CN105525344B - Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy - Google Patents
Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy Download PDFInfo
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- CN105525344B CN105525344B CN201510974331.XA CN201510974331A CN105525344B CN 105525344 B CN105525344 B CN 105525344B CN 201510974331 A CN201510974331 A CN 201510974331A CN 105525344 B CN105525344 B CN 105525344B
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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
- 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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- 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
- C30B25/12—Substrate holders or susceptors
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
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Abstract
The present invention is suitable for Diamond Synthesizing Technology field, there is provided a kind of seed crystal tray, base station component and its application for diamond single crystal homoepitaxy.The seed crystal tray is placed on the water-cooled platform of microwave plasma CVD device, and the seed crystal tray center offers the perforation for placing seed crystal.The base station component for diamond single crystal homoepitaxy, including water-cooled platform and the seed crystal tray being arranged on the water-cooled platform, the seed crystal tray is the above-mentioned seed crystal tray for diamond single crystal homoepitaxy.
Description
Technical field
The invention belongs to Diamond Synthesizing Technology field, more particularly to a kind of seed crystal for diamond single crystal homoepitaxy
Pallet, base station component and its application.
Background technology
Diamond integrates numerous excellent properties, has high hardness, thermal conductivity, wide transmitted spectrum band, broadband
The advantages that gap and high electron hole mobility, can be widely applied to cutter, coating, optical window and acoustic sensor, partly lead
The field such as body and electronic device.At present, the demand of diamond is big, and natural diamond reserves are seldom, therefore, synthesize big ruler
Very little, high quality diamond single crystal just seems particularly urgent.Microwave plasma CVD (MPCVD) method is with no electricity
Pole pollution, equipment are stable, plasma density is concentrated and indiffusion, sample quality such as can effectively repeat at a variety of advantages, very suitable
Next life long high quality, the single-crystal diamond of high-purity are shared, is one of most promising method of current diamond synthesis.
In MPCVD methods, the design of seed crystal tray determines whether growth temperature, plasma distribution and carbon source distribution are uniform, in diamond
Key effect is played in growth course.
The seed crystal tray that tradition uses is made of metal molybdenum, its property is stablized, pollution-free, and heat conduction is fast.Seed crystal tray
Center has pit sulculus to place diamond seed, is placed on the water-cooled platform in resonant cavity, by inputting microwave power and pressure
It is strong to obtain growth temperature, there is the advantages that quick heating, workable.However, there is growth in the seed crystal tray that tradition uses
The problem of temperature is difficult to be effectively controlled.
Chinese patent CN204281889 discloses a kind of new seed crystal tray for rapid growth of diamond single-crystal, its pallet
Center-side is equipped with pit, and the pit port of export with horizontal plane where pallet end face is connected by chamfered transition.The design can be in life
The discontinuity of electromagnetic field is reduced in growth process, suppression marginal growth is too fast, improves diamond quality.But use the seed crystal
When pallet grows diamond, in growth course, between seed crystal and groove, easy deposited graphite between substrate tray and water-cooled platform.It is heavy
Long-pending graphite can change the heat transfer path between diamond and water-cooled platform, so as to directly affect heat-conducting effect, make the life of seed crystal
Long temperature constantly raises, it is difficult to ensures that crystal stablizes growth conditions for a long time, hinders the synthesis of large dimond monocrystalline.
Control surface temperature when Chinese patent CN104775154A discloses a kind of isoepitaxial growth single-crystal diamond
Method, this method weld goldleaf among seed crystal and seed crystal tray, meanwhile, heat conduction is too fast in order to prevent adds under substrate tray
Heat-insulated silk, so that ensure that diamond and uniform plasma exposure, and then the uniformity in temperature field, make diamond growth
Obtain more preferably.Although the invention can effectively suppress contact of the graphite with seed crystal and seed crystal tray, there is provided stable growth temperature.But
It is that the goldleaf welded between seed crystal and seed crystal tray groove there are certain requirements growth temperature, and goldleaf can be melted at 1000 DEG C or so
Change, deposition temperature range when this is limited using this method to a certain extent.
The content of the invention
It is an object of the invention to provide a kind of seed crystal tray for diamond single crystal homoepitaxy, it is intended to solves at the same time
The problem of seed temperature hardly results in effective control in existing MPCVD (microwave plasma CVD) system.
Another object of the present invention is to provide a kind of base station component for diamond single crystal homoepitaxy, including it is above-mentioned
Seed crystal tray.
