CN109930202A - A kind of suitable ammonia heat method generates the heat isostatic apparatus of gallium nitride single crystal product - Google Patents
A kind of suitable ammonia heat method generates the heat isostatic apparatus of gallium nitride single crystal product Download PDFInfo
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- CN109930202A CN109930202A CN201910263191.3A CN201910263191A CN109930202A CN 109930202 A CN109930202 A CN 109930202A CN 201910263191 A CN201910263191 A CN 201910263191A CN 109930202 A CN109930202 A CN 109930202A
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- 239000013078 crystal Substances 0.000 title claims abstract description 119
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910002601 GaN Inorganic materials 0.000 title claims abstract description 100
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 65
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 47
- 238000009413 insulation Methods 0.000 claims abstract description 48
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 239000002826 coolant Substances 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 10
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- 238000001816 cooling Methods 0.000 claims description 4
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- 239000007924 injection Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 abstract description 4
- 238000005242 forging Methods 0.000 abstract description 3
- 230000006835 compression Effects 0.000 abstract description 2
- 238000007906 compression Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 239000007789 gas Substances 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 238000010586 diagram Methods 0.000 description 5
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- 238000004804 winding Methods 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
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- 229910000831 Steel Inorganic materials 0.000 description 3
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses the heat isostatic apparatus that a kind of suitable ammonia heat method generates gallium nitride single crystal product, it is characterized by comprising the working cylinders (2) of internal setting hot-zone, it is placed in the gallium nitride single crystal growing container (3) of the corresponding size that diameter is 200~400mm or bigger specification of generating in the hot-zone, the hot-zone, which is divided into, respectively corresponds the heating crystal region of gallium nitride single crystal growing container (3) and the upper heating zone of dissolution zone and lower heating zone, the corresponding hot-zone setting in baffle (18) position inside the gallium nitride single crystal growing container (3) makes baffle (18) lower regions generate the middle heat insulation loop (16) for being suitble to the step evolution temperature difference of ammonia heat method generation gallium nitride single crystal product, improving the gallium nitride single crystal growing container 3 i.e. working stress of autoclave simultaneously is compression, it can increase in this way Solid forging gallium nitride single crystal growing container (3) specification, growing diameter is 200~400mm, the gallium nitride single crystal product of even more big specification.
Description
Technical field
The present invention relates to the heat isostatic apparatus that a kind of suitable ammonia heat method generates gallium nitride single crystal product, more particularly to one kind
Suitable ammonia heat method generates big specification gallium nitride single crystal product or high-volume generates the heat isostatic apparatus of gallium nitride single crystal product.
Background technique
Third generation semiconductor material is prohibited using gallium nitride (GaN), silicon carbide (SiC), diamond, zinc oxide as the width of representative
Carrying semiconductor material is the hot spot of countries in the world semiconductor field research.Gallium nitride have forbidden bandwidth is big, breakdown electric field is high,
The unique performances such as thermal conductivity is big, electronics saturation drift velocity is high, dielectric constant is small, in opto-electronic device, power electronics, radio frequency
Microwave device, laser and detector etc. have a vast market foreground.
Gallium nitride single crystal growing technology has hydride gas-phase epitaxy also in developing stage, current main generation method
Method, high pressure nitrogen solwution method, ammonia heat method and sodium flux growth metrhod etc., wherein ammonia heat method is easily obtained the gallium nitride list of larger size
Crystalline substance, ammonia heat method belong to solvent-thermal method, refer under supercriticality or subcritical state or two states coexisting state with ammonia
For the process for producing crystal of solvent, the important equipment that ammonia heat method generates crystal is autoclave, belongs to A1 grades of ultrahigh pressure vessels, big ruler
Very little ammonia heat method gallium nitride single crystal product mostly uses seed crystal temperature difference method growth, i.e., the dissolution separated by baffle is arranged in autoclave
The stable temperature difference is established in area and crystal region, dissolution zone and crystal region, while more crystal more evenly in order to obtain, it is desirable that dissolution
Area and crystal region respectively keep temperature consistent as far as possible in region again, warm-natured this requires generating a step near baffle
Difference.The technological temperature that autoclave is born is generally 400~650 DEG C, and operation pressure is generally 100~200MPa, autoclave design
It is both needed to National Quality Supervision Bureau General's license with manufacture, since autoclave belongs to Integral forge type pressure vessel, and the working time is longer, protects
Thermophase was up to 20~80 days, therefore, is limited by structure design and working stress, is difficult to be made into large-sized autoclave, next life
It is the gallium nitride single crystal product of 200~400mm specification, even more big specification at diameter.
