CN104250852B - Sapphire crystal growth device and growing method - Google Patents
Sapphire crystal growth device and growing method Download PDFInfo
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- CN104250852B CN104250852B CN201410470974.6A CN201410470974A CN104250852B CN 104250852 B CN104250852 B CN 104250852B CN 201410470974 A CN201410470974 A CN 201410470974A CN 104250852 B CN104250852 B CN 104250852B
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- 239000013078 crystal Substances 0.000 title claims abstract description 133
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 113
- 239000010980 sapphire Substances 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 35
- 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 abstract description 43
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 42
- 239000010959 steel Substances 0.000 claims abstract description 42
- 238000009413 insulation Methods 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 50
- 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 10
- 239000007789 gas Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 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
- 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
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 230000005611 electricity Effects 0.000 description 9
- 229910052786 argon Inorganic materials 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
- 239000002826 coolant Substances 0.000 description 3
- 238000002109 crystal growth method Methods 0.000 description 3
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- 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
- 230000003287 optical effect Effects 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000008859 change Effects 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
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
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Abstract
Sapphire crystal growth device and growing method, including body of heater and vacuum extractor, body of heater is opening and closing type body of heater, and vacuum extractor connects with furnace interior；Furnace interior is provided with steel cage, and steel cage is the structure of upper and lower opening, is provided with heat-insulation layer at the upper shed of steel cage, and lower opening is provided with end heat-insulation layer, and the inner surface of steel cage is provided with side heat-insulation layer；The inside of steel cage is provided with pedestal, and pedestal is placed with crucible, and the top of body of heater is provided with lowering or hoisting gear, and lowering or hoisting gear is connected with steel cage by connecting rod；The upper surface of pedestal is provided with taper or circular arc counterbore, and the bottom shape of crucible is in the conical surface suitable with taper or circular arc counterbore shape or arc surface, and the side of crucible is provided with side heater and/or is arranged over heater top.The center of pedestal is provided with centre bore, can ventilate and carry out cooling and the crystal growth of seed crystal.Utilize assembly of the invention produce sapphire crystal cycle effective rate of utilization shorter, sapphire crystal higher, cost is relatively low.
Description
Technical field
The present invention relates to a kind of sapphire crystal growth device and growing method.
Background technology
Sapphire (Sapphire) is a kind of aluminium oxide (α-Al2O3) monocrystalline, be also called corundum, have excellence mechanical performance, chemical stability and optical property.Sapphire crystal hardness is the highest, is only second to diamond, has good wearability, and mechanical strength is high simultaneously, it is possible to bear the biggest load；Sapphire chemical property is sufficiently stable, the corrosion of general acid and alkali alkali, is difficult to deliquescence, and operating temperature is up to 2000 DEG C, it is possible to work under extremely rugged environment for a long time；It is the widest that sapphire optics penetrates band scope, good translucidus is suffered from near ultraviolet band to middle-infrared band, sapphire is also excellent laser host material simultaneously, has the widest tunable scope and the highest gain, is widely used in LED illumination industry and military window material.
In recent years, along with smart mobile phone, the touch screen type consumption electronic product such as panel computer widely available, sapphire can be widely used as the panel of electronic product.Sapphire optical permeability is good, and wearability is good, the most broken, has the probability replacing glass.
Meanwhile, along with the development of modern science and technology, size, quality and the cost of sapphire crystal material constantly being proposed new requirement, sapphire substrate is also towards large scale, high-quality simultaneously, and the direction of low cost is developed.Due to mobile phone, computer etc. belongs to quick consumer electronics product, it is desirable to price is the highest, but demand is huge, and its required panel also has identical characteristics, it is therefore desirable to sapphire, as panel rapidoprint, needs yield big, low cost.
Sapphire existing main growth methods has czochralski 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 sealed, be arranged around heater at crucible, and the alumina raw material that will be produced sapphire crystal by regulation heater power is melted；Crucible is placed on pedestal, and base bottom controls seed crystal by the flow of cooling medium circulation helium and is not melted and the further growth of crystal, and in growth course, crucible, seed crystal all keep static.