It is still another object of the present invention to provide a kind of method for preparing diamond single crystal using above-mentioned base station component.
The present invention is achieved in that a kind of seed crystal tray for diamond single crystal homoepitaxy, the seed crystal tray
It is placed on the water-cooled platform of microwave plasma CVD device, the seed crystal tray center is offered for placing seed crystal
Perforation.
Correspondingly, a kind of base station component for diamond single crystal homoepitaxy, including water-cooled platform and it is arranged on the water
Seed crystal tray in cold bench, the seed crystal tray are the above-mentioned seed crystal tray for diamond single crystal homoepitaxy.
And a kind of method for preparing diamond single crystal using above-mentioned base station component, comprise the following steps：
After the seed crystal and seed crystal tray are carried out surface cleaning processing respectively, the seed crystal tray is placed in the water cooling
On platform, the seed crystal is placed in the perforation of the seed crystal tray；
Reaction chamber door is closed, the air pressure for being pumped to the reaction chamber is 10-3-10-4Pa, is passed through hydrogen, inputs pressure and micro-
Wave power, the seed crystal is etched with hydrogen plasma；
Methane gas is passed through after etching, regulates and controls pressure and input power to adjust diamond growth temperature, prepares gold
Hard rock monocrystalline.
Provided by the present invention for the seed crystal tray of diamond single crystal homoepitaxy, the seed crystal tray center offers use
In the perforation for placing seed crystal, it is possible to achieve seed crystal is contacted with water-cooled platform, and the seed crystal does not connect directly with the seed crystal tray
Touch, so as to avoid temperature drift caused by deposited graphite, provided for seed crystal and stablize effective growing environment, make diamond single crystal
Continued propagation under high power density is maintained at, obtains excellent diamonds monocrystalline.Meanwhile the concave surface of the seed crystal tray can press down
The too fast growth of seed crystal edges processed, effectively suppressing twin etc. influences the factor of diamond quality, further improves diamond single crystal
Quality.In addition, the seed crystal tray provided by the present invention for diamond single crystal homoepitaxy, it is not necessary to weld goldleaf to suppress
Influence of the graphite to temperature, therefore, growth temperature extend its deposition temperature range from the limitation of goldleaf fusing point.
Provided by the present invention for the base station component of diamond single crystal homoepitaxy, containing above-mentioned seed crystal tray, accordingly, it is capable to
It is enough effectively to suppress temperature drift caused by graphite in growth course, further suppress the too fast growth in edge, stabilization is provided for seed crystal
Effective growing environment, makes diamond single crystal be maintained at continued propagation under high power density, obtains excellent diamonds monocrystalline.
The method provided by the invention that diamond single crystal is prepared using base station component, only need to be placed in the seed by the seed crystal
In the perforation of crystal holder disk, it is that the preparation of standby excellent diamonds monocrystalline can be achieved to set the parameters such as working gas, pressure, power.
This method is easy to operate, and controllability is strong, it is easy to accomplish the industrialization of single-crystal diamond.
Brief description of the drawings
Fig. 1 is the seed crystal tray structure diagram provided in an embodiment of the present invention for diamond single crystal homoepitaxy；
Fig. 2 is the base station component structure diagram provided in an embodiment of the present invention for diamond single crystal homoepitaxy；
Fig. 3 is the single-crystal diamond shape appearance figure that the embodiment of the present invention 1 provides；
Fig. 4 is the Raman spectrogram for the single-crystal diamond that the embodiment of the present invention 1 provides.
Embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining
The present invention, is not intended to limit the present invention.
It is described an embodiment of the present invention provides a kind of seed crystal tray 1 for diamond single crystal homoepitaxy with reference to Fig. 1
Seed crystal tray 1 is placed on the water-cooled platform 2 of microwave plasma CVD device, and 1 center of seed crystal tray offers
For placing the perforation 11 of seed crystal.
Specifically, MPCVD seed crystal tray materials commonly used in the art can be selected in the material of the seed crystal tray 1, the present invention
Embodiment preferably prepares the seed crystal tray 1 using refractory metal material molybdenum.The shape of the seed crystal tray 1 uses symmetrical junction
Structure, it is preferred to use using obtain uniform growth temperature, plasma distribution and carbon source substep it is cylindric.The embodiment of the present invention
Can be according to seed crystal thickness and the seed crystal tray 1 of growth technique selection different-thickness.As further preferred embodiments, the seed
The diameter R of crystal holder disk 1 is 25-50mm, and pallet thickness D is 3-20mm.Specifically, the thickness of the seed crystal is represented with d, the seed
The thickness of crystal holder disk 1 is preferably 1/2d-3/2d, so as to can not only ensure that growth remained at high power density, but also can be pressed down
Seed crystal edges growth processed, finally grows the diamond of higher caliper, high quality.