Summary of the invention
It is limited to solve of the existing technology designed by structure with working stress, is difficult to be made into large-sized high pressure
The problem of kettle, Lai Shengcheng diameter is the gallium nitride single crystal product of 200~400mm specification, even more big specification, the present invention provide one
The suitable ammonia heat method of kind generates the heat isostatic apparatus of gallium nitride single crystal product.A kind of suitable ammonia heat method of the invention generates gallium nitride
The heat isostatic apparatus of single crystal articles, it is characterised in that: the working cylinder 2 including internal setting hot-zone is placed in the hot-zone
The gallium nitride single crystal growing container 3 for generating the corresponding size that diameter is 200~400mm or bigger specification, the hot-zone point
It is divided into and respectively corresponds the heating crystal region of gallium nitride single crystal growing container 3 and the upper heating zone of dissolution zone and lower heating
The corresponding hot-zone setting in 18 position of baffle in area, 3 the inside of gallium nitride single crystal growing container produces 18 lower regions of baffle
Raw suitable ammonia heat method generates the middle heat insulation loop 16 of the step evolution temperature difference of gallium nitride single crystal product.
Further, the working cylinder 2 includes inner cylinder 4, the upper end cover 5 that 4 upper end of inner cylinder is arranged in and is arranged under inner cylinder 4
The lower cover 23 at end, the interior setting heat-insulation working platform 8 of the inner cylinder 4 and heating furnace module 9, the gallium nitride single crystal grow appearance
Device 3 is placed on the heat-insulation working platform 8 and is placed in the heating furnace module 9.
Further, the heating furnace module 9 includes heat screen 12, upper calandria 13, lower calandria 14, upper heat insulation loop
15, middle heat insulation loop 16 and lower heat insulation loop 17, the heat screen 12 is cup type to be placed on the heat-insulation working platform 8, described
Upper heat insulation loop 15, middle heat insulation loop 16 and lower heat insulation loop 17, which are arranged at intervals in the heat screen 12 and are separated into hot-zone, to be added
Hot-zone and lower heating zone, the upper heating zone are provided with calandria 13, and the lower heating zone is provided with lower calandria 14.
Further, coolant jacket 6,12 lower section of heat screen are provided with above the heat screen 12 in the inner cylinder 4
Heat-insulation working platform 8 outside be provided with lower coolant jacket 7, the upper coolant jacket 6, lower coolant jacket 7, heat screen 12 and heat-insulation working
The heat that platform 8 generates upper calandria 13 and lower calandria 14 carries out constraint shielding, and forming one can satisfy gallium nitride single crystal
The hot-zone that growth temperature requires.
Further, gas booster 11 is housed, the gas booster 11 passes through pipeline outside the working cylinder 2
It pressurizes into working cylinder 2, forms the external initial pressure that the gallium nitride single crystal growing container 3 requires, described is first
Beginning pressure is adjusted according to the pressure of liquefied ammonia in injection gallium nitride single crystal growing container 3, and nitrogen is realized when reaching desired temperature
The internal process pressure for changing algan single crystal growing container 3 is slightly below external operating pressure.
Further, the initial pressure is adjusted to realize gallium nitride single crystal growing container 3 when reaching desired temperature
Internal process pressure is slightly below the pressure value of 3~10MPa of external operating pressure.
Further, it is equipped with outside the working cylinder 2 and passes through inner cylinder 4, upper end cover 5, lower cover of the pipeline to working cylinder 2
23, upper coolant jacket 6 and lower coolant jacket 7 carry out cooling cooling water pump 10.
Further, pressure measurement sensor is set in the gallium nitride single crystal growing container 3, pressure measurement sensor
Signal wire draws working cylinder 2 by lower cover 23, and connect with the pressure gauge outside working cylinder 2.
Further, it is wound outside the inner cylinder 4 of the working cylinder 2 by compressor wire, the working cylinder 2 is arranged in machine
In frame 1, the rack 1 is the column by two sides and is placed in half circular beam at the column both ends through compressor wire winding production
Raw pressure is linked together to be formed, and the rack 1 is mounted on frame seat 20.
