CN104451892A - Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system - Google Patents
Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system Download PDFInfo
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- CN104451892A CN104451892A CN201410748950.2A CN201410748950A CN104451892A CN 104451892 A CN104451892 A CN 104451892A CN 201410748950 A CN201410748950 A CN 201410748950A CN 104451892 A CN104451892 A CN 104451892A
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Abstract
The invention belongs to the technical field of sapphire crystal growth furnace equipment, and provides a multistage graphite heating system of the sapphire crystal growth equipment and a using method of the multistage graphite heating system. The multistage graphite heating system comprises an upper heater, a middle heater, a bottom heater, three power supply devices, a growth furnace cavity, a crucible device and a heat preservation layer, wherein the growth furnace cavity comprises a small furnace cover, a large furnace cover, a furnace cylinder and a furnace base plate; the crucible device comprises a crucible, a crucible tray and a crucible supporting column; each of the upper heater and the middle heater comprise a continuous S-shaped fence-shaped graphite cylinder, four graphite round columns, two long water cooling copper electrodes and two short water cooling copper columns; the bottom heater comprises an S-shaped fence-shaped graphite disc, two graphite electrodes and a water cooling copper electrode; the three individually controlled power supplies are connected with water cooling cables of the upper heater, the middle heater and the bottom heater. The multistage graphite heating system of the sapphire crystal growth equipment and the using method of the multistage graphite heating system have the advantages that the temperature gradient requirement for the growth of large-sized sapphire crystals at each stage can be met, the cost can be reduced, and the quality can be improved.
Description
Technical field
The invention belongs to sapphire crystal growing furnace equipment technical field, particularly a kind of multi-stage type graphite heating system of sapphire crystal growth equipment and using method thereof.
Background technology
Sapphire crystal is a kind of single crystal of Alpha-alumina, fusing point is at about 2050 DEG C, boiling point is close to 3500 DEG C, can work under the mal-condition of 1900 DEG C of high temperature, light transmission is good, within the scope of ultraviolet, visible, infrared band, there is very high transmittance, under 3-5 μm of condition, transmitance is up to 85%, capability of resistance to radiation is strong, thermal shock resistance is good, there is superpower corrosion resistance nature, be widely used in the fields such as the window of infrared military installation, satellite spatial technology, the window material of high intensity laser beam, the bell jar of supersonjc missile and submarine; Further, due to sapphire crystalline network and gan relatively, be widely used in the epitaxially grown commercialization substrate material of gallium nitride based LED, the share more than 80% in all LED substrate material; Mohs' hardness is 9.0, is only second to diamond, has excellent adhesion strength, is widely used in the fields such as high-end watch dial, mobile phone screen, mobile phone camera protective guard and medical facilities.
Sapphire crystal belongs to superelevation melting crystals, very high to the requirement of crystal growth equipment, brings great difficulty to crystal growth.The growth method of conventional sapphire crystal has kyropoulos, heat-exchanging method, crystal pulling method, falling crucible method, EFG technique and temperature gradient method etc.In the growth apparatus of all sapphire crystals, thermal field is wherein the highest, most crucial, the design difficulty the best part of technology content, and well heater or be called that heating element is most important parts in thermal field.
Tungsten, molybdenum, tungstenalloy or other dystectic metal are usually used to the raw material making well heater.Metal or alloy attenuates after at high temperature having easy distortion, volatilization or oxidation, the grain growth of thicker after adsorbing volatilizing thing, metal and cause the problem that the heterogeneous microstructure of tungsten bar changes, and highly shortened the work-ing life of well heater.
In large-sized sapphire crystallization equipment, the metal heater of usual a set of price 30,000 yuan can only use 8 times, cause production cost very expensive, with dystectic metallographic phase ratio, graphite has excellent high-temperature behavior, comprise under high temperature and be difficult to the advantages such as distortion, intensity is high, volatile matter is few, therefore graphite is also used for the well heater of manufacture sapphire crystal growth equipment; The graphite heater of current existence is unistage type, can not overcome the shortcoming that thermograde is little, and cannot take into account end to end when growing large-size sapphire crystal, cause the quality of production poor.So far in the world also without any a graphite heater being applied to kyropoulos growing sapphire, the graphite heater of unistage type cannot be applied in the equipment of large-sized kyropoulos growing sapphire at all.