In the embodiment of the present invention, the center of the seed crystal tray 1 offers perforation 11, the perforation 11 can realize seed crystal and
The water-cooled platform 2 directly contacts, and ensures that diamond temperature is unlikely to excessive, power density is improved, to reach single-crystal diamond
The requirement of high power density growth.In addition, the perforation at 1 center of seed crystal tray can also suppress the extension of seed crystal edges, carry
Seedling height quality so that during the entire process of single-crystal diamond, growth temperature is stablized, and the growth of diamond is maintained at stable state
In, finally realize the synthesis of high quality, high thickness diamond single crystal.Due to the seed crystal shape more tend to it is square,
Stablize storage for the ease of the seed crystal, as the presently preferred embodiments, the perforation 11 is square perforation.Further, it is described
The length of side of square perforation should should not be too large or too small, to ensure the seed using the size of the seed crystal as according to being set
Certain space (i.e. described seed crystal and the seed crystal tray are not directly contacted with) is left between brilliant and described seed crystal tray, to prevent
Polycrystalline diamond is grown on the surface of the seed crystal tray, influences the quality of single-crystal diamond.As the presently preferred embodiments, the side
The length of side L of shape perforation is 3-10mm.
In the embodiment of the present invention, by seed crystal be placed in it is described perforation 11 in directly contacted with the water-cooled platform 2 when, due to Buddha's warrior attendant
Quickly, it is difficult to improve to cause the seed crystal face temperature described in growth course, so as to influence the growth of single-crystal diamond for stone heat conduction
Efficiency and quality.In order to effectively adjust the seed crystal face temperature, as the presently preferred embodiments, in the seed crystal and the water-cooled platform
Heat-insulated silk is provided between 2.The heat-insulated silk can be on the premise of avoiding deposited graphite from influencing temperature, described in flexible modulation
The temperature of seed crystal face, regulates and controls different growth temperatures.Material, the specification of the heat-insulated silk are used for diamond single crystal homogeneity following
It is described in detail in the base station component of extension.
Seed crystal tray provided in an embodiment of the present invention for diamond single crystal homoepitaxy, first, the seed crystal tray
Center offers the perforation for placing seed crystal, it is possible to achieve seed crystal is contacted with water-cooled platform, and the seed crystal not with the seed
Crystal holder disk directly contacts, and so as to avoid temperature drift caused by deposited graphite, ensures that power density continues surely in growth course
It is fixed, provided for seed crystal and stablize effective growing environment, diamond single crystal is stablized continued propagation, obtain excellent diamonds
Monocrystalline.Meanwhile the concave surface of the seed crystal tray can suppress the too fast growth of seed crystal edges, effectively suppressing twin etc. influences Buddha's warrior attendant
The factor of stone quality, further improves the quality of diamond single crystal.The embodiment of the present invention can also be high according to the seeded growth
Spend to select the seed crystal tray of different-thickness, ensure to realize the synthesis of thicker diamond under high power density.
Secondly, the embodiment of the present invention can place heat-insulated silk under diamond seed, can prevent the seed crystal with it is described
Water-cooled platform directly contacts, so as to avoid since heat conduction is too fast so that diamond temperature is too low to influence growth efficiency and diamond single crystal
The problem of quality.
Again, the embodiment of the present invention can adjust diamond single crystal according to the materials of the different heat-insulated silks of selection, diameter
Surface growth temperature (surface growth temperature during diamond single crystal homoepitaxy is controllable) during homoepitaxy, and controllable model
Enclose larger.It so not only can guarantee that and possessed larger growth temperature range of choice, but also be avoided that the temperature produced due to graphite deposits
Drift, simplifies experimental implementation, realizes seed crystal and stablizes continued propagation under high power density.
In addition, the seed crystal tray provided in an embodiment of the present invention for diamond single crystal homoepitaxy, it is not necessary to welding gold
Paper tinsel suppresses influence of the graphite to temperature, and therefore, growth temperature extends its depositing temperature model from the limitation of goldleaf fusing point
Enclose.