Further, the gallium nitride single crystal growing container 3 passes through lifting lower cover of the truck 21 from the working cylinder 2
Dress takes at 23, and the working cylinder 2 is loaded and unloaded from rack 1 by the cylinder jacket 19 connecting with track base 22.
The heat isostatic apparatus that a kind of suitable ammonia heat method of the invention generates gallium nitride single crystal product has following actively effect
Fruit, using heat isostatic apparatus, in conjunction with ammonia heat method gallium nitride single crystal growth technique technology, 2 hot-zone of design work cylinder, so that hot-zone
Temperature generates the step evolution temperature difference for being suitble to ammonia heat method to generate gallium nitride single crystal product, works at the same time the initial pressure of cylinder 2 according to note
The pressure for entering liquefied ammonia in gallium nitride single crystal growing container 3 is adjusted, and gallium nitride single crystal growth is realized when reaching desired temperature
The internal process pressure of container 3 is slightly below external operating pressure, improves the i.e. autoclave of gallium nitride single crystal growing container 3 in this way
Working stress can increase 3 specification of solid forging gallium nitride single crystal growing container, and growing diameter is 200~400mm, very
To the gallium nitride single crystal product of bigger specification.
Detailed description of the invention
Fig. 1 is the structural representation for the heat isostatic apparatus that a kind of suitable ammonia heat method of the present invention generates gallium nitride single crystal product
Figure.
Fig. 2 is the knot of the working cylinder for the heat isostatic apparatus that a kind of suitable ammonia heat method of the present invention generates gallium nitride single crystal product
Structure schematic diagram.
Fig. 3 is the cooling medium stream for the heat isostatic apparatus that a kind of suitable ammonia heat method of the present invention generates gallium nitride single crystal product
To schematic diagram.
Fig. 4 is the dress of the working cylinder for the heat isostatic apparatus that a kind of suitable ammonia heat method of the present invention generates gallium nitride single crystal product
Unload schematic diagram.
In figure: 1. racks, 2. working cylinders, 3. gallium nitride single crystal growing containers, 4. inner cylinders, 5. upper end covers, coolant jacket on 6.,
7. lower coolant jacket, 8. heat-insulation working platforms, 9. heating furnace modules, 10. cooling water pump, 11. gas booster, 12. heat screens, on 13
Calandria, 14. lower calandrias, heat insulation loop on 15., heat insulation loop in 16., 17. lower heat insulation loops, 18. baffles, 19. cylinder jackets,
20. frame seat, 21. lifting trucks, 22. track bases, 23. lower covers.
Specific embodiment
To further illustrate presently preferred embodiments of the present invention, and after cooperating attached drawing to be specified in, so as to be easier to for the present invention
In understanding.But as described below is only preferred embodiment used to explain the present invention, is not intended to do any shape to the present invention accordingly
Limitation in formula, all any type of modifications or change based on creative spirit of the invention, done, all still should belong to
The invention is intended to the scopes of protection.It should also be noted that, unless otherwise clearly defined and limited, term " setting " should be done extensively
Reason and good sense solution can understand above-mentioned term in the present invention specific for the ordinary skill in the art with concrete condition
Meaning.
Hot isostatic pressing technique is a kind of in closed ultrahigh pressure vessel, using nitrogen or argon gas as transmission medium, is added with electricity
Thermal technology forms hot-zone and handles under the collective effect of high temperature and high pressure product.Hot isostatic pressing technique has powder at present
Dense sintering, casting densification, diffusion connection, the big technique application of impregnation carbonization four, generate nitrogen using hot isostatic pressing technique
The fifth-largest technique application of hot isostatic pressing technique will be become by changing algan single crystal product.
Figures 1 and 2 show that a kind of suitable ammonia heat method of the invention generates the heat isostatic apparatus of gallium nitride single crystal product,
It is characterized by comprising the working cylinder 2 of internal setting hot-zone, the generation diameter being placed in the hot-zone be 200~400mm or
The gallium nitride single crystal growing container 3 of the corresponding size of bigger specification, the hot-zone, which is divided into, respectively corresponds the heating nitrogen
Change the crystal region of algan single crystal growing container 3 and the upper heating zone and lower heating zone of dissolution zone, the gallium nitride single crystal, which is grown, to be held
The lower regions that the corresponding hot-zone setting in 18 position of baffle of 3 the inside of device is divided into baffle 18, which generate, is suitble to ammonia heat method to generate nitridation
The middle heat insulation loop 16 of the step evolution temperature difference of algan single crystal product.