Therefore, sapphire crystal growing furnace equipment technical field is badly in need of a kind ofly meeting the requirement of each phase temperature gradient of crystal growth, reducing costs, put forward multi-stage type graphite heating system and the using method thereof of high-quality sapphire crystal growth equipment.
Summary of the invention
The invention provides multi-stage type graphite heating system and the using method of sapphire crystal growth equipment, technical scheme is as follows:
The multi-stage type graphite heating system of sapphire crystal growth equipment, wherein, comprising: upper portion heater, middle part well heater, bottom heater, supply unit, growth furnace cavity, crucible device and thermal insulation layer;
Growth furnace cavity, comprise: small furnace cover, large bell, stove cylinder and furnace hearth plate, and stove cylinder has upper and lower opening, large bell is circular ring structure, be connected with sealing-ring with the upper shed of stove cylinder, the external diameter of small furnace cover is slightly larger than the internal diameter of large bell, and the outer rim of small furnace cover is connected with large bell with sealing-ring, furnace hearth plate is connected with sealing-ring with the lower opening of stove cylinder, or furnace hearth plate is welded on the lower bottom part of stove cylinder;
Crucible device, comprise crucible, crucible pallet and crucible pillar, crucible pillar is positioned at the central position of furnace hearth plate, is connected with crucible pallet, and crucible pallet top is connected with crucible, and crucible is used for splendid attire sapphire growth raw material;
Thermal insulation layer is three-dimensional arrangement, is positioned at the inner side of the small furnace cover of growth furnace cavity, large bell, stove cylinder and furnace hearth plate, and is positioned at outside crucible;
Upper portion heater, with a complete graphite cylinder preparation, graphite cylinder cuts out groove, makes the paliform of continuous S type; 4 graphite cylinders are arranged on the position on edge on upper portion heater, the outer end of graphite cylinder is connected with water-cooled copper post, water-cooled copper post is fixed on stove cylinder sidewall, 1 pair of short water-cooled copper post is for supporting upper portion heater, another 1 is connected with the water-cooled cable outside stove cylinder through stove cylinder sidewall long water-cooled copper post, has conducting function for fixing upper portion heater;
Middle part well heater, 4 graphite cylinders are arranged on the position on edge under the well heater of middle part, other structure is consistent with upper portion heater;
Bottom heater, for discoid, comprise graphite disk and 2 Graphite Electrodess, the water-cooled copper electrodes of S type fence, 2 Graphite Electrodess are positioned at the bottom of graphite disk, be connected with graphite disk by screw thread, the bottom of 2 Graphite Electrodess is connected by screw thread with water-cooled copper electrode, and water-cooled copper electrode is fixed on furnace hearth plate, and is connected with outside water-cooled cable through furnace hearth plate;
Supply unit, is made up of 3 independent power supplys controlled, is connected respectively with upper portion heater, middle part well heater with the water-cooled cable of bottom heater.
The multi-stage type graphite heating system of sapphire crystal growth equipment as above, wherein, 3 independent power supplys controlled are IGBT direct supply, single phase alternating current power supply or three-phase alternating-current supply.
The multi-stage type graphite heating system of sapphire crystal growth equipment as above, wherein, the Modulating Power of 3 independent power supplys controlled is 0 ~ 200KW, and Adjustment precision is 0.1 ~ 5 ‰.
The multi-stage type graphite heating system of sapphire crystal growth equipment as above, wherein, 4 graphite cylinders become the angle of 90 ± 20 ° to be distributed on upper portion heater or middle part well heater respectively.
The multi-stage type graphite heating system of sapphire crystal growth equipment as above, wherein, crucible is tungsten crucible or molybdenum crucible.
The multi-stage type graphite heating system of sapphire crystal growth equipment as above, wherein, growth furnace cavity also comprises: vacuum pump, diffusion pump and mechanical pump, and vacuum pump, diffusion pump, mechanical pump are all connected with stove cylinder, and are all connected with controller.
