close oxygen valve, stop passing into oxygen;
7. methane gas valve, is opened, pass into methane gas, regulating methane gas gas flow to be 184sccm and hydrogen gas flow is 16sccm, adjustable pressure is 260mbar, the specimen surface temperature after etching is made to reach 940 DEG C, growth 40h, is namely 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 cleaned, specifically carry out according to the following steps: be under the condition of 200W at ultrasonic power, diamond seed and metal molybdenum substrate disk are placed in acetone successively and clean 15min, 10min is cleaned in deionized water, clean 20min in dehydrated alcohol, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning.
Fig. 4 is the adamantine growth morphology figure of Seed crystal substrate growing single-crystal not carrying out original position connection; Fig. 5 is the growth morphology figure that embodiment one original position connects the Seed crystal substrate isoepitaxial growth single-crystal diamond of preparation; As seen from the figure, embodiment one original position connects the Seed crystal substrate isoepitaxial growth single-crystal diamond surfacing of preparation, and pattern is good; And the Seed crystal substrate growing single-crystal diamond surface not carrying out original position connection is coarse, and there is a lot of coarse grain, prove that implementing original position connects the quality that can improve epitaxy single-crystal diamond.
Utilize Renishaw Raman spectroscopy instrument, Seed crystal substrate the present embodiment original position being connected to the isoepitaxial growth single-crystal diamond of preparation carries out Raman spectrum test, table 1 Raman spectrum data.As seen from table, Seed crystal substrate isoepitaxial growth single-crystal diamond the present embodiment original position being connected to preparation than the Seed crystal substrate growing single-crystal adamantine raman spectra peak position of not carrying out original position connection closer to the adamantine 1332cm of perfection
-1and the halfwidth at peak is narrower, prove that implementing original position connects the quality that can improve epitaxy single-crystal diamond.
Table 1 Raman spectrum data
Claims (10)
1. a Seed crystal substrate original position method of attachment for isoepitaxial growth single-crystal diamond, is characterized in that a kind of Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond is carried out according to following steps:
One, clean: diamond seed and metal molybdenum substrate disk are cleaned, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning;
Two, goldleaf is selected: selection thickness is the smooth goldleaf of 20 μm ~ 100 μm, smooth goldleaf is cut into the square piece of 0.5mm ~ 1.5mm all larger than diamond seed length and width, obtains welding medium;
Described smooth goldleaf purity is 18K ~ 24K;
Three, sample is placed:
Four metal molybdenum filaments are put into " well " font, obtain metal molybdenum filament base, metal molybdenum filament base is positioned in microwave plasma enhanced chemical vapor deposition instrument trays, then the diamond seed after the metal molybdenum substrate disk after cleaning, welding medium and cleaning is placed on metal molybdenum filament base successively, makes the diamond seed surface level after cleaning and be in metal molybdenum filament base center;
Described metal molybdenum filament length is 5mm ~ 20mm, and diameter is 0.3mm ~ 2mm;
Four, original position connects:
1., close microwave plasma enhanced chemical vapor deposition instrument hatch door, cabin body is vacuumized, makes cabin body vacuum tightness reach 3.0 × 10
-6mbar ~ 5.0 × 10
-6mbar;
2., opening program, setting hydrogen flowing quantity is 100sccm ~ 200sccm, and cabin body air pressure is 10mbar ~ 30mbar, start microwave generator, activate plasma;
3., be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure with speed, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 90mbar ~ 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 2800W ~ 3700W, diamond seed surface temperature reaches 1100 DEG C ~ 1300 DEG C, continue with speed to be that 0.5mbar/s ~ 2mbar/s raises cabin body air pressure, when rapid drawdown 50 DEG C ~ 150 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again redness is become again, welded in place completes,
4., with speed be that 1mbar/s ~ 3mbar/s reduces air pressure, make air pressure be down to 5mbar ~ 10mbar, power is down to 1680W ~ 1750W, and monitoring diamond seed surface temperature is reduced to room temperature;
5., to cabin body vacuumize, make vacuum tightness in the body of cabin reach 2.0 × 10
-6mbar ~ 8.0 × 10
-6mbar;
6., exit, after making cabin body internal gas pressure arrive 1atm, open the cabin, obtain the sample welded, namely complete the Seed crystal substrate original position method of attachment of isoepitaxial growth single-crystal diamond.
2. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, it is characterized in that in step one, diamond seed and metal molybdenum substrate disk being cleaned, specifically carry out according to the following steps: be under the condition of 100W ~ 400W at ultrasonic power, diamond seed and metal molybdenum substrate disk are placed in acetone successively and clean 15min ~ 30min, 15min ~ 30min is cleaned in deionized water, clean 15min ~ 30min in dehydrated alcohol, obtain the metal molybdenum substrate disk after the diamond seed after cleaning and cleaning.
3. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, is characterized in that the smooth goldleaf 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, is characterized in that selecting in step 2 thickness to be the smooth goldleaf of 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, it is characterized in that the metal molybdenum filament length described in step 3 is 1cm, diameter is 1mm.
6. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, is characterized in that 1. step 4 vacuumizes cabin body, makes cabin body vacuum tightness 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, it is characterized in that setting hydrogen flowing quantity during step 4 is 2. 200sccm, cabin body air pressure is 10mbar.
8. the Seed crystal substrate original position method of attachment of a kind of isoepitaxial growth single-crystal diamond according to claim 1, it is characterized in that 3. step 4 is that 0.5mbar/s raises cabin body air pressure with speed, Real-Time Monitoring diamond seed surface temperature, along with the rising of cabin body air pressure, diamond seed surface temperature raises, when cabin body air pressure is increased to 120mbar, now the power of microwave plasma enhanced chemical vapor deposition instrument is 3200W, diamond seed surface temperature reaches 1300 DEG C, continue with speed to be that 0.5mbar/s raises cabin body air pressure, when rapid drawdown 100 DEG C appears in diamond seed surface temperature, and diamond seed brightness deterioration, again redness is become again, 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, it is characterized in that 4. step 4 is that 1mbar/s ~ 3mbar/s reduces air pressure with speed, make air pressure be down to 8mbar, power is down to 1720W, and 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, is characterized in that 5. step 4 vacuumizes cabin body, makes vacuum tightness in the body of cabin reach 3.0 × 10
-6mbar.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105525344A (en) * | 2015-12-23 | 2016-04-27 | 中国科学院深圳先进技术研究院 | Seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and application thereof |
| CN107419329A (en) * | 2017-05-22 | 2017-12-01 | 北京科技大学 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
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| CN108360064A (en) * | 2018-02-26 | 2018-08-03 | 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 |
| CN111584382A (en) * | 2020-04-27 | 2020-08-25 | 哈尔滨工业大学 | Method for in-situ characterization of heterogeneous interface state by using diamond NV color center |
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| CN112111786A (en) * | 2020-09-15 | 2020-12-22 | 郑州大学 | Preparation method of optical-grade diamond wafer |
| 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 |
| CN114016130A (en) * | 2021-11-10 | 2022-02-08 | 哈尔滨工业大学 | Method for welding single crystal diamond seed crystal and sample holder |
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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 |
| CN105525344A (en) * | 2015-12-23 | 2016-04-27 | 中国科学院深圳先进技术研究院 | Seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and application thereof |
| 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 |
| CN107419329A (en) * | 2017-05-22 | 2017-12-01 | 北京科技大学 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
| CN107675249A (en) * | 2017-09-08 | 2018-02-09 | 西安电子科技大学 | The expanding growing method of single-crystal diamond |
| CN107675249B (en) * | 2017-09-08 | 2020-07-07 | 西安电子科技大学 | Diameter expanding growth method of single crystal diamond |
| CN108360064A (en) * | 2018-02-26 | 2018-08-03 | 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 |
| CN111584382A (en) * | 2020-04-27 | 2020-08-25 | 哈尔滨工业大学 | Method for in-situ characterization of heterogeneous interface state by using diamond NV color center |
| 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 |
| CN112030228A (en) * | 2020-09-11 | 2020-12-04 | 哈尔滨工业大学 | Bridging temperature control method for co-growth of multiple MPCVD single crystal diamonds |
| 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 |
| CN114016130A (en) * | 2021-11-10 | 2022-02-08 | 哈尔滨工业大学 | Method for welding single crystal diamond seed crystal and sample holder |
| 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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