Correspondingly, with reference to Fig. 2, the embodiment of the present invention additionally provides a kind of base station group for diamond single crystal homoepitaxy
Part, including water-cooled platform 2 and the seed crystal tray 1 that is arranged on the water-cooled platform 2, the seed crystal tray 1 are used for Buddha's warrior attendant for above-mentioned
The seed crystal tray 1 of stone monocrystalline homoepitaxy.
Specifically, the structure of the seed crystal tray 1, shape and the setting of the perforation are as it was noted above, in order to save
Length, details are not described herein again.
In the embodiment of the present invention, directly contacted with the water-cooled platform 2 as it was previously stated, seed crystal is placed in the perforation 11
When, it is difficult to improve to cause the seed crystal face temperature described in growth course due to diamond heat-conducting quickly, so as to influence monocrystalline gold
The growth efficiency and quality of hard rock.In order to effectively adjust the seed crystal face temperature, as the presently preferred embodiments, set in the perforation
The heat-insulated silk 3 for adjusting seed crystal face temperature is equipped with, the heat-insulated silk 3 is arranged on the water-cooled platform 2 of the punch position
Surface.The deposition that the heat-insulated silk avoids graphite causes temperature drift, and further, can avoid deposited graphite to temperature
On the premise of degree influences, the temperature of seed crystal face described in flexible modulation, regulates and controls different growth temperatures.
The length of the heat-insulated silk 3 should match with the size of the perforation, and the diameter of the heat-insulated silk 3 is by the seed
The needs of brilliant surface temperature are adjusted；The embodiment of the present invention is also an option that the heat-insulated silk 3 of different size to adjust the seed
Distance between brilliant and described water-cooled platform 2, so as to fulfill different growth techniques.It is common, when the seed crystal needs setting higher
Surface temperature when, selection is relatively large in diameter the heat-insulated silk 3 of (heat conduction is relatively poor)；When the seed crystal need to set it is relatively low
During surface temperature, the heat-insulated silk 3 of diameter smaller (heat conduction is relatively preferable) is selected.As the presently preferred embodiments, the heat-insulated silk 3
Length be 1-10mm, a diameter of 0.1-0.8mm.Specifically, the length of the heat-insulated silk 3 can be 1mm, 2mm, 3mm, 4mm,
The concrete numerical values such as 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, diameter can be 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm,
The concrete numerical values such as 0.6mm, 0.7mm, 0.8mm.
In the embodiment of the present invention, for the ease of the seed crystal stablize place, the heat-insulated silk 3 be preferably arranged to V-type or
Ellipse.The heat-insulated silk 3 made will ensure that heat-insulated silk is smooth, to ensure that the seed crystal is placed on the level of energy holding above, with
Uniform plasma exposure.Preferably, the material of the heat-insulated silk 3 is molybdenum filament, tantalum wire or tungsten filament, more preferably heat-conducting effect
Well, high temperature resistant molybdenum filament.The preferable heat-insulated silk 3 has characteristic uniform in material, makes the seed crystal and plasma uniform
Contact, ensures the uniform of the seed crystal face temperature and carbon source density, is further ensured that the quality of single-crystal diamond.
Base station component provided in an embodiment of the present invention for diamond single crystal homoepitaxy, containing above-mentioned seed crystal tray,
Therefore, it is possible to effectively suppress temperature drift caused by graphite in growth course, further suppress the too fast growth in edge, carried for seed crystal
For the effective growing environment of stabilization, diamond single crystal is maintained at continued propagation under high power density, obtain excellent diamonds
Monocrystalline.
Secondly, the embodiment of the present invention can place heat-insulated silk under diamond seed, can prevent the seed crystal with it is described
Water-cooled platform directly contacts, so as to avoid since heat conduction is too fast so that diamond temperature is too low to influence growth efficiency and diamond single crystal
The problem of quality.
Again, the embodiment of the present invention can be according to material, the diameter of the different heat-insulated silks of selection, to adjust diamond single crystal
Surface growth temperature (surface growth temperature during diamond single crystal homoepitaxy is controllable) during homoepitaxy, meets not equality of temperature
The growth technique requirement of degree, there is larger temperature range of choice.It so both can guarantee that and possessed larger growth temperature range of choice,
The temperature drift produced due to graphite deposits is avoided that again, simplifies experimental implementation, seed crystal is realized that stabilization is held under high power density
Continuous growth.