The using method of the multi-stage type graphite heating system of sapphire crystal growth equipment, comprises the steps:
Step one, high purity aluminium oxide raw material purity being greater than 99.99% is inserted in crucible, is installed on by crucible on crucible pallet;
Step 2, builds the thermal insulation layer above crucible, is arranged on by large bell above stove cylinder, and small furnace cover is arranged on above large bell, and centre sealing-ring ensures that its stopping property is good;
Step 3, opens mechanical pump and diffusion pump vacuumizes growth furnace cavity, until the vacuum tightness in growth furnace cavity is higher than 1 × 10
-2till Pa, start heating;
Step 4, regulated by 3 the independent power of power supply to upper portion heater, middle part well heater and bottom heater controlled, power proportions is set to 20:50:30; After electric current exports from power supply, successively through water-cooled cable, water-cooled copper electrode, Graphite Electrodes, heating after Graphite Electrodes conduction, realizes heating upper portion heater, middle part well heater and bottom heater;
Step 5, when the temperature of crucible is higher than 300 ± 20 DEG C, close diffusion pump, only keep mechanical pump to be the state opened, in growth furnace, slowly pass into argon gas, controlled the flow of argon gas by the mass flowmeter on mechanical pump, the pressure in growth furnace cavity is made to maintain within the scope of 0.1 ~ 5000Pa, improve the power of upper portion heater, middle part well heater and bottom heater, until the temperature of crucible is higher than 2050 ± 20 DEG C, the raw material in tungsten crucible melts completely;
Step 6, enter stable program, change the power proportions of upper portion heater, middle part well heater and bottom heater, lower total power, the amplitude that total power is lowered exceeds seeding temperature according to melt temperature and determines, until the core temperature of melt upper surface is a little more than melting temperature;
Step 7, enters seeding program, regulates the power proportions of upper portion heater, middle part well heater and bottom heater when seeding according to the situation of molten body fluid flow; Melt 2 ~ 20mm is inserted in seed crystal bottom, slowly upwards lifts, until the crystalline substance knot grown out is bright, till dislocation and crystal boundary are got rid of;
Step 8, seeding terminates rear slow reduction upper portion heater, the total power of middle part well heater and bottom heater, crystal is entered and expands shoulder and isometrical program, from expand shoulder to ending process in, longitudinal direction in crucible and radial thermograde can be more and more less, the needs of follow-up crystal growth are met in order to maintain enough thermogrades, more than 20kg is reached in crystal weight, need to adjust upper portion heater gradually, the power proportions of middle part well heater and bottom heater, simultaneously by the rising of total power with reduce and regulate crystalline growth velocity, show crystal weight until weigh and be slightly less than 120 ± 5kg, and crystal weight in 5 ± 2 hours without considerable change time, show that crystal growth terminates,
Step 9, crystal enters cycle of annealing, the power proportions of adjustment upper portion heater, middle part well heater and bottom heater, and total power slowly declines, in total power drops to after 0 24 hours, argon pressure to 5 × 10 in growth regulation furnace cavity
4pa, accelerates growth in-furnace temperature and declines, open small furnace cover, take out crystal, complete the production process of whole sapphire crystal when sapphire crystal temperature is reduced to below 50 DEG C after 48 hours.
Beneficial effect of the present invention:
1, because the process of growth of sapphire crystal comprises the stage such as intensification, material, stable, seeding, expansion shoulder, isometrical, ending, cooling annealing, and each stage needs corresponding temperature field, large-sized sapphire crystal due to volume very large, the otherness of the warm field that each stage needs is large, and the well heater of unistage type cannot meet the requirement of large-sized sapphire crystal growth at all.The present invention is by regulating the power proportions of upper portion heater, middle part well heater and bottom heater at any time, thus change the temperature distribution of whole temperature field, make warm field that large size sapphire crystal can be provided all the time to grow the required thermograde of different steps, improve the sapphire quality of production.
2, about 22 days are needed by the production process that the heating system of single well heater completes 1 120kg sapphire crystal, but only need about 19 days by the process of growth that multi-stage type graphite heating system of the present invention completes same sapphire crystal, save time and the energy consumption of more than 13%; And the head of sapphire crystal, middle part and Quality of Tail are all very excellent, there is no bubble, crystal boundary and large scattering particles, improve quality and the utilization ratio of single crystal, reduce production cost.
3, upper portion heater of the present invention, middle part well heater and bottom heater are made up of the graphite of the paliform of continuous S type, and heating effect is more even, ensure that same temperature homogeneity circumferentially.
