CN104250852A - Sapphire crystal growth device and growth method - Google Patents
Sapphire crystal growth device and growth method Download PDFInfo
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- CN104250852A CN104250852A CN201410470974.6A CN201410470974A CN104250852A CN 104250852 A CN104250852 A CN 104250852A CN 201410470974 A CN201410470974 A CN 201410470974A CN 104250852 A CN104250852 A CN 104250852A
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- 239000013078 crystal Substances 0.000 title claims abstract description 136
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 115
- 239000010980 sapphire Substances 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims description 39
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 43
- 239000010959 steel Substances 0.000 claims abstract description 43
- 238000001816 cooling Methods 0.000 claims abstract description 18
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 38
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 32
- 238000009413 insulation Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052721 tungsten Inorganic materials 0.000 claims description 14
- 239000010937 tungsten Substances 0.000 claims description 14
- 239000000112 cooling gas Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 230000005855 radiation Effects 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000000523 sample Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 235000015895 biscuits Nutrition 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002109 crystal growth method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000002015 acyclic group Chemical group 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- -1 quality and cost Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- 230000008646 thermal stress Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a sapphire crystal growth device and a sapphire crystal growth method. The sapphire crystal growth device comprises a furnace body and a vacuumizing device; the furnace body is an openable and closeable furnace body; the vacuumizing device is communicated with the inside of the furnace body; a steel cage is arranged inside the furnace body; the steel cage is of a structure with upper and lower openings; an upper insulating layer is arranged at the upper opening of the steel cage; a bottom insulating layer is arranged at the lower opening of the steel cage; a side insulating layer is arranged on the inner surface of the steel cage; a base is arranged inside the steel cage; a crucible is placed on the base; a lifting device is arranged at the top of the furnace body; the lifting device is connected with the steel cage through a connecting rod; a conical or circular-arc-shaped counter bore is formed in the upper surface of the base; the bottom surface of the crucible is a conical surface or circular-arc-shaped surface matched with the conical or circular-arc-shaped counter bore in shape; side heaters are arranged on the side surfaces of the crucible and/or top heaters are arranged above the crucible. A center hole is formed in the center of the base and can be filled with gas to carry out cooling on seed crystals and promote crystal growth. The device disclosed by the invention has the advantages that sapphire crystal production cycle is relatively short, the effective utilization rate of the sapphire crystals is high and the cost is relatively low.
Description
Technical field
The present invention relates to a kind of sapphire crystal growth device and growth method.
Background technology
Sapphire (Sapphire) is a kind of aluminum oxide (α-Al
2o
3) monocrystalline, be also called corundum, have excellent mechanical property, chemical stability and optical property.Sapphire crystal hardness is very high, is only second to diamond, has good wear resistance, and physical strength is high simultaneously, can bear very large load; Sapphire chemical property is very stable, the corrosion of general acid and alkali alkali, not easily deliquescence, and working temperature can reach 2000 DEG C, can work under extremely rugged environment for a long time; It is very wide that sapphire optics penetrates band scope, good translucidus is had near ultraviolet band to middle-infrared band, sapphire is also excellent laser host material simultaneously, has very wide tunable scope and very high gain, is widely used in LED illumination industry and military window material.
In recent years, along with smart mobile phone, extensively popularizing of the touch screen type consumption electronic products such as panel computer, sapphire can be widely used as the panel of electronic product.Sapphire optical perviousness is good, and wear resistance is good, not easily broken, has the possibility replacing glass.
Meanwhile, along with the development of modern science and technology, constantly propose new requirement to the size of sapphire crystal material, quality and cost, sapphire substrate is also towards large size simultaneously, high quality, the future development of low cost.Due to mobile phone, computer etc. belong to quick consumer electronics product, and require that price is not high, but demand is huge, the panel required for it also has identical characteristics, therefore need sapphire as panel work material, and need output large, cost is low.
