CN104499045B - Kyropoulos-method sapphire crystal growth furnace - Google Patents
Kyropoulos-method sapphire crystal growth furnace Download PDFInfo
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- CN104499045B CN104499045B CN201410854713.4A CN201410854713A CN104499045B CN 104499045 B CN104499045 B CN 104499045B CN 201410854713 A CN201410854713 A CN 201410854713A CN 104499045 B CN104499045 B CN 104499045B
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Abstract
The invention discloses a kyropoulos-method sapphire crystal growth furnace which is used for overcoming the problem that manual intervention is needed for completing a shouldering process by the existing kyropoulos-method device, belonging to a crystal growth device. The kyropoulos-method sapphire crystal growth furnace comprises a furnace body, a crucible, a crucible cover, a furnace lid and a crystal seed rod, wherein a side wall thermal insulation layer and a bottom thermal insulation layer are laid in the furnace body; a side surface heater and a bottom heater are arranged in the crucible surrounding the furnace body, and a side reflecting screen, a bottom reflecting screen and an upper reflecting screen are arranged on the crucible; the crucible cover is formed by a top circular plate and a lower cylinder which are integrally connected, and the bottom end of the lower cylinder is a sunken curved surface. During working, the sunken curved surface of the crucible cover contacts with melt, so that the shouldering process can be simplified, and melt natural convection and flow caused by surface tension are inhibited. The kyropoulos-method sapphire crystal growth furnace is used, so that manual intervention is not needed for completing the shouldering process; thermal fields are reasonably controlled, so that an orientated solidification process and a shouldering process are unified, the quality of the sapphire single crystal is effectively improved, the crystal yield is remarkably increased, and the production cost is lowered.
Description
Technical field
The invention belongs to crystal growing apparatus, and in particular to a kind of kyropoulos sapphire crystal growing furnace.
Technical background
Kyropoulos, also known as Ky methods, are a kind of most popular large-size sapphire single-crystal bulk-growth methods at present, occupy current
The special sapphire of LED component substrate prepares the market of industry more than 80%, the method set vertical pulling method (Cz) and directional solidification
The technology elite of method (DS), crystal growth initial stage observable growth interface, using oriented seed technology, carry out seeding, necking down,
Shouldering etc. obtains the small crystals block of early stage；The crystal block as follow-up directional solidification seed crystal, follow-up growing technology main points be similar to
Directional solidification, but growth interface thermograde is more much smaller than directional solidification.It is relatively low that kyropoulos can obtain dislocation density
Large-size sapphire single-crystal (more than 100 kilograms), for the preparation of LED component industry upstream GaN film material, to provide cost performance excellent
Different sapphire substrate sheet.
Existing kyropoulos crystal growing apparatus is (true by heating system (heating, temperature control and insulation), atmosphere control system
Sky, gas circuit, inflation), transmission system (lifting, rotation), crucible, crucible cover etc. constitute, however, existing apparatus are to operating personnel's
Skill requirement is higher, it is impossible to be automatically performed shouldering process, needs artificial determination shouldering end time point, is easily caused shouldering and terminates
Time point selection is improper and causes occur a large amount of crystal defects during subsequent growth；In the public affairs of some shortages skilled operation personnel
Department, yield rate only has 20-50%.
Due to the importance of kyropoulos, the patent applied at present is more, the disclosure of Chinese patent application 2014101356386
A kind of kyropoulos prepare the growing method of sapphire single-crystal, contribute to solving to be deposited inside traditional kyropoulos growing sapphire monocrystalline
In the problem of more bubble.Chinese patent application 2014104652678 discloses a kind of kyropoulos sapphire single crystal growth furnace and protects
Warm side screen, contributes to reducing the thermal stress and dislocation density in crystal, reduces power consumption, improves crystal mass.Chinese patent Shen
2014102291482 a kind of seeding methods of kyropoulos sapphire crystal growth please be disclosed, be favorably improved product homogeneity.
However, these inventions can not overcome existing kyropoulos grower to automatically determine shouldering end time point, need manually
Intervention completes the defect of shouldering process.