4, because sapphire crystal growth process can produce a lot of volatile matter, often complete once blue precious crystal growing process, just need to carry out cleaning to growth furnace 1 to safeguard once, tungsten and molybdenum material is after a sapphire crystal growth process, can become and be highly brittle, easily damage when cleaning is safeguarded, and the present invention does not need to connect by the mode of welding, whole employing is threaded, during cleaning, dismounting is very convenient, and graphite material has very high intensity when low temperature and high temperature, the situation of being out of shape and damaging is less likely to occur, reduces spoilage.Present invention greatly enhances the stability of thermal field, extend the work-ing life of thermal field, reduce the growth cost of sapphire crystal, have great meaning to the range of application widening sapphire crystal material.
5, multi-stage type graphite heating system of the present invention can be used in all sapphire crystal growth equipment, comprises in bubble raw stove, lifting furnace, heat-exchanging furnace, crucible decline stove, temperature gradient furnace, reverse mould stove and the zone melting furnace of the raw stove of bubble and improvement; Under the condition of vacuum or inert atmosphere, multi-stage type graphite heating system can also be applied in the equipment of other miscellaneous large size artificial lens of growth, has suitability widely.
Accompanying drawing explanation
The present invention is described in detail below in conjunction with the drawings and specific embodiments:
Fig. 1 is the composition structural representation of the multi-stage type graphite heating system of sapphire crystal growth equipment of the present invention.
Fig. 2 is the structural representation of upper portion heater of the present invention, middle part well heater and lower heater.
Embodiment
The measure realized to make the technology of the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
Fig. 1 is the composition structural representation of the multi-stage type graphite heating system of sapphire crystal growth equipment of the present invention.
As shown in Figure 1, the multi-stage type graphite heating system of sapphire crystal growth equipment, the multi-stage type graphite heating system of sapphire crystal growth equipment, wherein, comprising: upper portion heater 1, middle part well heater 2, bottom heater 3, supply unit, growth furnace cavity, crucible device and thermal insulation layer 8; Growth furnace cavity, comprise: small furnace cover 5, large bell 6, stove cylinder 7 and furnace hearth plate 14, and stove cylinder 7 has upper and lower opening, large bell 6 is circular ring structure, be connected with sealing-ring with the upper shed of stove cylinder 7, the external diameter of small furnace cover 5 is slightly larger than the internal diameter of large bell 6, and the outer rim of small furnace cover 5 is connected with large bell 6 with sealing-ring, furnace hearth plate 14 is connected with sealing-ring with the lower opening of stove cylinder 7, or furnace hearth plate 14 is welded on the lower bottom part of stove cylinder 7; Crucible device, comprise crucible 10, crucible pallet 12 and crucible pillar 13, crucible pillar 13 is positioned at the central position of furnace hearth plate 14, is connected with crucible pallet 12, and crucible pallet 12 top is connected with crucible 10, and crucible 10 is for splendid attire sapphire growth raw material; Thermal insulation layer 8 is three-dimensional arrangement, is positioned at the inner side of the small furnace cover 5 of growth furnace cavity, large bell 6, stove cylinder 7 and furnace hearth plate 14, and is positioned at outside crucible 10; Fig. 2 is the structural representation of upper portion heater of the present invention, middle part well heater and lower heater, and as shown in Figure 2, upper portion heater 1, prepares with a complete graphite cylinder 21, graphite cylinder cuts out groove 22, makes the paliform of continuous S type; 4 graphite cylinders 4 are arranged on the position on edge on upper portion heater 1, the outer end of graphite cylinder 4 is connected with water-cooled copper post, water-cooled copper post is fixed on stove cylinder 7 sidewall, 1 pair of short water-cooled copper post 23 is for supporting upper portion heater 1, another 1 is connected with the water-cooled cable 15 outside stove cylinder 7 through stove cylinder 7 sidewall long water-cooled copper post 24, has conducting function for fixing upper portion heater 1; Middle part well heater 2,4 graphite cylinders 4 are arranged on the position on well heater 2 times edges, middle part, other structure is consistent with upper portion heater 1; Bottom heater 3, for discoid, comprise graphite disk 31 and 2 Graphite Electrodess, the water-cooled copper electrodes of S type fence, 2 Graphite Electrodess are positioned at the bottom of graphite disk, be connected with graphite disk by screw thread, the bottom of 2 Graphite Electrodess 4 is connected by screw thread with water-cooled copper electrode, and water-cooled copper electrode is fixed on furnace hearth plate 14, and is connected with outside water-cooled cable 17 through furnace hearth plate 14; Supply unit, is made up of 3 independent power supplys 18,19,20 controlled, is connected respectively with upper portion heater 1, middle part well heater 2 with the water-cooled cable 15,16,17 of bottom heater 3.