Sapphire existing main growth methods has crystal pulling method (Cz), kyropoulos (Ky), heat-exchanging method (HEM), reverse mould method (EFG) and Horizontal Bridgman method, and wherein kyropoulos and heat-exchanging method are the main method of current growing large-size sapphire crystal.
The process of heat-exchanging method growing sapphire crystal is exactly the process of a simple melt crystallographic orientation.Existing method is: in the body of heater of sealing, around crucible, arrange well heater, is melted by the alumina raw material producing sapphire crystal by regulating heater power; Crucible is placed on pedestal, and base bottom controls seed crystal by the flow of heat-eliminating medium circulation helium and is not melted and the further growth of crystal, and in process of growth, crucible, seed crystal all keep static.
In traditional heat-exchanging method growing sapphire crystal process, be not melted to control seed crystal, the major measure taked is, is lowered the temperature by heat-eliminating medium helium in base bottom to seed crystal, wherein heat-eliminating medium helium adopts the radiating mode of circulation, and radiating effect is poor; Secondly, because recuperated gas requires high flow rate, pipeline is all thinner, internal diameter is in 8 millimeter, and the initial temperature of the cold helium passed into is generally room temperature, and the temperature of hot helium is out about 1000 DEG C, heat is limited, only there is 3 ~ 5KW, therefore, for the further large-sized sapphire crystal of growth, growth velocity is slow, growth cycle is longer, and generally need about 17 ~ 19 days, cost is higher.
Simultaneously, pedestal is plane with the contact surface of the crucible placing seed crystal, and heat interchanging area is less, is unfavorable for that crucible dispels the heat, because this caloric requirement is exchanged by very little heat interchanging area, the heat flow density in this region is very high, and cause the localized temperature gradients of sapphire seed crystal above this heat-transfer surface very large, thermal stresses is bigger than normal, the inner easily pressurized of seed crystal forms the defects such as dislocation, defect is propagated to crystals, and then affects crystal mass, and wherein the effective rate of utilization of sapphire crystal is about 35%.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the deficiency of above-mentioned background technology, provides higher, the lower-cost sapphire crystal growth device of effective rate of utilization that is shorter, sapphire crystal of a kind of production cycle and growth method.
The technical scheme that the present invention solves the employing of its technical problem is that a kind of sapphire crystal growth device, comprises body of heater and vacuum extractor, and described body of heater is opening and closing type body of heater, and described vacuum extractor is communicated with furnace interior; Described furnace interior is provided with steel cage, and steel cage is the structure of upper and lower opening, and upper shed place of steel cage is provided with thermal insulation layer, and lower opening is provided with end thermal insulation layer, and the internal surface of steel cage is provided with side thermal insulation layer; The inside of steel cage is provided with pedestal, and pedestal is placed with crucible, and the top of described body of heater is provided with lifting device, and described lifting device is connected with steel cage by union lever; The upper surface of described pedestal is provided with taper or circular arc counterbore, the bottom shape of described crucible in taper or the suitable conical surface of circular arc counterbore shape or arc surface, the side of described crucible is provided with side well heater and/or top is provided with heater top.
Further, the surface of described taper or circular arc counterbore is provided with air slot, the quantity of air slot preferably >=2, more preferably 6 ~ 20, described air slot in taper or circular arc counterbore surrounding along divergent shape.
Further, the width of described air slot is 3 ~ 20mm, and the degree of depth is 0.1 ~ 20mm.
Further, the width of described air slot is 5 ~ 10mm, and the degree of depth is 0.5 ~ 5mm.
Further, describedly one deck conductive graphite paper between crucible and pedestal, is lined with.
Further, the center of described pedestal and the center of end thermal insulation layer are equipped with centre hole.
