CN105177711A - Sapphire crystal growing furnace heat field, crystal growing furnace with heat field and crystal growing process of crystal growing furnace - Google Patents

Sapphire crystal growing furnace heat field, crystal growing furnace with heat field and crystal growing process of crystal growing furnace Download PDF

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CN105177711A
CN105177711A CN201510676049.3A CN201510676049A CN105177711A CN 105177711 A CN105177711 A CN 105177711A CN 201510676049 A CN201510676049 A CN 201510676049A CN 105177711 A CN105177711 A CN 105177711A
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crystal
crystallization furnace
sapphire crystallization
seed
thermal field
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朱剑啸
吉爱华
曲海峰
侯乃生
吉慕璇
吉磊
张志伟
董俊杰
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Abstract

The invention discloses a sapphire crystal growing furnace heat field, a crystal growing furnace with the heat field and a crystal growing process of the crystal growing furnace, wherein a crucible of a tungsten tube of the sapphire crystal growing furnace heat field is arranged in a way of being supported by a crucible support frame; a lower heat insulation molybdenum screen is arranged between the crucible support frame and the tungsten tube; a zirconium oxide fiber plate is arranged on the lower heat insulation molybdenum screen, so that the temperature gradient of the heat field is constant. The sapphire crystal growing furnace heat field also comprises a seed crystal clamping head assembly; a seed crystal rod of the seed crystal clamping head assembly is suspended in a heating cage assembly and extends into the crucible, so that the seed crystals can maintain the sealing performance of the heat field during the pulling; the temperature gradient uniformity is also ensured. The crystals have high quality, small dislocation density, few crystal boundaries and few bubbles due to the good temperature gradient. The sapphire crystal growing furnace is provided with the heat field, so that high-quality crystals can be produced; the temperature gradient is constant, so that the production efficiency is high; the cost of enterprises can be saved. Therefore after the crystal growing process is used, the quality and the acceptance rate of produced crystals are respectively improved; the cost is reduced; the production efficiency is improved.

Description

Sapphire crystallization furnace thermal field and be provided with the brilliant stove of length of this thermal field and long brilliant technique thereof
Technical field
The present invention relates to sapphire production technical field, particularly relate to a kind of sapphire crystallization furnace thermal field and be provided with the brilliant stove of length of this thermal field and long brilliant technique thereof.
Background technology
Sapphire (Sapphire) is the monocrystalline of a kind of aluminum oxide (α-Al2O3), be also called corundum, with regard to color, simple alumina crystal presents clear, colorless, at nature sapphire when growing, time in crystal containing titanium ion (Ti3+) and iron ion (Fe3+), crystal can be made to present blueness, and become blue sapphire (BlueSapphire).Sapphire crystal chemical property is highly stable, generally water insoluble and acid and alkali, caustic corrosion, and hardness of crystals is very high, is Mohs' hardness 9 grades, is only second to the hardest diamond.It has good light transmission, heat conductivity and electric insulating quality, mechanics good mechanical property, and has wear-resisting and weather-proof feature.The crystalline network of its uniqueness, excellent mechanical property, good thermal property make sapphire crystal become the ideal substrate material such as LED, large-scale integrated circuit SOI and SOS, along with the development of modern science and technology, new requirement is constantly proposed to the size of sapphire crystal material, quality.At present, low cost, high-quality large-size sapphire single-crystal have the increasing market requirement.
Along with technical progress, the method of artificial production sapphire crystal gets more and more, but no matter any good method, only reach the brilliant temperature of length of sapphire crystal, sapphire crystal could grow, if there is no thermal insulation layer, in stove, the high temperature of degree more than 2000 is difficult to ensure, reach the temperature of sapphire crystal growth, must ceaselessly heat, huge to the consumption of electricity, energy dissipation is serious, the more important thing is the sapphire crystal quality product having a strong impact on and grow, on the other hand, for improved large size 100-500KG level sapphire crystallization furnace, how to find out the brilliant technique of applicable 100-500KG level sapphire crystallization furnace superintendent also particularly important, the brilliant technique of domestic length is groped, the crystal grown has lattice imperfection, numerical value is greater than 1000 dislocation desities/pits.cm-2, crystal crystal boundary is many, bubble is many, this can have a strong impact on internal structure and the quality of sapphire leading product Sapphire Substrate sheet and diaphragm, yield rate is extremely low, waste huge, cost is high, efficiency is low, be difficult to scale operation.Sapphire crystal growing furnace thermal field adopts any lagging material outward and adopts what technique to make it be reduced to dislocation density, becomes the technical problem that domestic sapphire industry is paid close attention to.
