CN106435717A - Growth equipment and growth technology for 200-kg sapphire crystals - Google Patents
Growth equipment and growth technology for 200-kg sapphire crystals Download PDFInfo
- Publication number
- CN106435717A CN106435717A CN201610716767.3A CN201610716767A CN106435717A CN 106435717 A CN106435717 A CN 106435717A CN 201610716767 A CN201610716767 A CN 201610716767A CN 106435717 A CN106435717 A CN 106435717A
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- Prior art keywords
- crucible
- growth
- tungsten
- crystal
- circular
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Classifications
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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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
Abstract
The invention belongs to the technical field of crystal growth, relates to a crystal growth method, in particular to a growth method for 200-kg large-size sapphire crystals, and further relates to growth equipment for 200-kg sapphire crystals. The growth equipment comprises a stainless steel barrel, the inner side of the stainless steel barrel is provided with a heat insulating layer, a round tungsten cage heating body is arranged in the heat insulating layer, and a round crucible is arranged in an inner cavity of the round tungsten cage heating body. According to the growth equipment for the 200-kg sapphire crystals, the round crucible and the round tungsten cage heating body are arranged, temperature field distribution of the equipment is uniform and stable, and few bubble groups are generated on the upper portions of the prepared crystals; in addition, different length-width-height ratios can be designed for a heat field of the round crucible according to the actual needs of the crystal drawing bar specifications.
Description
Technical field
A kind of the invention belongs to technical field of crystal growth, the present invention relates to growth apparatus of 200kg level sapphire crystal;
It is related to a kind of growing method, more particularly to a kind of growth technique of 200kg level sapphire crystal.
Background technology
Sapphire consist of aluminium oxide Al2O3, be by three oxygen atoms and two aluminium atoms so that covalent bond form is combined
Become, its crystal structure is hexagonal crystallographic texture.As sapphire has the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, high printing opacity
Property, the features such as fusing point is high 2050 DEG C, is therefore often used as the material of photoelectric cell.At present super brightness white/blue-ray LED
Quality depending on gallium nitride GaN epitaxial layer material quality, and epitaxial layer of gallium nitride quality then with the Sapphire Substrate for being used
Surface Machining quality is closely bound up.Due to sapphire single-crystal Al2O3Lattice between C face and III-V and II-VI race's deposition film
Constant mismatch rate is little, while can be high temperature resistant so that sapphire wafer becomes the critical material for making white/blue green light LED.
Cold core float die SAPMAC is on the basis of traditional kyropoulos, develops in conjunction with the advantage of czochralski method
A kind of method for being suitable to growing high quality sapphire single-crystal.Although the technique has larger carrying in terms of crystal mass and cost
Height, but also inherit some basic characteristics of traditional kyropoulos, that is, the sapphire single-crystal for growing be pyriform, and in weight and
There is larger restriction in terms of size, in terms of processing large-sized wafer and other shapes chip, greatly limit the material profit of crystal
With rate.Therefore, in order to meet the wilderness demand of Mobile phone screen and other potential large scale product markets, in the base of original SAPMAC
Improve on plinth, grow 200kg level sapphire single-crystal and be conducive to shortening the R&D cycle, reduce Innovation Input, improve material
Utilization rate, reduces cost.Further, the different size product of the huge market demand can be directed to, thermal field be adjusted, be grown
The sapphire crystal of all size, makes stock utilization reach maximization.
Content of the invention
It is an object of the invention to provide a kind of a kind of growth apparatus of 200kg level sapphire crystal and growth technique, increase
The single crystal weight of sapphire crystal, effectively improves crystalline material utilization rate, solves 200kg level sapphire single-crystal and is giving birth to
Stress concentration, the larger problem of crystal stress can be easily produced in growth process.In addition, also there is seeding difficulty in 200kg level thermal field
Problem.In addition, want to lift the yield rate of 200kg level sapphire single-crystal, except needing thermal field reasonable in design, must also be more
Focus on the control to seeding form, by technology controlling and process, reduce the stress of crystals to greatest extent, reduce crystal defect.