Further, be also provided with external admission air-cooling apparatus, external admission air-cooling apparatus comprises source of the gas, valve, external feed stream pipe, bottom inflow pipe, and source of the gas is connected by the first pipe connecting with valve; Valve is connected with external feed stream pipe, is provided with under meter between valve and external feed stream pipe, is connected between under meter with valve by the second pipe connecting; External feed stream pipe is connected with bottom inflow pipe, and the junction of bottom inflow pipe and external feed stream pipe is provided with sleeve pipe, and bottom inflow pipe, through the centre hole of end thermal insulation layer and the centre hole of pedestal, extend into below crucible bottom.
A growth method for sapphire crystal, utilizes described sapphire crystal growth device to carry out, specifically comprises the following steps:
(1) sapphire seed crystal is placed: lay sapphire seed crystal in crucible bottom, make sapphire seed crystal be positioned at directly over bottom inflow pipe;
(2) feed: high purity aluminium oxide raw material is put into crucible, close body of heater;
(3) vacuumize: start vacuum extractor, the pressure in body of heater is evacuated to below 3Pa;
(4) material is heated: start side well heater or/and heater top, make the temperature in steel cage rise to 2050 ~ 2150 DEG C, high purity aluminium oxide raw material starts fusing; With the position of solid-liquid interface in tungsten tipped probe detection crucible, determine whether sapphire seed crystal starts to melt, when sapphire seed crystal starts to melt, start external admission air-cooling apparatus, cooling gas is passed into crucible bottom, until sapphire seed crystal is partially melted with the flow velocity of 10 ~ 200L/min;
(5) crystal growth: by the elevated height 1 ~ 350mm of lifting device by steel cage, steel cage is separated with end thermal insulation layer, and then makes pedestal be exposed in body of heater, the outside heat loss through radiation of pedestal, reduce the temperature near crucible bottom sapphire seed crystal, sapphire seeded growth; Cooling gas is passed into crucible bottom, until the whole crystallization of melt in crucible with the flow velocity of 10 ~ 50L/min;
(6) annealing cooling: steel cage is promoted to extreme higher position by lifting device; Cooling gas is passed into crucible bottom, until the crystal in crucible 8 is cooled to room temperature with the flow velocity of 10 ~ 100L/min;
(7) come out of the stove: be down to after below 400 DEG C until the temperature in body of heater, open body of heater, take out crystal.
Further, high purity aluminium oxide raw material described in step (2), (4) is any one or a few in alumina powder, aluminum oxide biscuit, alumina block material.
Further, crucible described in step (1), (2), (4), (5), (6) is any one in tungsten crucible, molybdenum crucible, iridium crucible.
Further, described in step (4), (5), (6), cooling gas is argon gas.
Compared with prior art, advantage of the present invention is as follows:
(1) upper surface of pedestal is provided with taper or circular arc counterbore, the bottom shape of crucible in taper or the suitable conical surface of circular arc counterbore shape or arc surface, can effective increasing heat radiation area; Steel cage can promote by lifting device, and steel cage is separated with end thermal insulation layer, and then makes pedestal be exposed in body of heater, the heat loss through radiation amount of pedestal is comparatively large, and reach the thermograde required for crystal growth, the speed of growth of crystal is very fast, growth cycle is shorter, growth cycle can be shortened 3 ~ 5 days; The crystal mass of growth is better, and the effective rate of utilization of sapphire crystal can be increased to 36% ~ 37%, the growth cost of crystal is lower.
(2) taper of pedestal or the surface of circular arc counterbore are provided with air slot, and air slot is conducive to airflow, form airflow radiating, are conducive to the thermograde reached required for crystal growth.
(3) external admission air-cooling apparatus and vacuum extractor is provided with, cooling gas (as argon gas) is passed in crucible bottom by external admission air-cooling apparatus, crucible is dispelled the heat, cooling gas flows in body of heater after taking away the heat of crucible, then the cooling gas in vacuum extractor extraction body of heater is utilized, make cooling gas form acyclic radiating mode, radiating effect is better.
Accompanying drawing explanation
Fig. 1 is the structural representation of sapphire crystal growth device embodiment of the present invention.
Fig. 2 is the vertical view of pedestal embodiment illustrated in fig. 1.