Preferably, 3 of the present embodiment independent power supplys controlled are IGBT direct supply, single phase alternating current power supply or three-phase alternating-current supply.
Preferably, the Modulating Power of 3 independent power supplys controlled of the present embodiment is 0 ~ 200KW, and Adjustment precision is 0.1 ~ 5 ‰.
Preferably, 4 graphite cylinders of the present embodiment become the angle of 90 ± 20 ° to be distributed on upper portion heater or middle part well heater respectively.
Preferably, the crucible of the present embodiment is tungsten crucible or molybdenum crucible.
Preferably, the growth furnace cavity of the present embodiment also comprises: vacuum pump, diffusion pump and mechanical pump, and vacuum pump, diffusion pump, mechanical pump are all connected with stove cylinder, and are all connected with controller.
The using method of the multi-stage type graphite heating system of sapphire crystal growth equipment, comprises the steps:
Step one, high purity aluminium oxide raw material purity being greater than 99.99% is inserted in crucible 10, is installed on by crucible 10 on crucible pallet 12;
Step 2, builds the thermal insulation layer 8 above crucible 10, is arranged on above stove cylinder 7 by large bell 6, and small furnace cover 5 is arranged on above large bell 6, and centre sealing-ring ensures that its stopping property is good;
Step 3, opens mechanical pump and diffusion pump vacuumizes growth furnace cavity, until the vacuum tightness in growth furnace cavity is higher than 1 × 10
-2till Pa, start heating;
Step 4, regulated by the power of 3 the independent power supply 18,19,20 pairs of upper portion heaters 1, middle part well heater 2 and the bottom heaters 3 that control, power proportions is set to 20:50:30; After electric current exports from power supply, successively through water-cooled cable 15,16,17, water-cooled copper electrode 24, Graphite Electrodes 4, Graphite Electrodes 4 conducts electricity rear heating, realizes heating upper portion heater 1, middle part well heater 2 and bottom heater 3;
Step 5, when the temperature of crucible 10 is higher than 300 ± 20 DEG C, close diffusion pump, only keep mechanical pump to be the state opened, in growth furnace cavity, slowly pass into argon gas, controlled the flow of argon gas by the mass flowmeter on mechanical pump, the pressure in growth furnace is made to maintain within the scope of 0.1 ~ 5000Pa, improve the power of upper portion heater 1, middle part well heater 2 and bottom heater 3, until the temperature of crucible 10 is higher than 2050 ± 20 DEG C, the raw material in tungsten crucible is fused into melt 11 completely;
Step 6, enter stable program, change the power proportions of upper portion heater 1, middle part well heater 2 and bottom heater 3, lower total power, the amplitude that total power is lowered exceeds seeding temperature according to melt temperature and determines, until the core temperature of melt 11 upper surface is a little more than melting temperature;
Step 7, enters seeding program, regulates the power proportions of upper portion heater 1, middle part well heater 2 and bottom heater 3 when seeding according to the situation of molten body fluid flow; Melt 2 ~ 20mm is inserted in seed crystal bottom, slowly upwards lifts, until the crystalline substance knot grown out is bright, till dislocation and crystal boundary are got rid of;
Step 8, seeding terminates rear slow reduction upper portion heater 1, the total power of middle part well heater 2 and bottom heater 3, crystal 9 is entered and expands shoulder and isometrical program, from expand shoulder to ending process in, longitudinal direction in crucible 10 and radial thermograde can be more and more less, the needs of follow-up crystal growth are met in order to maintain enough thermogrades, more than 20kg is reached in crystal 9 weight, need to adjust upper portion heater 1 gradually, the power proportions of middle part well heater 2 and bottom heater 3, simultaneously by the rising of total power with reduce and regulate crystalline growth velocity, show crystal weight until weigh and be slightly less than 120 ± 5kg, and crystal weight in 5 ± 2 hours without considerable change time, show that crystal growth terminates,
Step 9, crystal 9 enters cycle of annealing, the power proportions of adjustment upper portion heater 1, middle part well heater 2 and bottom heater 3, and total power slowly declines, in total power drops to after 0 24 hours, argon pressure to 5 × 10 in growth regulation furnace cavity
4pa, accelerates growth in-furnace temperature and declines, open small furnace cover, take out crystal, complete the production process of whole sapphire crystal when sapphire crystal temperature is reduced to below 50 DEG C after 48 hours.