The content of the invention
The present invention provides a kind of kyropoulos sapphire crystal growing furnace, and overcoming cannot be automatically true using existing kyropoulos device
Determine shouldering end time point, need manual intervention to complete the problem of shouldering process, can not only effectively improve system stability, can
By property and repeatability, it is also possible to save growth cost, improve the quality and yield rate of sapphire single-crystal.
A kind of kyropoulos sapphire crystal growing furnace provided by the present invention, including body of heater, crucible, crucible cover, bell and
Seed rod；The body of heater is the cylinder of bottom end closure, and around inboard wall of furnace body side wall heat-insulation layer is laid with, and body of heater inner bottom part is laid with
Bottom heat-insulation layer；The crucible for bottom end closure cylinder, crucible bottom is placed on half-set, half-set by flat board and
Be fixed on planar bottom surface center pole constitute, the pole vertical support on the heat-insulation layer of bottom, during the crucible cover has
Heart through hole, is covered in crucible top, and the bell is disc, and with outlet duct, top heat-insulation layer is laid in bell bottom surface；Work
Bell is covered in the top of the body of heater when making, and the seed rod upper end is through top heat-insulation layer and the venthole of the bell
The central through hole of the crucible cover is stretched in road, seed rod lower end, and seed rod lower surface is placed with seed crystal, seed crystal contact bath surface；
It is characterized in that：
The crucible cover is rotary body, is coaxially connected as a single entity by top disc and lower cylindrical and is constituted, the top disc
Center has the central through hole for axially penetrating through top disc and lower cylindrical；Lower cylindrical has ring with top disc coupling part
Connected in star, the bottom of lower cylindrical is inner sunken face, the monocrystalline that the inner sunken face is produced with the stove in the case of without crucible cover
Sapphire crystal ingot top curve surface shape is consistent, presents smooth streamlined；
Around the crucible, side heater is provided with, its profile is cylindrical shape, top insulation is hung on by support bar
Layer bottom；Bottom heater is set around pole below the flat board of the half-set, its profile is annular, by propping up
Strut is fixed on the flat board bottom of half-set；
Lateral reflection screen is provided between the side heater and the side wall heat-insulation layer, the lateral reflection screen is cylinder
Shape, is made up of 5～10 layers of coaxial cylinders nesting, and by support bar side wall heat-insulation layer inner side is fixed on；The bottom heater and
Bottom reflection screen is set around pole between the bottom heat-insulation layer, the bottom reflection screen is annular, same by 5 layers～10 layers
Heart annulus stacking is constituted, and is fixed on the heat-insulation layer of bottom by support bar；
The crucible cover top, around seed rod top radiation shield is provided with, and the top radiation shield is annular, by 5
～10 layers of donut stacking are constituted, and are hung under the heat-insulation layer of top by support bar；
During work, the top disc of crucible cover is ridden over above crucible, as support, and plays a part of to be incubated liquation；Under
The inner sunken face of portion cylinder bottom is contacted with liquation, and the inner sunken face can simplify shouldering process, i.e., when growing on seed rod
Centered on the size of clear size of opening 3/4 crystal when, now seed rod stop lifting, directional solidification is directly entered, by temperature field
Regulation and control make crystal grow downwards along the curved-surface natural, until shouldering process is automatically performed, while shouldering process is simplified, it is to avoid
Crystal growth caused by artificial selection shouldering end time (being switched to the time of directional solidification in i.e. common growth furnace by lifting)
Failure problem；Play a part of the flowing for suppressing liquation free convection and surface tension to cause simultaneously.