During traditional heat-exchanging method growing sapphire crystal, not being melted to control seed crystal, the major measure taked is, is lowered the temperature seed crystal by cooling medium helium in base bottom, wherein cooling medium helium uses the radiating mode of circulation, and radiating effect is poor；Secondly as recuperated gas requires high flow rate, pipeline is the most thinner, internal diameter is in 8 millimeter, and the initial temperature of the cold helium being passed through is generally room temperature, and the temperature of hot helium out is about 1000 DEG C, change thermal Finite, only have 3～5KW, therefore, for growing further large-sized sapphire crystal, growth rate is slow, growth cycle is longer, it is generally required to about 17～19 days, relatively costly.
Simultaneously, pedestal is plane with the contact surface of the crucible placing seed crystal, and heat exchange area is less, is unfavorable for that crucible dispels the heat, owing to this heat needs to be exchanged by the least heat exchange area, the heat flow density in this region is the highest, causes the localized temperature gradients of sapphire seed crystal above this heat-transfer surface very big, and thermal stress is bigger than normal, the internal 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
The technical problem to be solved is, overcomes the deficiency of above-mentioned background technology, it is provided that effective rate of utilization shorter, sapphire crystal sapphire crystal growth device higher, lower-cost of a kind of production cycle and growing method.
The present invention solves its technical problem and employed technical scheme comprise that, a kind of sapphire crystal growth device, including body of heater and vacuum extractor, described body of heater is opening and closing type body of heater, and described vacuum extractor connects with furnace interior；Described furnace interior is provided with steel cage, and steel cage is the structure of upper and lower opening, is provided with heat-insulation layer at the upper shed of steel cage, and lower opening is provided with end heat-insulation layer, and the inner surface of steel cage is provided with side heat-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 lowering or hoisting gear, and described lowering or hoisting gear is connected with steel cage by connecting rod；The upper surface of described pedestal is provided with taper or circular arc counterbore, and the bottom shape of described crucible is in the conical surface suitable with taper or circular arc counterbore shape or arc surface, and the side of described crucible is provided with side heater and/or is arranged over 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, described one layer of conductive graphite paper between crucible and pedestal, it is lined with.
Further, the center of described pedestal and the center of end heat-insulation layer are equipped with centre bore.
Further, being additionally provided with external admission air-cooling apparatus, external admission air-cooling apparatus includes source of the gas, valve, external feed stream pipe, bottom inflow pipe, and source of the gas is connected by the first connecting tube with valve；Valve is connected with external feed stream pipe, is provided with effusion meter between valve and external feed stream pipe, is connected by the second connecting tube between effusion meter with valve；External feed stream pipe is connected with bottom inflow pipe, and bottom inflow pipe is provided with sleeve pipe with the junction of external feed stream pipe, and bottom inflow pipe passes centre bore and the centre bore of pedestal of end heat-insulation layer, extend into below crucible bottom.
The growing method of a kind of sapphire crystal, utilizes described sapphire crystal growth device to carry out, and specifically includes following steps:
(1) sapphire seed crystal is placed: lay sapphire seed crystal in crucible bottom, make sapphire seed crystal be positioned at the surface of bottom inflow pipe；
(2) charging: high purity aluminium oxide raw material is put into crucible, closes body of heater；
(3) evacuation: start vacuum extractor, the pressure in body of heater is evacuated to below 3Pa；
(4) heating material: startup side heater, or/and heater top, makes the temperature in steel cage rise to 2050～2150 DEG C, and 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, flow velocity with 10～200L/min is passed through cooling gas to crucible bottom, until sapphire seed crystal is partially melted；
(5) crystal growth: by lowering or hoisting gear by the elevated height 1～350mm of steel cage, make steel cage separate with end heat-insulation layer, and then make 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；Flow velocity with 10～50L/min is passed through cooling gas to crucible bottom, until the melt in crucible all crystallizes；
(6) annealing cooling: steel cage is promoted to extreme higher position by lowering or hoisting gear；Flow velocity with 10～100L/min is passed through cooling gas to crucible bottom, until the crystal in crucible 8 is cooled to room temperature；
(7) come out of the stove: after the temperature in body of heater is down to below 400 DEG C, open body of heater, take out crystal.