Process of growth due to sapphire crystal comprises the stage such as intensification, material, stable, seeding, expansion shoulder, isometrical, ending, cooling annealing, and each stage needs corresponding temperature field, large-sized sapphire crystal due to volume very large, the otherness of the warm field that each stage needs is large, and the well heater of unistage type cannot meet the requirement of large-sized sapphire crystal growth at all.The present invention is by regulating the power proportions of upper portion heater, middle part well heater and bottom heater at any time, thus change the temperature distribution of whole temperature field, make warm field that large size sapphire crystal can be provided all the time to grow the required thermograde of different steps, improve the sapphire quality of production.
The production process completing 1 120kg sapphire crystal by the heating system of single well heater needs about 22 days, but only need about 19 days by the process of growth that multi-stage type graphite heating system of the present invention completes same sapphire crystal, save time and the energy consumption of more than 13%; And the head of sapphire crystal, middle part and Quality of Tail are all very excellent, there is no bubble, crystal boundary and large scattering particles, improve quality and the utilization ratio of single crystal, reduce production cost.
Upper portion heater of the present invention, middle part well heater and bottom heater are made up of the graphite of the paliform of continuous S type, and heating effect is more even, ensure that same temperature homogeneity circumferentially.
Because sapphire crystal growth process can produce a lot of volatile matter, often complete once blue precious crystal growing process, just need to carry out cleaning to growth furnace 1 to safeguard once, tungsten and molybdenum material is after a sapphire crystal growth process, can become and be highly brittle, easily damage when cleaning is safeguarded, and the present invention does not need to connect by the mode of welding, whole employing is threaded, during cleaning, dismounting is very convenient, and graphite material has very high intensity when low temperature and high temperature, the situation of being out of shape and damaging is less likely to occur, reduces spoilage.Present invention greatly enhances the stability of thermal field, extend the work-ing life of thermal field, reduce the growth cost of sapphire crystal, have great meaning to the range of application widening sapphire crystal material.
Multi-stage type graphite heating system of the present invention can be used in all sapphire crystal growth equipment, comprises in bubble raw stove, lifting furnace, heat-exchanging furnace, crucible decline stove, temperature gradient furnace, reverse mould stove and the zone melting furnace of the raw stove of bubble and improvement; Under the condition of vacuum or inert atmosphere, multi-stage type graphite heating system can also be applied in the equipment of other miscellaneous large size artificial lens of growth, has suitability widely.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. the multi-stage type graphite heating system of sapphire crystal growth equipment, is characterized in that, comprising: upper portion heater, middle part well heater, bottom heater, supply unit, growth furnace cavity, crucible device and thermal insulation layer;
Described growth furnace cavity, comprise: small furnace cover, large bell, stove cylinder and furnace hearth plate, and described stove cylinder has upper and lower opening, described large bell is circular ring structure, be connected with sealing-ring with the upper shed of described stove cylinder, the external diameter of described small furnace cover is slightly larger than the internal diameter of large bell, and the outer rim of described small furnace cover is connected with large bell with sealing-ring, described furnace hearth plate is connected with sealing-ring with the lower opening of stove cylinder, or described furnace hearth plate is welded on the lower bottom part of stove cylinder;
Described crucible device, comprise crucible, crucible pallet and crucible pillar, described crucible pillar is positioned at the central position of furnace hearth plate, is connected with described crucible pallet, and described crucible pallet top is connected with crucible, and described crucible is used for splendid attire sapphire growth raw material;
Described thermal insulation layer is three-dimensional arrangement, is positioned at the inner side of the small furnace cover of described growth furnace cavity, large bell, stove cylinder and furnace hearth plate, and is positioned at outside described crucible;
Described upper portion heater, with a complete graphite cylinder preparation, described graphite cylinder cuts out groove, makes the paliform of continuous S type; 4 graphite cylinders are arranged on the position on edge on described upper portion heater, the outer end of described graphite cylinder is connected with water-cooled copper post, described water-cooled copper post is fixed on stove cylinder sidewall, 1 pair of short described water-cooled copper post is for supporting upper portion heater, another 1 is connected with the water-cooled cable outside stove cylinder through stove cylinder sidewall long described water-cooled copper post, for fixing described upper portion heater and having conducting function;
Described middle part well heater, 4 described graphite cylinders are arranged on the position on edge under the well heater of middle part, other structure is consistent with described upper portion heater;
Described bottom heater, for discoid, comprise graphite disk and 2 Graphite Electrodess, the water-cooled copper electrodes of S type fence, 2 described Graphite Electrodess are positioned at the bottom of graphite disk, be connected with described graphite disk by screw thread, the bottom of 2 described Graphite Electrodess is connected by screw thread with water-cooled copper electrode, and described water-cooled copper electrode is fixed on furnace hearth plate, and is connected with outside water-cooled cable through described furnace hearth plate;
Described supply unit, is made up of 3 independent power supplys controlled, is connected respectively with described upper portion heater, middle part well heater with the water-cooled cable of bottom heater.