Summary of the invention
The first object of the present invention is to provide a kind of sapphire crystallization furnace thermal field, and this thermal field improves heat insulation effect, improve crystal mass and crystal yield rate, and this thermal field structure is reasonable in design, is suitable for producing in enormous quantities.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of sapphire crystallization furnace thermal field comprises stainless steel cask, tungsten cylinder is provided with in described stainless steel cask, heating basket assembly is provided with in described tungsten cylinder, crucible is provided with in described heating basket assembly, bottom in described tungsten cylinder is provided with crucible holder, described crucible is arranged on described crucible holder, is provided with lower heat insulation molybdenum shield between described crucible holder and described tungsten cylinder inwall; Also comprise seed chuck assembly, described seed chuck assembly comprises seed rod, and described seed rod is suspended in described heating basket assembly, and described seed rod stretches in described crucible.
Optimal way is, described lower heat insulation molybdenum shield is provided with Zirconium oxide fibre base plate.
Optimal way is, described lower heat insulation molybdenum shield is provided with interlayer, and described Zirconium oxide fibre base plate is fixed in described interlayer.
The second object of the present invention is to provide a kind of sapphire crystallization furnace, the furnace sealing of this long brilliant stove is good, makes the thermograde consistence of its inside good, thus improves its crystal mass produced and product rate, also improve production efficiency, be suitable for producing crystal in enormous quantities.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of sapphire crystallization furnace comprises above-mentioned sapphire crystallization furnace thermal field.
Optimal way is, is provided with well heater, thermal insulation layer, body of heater inner casing and body of heater shell outside described stainless steel cask successively.
Optimal way is, described thermal insulation layer is made up of zirconium white.
Optimal way is, also comprise intelligent control system, described intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with described CPU module, described CPU module is also electrically connected with the described heating basket assembly of described well heater and described sapphire crystallization furnace respectively, described power module is electrically connected with electrical network, described intelligent control system also comprises photovoltaic cell component, and described photovoltaic cell component is electrically connected with described power module by photovoltaic processing module.
Optimal way is, also comprise intelligent control system, described intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with described CPU module, described CPU module is also electrically connected with the described heating basket assembly of described well heater and described sapphire crystallization furnace respectively, described power module is electrically connected with electrical network, described intelligent control system also comprises wind energy system, and described wind energy system is electrically connected with described power module by inverter.
Optimal way is, also comprises the seed chuck Component driver portion be electrically connected with described CPU module, and described seed chuck Component driver portion and described seed chuck assembly are in transmission connection.
The third object of the present invention is to provide a kind of sapphire crystallization furnace superintendent brilliant technique, and this technique obtains optimization, and production efficiency is high, is suitable for producing crystal in enormous quantities.
For solving the problems of the technologies described above, technical scheme of the present invention is:
The brilliant technique of a kind of sapphire crystallization furnace superintendent, comprises step: get the raw materials ready, prepares three pure dichlorine monoxides as raw material, further comprising the steps of:
S (5), filler and frame are brilliant, are packed into by described aluminium sesquioxide in the described crucible of described sapphire crystallization furnace thermal field, and are clipped in by crystal seed on the described seed rod of described seed chuck assembly of described sapphire crystallization furnace thermal field;
S (10), to vacuumize, vacuum in the described stainless steel cask making described sapphire crystallization furnace thermal field;
S (15), heating, start described sapphire crystallization furnace to described sapphire crystallization furnace thermal field heating;
S (20), melting sources, when the power in described sapphire crystallization furnace thermal field is in 501 ~ 505KW power range, described aluminium sesquioxide be melted into liquid; When temperature in the described tungsten cylinder of described sapphire crystallization furnace thermal field falls into 2030 ° ~ 2050 ° of scopes, carry out seeding;
S (25), welding crystal seed, the described seed chuck assembly of described sapphire crystallization furnace thermal field makes seed crystal decline close to described aluminium sesquioxide liquid level, then contacts described aluminium sesquioxide liquid level, then mentions seed crystal; Repetition aforesaid operations completes washes crystalline substance; After washing crystalline substance, under seed crystal being dropped to described aluminium sesquioxide liquid level, carry out welding crystal seed; When carrying out described welding crystal seed, the power range in described sapphire crystallization furnace thermal field is 500 ~ 504KW;
S (30), brilliant Diameter growth, after welding crystal seed, the described seed chuck assembly of described sapphire crystallization furnace thermal field continues lift, makes the diameter of crystal become large, until crystal weight is in 5 ~ 10KG weight range;
S (35), crystal growth, crystal enters the production phase from growth phase, according to the pace of change of crystal weight in process of growth, adjusts the power in described sapphire crystallization furnace thermal field; Crystal weight continues constant production and completes;
S (40), brilliant footpath are separated with crucible, make the described seed chuck assembly pull-up of described sapphire crystallization furnace thermal field, are separated in brilliant footpath with crucible;
Crystal is taken out in S (50), cooling, when the described stainless steel cask internal pressure of described sapphire crystallization furnace thermal field is normal atmosphere, opens the described stainless steel cask naturally cooling of described sapphire crystallization furnace thermal field, after 36 hours, takes out crystal.