The inner sunken face of the crucible cover lower cylindrical bottom, can be generated by following step：
A, in the case of without crucible cover, sapphire crystal ingot is produced using the body of heater, whether detect the sapphire crystal ingot
For monocrystalline sapphire crystal ingot, it is, carries out step B；Otherwise sapphire crystal ingot is produced again by adjustment shouldering technique, it is so anti-
Multiple operation carries out step B up to monocrystalline sapphire crystal ingot is finally given；
Whether B, the defect concentration of detection monocrystalline sapphire crystal ingot, impurity content and distribution are satisfied by product quality requirement,
It is to carry out step C；Otherwise return to step A；
C, monocrystalline sapphire crystal ingot will be obtained die will be obtained Jing after reverse mould, after the molding surface is polished flat, is polished,
Again punch is obtained after reverse mould, using the punch inner sunken face of the crucible cover lower cylindrical bottom is manufactured.
The side heater and bottom heater, can be made up of molybdenum or tungsten material；
The material of the side wall heat-insulation layer, bottom heat-insulation layer and top heat-insulation layer can press quality by zirconium oxide, aluminum oxide
Than 1:4～1:20 are mixed；
The material of the lateral reflection screen, bottom reflection screen and top radiation shield can adopt metal molybdenum；
The crucible cover can be made with crucible using identical material of tungsten, it is to avoid the complication of liquation polluter.
The present invention includes common crucible and special crucible cover, and crucible cover top is ridden over above crucible, as support, and
Play a part of to be incubated liquation.Special inner sunken face is made in crucible cover bottom, the shape of the inner sunken face by optimization, and most
Suitable sapphire crystal ingot outer shape is consistent, presents smooth streamlined.Bottom invade crucible liquation in, crystal growth each
Stage provides and the harmonious growing environment of crystal shape, while shouldering is limited, also functions to suppress liquation free convection
The effect of the flowing caused with surface tension.
The side heater and bottom heater disclosure satisfy that 2300 DEG C of high temperature above heating requirements；Seeding, stable state life
Long and cooling procedure requires that side heater and bottom heater have corresponding power curve matching, crucible and crucible cover
Requirement has suitable heater power curve matching, so as to the distribution of regulating and controlling temperature field in process of production, side heat
The power regulation of device and bottom heater is related to body of heater size and concrete production process, needs by early stage numerical simulation and body of heater
After the completion of manufacture obtained by test adjustment.
The heat-insulation system of the present invention is made up of heat-insulation layer and radiation shield, and their setting is matched with crucible structure, on the one hand
With reduces cost, the reliability and stability of system can be on the other hand improved.
Using kyropoulos sapphire crystal growing furnace provided by the present invention, shouldering process is completed without the need for manual intervention, led to
Thermal field is controlled after rationally, directional solidification process can be united with shouldering process, effectively improve the quality of sapphire single-crystal,
And crystal yield rate is significantly improved, production cost is reduced, so as to realize high efficiency growth prepared by large-size sapphire single-crystal.
Description of the drawings
Fig. 1 is the structural representation of the present invention；
Fig. 2 is crucible cover schematic diagram.
Specific embodiment
Below in conjunction with drawings and Examples, the present invention is further described.It should be appreciated that described herein be embodied as
Example is not intended to limit the present invention only to explain the present invention.