A kind of growth apparatus of 200kg level sapphire crystal, including stainless steel cask 1,1 inner side of the stainless steel cask is provided with
Heat-insulation layer 2, is provided with circular tungsten cage heater, is provided with circle in the circle tungsten cage heating intracoelomic cavity in the heat-insulation layer 2
Crucible 5.
Further, the center of the heat-insulation layer 2 is that zirconia brick, outside is wrapped up by molybdenum sheet.
Further, the circle tungsten cage heater includes on sidepiece circular tungsten cage under circular tungsten cage heater 3 and sidepiece
Heater 4.
Further, on the sidepiece under circular tungsten cage heater 3 and sidepiece circular tungsten cage heater 4 for inlaying combination knot
Structure.
Further, the circle crucible 5 is supported by crucible supporting structure 8;Circle 5 upper end of crucible is provided with crucible
Lid 13, is placed with heat screen 14 on crucible cover.
Further, the crucible supporting structure 8 includes crucible pallet 10 and tungsten pillar 9, and crucible pallet 10 is placed in tungsten and props up
On post 9, crucible pallet 10 is contacted with the bottom of circular crucible 5, is arranged with the contact portion of circular crucible 5 in crucible pallet 10
There is zirconia coating.
Further, 5 lower section of circle crucible is provided with bottom heating element of tungsten 7, and 7 lower section of the bottom heating element of tungsten sets
It is equipped with the heat-insulation layer 6 that bottom molybdenum sheet wraps up zirconia brick structure.
Present invention also offers produce the growth technique of 200kg level sapphire crystal using above-mentioned growth apparatus, step is such as
Under:
(1), high voltage is risen, until the raw material in circular crucible melts;
(2), voltage being adjusted, bath surface convection current form stable in circular crucible is made, and the cold heart is made with circular crucible geometry
Center is deviateed less than 20mm;
(3), seeding, adjusts seed crystal position and is close to melt liquid level, while adjusting voltage, it is to avoid seed crystal is melted;Seed crystal
10~60min is preheated at its lower end with 2~10mm of melt liquid level, eliminate stress;
(4), lift, coordinate rotation, the speed of rotation is 0.2~10rpm;While adjusting the temperature to crystallization end to cover the cold heart
And start shouldering;
(5), shouldering, rises high voltage and promotes shouldering to complete, lower the temperature thereafter so that crystal growth shapes, during to growth end,
High voltage is risen again, so that crystal growth smoothly finishes up;
(6), reduce voltage until power supply is closed, crystal is cooled to 200-300 DEG C, and long crystalline substance terminates.
Growth apparatus and growth technique provided by the present invention for 200kg level sapphire crystal, its thermal field is evenly distributed
Stable, the crystal top bubble population for preparing is less.Also, this circle crucible thermal field can draw the reality of bar gauge lattice according to crystal
Need to design different length ratios, utilization rate of crystal height.
Description of the drawings
Fig. 1 is growth apparatus structural representation of the present invention;
In figure:1st, stainless steel cask;2nd, heat-insulation layer;3rd, circular tungsten cage heater on sidepiece;4th, circular tungsten cage heating under sidepiece
Body;5th, circular crucible;6th, bottom molybdenum sheet parcel zirconia brick heat-insulation layer 7,7- bottom heating element of tungsten;8- crucible supporting structure;9-
Tungsten pillar;10- crucible pallet;11st, 200kg level sapphire crystal;12nd, long crystalline substance seed crystal;13rd, crucible cover;14th, upper heat screen.
Specific embodiment
Embodiment one
As shown in figure 1, a kind of growth apparatus of 200kg level sapphire crystal, this equipment is thermal field structure of single crystal furnace, bag
Stainless steel cask 1 is included, 1 inner side of stainless steel cask is provided with molybdenum sheet parcel zirconia brick heat-insulation layer 2, in molybdenum sheet parcel zirconia brick guarantor
2 inner side of warm layer is provided with circular tungsten cage heater, including circular tungsten cage heater 3 and side on the sidepiece of upper and lower mosaic combined structure
Subordinate's circle tungsten cage heater 4, is provided with circular crucible 5 in the inner chamber of circular tungsten cage heater.Described lateral cross
For tetragon.
In the present embodiment, in order that its thermal field distribution is more uniform, on sidepiece described in the aspect ratio of the circle crucible 5
Circular 3 high 20cm of tungsten cage heater.