After adopting technique scheme, the invention has the beneficial effects as follows: because the crucible in the tungsten cylinder of sapphire crystallization furnace thermal field of the present invention is supported setting by crucible holder, wherein crucible holder comprises zirconium oxide fiber board and lower heat insulation molybdenum shield, and the thermograde in thermal field can be made consistent.The seed rod of seed chuck assembly is also suspended in heating basket assembly by the present invention simultaneously, and allowing seed rod stretch in crucible, making seed crystal when lifting, the stopping property of thermal field also keeps good, makes the thermograde in thermal field consistent further.And thermograde consistence is good, make the quality of crystal high, dislocation desity is little, and crystal crystal boundary is few, bubble is few.And sapphire crystallization furnace of the present invention, because it is provided with thermal field of the present invention, when making it produce crystal, the crystal of high-quality can be produced, and because of thermograde consistent, make its production efficiency high.Therefore utilize the crystal of the brilliant explained hereafter of the length of sapphire crystallization furnace of the present invention, its crystal mass and product rate are all improved, and provide cost savings, improve production efficiency.
Because lower heat insulation molybdenum shield is provided with Zirconium oxide fibre base plate; This structure makes the heat insulation effect in thermal field better.
Owing to being provided with well heater, thermal insulation layer, body of heater inner casing and body of heater shell outside stainless steel cask successively; This structure makes thermal field of the present invention have dual-heated, also has dual insulation, also makes the stopping property of thermal field good, thus ensure that the thermograde consistence in thermal field.
Because thermal insulation layer is made up of zirconium white; Because zirconium white is a kind of senior refractory raw material, its melt temperature is about 2900 DEG C, chooses zirconium white because the high and high insulating effect of its heatproof, further ensures the consistence of thermograde.
Owing to also comprising intelligent control system, intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with CPU module, CPU module is also electrically connected with the heating basket assembly of well heater and sapphire crystallization furnace respectively, power module is electrically connected with electrical network, intelligent control system also comprises photovoltaic cell component, and photovoltaic cell component is electrically connected with power module by photovoltaic processing module; Solar energy converting can be become electric energy by this photovoltaic cell component, thus makes to present invention saves the energy; The power supply that simultaneously can also continue, indirectly ensure that the consistence of thermograde.
Owing to also comprising intelligent control system, intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with CPU module, CPU module is also electrically connected with the heating basket assembly of well heater and described sapphire crystallization furnace respectively, power module is electrically connected with electrical network, intelligent control system also comprises wind energy system, and wind energy system is electrically connected with power module by inverter; Wind resource change can be become electric energy by this wind energy system, thus makes to present invention saves the energy; The power supply that simultaneously can also continue, indirectly ensure that the consistence of thermograde.
In sum, sapphire crystallization furnace thermal field of the present invention and be provided with the brilliant stove of length of this thermal field and long brilliant technique thereof compared to prior art, in the technical problem crystal growing process solved, thermograde is inconsistent, crystal is caused to have lattice imperfection, numerical value is greater than 1000 dislocation desities/pits.cm-2, crystal crystal boundary is many, bubble is many, this can have a strong impact on internal structure and the quality of sapphire leading product Sapphire Substrate sheet and diaphragm, yield rate is extremely low, waste huge, cost is high, and efficiency is low, is difficult to the technical problem of scale operation; And sapphire thermal field of the present invention and be provided with the sapphire crystallization furnace of this thermal field and long brilliant technique thereof, can ensure that the thermograde of crystal production is consistent, make the crystal mass of production and crystal yield rate high, also save the cost of enterprise, improve production efficiency, improve quality product, production technology optimization, production efficiency is high, is suitable for producing in enormous quantities.