As shown in Figure 1 and Figure 2, the present invention includes body of heater 1, crucible 2, crucible cover 3, bell 4 and seed rod 5；The body of heater 1
For the cylinder of bottom end closure, side wall heat-insulation layer 6 is laid with around inboard wall of furnace body, body of heater inner bottom part is laid with bottom heat-insulation layer 7；Institute
The cylinder that crucible 2 is bottom end closure is stated, the bottom of crucible 2 is placed on half-set 8, half-set 8 is by flat board and is fixed on flat
The pole of plate bottom center is constituted, and on bottom heat-insulation layer 7, the crucible cover 3 has central through hole to the pole vertical support,
The top of crucible 2 is covered in, the bell 4 is disc, and its center has outlet duct, and top heat-insulation layer 9 is laid in bell bottom surface；
Bell 4 is covered in the top of the body of heater 1 during work, and the upper end of the seed rod 5 goes out through top heat-insulation layer 9 and the bell
The central through hole of the crucible cover 3 is stretched in pore road, seed rod lower end, contacts bath surface；
The crucible cover 3 is rotary body, is coaxially connected as a single entity by top disc 3-1 and lower cylindrical 3-2 and is constituted, the top
Portion disk 3-1 centers have the central through hole 3-1A for axially penetrating through top disc 3-1 and lower cylindrical 3-2；Lower cylindrical 3-2 with
Top disc 3-1 coupling part has an annular groove 3-2A, and the bottom of lower cylindrical 3-2 is inner sunken face 3-2B, the indent
Curved surface 3-2B is consistent with the monocrystalline sapphire crystal ingot top curve surface shape that the stove is produced in the case of without crucible cover, and light slip-stream is presented
Line style；
Around the crucible, side heater 10 is provided with, its profile is cylindrical shape, top is hung on by support bar and is protected
The bottom of warm layer 9；Bottom heater 11 is set around pole below the flat board of the half-set 8, its profile is annular,
The flat board bottom of half-set 8 is fixed on by support bar；
Lateral reflection screen 12, the lateral reflection screen 12 are provided between the side heater 10 and the side wall heat-insulation layer 6
For cylindrical shape, it is made up of 5～10 layers of coaxial cylinders nesting, the inner side of side wall heat-insulation layer 6 is fixed on by support bar；The bottom adds
Bottom reflection screen 13 is set around pole between hot device 11 and the bottom heat-insulation layer 7, the bottom reflection screen 13 is annular,
It is made up of 5 layers～10 layers donut stacking, is fixed on bottom heat-insulation layer 7 by support bar；
The top of the crucible cover 3, around seed rod top radiation shield 14 is provided with, and the top radiation shield 14 is annulus
Shape, is made up of 5～10 layers of donut stacking, is hung under the heat-insulation layer 9 of top by support bar；
During work, top disc 3-1 of crucible cover 3 is ridden over above crucible, as support, and plays the work of insulation liquation
With；The inner sunken face 3-2B of lower cylindrical 3-2 bottom is contacted with liquation, and the inner sunken face can simplify shouldering process, while rising
To the effect of the flowing for suppressing liquation free convection and surface tension to cause.
In embodiments of the invention：
The side heater 10 is that cylinder heater is made in the coiling of tungsten wire, and power can in 0～300KW scopes
Adjust；
The bottom heater 11 is that disc heater is made in the coiling of tungsten wire, and power is adjustable in 0～80KW scopes；
The material of the side wall heat-insulation layer 6, bottom heat-insulation layer 7 and top heat-insulation layer 9 by zirconium oxide, aluminum oxide in mass ratio
1：9 are mixed；
The material of the lateral reflection screen 12, bottom reflection screen 13 and top radiation shield 14 is by high reflectance, high-melting-point, Gao Wen
Qualitatively metal molybdenum is made；
The crucible cover 3 is made up with crucible 2 of identical material of tungsten.
Implement the czochralski method techniques such as seeding, necking down using the present invention is carried out in the little space in the top of crucible cover 3, in order to ensure have
Enough gradients, the internal water cooling speed in seed rod 5 will be accelerated.Peep hole can be arranged on higher position, convenient to overlook
Seed rod top；
Seeding reaches 3/4 visible molten surface (being located at the middle and upper part of crucible cover 3), you can to start directional solidification control, this
When, crystal grows downwards naturally along crucible cover lower curved face, until being automatically performed shouldering process.
During steady-state growth, the power of side heater 10 and bottom heater 11 is controlled, liquation inside temperature is maintained as far as possible
The uniformity of degree field；The power of side heater 10 first declines on the basis of the heating power of original steady-state growth during cooling
10%-20%, restarts bottom heater 11, and Jing test of many times determines after bottom heater is completed by the manufacture of this device
Power curve is gradually reduced heating power, until completing directional solidification process.