2. the multi-stage type graphite heating system of sapphire crystal growth equipment according to claim 1, is characterized in that, 3 independent described power supplys controlled are IGBT direct supply, single phase alternating current power supply or three-phase alternating-current supply.
3. the multi-stage type graphite heating system of sapphire crystal growth equipment according to claim 1, is characterized in that, the Modulating Power of 3 independent described power supplys controlled is 0 ~ 200KW, and Adjustment precision is 0.1 ~ 5 ‰.
4. the multi-stage type graphite heating system of sapphire crystal growth equipment according to claim 1, is characterized in that, 4 described graphite cylinders become the angle of 90 ± 20 ° to be distributed on upper portion heater or middle part well heater respectively.
5. the multi-stage type graphite heating system of sapphire crystal growth equipment according to claim 1, is characterized in that, described crucible is tungsten crucible or molybdenum crucible.
6. the multi-stage type graphite heating system of sapphire crystal growth equipment according to claim 1, it is characterized in that, described growth furnace cavity also comprises: vacuum pump, diffusion pump and mechanical pump, and described vacuum pump, diffusion pump, mechanical pump are all connected with stove cylinder, and are all connected with controller.
7. the using method of the multi-stage type graphite heating system of sapphire crystal growth equipment, comprises the steps:
Step one, high purity aluminium oxide raw material purity being greater than 99.99% is inserted in crucible, is installed on by crucible on crucible pallet;
Step 2, builds the thermal insulation layer above crucible, is arranged on by large bell above stove cylinder, and small furnace cover is arranged on above large bell, and centre sealing-ring ensures that its stopping property is good;
Step 3, opens mechanical pump and diffusion pump vacuumizes growth furnace cavity, until the vacuum tightness in growth furnace cavity is higher than 1 × 10
-2till Pa, start heating;
Step 4, regulated by 3 the independent power of power supply to upper portion heater, middle part well heater and bottom heater controlled, power proportions is set to 20:50:30; After electric current exports from power supply, successively through water-cooled cable, water-cooled copper electrode, Graphite Electrodes, heating after Graphite Electrodes conduction, realizes heating upper portion heater, middle part well heater and bottom heater;
Step 5, when the temperature of crucible is higher than 300 ± 20 DEG C, close diffusion pump, only keep mechanical pump to be the state opened, in growth furnace cavity, slowly pass into argon gas, controlled the flow of argon gas by the mass flowmeter on mechanical pump, the pressure in growth furnace is made to maintain within the scope of 0.1 ~ 5000Pa, improve the power of upper portion heater, middle part well heater and bottom heater, until the temperature of crucible is higher than 2050 ± 20 DEG C, the raw material in tungsten crucible melts completely;
Step 6, enter stable program, change the power proportions of upper portion heater, middle part well heater and bottom heater, lower total power, the amplitude that total power is lowered exceeds seeding temperature according to melt temperature and determines, until the core temperature of melt upper surface is a little more than melting temperature;
Step 7, enters seeding program, regulates the power proportions of upper portion heater, middle part well heater and bottom heater when seeding according to the situation of molten body fluid flow; Melt 2 ~ 20mm is inserted in seed crystal bottom, slowly upwards lifts, until the crystalline substance knot grown out is bright, till dislocation and crystal boundary are got rid of;
Step 8, seeding terminates rear slow reduction upper portion heater, the total power of middle part well heater and bottom heater, crystal is entered and expands shoulder and isometrical program, from expand shoulder to ending process in, longitudinal direction in crucible and radial thermograde can be more and more less, the needs of follow-up crystal growth are met in order to maintain enough thermogrades, more than 20kg is reached in crystal weight, need to adjust upper portion heater gradually, the power proportions of middle part well heater and bottom heater, simultaneously by the rising of total power with reduce and regulate crystalline growth velocity, show crystal weight until weigh and be slightly less than 120 ± 5kg, and crystal weight in 5 ± 2 hours without considerable change time, show that crystal growth terminates,