Fig. 3 is partial enlarged drawing embodiment illustrated in fig. 1.
Fig. 4 is the view after steel cage embodiment illustrated in fig. 1 promotes.
In figure: 1-lifting device, 2-union lever, 3-steel cage, 4-upper thermal insulation layer, 5-heater top, 6-side well heater, 7-side thermal insulation layer, 8-crucible, 9-sapphire seed crystal, 10-pedestal, 11-end thermal insulation layer, 12-bottom inflow pipe, 13-air slot, 14-body of heater, 15-centre hole.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Embodiment 1
With reference to Fig. 1, sapphire crystal growth device embodiment of the present invention comprises body of heater 14, vacuum extractor and external admission air-cooling apparatus, and vacuum extractor is communicated with body of heater 14 inside; Body of heater 14 is opening and closing type body of heater, and the top of body of heater 14 is provided with lifting device 1, and body of heater 14 inside is provided with steel cage 3, and lifting device 1 is connected with steel cage 3 by union lever 2; The structure of steel cage 3 in upper and lower opening, upper shed place of steel cage 3 is provided with thermal insulation layer 4, and lower opening is provided with end thermal insulation layer 11, and the internal surface of steel cage 3 is provided with side thermal insulation layer 7; The inside of steel cage 3 is provided with pedestal 10, with reference to Fig. 2, Fig. 3, the upper surface of pedestal 10 is provided with taper or circular arc counterbore, the surface of taper or circular arc counterbore is provided with 2 air slots 13, air slot 13 is along divergent shape in taper or circular arc counterbore surrounding, the width of air slot 13 is 20mm, and the degree of depth is 20mm; The center of pedestal 10 and the center of end thermal insulation layer 11 are equipped with centre hole 15; With reference to Fig. 1, pedestal 10 being placed with crucible 8, in order to make crucible 8 and pedestal 10 can sharp separation, between crucible 8 and pedestal 10, being lined with one deck conductive graphite paper, the bottom shape of crucible 8 in taper or the suitable conical surface of circular arc counterbore or arc surface, the side of crucible 8 is provided with side well heater 6.
External admission air-cooling apparatus comprises source of the gas, valve, external feed stream pipe, bottom inflow pipe 12, and source of the gas is connected by the first pipe connecting with valve; Valve is connected with external feed stream pipe, is provided with under meter between valve and external feed stream pipe, is connected between under meter with valve by the second pipe connecting; External feed stream pipe is connected with bottom inflow pipe 12, and bottom inflow pipe 12 is provided with sleeve pipe with the junction of external feed stream pipe, and bottom inflow pipe 12, through the centre hole 15 of end thermal insulation layer 11 and the centre hole 15 of pedestal 10, extend into crucible 8 bottom part down.
The growth method embodiment of sapphire crystal of the present invention comprises the following steps:
(1) place sapphire seed crystal: bottom tungsten crucible, lay diameter is 20mm, the sapphire seed crystal 9 of height 10mm, makes sapphire seed crystal 9 be positioned at directly over bottom inflow pipe 12;
(2) feed: the alumina powder of 100 kilograms is put into tungsten crucible, close body of heater 14;
(3) vacuumize: start vacuum extractor, the pressure in body of heater 14 is evacuated to 2Pa;
(4) heat material: start side well heater 6, make the temperature in steel cage 3 rise to 2050 DEG C, alumina powder starts fusing; With the position of solid-liquid interface in tungsten tipped probe detection tungsten crucible, determine whether sapphire seed crystal 9 starts to melt, when probe starts to melt to sapphire seed crystal 9, start external admission air-cooling apparatus, bottom tungsten crucible, argon gas is passed into, until sapphire seed crystal 9 is only partially melted with the flow velocity of 100L/min;
(5) crystal growth: with reference to Fig. 4, by the elevated height 1 ~ 350mm of lifting device 1 by steel cage 3, steel cage 3 is separated with end thermal insulation layer 11, and then make pedestal 10 be exposed in body of heater 14, pedestal 10 is heat loss through radiation outwards, reduce the temperature near sapphire seed crystal 9 bottom tungsten crucible, sapphire seed crystal 9 grows; Bottom tungsten crucible, argon gas is passed into, until the whole crystallization of melt in tungsten crucible with the flow velocity of 20L/min;
(6) annealing cooling: steel cage 3 is promoted to extreme higher position by lifting device 1; Bottom tungsten crucible, argon gas is passed into, until the crystal in tungsten crucible is cooled to room temperature with the flow velocity of 50L/min;
(7) come out of the stove: after the temperature in body of heater 14 is down to 200 DEG C, open body of heater 14, take out crystal, the weight obtaining crystal is 100 kilograms.