Further, any one or a few during high purity aluminium oxide raw material is alumina powder, aluminium oxide biscuit, aluminium oxide block described in step (2), (4).
Further, crucible described in step (1), (2), (4), (5), (6) is any one in tungsten crucible, molybdenum crucible, iridium crucible.
Further, cooling down gas described in step (4), (5), (6) is argon.
Compared with prior art, advantages of the present invention is as follows:
(1) upper surface of pedestal is provided with taper or circular arc counterbore, and the bottom shape of crucible is in the conical surface suitable with taper or circular arc counterbore shape or arc surface, it is possible to effectively increasing heat radiation area；Steel cage can be promoted by lowering or hoisting gear, makes steel cage separate with end heat-insulation layer, and then makes pedestal be exposed in body of heater, the heat loss through radiation amount of pedestal is relatively big, reaches the thermograde required for crystal growth, and 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 preferable, can improve the effective rate of utilization of sapphire crystal to 36%～37%, and the growth cost of crystal is relatively low.
(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 reaching the thermograde required for crystal growth.
(3) external admission air-cooling apparatus and vacuum extractor it are provided with, it is passed through cooling gas (such as argon) 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 vacuum extractor is utilized to extract the cooling gas in body of heater out, making cooling gas form acyclic radiating mode, radiating effect is preferable.
Accompanying drawing explanation
Fig. 1 is the structural representation of sapphire crystal growth device embodiment of the present invention.
Fig. 2 is the top view of the pedestal of embodiment illustrated in fig. 1.
Fig. 3 is the partial enlarged drawing of embodiment illustrated in fig. 1.
Fig. 4 is the view after the steel cage lifting of embodiment illustrated in fig. 1.
In figure: 1 lowering or hoisting gear, 2 connecting rods, 3 steel cages, heat-insulation layer on 4,5 heater tops, 6 side heaters, 7 side heat-insulation layers, 8 crucibles, 9 sapphire seed crystals, 10 pedestals, 11 end heat-insulation layers, 12 bottom inflow pipes, 13 air slots, 14 bodies of heater, 15 centre bores.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is described in further detail by specific embodiment.
Embodiment 1
With reference to Fig. 1, sapphire crystal growth device embodiment of the present invention includes body of heater 14, vacuum extractor and external admission air-cooling apparatus, and vacuum extractor is internal with body of heater 14 to be connected；Body of heater 14 is opening and closing type body of heater, and the top of body of heater 14 is provided with lowering or hoisting gear 1, and the internal steel cage 3 that is provided with of body of heater 14, lowering or hoisting gear 1 is connected with steel cage 3 by connecting rod 2；The steel cage 3 structure in upper and lower opening, is provided with heat-insulation layer 4 at the upper shed of steel cage 3, lower opening is provided with end heat-insulation layer 11, and the inner surface of steel cage 3 is provided with side heat-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 in taper or circular arc counterbore surrounding along divergent shape, 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 heat-insulation layer 11 are equipped with centre bore 15；With reference to Fig. 1, crucible 8 it is placed with, so that crucible 8 and pedestal 10 can be lined with one layer of conductive graphite paper with sharp separation between crucible 8 and pedestal 10 on pedestal 10, the bottom shape of crucible 8 is in the conical surface suitable with taper or circular arc counterbore or arc surface, and the side of crucible 8 is provided with side heater 6.
External admission air-cooling apparatus includes source of the gas, valve, external feed stream pipe, bottom inflow pipe 12, and source of the gas is connected by the first connecting tube with valve；Valve is connected with external feed stream pipe, is provided with effusion meter between valve and external feed stream pipe, is connected by the second connecting tube between effusion meter with valve；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 passes centre bore 15 and the centre bore 15 of pedestal 10 of end heat-insulation layer 11, extend into crucible 8 bottom part down.