Under the sidepiece, the lower section of circular tungsten cage heater 4 is provided with bottom molybdenum sheet and wraps up zirconia brick heat-insulation layer 6, the bottom of at
Portion's molybdenum sheet wraps up the top of zirconia brick heat-insulation layer 6 and is provided with bottom heating element of tungsten 7.The circle crucible 5 is by the crucible of bottom
Supporting construction 8 is supported, and the crucible supporting structure 8 is made up of tungsten pillar 9 and crucible pallet 10, crucible pallet 10 and circular crucible
5 bottom contact, is provided with zirconia coating in crucible pallet 10 with the contact portion of circular crucible 5, and crucible pallet 10 is placed in
On tungsten pillar 9;Circle 5 upper end of crucible is provided with crucible cover 12, on crucible cover 12, is placed with heat screen 13.
The present invention additionally provides a kind of growth technique for producing 200kg sapphire crystal using above-mentioned growth apparatus simultaneously,
Step is as follows:
1st, high voltage is risen, until the raw material in circular crucible melts;
2nd, voltage is adjusted, makes bath surface convection current form stable in circular crucible, and make in the cold heart and circular crucible geometry
Heart positional deviation 15mm;
3rd, seeding, adjusts seed crystal position and is close to melt liquid level, while adjusting voltage, it is to avoid seed crystal is melted;Seed crystal exists
10min is preheated at its lower end and melt liquid level 2mm, eliminate stress;
4th, lift, coordinate rotation, the speed of rotation is 0.2rpm;While adjust the temperature to crystallization end and covering the cold heart and starting
Shouldering;
5th, shouldering, rises high voltage and promotes shouldering to complete, lower the temperature thereafter so that crystal is grown into shaping, to growth end
When, high voltage is risen so that crystal growth smoothly finishes up;
6th, reduce voltage until power supply is closed, crystal is cooled to 200 DEG C, and long crystalline substance terminates.
Embodiment two
Other are with embodiment one, and difference is, produce the growth of 200kg sapphire crystal using above-mentioned growth apparatus
Technique, step is as follows:
1st, high voltage is risen, until the raw material in circular crucible melts;
2nd, voltage is adjusted, makes bath surface convection current form stable in circular crucible, and make in the cold heart and circular crucible geometry
Heart positional deviation 10mm;
3rd, seeding, adjusts seed crystal position and is close to melt liquid level, while adjusting voltage, it is to avoid seed crystal is melted;Seed crystal exists
30min is preheated at its lower end and melt liquid level 5mm, eliminate stress;
4th, lift, coordinate rotation, the speed of rotation is 5rpm, while adjust the temperature to crystallization end and covering the cold heart and starting to put
Shoulder;
5th, shouldering, rises high voltage and promotes shouldering to complete, lower the temperature thereafter so that crystal is grown into shaping, to growth end
When, high voltage is risen so that crystal growth smoothly finishes up;
6th, reduce voltage until power supply is closed, crystal is cooled to 250 DEG C, and long crystalline substance terminates.
Embodiment three
1st, high voltage is risen, until the raw material in circular crucible melts;
2nd, voltage is adjusted, makes bath surface convection current form stable in circular crucible, and make in the cold heart and circular crucible geometry
Heart positional deviation 18mm;
3rd, seeding, adjusts seed crystal position and is close to melt liquid level, while adjusting voltage, it is to avoid seed crystal is melted.Seed crystal exists
60min is preheated at its lower end and melt liquid level 10mm, eliminate stress;
4th, lift, coordinate rotation, the speed of rotation is 10rpm;While adjust temperature crystallization end and covering the cold heart and starting to put
Shoulder;
5th, shouldering, rises high voltage and promotes shouldering to complete, lower the temperature thereafter so that crystal growth shapes, and during to growth end, rises
High voltage, so that crystal growth smoothly finishes up;
6th, reduce voltage until power supply is closed, crystal is cooled to 300 DEG C, and long crystalline substance terminates.
Prepare after 200kg level crystal and draw rod scheme and be adjusted to default further according to habit, in order to optimum
Change ground and utilize 200kg level sapphire crystal.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be defined by the scope of the claims.