After the thermal field components such as argon gas and pedestal 10 complete fluid interchange, be directly expelled to outside body of heater 14 by vacuum extractor, form the acyclic radiating mode of gas cooling, compared with traditional gas cooling circulation cooling, radiating effect is better.
Add up according to testing data, in the growth method of the sapphire crystal of the present embodiment, the growth cycle of sapphire crystal is 15 days, and traditional growth cycle is 18 days, compares traditional growth cycle, the growth cycle of the present embodiment shortens 3 days, sapphire crystal is in the process of growth, and the firm power of well heater is about 40 ~ 50KW, can save power about 2880 ~ 3600 KWh, often to spend electricity 0.8 yuan of calculating (1 degree of electricity=1KWh), cost-saved about 2304 ~ 2880 yuan.
In the growth method of the sapphire crystal of the present embodiment, in the 100 kilograms of crystal obtained, effective sapphire crystal is 36 kilograms, and the effective rate of utilization of sapphire crystal is 36%, and the effective rate of utilization of traditional sapphire crystal is 35%, compare traditional sapphire crystal growth method, in the present embodiment, in the crystal of every 100 kilograms, can fecund 1 kilogram of sapphire crystal, with per kilogram sapphire crystal 700 yuan calculating, 700 yuan can be made a profit more.
Therefore, the growth method of the sapphire crystal of the present embodiment, often grows 100 kilograms of crystal, cost-saved about 3004 ~ 3580 yuan.
Embodiment 2
The difference of the sapphire crystal growth device of the present embodiment and the sapphire crystal growth device of embodiment 1 is only: the surface of taper or circular arc counterbore is provided with 12 air slots 13, and the width of air slot 13 is 10mm, and the degree of depth is 5mm; Crucible 8 is molybdenum crucible, and the top of crucible 8 is provided with heater top 5.All the other are with embodiment 1.
The difference of the growth method of the growth method of the sapphire crystal of the present embodiment and the sapphire crystal of embodiment 1 is only: the diameter of sapphire seed crystal 9 is 25mm, height 20mm; Crucible 8 is molybdenum crucible, and high purity aluminium oxide raw material is aluminum oxide biscuit; Start heater top 5 in step (4), make the temperature in steel cage 3 rise to 2100 DEG C.All the other are with embodiment 1.
Add up according to testing data, in the growth method of the sapphire crystal of the present embodiment, the growth cycle of sapphire crystal is 14 days, and traditional growth cycle is 18 days, compares traditional growth cycle, the growth cycle of the present embodiment shortens 4 days, sapphire crystal is in the process of growth, and the firm power of well heater is about 40 ~ 50KW, can save power about 3840 ~ 4800KWh, often to spend electricity 0.8 yuan of calculating (1 degree of electricity=1KWh), cost-saved about 3072 ~ 3840 yuan.
In the growth method of the sapphire crystal of the present embodiment, in the 100 kilograms of crystal obtained, effective sapphire crystal is 37 kilograms, and the effective rate of utilization of sapphire crystal is 37%, and the effective rate of utilization of traditional sapphire crystal is 35%, compare traditional sapphire crystal growth method, in the present embodiment, in the crystal of every 100 kilograms, can fecund 2 kilograms of sapphire crystals, with per kilogram sapphire crystal 700 yuan calculating, 1400 yuan can be made a profit more.