Step 9, crystal enters cycle of annealing, the power proportions of adjustment upper portion heater, middle part well heater and bottom heater, and total power slowly declines, in total power drops to after 0 24 hours, argon pressure to 5 × 10 in growth regulation furnace cavity
4pa, accelerates growth in-furnace temperature and declines, open small furnace cover, take out crystal, complete the production process of whole sapphire crystal when sapphire crystal temperature is reduced to below 50 DEG C after 48 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410748950.2A CN104451892A (en) | 2014-12-10 | 2014-12-10 | Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system |
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| CN201410748950.2A CN104451892A (en) | 2014-12-10 | 2014-12-10 | Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system |
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| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN105088333A (en) * | 2015-09-09 | 2015-11-25 | 华中科技大学 | Kyropoulos sapphire crystal growth furnace |
| CN105200529A (en) * | 2015-09-29 | 2015-12-30 | 郎业方 | Double-region heater for single-crystal furnace |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN106637386A (en) * | 2015-10-30 | 2017-05-10 | 西安通鑫半导体辅料有限公司 | Single crystal straight-pulling heater capable of increasing crystal pulling rate, and single crystal straight-pulling method |
| CN108277534A (en) * | 2018-04-27 | 2018-07-13 | 济南金曼顿自动化技术有限公司 | A kind of graphite resistance heating SiC crystal growth furnace |
| CN108588832A (en) * | 2018-04-28 | 2018-09-28 | 内蒙古恒嘉晶体材料有限公司 | Prepare the improved kyropoulos and crystal growing furnace of sapphire crystal |
| CN109338469A (en) * | 2018-11-26 | 2019-02-15 | 国宏中晶集团有限公司 | A kind of sapphire crystal growth power supply and its method |
| CN109487332A (en) * | 2018-10-15 | 2019-03-19 | 广州恩锐施智能科技有限公司 | A kind of crystal oven control method and system |
| CN109922545A (en) * | 2017-12-08 | 2019-06-21 | 北京机电工程研究所 | Graphite heating component, graphite heater and design method |
| CN111607823A (en) * | 2020-06-19 | 2020-09-01 | 山东新升光电科技有限责任公司 | Sapphire single crystal pulling method preparation device and method |
| CN113373518A (en) * | 2021-07-16 | 2021-09-10 | 济南大学 | Device and method for growing oversized long equal-diameter lithium niobate |
| CN114040522A (en) * | 2021-11-05 | 2022-02-11 | 中国电子科技集团公司第四十八研究所 | Semiconductor equipment heating device |
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| CN104711676B (en) * | 2015-03-16 | 2017-05-24 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN104711676A (en) * | 2015-03-16 | 2015-06-17 | 内蒙古京晶光电科技有限公司 | Gem single crystal growth method |
| CN105088333A (en) * | 2015-09-09 | 2015-11-25 | 华中科技大学 | Kyropoulos sapphire crystal growth furnace |
| CN105200529A (en) * | 2015-09-29 | 2015-12-30 | 郎业方 | Double-region heater for single-crystal furnace |
| CN106637386A (en) * | 2015-10-30 | 2017-05-10 | 西安通鑫半导体辅料有限公司 | Single crystal straight-pulling heater capable of increasing crystal pulling rate, and single crystal straight-pulling method |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN109922545A (en) * | 2017-12-08 | 2019-06-21 | 北京机电工程研究所 | Graphite heating component, graphite heater and design method |
| CN108277534A (en) * | 2018-04-27 | 2018-07-13 | 济南金曼顿自动化技术有限公司 | A kind of graphite resistance heating SiC crystal growth furnace |
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| CN111607823A (en) * | 2020-06-19 | 2020-09-01 | 山东新升光电科技有限责任公司 | Sapphire single crystal pulling method preparation device and method |
| CN113373518A (en) * | 2021-07-16 | 2021-09-10 | 济南大学 | Device and method for growing oversized long equal-diameter lithium niobate |
| CN114040522A (en) * | 2021-11-05 | 2022-02-11 | 中国电子科技集团公司第四十八研究所 | Semiconductor equipment heating device |
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