And an embodiment of the present invention provides a kind of method for preparing diamond single crystal using above-mentioned base station component, including
Following steps：
S01. after the seed crystal and seed crystal tray being carried out surface cleaning processing respectively, the seed crystal tray is placed in described
On water-cooled platform, the seed crystal is placed in the perforation of the seed crystal tray；
S02. reaction chamber door is closed, the air pressure for being pumped to the reaction chamber is 10-3-10-4Pa, is passed through hydrogen, inputs pressure
And microwave power, etch the seed crystal with hydrogen plasma；
S03. methane gas is passed through after etching, regulates and controls pressure and input power to adjust diamond growth temperature, makes
Standby diamond single crystal.
Specifically, in above-mentioned steps S01, the seed crystal and seed crystal tray pass through respectively shows cleaning treatment, described in guarantee
Seed crystal and seed crystal tray are clean, pollution-free.Specifically, the method for the seed crystal face cleaning treatment is preferably：By the seed crystal
It is sequentially placed into mixed acid, deionized water, acetone and is cleaned by ultrasonic；The method of seed crystal tray surface cleaning processing is preferably：
The seed crystal tray is placed in acetone and is cleaned by ultrasonic.
The seed crystal tray is placed on the water-cooled platform, the seed crystal is placed in the perforation of the seed crystal tray, can
To ensure the high power density of single crystal diamond film.As the presently preferred embodiments, between the seed crystal and water-cooled platform, place every
Heated filament.Specifically, the seed crystal tray is placed on the water-cooled platform, selected according to the seed crystal thickness and growth technique different
The heat-insulated silk, is placed on the central hole of the seed crystal tray by the heat-insulated silk of the seed crystal tray and different size of thickness
In, then the seed crystal cleaned up is placed on the heat-insulated silk, the seed crystal is steadily placed, is ensured uniform with plasma
Contact, temperature are uniform.Preferably, V-type or ellipse is made in heat-insulated silk to meet different growth techniques.
In above-mentioned steps S02, the pumping process can be evacuated using mechanical pump and molecular pump respectively, be pumped to the reaction
The air pressure of chamber is 10-3-10-4Pa, and ensure that foreign gas is discharged in reaction cavity.
In above-mentioned steps S03, methane gas is passed through after etching, set the flow-rate ratio of methane and hydrogen to set methane
Concentration, it is preferred that the volumetric concentration of the methane between 1%-10%, concretely 1%, 2%, 3%, 4%, 5%, 6%,
7%th, 8%, 9%, 10%.Regulate and control pressure and input power to adjust diamond growth temperature, the preferred 800- of growth temperature
Between 1300 DEG C, concretely 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, 1300 DEG C.
After growth, the means such as light microscope, Raman spectrum characterization diamond quality can be used.
The seed crystal, need to be only placed in by the method provided in an embodiment of the present invention that diamond single crystal is prepared using base station component
In the perforation of the seed crystal tray, it is that standby excellent diamonds monocrystalline can be achieved to set the parameters such as working gas, pressure, power
Prepare.This method is easy to operate, and controllability is strong, it is easy to accomplish the industrialization of single-crystal diamond.
Illustrated with reference to specific embodiment.
Embodiment 1
A kind of method for preparing diamond single crystal using above-mentioned base station component, comprises the following steps：
S11. after the seed crystal and seed crystal tray being carried out surface cleaning processing respectively, the seed crystal tray is placed in described
On water-cooled platform, heat-insulated silk is placed in the perforation of the seed crystal tray, the seed crystal is placed on heat-insulated silk；Specifically,
Select seed crystal, thickness 1.07mm, in mixed acid (HNO3：H2SO4=1:1) it is cleaned by ultrasonic 30min in, except remove seed
The impurity such as brilliant surface metal；Then it is placed in deionization water-bath and is cleaned by ultrasonic the acid solution that 30min removes remnants；Then seed crystal is existed
Ultrasound 30min washes away the impurity such as organic matter in acetone.It is meanwhile seed crystal tray described in the embodiment of the present invention is also ultrasonic in acetone
30min is cleaned, obtains the seed crystal and seed crystal tray of cleaning；
Selecting molybdenum filament, a diameter of 0.18mm of molybdenum filament, rolls over shape in 90 ° by molybdenum filament as heat-insulated silk；
The seed crystal tray cleaned up is placed on water-cooled platform, the molybdenum filament made is smooth to be placed in wearing for seed crystal tray center
Kong Zhong, is then placed in ready seed crystal.
S12. reaction cavity is closed, is evacuated to 10-4Pa, is passed through hydrogen 300sccm, with hydrogen plasma etched seed.