The hot-zone diameter of the current general requirements of heat isostatic apparatus is 150~φ of φ 800mm, the hot-zone diameter of larger specification
For φ 800~φ 1600mm, the hot-zone diameter of maximum specification is φ 2040mm at present, can satisfy generate diameter be 200~
The requirement of the gallium nitride single crystal growing container 3 of 400mm or the corresponding size of bigger specification.
Further, the working cylinder 2 includes inner cylinder 4, the upper end cover 5 that 4 upper end of inner cylinder is arranged in and is arranged under inner cylinder 4
The lower cover 23 at end, the interior setting heat-insulation working platform 8 of the inner cylinder 4 and heating furnace module 9, the gallium nitride single crystal grow appearance
Device 3 is placed on the heat-insulation working platform 8 and is placed in the heating furnace module 9.
Further, the heating furnace module 9 includes heat screen 12, upper calandria 13, lower calandria 14, upper heat insulation loop
15, middle heat insulation loop 16 and lower heat insulation loop 17, the cup type inner cylinder for being placed in 8 top of heat-insulation working platform of the heat screen 12
In 4, the upper heat insulation loop 15, middle heat insulation loop 16 and lower heat insulation loop 17 are arranged at intervals in the heat screen 12 and by hot-zones
It is separated into heating zone and lower heating zone, upper calandria 13 is arranged in the upper heating zone, and the lower heating zone setting is lower to be added
Hot body 14, while the heating power input of upper calandria 13 and lower calandria 14 is controlled respectively, middle heat insulation loop 16 is selected compared with brief biography
The thermal insulation material of hot coefficient, while using suitable width, it is ensured that the inside of gallium nitride single crystal growing container 3 baffle 18 it is upper
Side and lower section generate the step evolution temperature difference.
Further, coolant jacket 6,12 lower section of heat screen are provided with above the heat screen 12 in the inner cylinder 4
Heat-insulation working platform 8 outside be provided with lower coolant jacket 7, the upper coolant jacket 6, lower coolant jacket 7, heat screen 12 and heat-insulation working
The heat that platform 8 generates upper calandria 13 and lower calandria 14 carries out constraint shielding, and forming one can satisfy gallium nitride single crystal
The hot-zone that growth temperature requires.
Heat screen generally uses multiple layer metal cylinder or carbon fiber cylinder to be supported, inside filling alumina silicate heat-barrier material
Or ceramic fiber blanket heat-barrier material or carbon fiber blanket heat-barrier material.
Further, gas booster 11 is housed, the gas booster 11 passes through pipeline outside the working cylinder 2
It pressurizes into working cylinder 2, forms the external initial pressure that the gallium nitride single crystal growing container 3 requires, described is first
Beginning pressure is adjusted according to the pressure of liquefied ammonia in injection gallium nitride single crystal growing container 3, and nitrogen is realized when reaching desired temperature
The internal process pressure for changing algan single crystal growing container 3 is slightly below external operating pressure.Simultaneously during heat-insulation pressure keeping, if work
The sealing for making cylinder 2 occurs leakage and pressure reduction situation occurs, then can be mended by gas booster 11 into working cylinder 2
Pressure.
Due to using electric heating tube in drier, the pressure medium of gas booster 11 uses the gas or inert gas for being not easy to react
Body.Its pressure controling mode is generally there are three types of temperature, pressure control model: first pressurize heat up afterwards, first heat up pressurize afterwards, side is pressurizeed
Side heating, wherein heating mode is consistent with the temperature, pressure control mode that ammonia heat method gallium nitride single crystal is grown after first pressurizeing.
Further, the initial pressure is adjusted to realize gallium nitride single crystal growing container 3 when reaching desired temperature
Internal process pressure is slightly below the pressure value of 3~10MPa of external operating pressure.
A kind of suitable ammonia heat method of the content of present invention generates the working cylinder 2 of the heat isostatic apparatus of gallium nitride single crystal product, most
High operating pressure 200MPa, 800 DEG C of maximum operating temperature, the working media that gas booster 11 pressurizes is high pure nitrogen.