Accompanying drawing explanation
Fig. 1 is the structural representation of sapphire crystallization furnace thermal field of the present invention;
Fig. 2 is the structural representation of sapphire crystallization furnace of the present invention;
Fig. 3 is the functional block diagram of sapphire crystallization furnace of the present invention;
Fig. 4 is the schema of the brilliant technique of sapphire crystallization furnace superintendent of the present invention;
In figure: 1-photovoltaic cell component, 2-photovoltaic processing module, 3-wind energy system, 4-inverter, 5-electrical network, 6-power module, 7-CPU module, 8-control panel, 9-sapphire crystallization furnace thermal field, 90-stainless steel cask, 91-baffle plate, 92-tungsten cylinder, 93-crucible heat insulation layer, 94-Zirconium oxide fibre side is shielded, 95-tungsten crucible, 96-lower heat insulation molybdenum shield, 97-Zirconium oxide fibre base plate, 98-crucible holder, 99-heating basket assembly, 911-seed chuck assembly, 912-upper heat insulation molybdenum shield, 10-well heater, 11-thermal insulation layer, 12-body of heater inner casing, 13-body of heater shell, 14-water system, 15-vacuum system.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
As shown in Figure 1, a kind of sapphire crystallization furnace thermal field comprises stainless steel cask 90, and be provided with bung above stainless steel cask 90, bung offers vision slit, and position relative with vision slit inside bung is provided with baffle plate 91, and baffle plate 91 selects zirconium white material to make.Be provided with tungsten cylinder 92 in stainless steel cask 90, between stainless steel cask 90 and tungsten cylinder 92, be provided with Zirconium oxide fibre side shield 94.Be provided with heating basket assembly 99 in tungsten cylinder 92, the upper end of heating basket assembly 99 is provided with heat insulation molybdenum shield 912, is provided with crucible, the preferred tungsten crucible 95 of crucible in heating basket assembly 99.Tungsten crucible 95 side of the present embodiment, end face, bottom thickness are 0.5 ± 0.01mm.Crucible heat insulation layer 93 is provided with above tungsten crucible 95.Tungsten crucible 95 is arranged on crucible holder 98, and crucible holder 98 is cylindricality, is filled with lower heat insulation molybdenum shield 96 between itself and tungsten cylinder 92.Lower heat insulation molybdenum shield 96 is provided with interlayer, is installed with Zirconium oxide fibre base plate 97 in interlayer.The Zirconium oxide fibre base plate 97 of the present embodiment is disc structure.
Sapphire crystallization furnace thermal field 9 of the present invention also comprises seed chuck assembly 911, and seed chuck assembly 911 comprises seed rod, and this seed rod is suspended in heating basket assembly 99, and stretches in tungsten crucible 95.
Sapphire crystallization furnace thermal field 9 of the present invention, when producing, because being provided with Zirconium oxide fibre base plate 97 in the bottom of tungsten crucible 95, makes the thermograde in thermal field consistent.The seed chuck assembly 911 heated in basket assembly 99 has been located at thermal field inside simultaneously, making its seed rod when carrying out lift operation, can not affect the stopping property of thermal field, also making the thermograde in thermal field consistent.Therefore sapphire crystallization furnace thermal field 9 of the present invention improves heat insulation effect, improves crystal mass and crystal yield rate, for enterprise is cost-saving, enhance productivity, improve quality product, thermal field is reasonable in design, production technology optimization, production efficiency is high, is suitable for producing in enormous quantities.
As shown in Figures 2 and 3, a kind of sapphire crystallization furnace comprises sapphire crystallization furnace thermal field 9, well heater 10, thermal insulation layer 11, body of heater inner casing 12 and body of heater shell 13 is provided with successively outside the stainless steel cask 90 of sapphire crystallization furnace thermal field 9, wherein thermal insulation layer 11 selects zirconium white material to make, and body of heater inner casing 12 material is tetrafluoroethylene.
Sapphire crystallization furnace of the present invention also comprises water system 14 and vacuum system 15, and water system 14 is all connected with stove outer covering body with vacuum system 15; Seed chuck assembly 911 is in transmission connection with seed chuck assembly 911 driving part outside stainless steel cask 90.