The growing method embodiment of sapphire crystal of the present invention comprises the following steps:
(1) sapphire seed crystal is placed: bottom tungsten crucible, lay the sapphire seed crystal 9 of a diameter of 20mm, highly 10mm, make sapphire seed crystal 9 be positioned at the surface of bottom inflow pipe 12；
(2) charging: the alumina powder of 100 kilograms is put into tungsten crucible, closes body of heater 14；
(3) evacuation: start vacuum extractor, the pressure in body of heater 14 is evacuated to 2Pa；
(4) heating material: start side 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 to sapphire seed crystal 9 starts to melt, start external admission air-cooling apparatus, bottom tungsten crucible, argon it is passed through, 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 lowering or hoisting gear 1 by the elevated height 1～350mm of steel cage 3, steel cage 3 is made to separate with end heat-insulation layer 11, and then make pedestal 10 be exposed in body of heater 14, the outside heat loss through radiation of pedestal 10, reducing the temperature near sapphire seed crystal 9 bottom tungsten crucible, sapphire seed crystal 9 grows；Bottom tungsten crucible, argon it is passed through, until the melt in tungsten crucible all crystallizes with the flow velocity of 20L/min；
(6) annealing cooling: steel cage 3 is promoted to extreme higher position by lowering or hoisting gear 1；Bottom tungsten crucible, argon it is passed through, until the crystal in tungsten crucible is cooled to room temperature with the flow velocity of 50L/min；
(7) coming 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 argon and pedestal 10 thermal field component such as grade complete fluid interchange, being directly expelled to outside body of heater 14 by vacuum extractor, form gas and cool down acyclic radiating mode, compared with traditional gas cooling circulation cooling, radiating effect is preferable.
Add up according to test data, in the growing 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 during growth, and the firm power of heater is about 40～50KW, can save electricity about 2880～3600 KW h, often to spend 0.8 yuan of calculating (1 degree of electricity=1KW h) of electricity, cost-saved about 2304～2880 yuan.
In the growing 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 growing method of the sapphire crystal of the present embodiment, often 100 kilograms of crystal of growth, cost-saved about 3004～3580 yuan.
Embodiment 2
Differing only in of the sapphire crystal growth device of the sapphire crystal growth device of the present embodiment and embodiment 1: 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, crucible 8 be arranged over heater top 5.Remaining is with embodiment 1.
The growing method of the sapphire crystal of the present embodiment differs only in the growing method of the sapphire crystal of embodiment 1: a diameter of 25mm of sapphire seed crystal 9, highly 20mm；Crucible 8 is molybdenum crucible, and high purity aluminium oxide raw material is aluminium oxide biscuit；Step (4) starts heater top 5, makes the temperature in steel cage 3 rise to 2100 DEG C.Remaining is with embodiment 1.
Add up according to test data, in the growing 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 during growth, and the firm power of heater is about 40～50KW, can save electricity about 3840～4800KW h, often to spend 0.8 yuan of calculating (1 degree of electricity=1KW h) of electricity, cost-saved about 3072～3840 yuan.
In the growing 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 growing method of the sapphire crystal of the present embodiment, often 100 kilograms of crystal of growth, cost-saved about 4472～5240 yuan.
Embodiment 3
Differing only in of the sapphire crystal growth device of the sapphire crystal growth device of the present embodiment and embodiment 1: 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 heater 6 and is arranged over heater top 5.Remaining is with embodiment 1.
The growing method of the sapphire crystal of the present embodiment differs only in the growing method of the sapphire crystal of embodiment 1: a diameter of 30mm of sapphire seed crystal 9, highly 30mm；Crucible 8 is iridium crucible, and high purity aluminium oxide raw material is aluminium oxide block；Step (4) starts side heater 6 and heater top 5, makes the temperature in steel cage 3 rise to 2150 DEG C.Remaining is with embodiment 1.
Add up according to test data, in the growing 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 during growth, and the firm power of heater is about 40～50KW, can save electricity about 4800～6000KW h, often to spend 0.8 yuan of calculating (1 degree of electricity=1KW h) of electricity, cost-saved about 3840～4800 yuan.
In the growing 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 growing method of the sapphire crystal of the present embodiment, often 100 kilograms of crystal of growth, 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 amendments and modification are also within protection scope of the present invention.
The prior art that the content not described in detail in description is known to the skilled person.