Further, it is equipped with outside the working cylinder 2 and passes through inner cylinder 4, upper end cover 5, lower cover of the pipeline to working cylinder 2
23, upper coolant jacket 6 and lower coolant jacket 7 carry out cooling cooling water pump 10.Temperature outside heat screen exceeds up to 200~400 DEG C
The value may impact in inner cylinder 4 to working cylinder, the safety of upper end cover 5 and lower cover 23 and service life, therefore, setting cooling
Water pump 10 cools down inner cylinder 4, the end cap of working cylinder, to guarantee the safety of equipment, and obtains gallium nitride single crystal growing container 3
Temperature required for both ends.Fig. 3 shows cooling medium and flows to schematic diagram.Cooling medium forms three after cooling water pump 10 pumps out
A cooling circuit, one through lower cover 23 and lower 7 reflow tank of coolant jacket, the second tunnel around reflow tank, third road after inner cylinder 4
Converge reflow tank with the second tunnel cooling medium after upper end cover 5 and upper coolant jacket 6.
Further, pressure measurement sensor is set in the gallium nitride single crystal growing container 3, pressure measurement sensor
Signal wire draws working cylinder 2 by lower cover 23, and connect with the pressure gauge outside working cylinder 2.
Further, it is wound outside the inner cylinder 4 of the working cylinder 2 by compressor wire, 2 inner cylinder of working cylinder is through prestress steel
After silk winding, it is in compression and compressive strain state always, safety is good, ensure that long service life.The working cylinder 2
It is arranged in rack 1, the rack 1 is the column by two sides and is placed in half circular beam at the column both ends through prestress steel
The pressure that silk winding generates is linked together to be formed, and the rack 1 is mounted on frame seat 20.Heat isostatic apparatus is typically tied
Configuration formula has compressor wire winding and two kinds of forms of solid forging, and under normal circumstances, Integral forge type is suitable only for middle-size and small-size
Heat isostatic apparatus, and compressor wire winding form is then suitble to from small-sized to the heat isostatic apparatus of large size or even ultra-large type,
The heat isostatic apparatus of hot-zone diameter phi 800mm or more should wind form using compressor wire.Working cylinder 2 bears radial force,
Rack 1 bears the axial force passed over by the upper end cover 5 and lower cover 23 of floating structure.
Fig. 4 is the dress of the working cylinder for the heat isostatic apparatus that a kind of suitable ammonia heat method of the present invention generates gallium nitride single crystal product
Unload schematic diagram.The gallium nitride single crystal growing container 3 is filled from the lower cover 23 of the working cylinder 2 by going up and down truck 21
It takes, the working cylinder 2 is realized to promote from rack 1 and removes and load and unload by the cylinder jacket 19 connecting with track base 22.Heat
The dress feeding mode of isopressing device, can be divided into charging and lower charging two ways, upper charging method is simple and easy, cost compared with
It is low, it is all made of charging method under normal circumstances.But in some special cases, as heat isostatic apparatus work hot-zone height compared with
Height needs to increase factory building height, or deep-cut melt pit be just able to satisfy dress feeding requirement, or certain impregnation carbonization industries need through
When the dust accumulation in normal cleaning works cylinder bottom portion, then lower charging method can be selected.Lower charging method is selected to grow gallium nitride single crystal
It is convenient that the dress of container 3 takes.
It is the method and tool for generating gallium nitride single crystal product based on ammonia heat method using heat isostatic apparatus of the invention below
Body step.