Sapphire crystallization furnace of the present invention also comprises intelligent control system, intelligent control system comprises CPU module 7 and the power module 6 of electrical connection, also comprise and being electrically connected with the control panel 8 be electrically connected with CPU module 7, CPU module 7 is also respectively with well heater 10 with heat basket assembly 99 and be electrically connected, and power module 6 is electrically connected with electrical network 5.The present embodiment also comprises photovoltaic cell component 1, and it comprises high-performance flexible photovoltaic cell component 1, sensor, turbine and worm and push-rod electric machine; And photovoltaic cell component 1 is electrically connected with power module 6 by photovoltaic processing module 2.Namely photovoltaic cell component 1 absorbs sun power, and converts thereof into electric energy, is transferred to power module 6.
The present invention also comprises wind energy system 3, and wind energy system 3 is electrically connected with power module 6 by inverter 4, and power module 6 is also electrically connected with electrical network 5 simultaneously.Namely the present invention can use sun power, wind energy and electrical network 5 to power to sapphire crystallization furnace, thus saves the energy, and what also make sapphire crystallization furnace can stablize lasting work, indirectly ensure that the temperature in thermal field, the temperature of crystal growth.
CPU module 7 is also electrically connected with seed chuck assembly 911 driving part, water system 14 and vacuum system 15 respectively.Therefore sapphire crystallization furnace of the present invention can be controlled easily by control panel 8, improves the intelligent of equipment, also improves production efficiency.
The present invention adopts wind energy and solar electrical energy generation, and a part uses unnecessary grid-connected, double-heater, and thermal field has added again well heater outward; Thermal field simulate effect and actual effect basically identical, temperature of thermal field gradient basically identical you, present invention ensures that long brilliant stove good seal and the consistence of in-furnace temperature and the consistence of thermograde, combine again for this sapphire crystal furnace technique, saved energy consumption, improve heat insulation effect, improve crystal mass and crystal yield rate, for enterprise is cost-saving, enhance productivity, improve quality product, long crystal structure is reasonable in design, production technology optimization, production efficiency is high, is suitable for producing in enormous quantities.
As shown in Figure 4, the brilliant technique of a kind of length of sapphire crystallization furnace comprises the following steps:
A, preparation raw material, get out pure aluminium sesquioxide starting material.
B, filler and frame are brilliant, fill pure aluminium sesquioxide starting material and enter in tungsten crucible 95, and be erected at by crystal seed on the assembly chuck of seed chuck assembly 911.
C, to vacuumize, open vacuum system 15, make vacuum in stainless steel cask 90.
D, heating, operation control panel 8 allows power module 6 provide voltage to well heater 10 and heating basket assembly 99, makes to heat up in tungsten cylinder 92.
E, melting sources, the critical power of melting sources is 501-505kw; For 500KG level sapphire crystallization furnace, the power of melting sources is 500KW.
When power in tungsten cylinder 92 is 500KW, the raw material checked in tungsten crucible 95 by vision slit melts situation.As raw material in tungsten crucible 95 maintains the original state and no change, then illustrate that now power is on the low side and also do not reach material power.Then operation control panel 8, makes power module 6 adjust; Tungsten cylinder 92 internal power is increased within the scope of 502 ~ 505KW, continues to observe the material situation in tungsten crucible 95.As raw material in tungsten crucible 95 starts landslide, then illustrate that now material power is applicable to, note observing until raw material all melts, in tungsten crucible 95, raw material becomes liquid.By observing the liquid level after melting, the velocity of flow of liquid fluid line judges the height of temperature in tungsten cylinder 92.
Enter into range of stability when the material stage, control temperature in tungsten cylinder 92 by range of stability, when temperature reaches seeding temperature scope 2040 ± 10 °, start seeding temperature.Operation control panel 8, makes it control seed chuck assembly 911 and works, and allows the slow uniform descent of seed chuck to secure location, and the secure location of the slow uniform descent of seed chuck is 280 ± 10m.Preparation enters welding seed crystal process.
F, welding crystal seed:
1., after seed crystal drops to secure location, slowly seed crystal is dropped to liquid level;
If 2. in seed crystal decline process, in-furnace temperature is too high, seed crystal from liquid level more close to, temperature can be higher, and seed crystal face can be melted, i.e. roasting seed crystal;
If 3. run into this situation, tungsten cylinder 92 internal power is lowered a little, so that reaches suitable temperature spot, be convenient to seed crystal and decline, contact liquid level;
4., when seed crystal contact liquid level, record the particular location of contact liquid level, so that seeding is as reference position;
5. seed crystal is down to below liquid level, reintroduces liquid level, several circulation like this, reach and wash brilliant object;
6. washing crystalline substance is in order to the volatile matter wash clean by seed crystal face, so that the temperature of seed crystal is consistent to arriving with the temperature of one side;
7. at a suitable temperature, seed crystal is dropped to below liquid level, allow liquid level slowly grow up to solid-state form along with seed crystal;
8. in welding seed crystal process, must according to the size of the Authority Contro1 crystalline substance knot of operating process.