Apply suitable pressure and power, seed temperature is maintained at 850 DEG C, etches one hour.Methane, methane concentration are passed through after etching
For 8%, power and pressure are adjusted, ensures seed crystal in 950 DEG C of growths.At this time because there is heat-insulated silk between seed crystal and water-cooled platform, deposit
Graphite seed temperature will not be impacted, whole growth course keeps stablizing；
S13. after growing 92h, seed crystal is placed in thicker seed crystal tray and is grown, keep high power density, seed crystal after 25h
CVD layer thickness is 3.08mm.
After growth, diamond quality is characterized using means such as light microscope, Raman spectrums, the embodiment of the present invention obtains
Single-crystal diamond pattern as shown in figure 3, Raman spectrogram as shown in figure 4, as seen from the figure, the shape of the single-crystal diamond
Looks are good, purity is high.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of seed crystal tray for diamond single crystal homoepitaxy, the seed crystal tray is placed in microwave plasma chemical gas
On the water-cooled platform of phase precipitation equipment, it is characterised in that the seed crystal tray center offers the perforation for placing seed crystal, described
The thickness of seed crystal represents that the thickness of the seed crystal tray is 1/2d-3/2d with d.
2. it is used for the seed crystal tray of diamond single crystal homoepitaxy as claimed in claim 1, it is characterised in that the perforation is
Square perforation, the length of side of the square perforation is 3-10mm.
3. a kind of base station component for diamond single crystal homoepitaxy, including water-cooled platform and the seed that is arranged on the water-cooled platform
Crystal holder disk, it is characterised in that the seed crystal tray is to be used for diamond single crystal homoepitaxy described in claim 1-2 any
Seed crystal tray.
4. it is used for the base station component of diamond single crystal homoepitaxy as claimed in claim 3, it is characterised in that in the perforation
The heat-insulated silk for adjusting seed crystal face temperature is provided with, the heat-insulated silk is arranged on the water-cooled platform table of the punch position
Face.
5. it is used for the base station component of diamond single crystal homoepitaxy as claimed in claim 4, it is characterised in that the heat-insulated silk
Length be 1-10mm, a diameter of 0.1-0.8mm.
6. it is used for the base station component of diamond single crystal homoepitaxy as claimed in claim 5, it is characterised in that the heat-insulated silk
It is arranged to V-type or ellipse.
7. the base station component for diamond single crystal homoepitaxy as described in claim 4-6 is any, it is characterised in that described
Heat-insulated silk material matter is molybdenum filament, tantalum wire or tungsten filament.
8. a kind of usage right requires the method that any base station components of 3-7 prepare diamond single crystal, comprise the following steps：
After the seed crystal and seed crystal tray are carried out surface cleaning processing respectively, the seed crystal tray is placed in the water-cooled platform
On, the seed crystal is placed in the perforation of the seed crystal tray；
Reaction chamber door is closed, the air pressure for being pumped to the reaction chamber is 10-3-10-4Pa, is passed through hydrogen, inputs pressure and microwave work(
Rate, the seed crystal is etched with hydrogen plasma；
Methane gas is passed through after etching, regulates and controls pressure and input power to adjust diamond growth temperature, prepares diamond
Monocrystalline.
9. the method for preparing diamond single crystal using base station component as claimed in claim 8, it is characterised in that in the seed crystal
Between water-cooled platform, heat-insulated silk is placed.
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| CN106012003B (en) * | 2016-06-07 | 2018-06-08 | 武汉工程大学 | The two-dimentional expansion method of CVD single-crystal diamonds |
| CN107955967A (en) * | 2017-11-30 | 2018-04-24 | 河北普莱斯曼金刚石科技有限公司 | Growth of Single Crystal Diamond device and method |
| 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 |
| CN109355702B (en) * | 2018-12-19 | 2022-03-18 | 长沙新材料产业研究院有限公司 | Method for reducing impurity content of CVD synthetic diamond |
| CN111663179A (en) * | 2019-03-05 | 2020-09-15 | 中国科学院物理研究所 | Seed crystal support for growth of single crystal diamond |
| CN110042464A (en) * | 2019-04-02 | 2019-07-23 | 西安电子科技大学 | A kind of method of multi-disc single-crystal diamond expanding growth simultaneously |
| CN110820044B (en) * | 2019-12-02 | 2021-10-01 | 长沙新材料产业研究院有限公司 | High-quality diamond growth method and system |
| CN113957516B (en) * | 2021-10-29 | 2024-01-30 | 中国电子科技集团公司第二十六研究所 | Tray device for growing crystals by horizontal directional crystallization method and use method |
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