The preparation of heat isostatic apparatus: the list that the heat isostatic apparatus of pressure must be authorized through National Quality Supervision Bureau General is carried
Prison inspection is completed in position, stamps steel seal and provides prison probatio inspectionem pecuoarem book, each pressure gauge, thermometric instrument must be had the verification of the unit of corresponding qualification
Qualification, each functional component is experiment proves that functional performance is qualified, including heats furnace module 9, cooling water pump 10, gas booster 11
With pressure measurement sensor etc.；
3 preparation of gallium nitride single crystal growing container: the unit that gallium nitride single crystal growing container 3 must be authorized through National Quality Supervision Bureau General
Prison inspection is completed, and provides prison probatio inspectionem pecuoarem book, completes corresponding test according to its design specification, including is outer limits pressure testing, interior
Portion's extreme pressure test, experiments of sealing performance, container corrosion performance test etc.；
The charging work of gallium nitride single crystal growing container 3: by solid matter, including seed crystal, polycrystalline compost or mineralizer etc. and gear
Plate 18 is put into gallium nitride single crystal growing container 3, be refrigerated to -50 DEG C hereinafter, and vacuumize, then injected by liquefied ammonia injected system
Liquefied ammonia requires to avoid being mixed into for the oxygenatedchemicals such as oxygen and water as far as possible when injecting liquefied ammonia；
Gallium nitride single crystal growing container 3 is placed on lifting truck 21, its pressure measurement sensor signal wire is connected and is drawn
Outside the lower cover 23 of lower section, gallium nitride single crystal growing container 3 is packed into working cylinder from the bottom of working cylinder 2 by operation lifting truck 21
In 2；
Using heating mode after first pressurizeing, according to technological temperature and pressure requirements that gallium nitride single crystal is grown, cooling water pump 10 is held
Continuous to be pumped into cooling water, gas booster 11 is forced into initial pressure into working cylinder 2, then starts heating work, by heating furnace
Component 9 carries out the dissolution zone of gallium nitride single crystal growing container 3 and crystal region to be heated to setting technological temperature, into holding stage
20~80 days, the pressure of the nitrogen of the liquefied ammonia contained inside gallium nitride single crystal growing container 3 and outside all can be with the liter of temperature
It is high and increases, when reaching technological temperature that gallium nitride single crystal growth needs and operation pressure enters heat-insulation pressure keeping state, nitrogenize
Operation pressure inside algan single crystal growing container 3 should be slightly below 3~10MPa of external pressure, during heat-insulation pressure keeping, by electrical
Control system control heating furnace module 9 provides heat preservation power, automatic adjustment, in heat-insulation pressure keeping to gallium nitride single crystal growing container 3
In the process, if the sealing of the heat isostatic apparatus of carrying pressure leaks, lead to the outside of gallium nitride single crystal growing container 3
Pressure and internal pressure are unsatisfactory for requiring, then ftercompction can be carried out to working cylinder 2 by gas booster 11, in heat-insulation pressure keeping process
In, when feeling the need to the case where stopping working if there is power failure or other operators, then it can pass through heat isostatic apparatus
Standby generator sets provide necessary safety utilization of electric power, it is ensured that the safety of heat isostatic apparatus；
Enter decrease temperature and pressure process after the completion of heat-insulation pressure keeping, external pressure and the inside of gallium nitride single crystal growing container 3 need to be monitored
Pressure should be disposed suitably if being unsatisfactory for；
After the completion of decrease temperature and pressure, operation lifting truck 21 moves on to gallium nitride single crystal growing container 3 outside working cylinder 2, then removes nitrogen
The connection for changing 3 pressure measurement sensor signal wire of algan single crystal growing container, can hang away gallium nitride single crystal growing container 3 at this time；
Ammonia in gallium nitride single crystal growing container 3 is discharged into water, container is opened, takes out crystal, and it is soaked in chloroazotic acid
Bubble removes surface impurity, obtains the gallium nitride single crystal product that diameter is 200~400mm or bigger specification.
If heat isostatic apparatus is when not in use, lifting truck 21 should be run, lower cover 23 is fitted into working cylinder 2, make machine
Frame 1 and working cylinder 2 are in center overlapping positions, and the high pure nitrogen of a small amount of≤0.1MPa is passed through to working cylinder 2, protect working cylinder
Structural member in 2.
The above is only the preferred embodiment of the present invention, therefore cannot be limited the scope of implementation of the present invention with this, i.e., according to
Equivalent changes and modifications made by scope of the present invention patent and description should still belong to the model that the invention patent covers
In enclosing.
Claims (9)
1. the heat isostatic apparatus that a kind of suitable ammonia heat method generates gallium nitride single crystal product, it is characterised in that: be arranged including inside
The working cylinder (2) of hot-zone is placed in the corresponding size that diameter is 200~400mm or bigger specification of generating in the hot-zone
Gallium nitride single crystal growing container (3), the hot-zone, which is divided into, respectively corresponds the heating gallium nitride single crystal growing container (3)
Crystal region and dissolution zone upper heating zone and lower heating zone, the baffle inside the gallium nitride single crystal growing container (3)
(18) the corresponding hot-zone setting in position makes baffle (18) lower regions generate the rank for being suitble to ammonia heat method to generate gallium nitride single crystal product
The middle heat insulation loop (16) for the warm-natured difference that jumps.