Claims (9)
1. a sapphire crystal growth device, including body of heater (14) and vacuum extractor, described body of heater (14) is opening and closing type body of heater, and described vacuum extractor is internal with body of heater (14) to be connected；Described body of heater (14) is internal is provided with steel cage (3), the described steel cage (3) structure in upper and lower opening, being provided with heat-insulation layer (4) at the upper shed of steel cage (3), lower opening is provided with end heat-insulation layer (11), and the inner surface of steel cage (3) is provided with side heat-insulation layer (7)；The inside of steel cage (3) is provided with pedestal (10), and described pedestal (10) is placed with crucible (8), it is characterised in that: the top of described body of heater (14) is provided with lowering or hoisting gear (1), and described lowering or hoisting gear (1) is connected with steel cage (3) by connecting rod (2)；The upper surface of described pedestal (10) is provided with taper or circular arc counterbore, and the surface of described taper or circular arc counterbore is provided with air slot (13), described air slot (13) in taper or circular arc counterbore surrounding along divergent shape；The bottom shape of described crucible (8) is in the conical surface suitable with taper or circular arc counterbore shape or arc surface, and the side of described crucible (8) is provided with side heater (6) and/or is arranged over heater top (5).
2. sapphire crystal growth device as claimed in claim 1, it is characterised in that: the width of described air slot (13) is 3～20mm, and the degree of depth is 0.1～20mm.
3. sapphire crystal growth device as claimed in claim 2, it is characterised in that: the width of described air slot (13) is 5～10mm, and the degree of depth is 0.5～5mm.
4. the sapphire crystal growth device as described in one of claims 1 to 3, it is characterised in that: it is lined with one layer of conductive graphite paper between described crucible (8) and pedestal (10).
5. the sapphire crystal growth device as described in one of claims 1 to 3, it is characterised in that: the center of described pedestal (10) and the center of end heat-insulation layer (11) are equipped with centre bore (15).
6. sapphire crystal growth device as claimed in claim 5, it is characterised in that: being additionally provided with external admission air-cooling apparatus, external admission air-cooling apparatus includes source of the gas, valve, external feed stream pipe, bottom inflow pipe (12), and source of the gas is connected by the first connecting tube with valve；Valve is connected with external feed stream pipe, is provided with effusion meter between valve and external feed stream pipe, is connected by the second connecting tube between effusion meter with valve；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, bottom inflow pipe (12) passes centre bore (15) and the centre bore (15) of pedestal (10) of end heat-insulation layer (11), extend into crucible (8) bottom part down.
7. the growing method of a sapphire crystal, it is characterised in that: utilizing the sapphire crystal growth device described in claim 6 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 the surface of bottom inflow pipe (12)；
(2) charging: high purity aluminium oxide raw material is put into crucible (8), closes body of heater (14)；
(3) evacuation: start vacuum extractor, the pressure in body of heater (14) is evacuated to below 3Pa；
(4) heating material: startup side heater (6), or/and heater top (5), makes 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, flow velocity with 10～200L/min is passed through cooling gas, until sapphire seed crystal (9) is partially melted to crucible (8) bottom；
(5) crystal growth: by lowering or hoisting gear (1) by the elevated height 1～350mm of steel cage (3), steel cage (3) is made to separate with end heat-insulation layer (11), and then make pedestal (10) be exposed in body of heater (14), pedestal (10) outwards heat loss through radiation, reducing the temperature near crucible (8) bottom sapphire seed crystal (9), sapphire seed crystal (9) grows；Flow velocity with 10～50L/min is passed through cooling gas, until the melt in crucible (8) all crystallizes to crucible (8) bottom；
(6) annealing cooling: steel cage (3) is promoted to extreme higher position by lowering or hoisting gear (1)；Flow velocity with 10～100L/min is passed through cooling gas, until the crystal in crucible 8 is cooled to room temperature to crucible (8) bottom；
(7) come out of the stove: after the temperature in body of heater (14) is down to below 400 DEG C, open body of heater (14), take out crystal.
8. the growing method of sapphire crystal as claimed in claim 7, it is characterised in that: any one or a few during high purity aluminium oxide raw material is alumina powder, aluminium oxide biscuit, aluminium oxide block described in step (2), (4).
9. the growing method of sapphire crystal as claimed in claim 7, it is characterised in that: crucible (8) described in step (1), (2), (4), (5), (6) is any one in tungsten crucible, molybdenum crucible, iridium crucible.
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