Claims (8)
1. a kind of growth apparatus of 200kg level sapphire crystal, including stainless steel cask (1), it is characterised in that:The stainless steel cask
(1) heat-insulation layer (2) is provided with the inside of, is provided with circular tungsten cage heater, the circle tungsten cage heater in heat-insulation layer (2)
Circular crucible (5) is provided with inner chamber.
2. growth apparatus of a kind of 200kg level sapphire crystal according to claim 1, it is characterised in that:The insulation
The center of layer (2) is zirconia brick, and outside is wrapped up by molybdenum sheet.
3. growth apparatus of a kind of 200kg level sapphire crystal according to claim 1, it is characterised in that:The circle
Tungsten cage heater includes on sidepiece circle tungsten cage heater (4) under circular tungsten cage heater (3) and sidepiece.
4. growth apparatus of a kind of 200kg level sapphire crystal according to claim 3, it is characterised in that:The sidepiece
Under upper circle tungsten cage heater (3) and sidepiece, circular tungsten cage heater (4) is mosaic combined structure.
5. growth apparatus of a kind of 200kg level sapphire crystal according to claim 1, it is characterised in that:The circle
Crucible (5) is supported by crucible supporting structure (8);Circle crucible (5) upper end is provided with crucible cover (13), puts on crucible cover
It is equipped with heat screen (14).
6. growth apparatus of a kind of 200kg level sapphire crystal according to claim 5, it is characterised in that:The crucible
Supporting construction (8) includes crucible pallet (10) and tungsten pillar (9), and crucible pallet (10) is placed on tungsten pillar (9), crucible pallet
(10) contact with the bottom of circular crucible (5), in crucible pallet (10), the contact portion of circular crucible (5) is provided with zirconium oxide
Coating.
7. growth apparatus of a kind of 200kg level sapphire crystal according to claim 1, it is characterised in that:The circle
Bottom heating element of tungsten (7) is provided with below crucible (5), is provided with bottom molybdenum sheet parcel oxygen below bottom heating element of tungsten (7)
Change the heat-insulation layer (6) of zirconia block structure.
8. using a kind of 200kg level sapphire crystal growth equipment production 200kg level sapphire crystal described in claim 1-7
Production technology, step is as follows:
(1), high voltage is risen, until the raw material in circular crucible melts;
(2), voltage being adjusted, bath surface convection current form stable in circular crucible is made, and the cold heart is made with circular crucible geometric center
Positional deviation is less than 20mm;
(3), seeding, adjusts seed crystal position and is close to melt liquid level, while adjusting voltage, it is to avoid seed crystal is melted;Seed crystal is at which
10~60min is preheated at lower end and 2~10mm of melt liquid level, eliminate stress;
(4), lift, coordinate rotation, the speed of rotation is 0.2~10rpm;While adjust the temperature to crystallization end and covering the cold heart and opening
Beginning shouldering;
(5), shouldering, rises high voltage and promotes shouldering to complete, lower the temperature thereafter so that crystal growth shapes, and during to growth end, then rises
High voltage, so that crystal growth smoothly finishes up;
(6), reduce voltage until power supply is closed, crystal is cooled to 200-300 DEG C, and long crystalline substance terminates.
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CN201610716767.3A CN106435717A (en) | 2016-08-24 | 2016-08-24 | Growth equipment and growth technology for 200-kg sapphire crystals |
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CN201610716767.3A CN106435717A (en) | 2016-08-24 | 2016-08-24 | Growth equipment and growth technology for 200-kg sapphire crystals |
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CN105088333A (en) * | 2015-09-09 | 2015-11-25 | 华中科技大学 | Kyropoulos sapphire crystal growth furnace |
CN205934117U (en) * | 2016-08-24 | 2017-02-08 | 天通银厦新材料有限公司 | Growth equipment of 200kg level sapphire crystal |
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Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102051674A (en) * | 2011-01-20 | 2011-05-11 | 王楚雯 | Monocrystal ingot manufacturing device |
CN203007477U (en) * | 2012-12-13 | 2013-06-19 | 无锡鼎晶光电科技有限公司 | Structure of single-crystal furnace thermal field for growth of sapphire crystal |
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