2. a kind of suitable ammonia heat method according to claim 1 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: the working cylinder (2) includes inner cylinder (4), is arranged in the upper end cover (5) of inner cylinder (4) upper end and setting in inner cylinder (4)
The lower cover (23) of lower end, interior setting heat-insulation working platform (8) of the inner cylinder (4) and heating furnace module (9), the gallium nitride
Crystal growth container (3) is placed on the heat-insulation working platform (8) and is placed in the heating furnace module (9).
3. a kind of suitable ammonia heat method according to claim 2 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: the heating furnace module (9) includes heat screen (12), upper calandria (13), lower calandria (14), upper heat insulation loop
(15), middle heat insulation loop (16) and lower heat insulation loop (17), the heat screen (12), which falls, cup type is placed in the heat-insulation working platform (8)
On, the upper heat insulation loop (15), middle heat insulation loop (16) and lower heat insulation loop (17) are arranged at intervals in the heat screen (12)
And hot-zone is separated into upper heating zone and lower heating zone, the upper heating zone is provided with calandria (13), it is described lower plus
Hot-zone is provided with lower calandria (14).
4. a kind of suitable ammonia heat method according to claim 3 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: being provided with coolant jacket (6) above the heat screen (12) in the inner cylinder (4), below the heat screen (12)
Heat-insulation working platform (8) outside be provided with lower coolant jacket (7), the upper coolant jacket (6), lower coolant jacket (7), heat screen (12)
The heat generated with heat-insulation working platform (8) to upper calandria (13) and lower calandria (14) carries out constraint shielding, forms an energy
Enough meet the hot-zone of gallium nitride single crystal growth temperature requirement.
5. a kind of suitable ammonia heat method according to claim 4 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: gas booster (11) being housed outside the working cylinder (2), the gas booster (11) passes through pipeline to work
Make to pressurize in cylinder (2), form the external initial pressure that the gallium nitride single crystal growing container (3) requires, described is first
Beginning pressure is adjusted according to the pressure of liquefied ammonia in injection gallium nitride single crystal growing container (3), the realization when reaching desired temperature
The internal process pressure of gallium nitride single crystal growing container (3) is slightly below external operating pressure.
6. a kind of suitable ammonia heat method according to claim 5 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: being equipped with outside the working cylinder (2) and passes through inner cylinder (4), upper end cover (5), lower cover of the pipeline to working cylinder (2)
(23), upper coolant jacket (6) and lower coolant jacket (7) carry out cooling cooling water pump (10).
7. a kind of suitable ammonia heat method according to claim 6 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: pressure measurement sensor, the signal wire of pressure measurement sensor being arranged in the gallium nitride single crystal growing container (3)
Working cylinder (2) are drawn by lower cover (23), and are connect with mounted in the pressure gauge of working cylinder (2) outside.
8. a kind of suitable ammonia heat method according to claim 7 generates the heat isostatic apparatus of gallium nitride single crystal product, special
Sign is: being wound outside the inner cylinder (4) of the working cylinder (2) by compressor wire, the working cylinder (2) is arranged in rack
(1) in, the rack (1) is wound with half circular beam for being placed in the column both ends through compressor wire by the column of two sides
The pressure of generation is linked together to be formed, and the rack (1) is mounted on frame seat (20).
9. a kind of according to claim 1, the described in any item suitable ammonia heat method generation gallium nitride single crystal systems in 2,3,4,5,6,7 or 8
The heat isostatic apparatus of product, it is characterised in that: the gallium nitride single crystal growing container (3) is by lifting truck (21) from described
Working cylinder (2) lower cover (23) at fill and take, the working cylinder (2) passes through the cylinder jacket that connect with track base (22)
(19) it is loaded and unloaded from rack (1).
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| CN111304732A (en) * | 2020-03-27 | 2020-06-19 | 上海玺唐半导体科技有限公司 | Crystal growth device, hot isostatic pressing equipment and crystal growth method |
| CN111455450A (en) * | 2020-05-13 | 2020-07-28 | 上海玺唐半导体科技有限公司 | GaN single crystal growth device and heating method thereof |
| CN111485289A (en) * | 2020-04-13 | 2020-08-04 | 上海玺唐半导体科技有限公司 | Heating device and heating method |
| CN112048771A (en) * | 2020-08-04 | 2020-12-08 | 上海玺唐半导体科技有限公司 | Reaction kettle, device and method for growing gallium nitride crystal |
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