Therefore, in the growth method of the sapphire crystal of the present embodiment, often grow 100 kilograms of crystal, cost-saved about 4472 ~ 5240 yuan.
Embodiment 3
The difference of the sapphire crystal growth device of the present embodiment and the sapphire crystal growth device of embodiment 1 is only: the surface of taper or circular arc counterbore is provided with 20 air slots 13, and the width of air slot 13 is 5mm, and the degree of depth is 0.5mm; Crucible 8 is iridium crucible, and the side of crucible 8 is provided with side well heater 6 and top is provided with heater top 5.All the other are with embodiment 1.
The difference of the growth method of the growth method of the sapphire crystal of the present embodiment and the sapphire crystal of embodiment 1 is only: the diameter of sapphire seed crystal 9 is 30mm, height 30mm; Crucible 8 is iridium crucible, and high purity aluminium oxide raw material is alumina block material; Start side well heater 6 and heater top 5 in step (4), make the temperature in steel cage 3 rise to 2150 DEG C.All the other are with embodiment 1.
Add up according to testing data, in the growth method of the sapphire crystal of the present embodiment, the growth cycle of sapphire crystal is 13 days, and traditional growth cycle is 18 days, compares traditional growth cycle, the growth cycle of the present embodiment shortens 5 days, sapphire crystal is in the process of growth, and the firm power of well heater is about 40 ~ 50KW, can save power about 4800 ~ 6000KWh, often to spend electricity 0.8 yuan of calculating (1 degree of electricity=1KWh), cost-saved about 3840 ~ 4800 yuan.
In the growth method of the sapphire crystal of the present embodiment, in the 100 kilograms of crystal obtained, effective sapphire crystal is 37 kilograms, and the effective rate of utilization of sapphire crystal is 37%, and the effective rate of utilization of traditional sapphire crystal is 35%, compare traditional sapphire crystal growth method, in the present embodiment, in the crystal of every 100 kilograms, can fecund 2 kilograms of sapphire crystals, with per kilogram sapphire crystal 700 yuan calculating, 1400 yuan can be made a profit more.
Therefore, in the growth method of the sapphire crystal of the present embodiment, often grow 100 kilograms of crystal, cost-saved about 5240 ~ 6200 yuan.
Those skilled in the art can carry out various modifications and variations to the embodiment of the present invention, if these amendments and modification are within the scope of the claims in the present invention and equivalent technologies thereof, then these revise and modification also within protection scope of the present invention.
The prior art that the content do not described in detail in specification sheets is known to the skilled person.
Claims (10)
1. a sapphire crystal growth device, comprises body of heater (14) and vacuum extractor, and described body of heater (14) is opening and closing type body of heater, and described vacuum extractor is communicated with body of heater (14) inside; Described body of heater (14) inside is provided with steel cage (3), the structure of described steel cage (3) in upper and lower opening, upper shed place of steel cage (3) is provided with thermal insulation layer (4), and lower opening is provided with end thermal insulation layer (11), and the internal surface of steel cage (3) is provided with side thermal insulation layer (7); The inside of steel cage (3) is provided with pedestal (10), described pedestal (10) is placed with crucible (8), it is characterized in that: the top of described body of heater (14) is provided with lifting device (1), and described lifting device (1) is connected with steel cage (3) by union lever (2); The upper surface of described pedestal (10) is provided with taper or circular arc counterbore, the bottom shape of described crucible (8) in taper or the suitable conical surface of circular arc counterbore shape or arc surface, the side of described crucible (8) is provided with side well heater (6) and/or top is provided with heater top (5).
2. sapphire crystal growth device as claimed in claim 1, is characterized in that: the surface of described taper or circular arc counterbore is provided with air slot (13), and described air slot (13) is along divergent shape in taper or circular arc counterbore surrounding.