Claims (4)
1. a kind of kyropoulos sapphire crystal growing furnace, including body of heater (1), crucible (2), crucible cover (3), bell (4) and seed crystal
Bar (5)；The body of heater (1) is the cylinder of bottom end closure, and around inboard wall of furnace body side wall heat-insulation layer (6), body of heater inner bottom part are laid with
It is laid with bottom heat-insulation layer (7)；The crucible (2) for bottom end closure cylinder, crucible (2) bottom is placed in half-set (8)
On, half-set (8) is made up of flat board with the pole for being fixed on planar bottom surface center, and the pole vertical support is protected in bottom
On warm layer (7), the crucible cover (3) is covered in crucible (2) top with central through hole, and the bell (4) is disc, tool
There is outlet duct, top heat-insulation layer (9) is laid in bell bottom surface；Bell (4) is covered in the top of the body of heater (1), institute during work
Seed rod (5) upper end is stated through top heat-insulation layer (9) and the outlet duct of the bell (4), the earthenware is stretched in seed rod lower end
The central through hole of crucible lid (3), seed rod lower surface is placed with seed crystal, seed crystal contact bath surface；
It is characterized in that：
The crucible cover (3) is rotary body, is coaxially connected as a single entity and is constituted by top disc (3-1) and lower cylindrical (3-2), described
Top disc (3-1) center has the central through hole (3-1A) for axially penetrating through top disc (3-1) and lower cylindrical (3-2)；Under
Portion's cylinder (3-2) has annular groove (3-2A) with top disc (3-1) coupling part, and the bottom of lower cylindrical (3-2) is interior
Concave curved surface (3-2B), at the top of the monocrystalline sapphire crystal ingot that the inner sunken face (3-2B) produces with the stove in the case of without crucible cover
Curve form is consistent, presents smooth streamlined；
Around the crucible, side heater (10) is provided with, its profile is cylindrical shape, and by support bar top insulation is hung on
Layer (9) bottom；Bottom heater (11) is set around pole in the flat board lower section of the half-set (8), its profile is annulus
Shape, by support bar the flat board bottom of half-set (8) is fixed on；
Lateral reflection screen (12), the lateral reflection screen are provided between the side heater (10) and the side wall heat-insulation layer (6)
(12) it is cylindrical shape, is made up of 5～10 layers of coaxial cylinders nesting, side wall heat-insulation layer (6) inner side is fixed on by support bar；It is described
Bottom reflection screen (13), the bottom reflection are set around pole between bottom heater (11) and the bottom heat-insulation layer (7)
Screen (13) is annular, is made up of 5 layers～10 layers donut stacking, is fixed on bottom heat-insulation layer 7 by support bar；
Crucible cover (3) top, around seed rod top radiation shield (14) is provided with, and the top radiation shield (14) is annulus
Shape, is made up of 5～10 layers of donut stacking, is hung under top heat-insulation layer (9) by support bar；
During work, the top disc (3-1) of crucible cover (3) is ridden over above crucible, as support, and plays the work of insulation liquation
With；The inner sunken face (3-2B) of lower cylindrical (3-2) bottom is contacted with liquation, and the inner sunken face can simplify shouldering process, together
When play a part of the flowing that suppresses liquation free convection and surface tension to cause.
2. kyropoulos sapphire crystal growing furnace as claimed in claim 1, it is characterised in that：
The inner sunken face (3-2B) of crucible cover (3) lower cylindrical (3-2) bottom, is generated by following step：
A, in the case of without crucible cover, sapphire crystal ingot is produced using the body of heater, detect whether the sapphire crystal ingot is single
Brilliant sapphire crystal ingot, is to carry out step B；Otherwise sapphire crystal ingot is produced again by adjustment shouldering technique, so grasped repeatedly
Make, up to monocrystalline sapphire crystal ingot is finally given, to carry out step B；
Whether B, the defect concentration of detection monocrystalline sapphire crystal ingot, impurity content and distribution are satisfied by product quality requirement, are then
Carry out step C；Otherwise return to step A；
C, monocrystalline sapphire crystal ingot will be obtained die will be obtained Jing after reverse mould, to molding surface polishing, polishing after, reverse mould again
After obtain punch, manufacture the inner sunken face (3-2B) of crucible cover (3) lower cylindrical (3-2) bottom using the punch.
3. kyropoulos sapphire crystal growing furnace as claimed in claim 1 or 2, it is characterised in that：
The side heater (10) and bottom heater (11), are made up of molybdenum or tungsten material.
4. kyropoulos sapphire crystal growing furnace as claimed in claim 3, it is characterised in that：
The material of the side wall heat-insulation layer (6), bottom heat-insulation layer (7) and top heat-insulation layer (9) presses quality by zirconium oxide, aluminum oxide
Than 1:4～1:20 are mixed；
The material of the lateral reflection screen (12), bottom reflection screen (13) and top radiation shield (14) adopts metal molybdenum；
The crucible cover (3) is made with crucible (2) using identical material of tungsten.
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| CN201410854713.4A CN104499045B (en) | 2014-12-31 | 2014-12-31 | Kyropoulos-method sapphire crystal growth furnace |
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| CN201410854713.4A CN104499045B (en) | 2014-12-31 | 2014-12-31 | Kyropoulos-method sapphire crystal growth furnace |
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| CN104499045B true CN104499045B (en) | 2017-04-19 |
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| CN105088333A (en) * | 2015-09-09 | 2015-11-25 | 华中科技大学 | Kyropoulos sapphire crystal growth furnace |
| CN105463565A (en) * | 2015-11-25 | 2016-04-06 | 四川神光石英科技有限公司 | Quartz glass melting furnace |
| CN106119963A (en) * | 2016-02-03 | 2016-11-16 | 江苏浩瀚蓝宝石科技有限公司 | The impact on thermal field of a kind of kyropoulos sapphire single-crystal furnace heat shielding |
| CN105926041A (en) * | 2016-05-05 | 2016-09-07 | 中国科学院合肥物质科学研究院 | Supporting device for crucible used in crystal growth of super-high temperature melt method |
| CN105887197A (en) * | 2016-05-05 | 2016-08-24 | 中国科学院合肥物质科学研究院 | Crystal growing device of rare earth sesquioxide by Czochralski method |
| CN106435729A (en) * | 2016-10-09 | 2017-02-22 | 英利能源（中国）有限公司 | Seeding and shoulder expanding device and technique for single crystal rods and single crystal furnace |
| CN107300321B (en) * | 2017-07-21 | 2023-10-13 | 中联精工（天津）有限公司 | Crucible furnace for die castings |
| CN109797427A (en) * | 2019-03-27 | 2019-05-24 | 石河子市鑫磊光电科技有限公司 | A kind of KY method Sapphire Crystal Growth suspension type crucible cover and KY method Sapphire Crystal Growth device for adjusting height immediately |
| CN112501686A (en) * | 2019-09-16 | 2021-03-16 | 新疆紫晶光电技术有限公司 | Thermal field device for sapphire growth by kyropoulos method |
| CN111850687A (en) * | 2020-07-22 | 2020-10-30 | 哈尔滨秋硕半导体科技有限公司 | Crucible cover structure for sapphire single crystal furnace by kyropoulos method |
| CN111850688A (en) * | 2020-07-22 | 2020-10-30 | 哈尔滨秋硕半导体科技有限公司 | Cooling device for inhibiting shoulder shrinkage of sapphire single crystal by kyropoulos method |
| CN113550008B (en) * | 2021-07-14 | 2023-06-23 | 山东恒元半导体科技有限公司 | Device and method for growing oversized lithium niobate crystal |
| CN113970243A (en) * | 2021-10-14 | 2022-01-25 | 中国科学院沈阳科学仪器股份有限公司 | Thin-wall heat-insulating layer structure of beam source furnace |
| CN114108075B (en) * | 2021-11-12 | 2023-08-04 | 赣州海盛钨业股份有限公司 | Tungsten alloy protective cover for sapphire growth by kyropoulos method |
| CN116949562B (en) * | 2023-09-19 | 2024-02-13 | 内蒙古晶环电子材料有限公司 | Sapphire crystal growth furnace |
| CN116926661B (en) * | 2023-09-19 | 2024-02-06 | 内蒙古晶环电子材料有限公司 | Sapphire crystal growth furnace and sapphire crystal growth method |
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