3. sapphire crystal growth device as claimed in claim 2, is characterized in that: the width of described air slot (13) is 3 ~ 20mm, and the degree of depth is 0.1 ~ 20mm.
4. sapphire crystal growth device as claimed in claim 3, is characterized in that: the width of described air slot (13) is 5 ~ 10mm, and the degree of depth is 0.5 ~ 5mm.
5. the sapphire crystal growth device as described in one of Claims 1 to 4, is characterized in that: be lined with one deck conductive graphite paper between described crucible (8) and pedestal (10).
6. the sapphire crystal growth device as described in one of Claims 1 to 4, is characterized in that: the center of described pedestal (10) and the center of end thermal insulation layer (11) are equipped with centre hole (15).
7. sapphire crystal growth device as claimed in claim 6, it is characterized in that: be also provided with external admission air-cooling apparatus, external admission air-cooling apparatus comprises source of the gas, valve, external feed stream pipe, bottom inflow pipe (12), and source of the gas is connected by the first pipe connecting with valve; Valve is connected with external feed stream pipe, is provided with under meter between valve and external feed stream pipe, is connected between under meter with valve by the second pipe connecting; External feed stream pipe is connected with bottom inflow pipe (12), bottom inflow pipe (12) is provided with sleeve pipe with the junction of external feed stream pipe, the centre hole (15) of bottom inflow pipe (12) through end thermal insulation layer (11) and the centre hole (15) of pedestal (10), extend into crucible (8) bottom part down.
8. a growth method for sapphire crystal, is characterized in that: utilize the sapphire crystal growth device described in claim 7 to carry out, concrete operation step is as follows:
(1) sapphire seed crystal is placed: lay sapphire seed crystal (9) in crucible (8) bottom, make sapphire seed crystal (9) be positioned at directly over bottom inflow pipe (12);
(2) feed: high purity aluminium oxide raw material is put into crucible (8), close body of heater (14);
(3) vacuumize: start vacuum extractor, the pressure in body of heater (14) is evacuated to below 3Pa;
(4) material is heated: start side well heater (6) or/and heater top (5), make the temperature in steel cage (3) rise to 2050 ~ 2150 DEG C, high purity aluminium oxide raw material starts fusing; The position of crucible (8) interior solid-liquid interface is detected with tungsten tipped probe, determine whether sapphire seed crystal (9) starts to melt, when sapphire seed crystal (9) starts to melt, start external admission air-cooling apparatus, cooling gas is passed into, until sapphire seed crystal (9) is partially melted to crucible (8) bottom with the flow velocity of 10 ~ 200L/min;
(5) crystal growth: by the elevated height 1 ~ 350mm of lifting device (1) by steel cage (3), steel cage (3) is separated with end thermal insulation layer (11), and then make pedestal (10) be exposed in body of heater (14), pedestal (10) is heat loss through radiation outwards, reduce the temperature near crucible (8) bottom sapphire seed crystal (9), sapphire seed crystal (9) grows; Cooling gas is passed into, until the whole crystallization of melt in crucible (8) to crucible (8) bottom with the flow velocity of 10 ~ 50L/min;
(6) annealing cooling: steel cage (3) is promoted to extreme higher position by lifting device (1); Cooling gas is passed into, until the crystal in crucible 8 is cooled to room temperature to crucible (8) bottom with the flow velocity of 10 ~ 100L/min;
(7) come out of the stove: be down to after below 400 DEG C until the temperature in body of heater (14), open body of heater (14), take out crystal.
9. the growth method of sapphire crystal as claimed in claim 8, is characterized in that: high purity aluminium oxide raw material described in step (2), (4) is any one or a few in alumina powder, aluminum oxide biscuit, alumina block material.
10. the growth method of sapphire crystal as claimed in claim 8, is characterized in that: crucible (8) described in step (1), (2), (4), (5), (6) is tungsten crucible, any one in molybdenum crucible, iridium crucible.
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