G, brilliant Diameter growth
1. brilliant Diameter growth is an operation steps after welding crystal seed reaches certain length.
2. brilliant Diameter growth allows crystal slowly become large, and diameter slowly amplifies on the basis that crystalline substance is tied.
3., during brilliant Diameter growth, the rotating speed of speed and the seed chuck lifted be noted more.
4. brilliant Diameter growth initial stage crystal weight is generally at 5-10KG.
5. the brilliant Diameter growth middle and later periods will note the range of decrease and other each important parameters of power per hour.
6., after the brilliant Diameter growth stage reaches the standard of working specification, crystal can enter growth phase.
H, crystal growth
1. crystal enters the production phase from the brilliant Diameter growth stage;
2. in production process early stage, crystal production is comparatively slow, note observing more, per hourly carries out important parameter record form;
3. crystal growth weight hourly is with reference to production operation normative form;
4., as crystal growth is excessively slow, crystalline growth velocity can be controlled by the method increasing the power range of decrease;
5., as crystal growth is too fast, crystalline growth velocity can be controlled by the method reducing the power range of decrease;
6., as crystal produces sticky pot situation, operation can be suspended to control crystal growth;
7. crystal enters Later growth, note carrying de-;
8., after crystal growth weight reaches weight of loading, substantially can judge that crystal growth arrives coda;
9. crystal weight is always constant, and growth curve changes not quite always, and seed rod pulling rate improves;
10. in above-mentioned parameter operating process, crystal weight is always constant, and crystal can enter brilliant footpath and tungsten crucible 95 separation phase.
I, brilliant footpath are separated with tungsten crucible 95;
1., after crystal production completes, system enters brilliant footpath and tungsten crucible 95 separation phase automatically;
2. brilliant footpath is separated in rear process with tungsten crucible 95, will operate in strict accordance with system parameter settings value;
3. the situation of observing when crystal footpath is separated with tungsten crucible 95 more;
4. the important parameter such as weight of power, time, crystal when brilliant footpath is separated with tungsten crucible 95, will be noted;
5. brilliant footpath is separated with tungsten crucible 95 is the stage of eliminating crystals stress, is also the process slowly declined by crystalline temp;
6., when brilliant footpath and tungsten crucible 95 separative power reach 0KW, annealing terminates.
J, cooling take out crystal;
1. brilliant footpath is separated after end with crucible, puts to normal atmosphere, opens bell, naturally cooling by body of heater internal gas pressure;
2., after naturally cooling reaches 36h, detect the temperature of plane of crystal with infrared temperature-measuring gun;
3., after determining that plane of crystal temperature is within safety temperature, take out crystal;
4. the crystal of taking-up is transferred quality inspection together with recorder;
5., after quality inspection Primary Evaluation, finished product crystal is put in storage.
The above preferred embodiment of the present invention; not in order to limit the present invention; all any amendments done within the spirit and principles in the present invention, etc. same sapphire crystallization furnace thermal field and be provided with the brilliant stove of length of this thermal field and the improvement etc. of long brilliant process structure thereof, all should be included within protection scope of the present invention.

Claims (10)

1. sapphire crystallization furnace thermal field, comprise stainless steel cask, tungsten cylinder is provided with in described stainless steel cask, heating basket assembly is provided with in described tungsten cylinder, be provided with crucible in described heating basket assembly, it is characterized in that, the bottom in described tungsten cylinder is provided with crucible holder, described crucible is arranged on described crucible holder, is provided with lower heat insulation molybdenum shield between described crucible holder and described tungsten cylinder inwall; Also comprise seed chuck assembly, described seed chuck assembly comprises seed rod, and described seed rod is suspended in described heating basket assembly, and described seed rod stretches in described crucible.
2. sapphire crystallization furnace thermal field according to claim 1, is characterized in that, described lower heat insulation molybdenum shield is provided with Zirconium oxide fibre base plate.
3. sapphire crystallization furnace thermal field according to claim 1 and 2, is characterized in that, described lower heat insulation molybdenum shield is provided with interlayer, and described Zirconium oxide fibre base plate is fixed in described interlayer.
4. a sapphire crystallization furnace, is characterized in that, comprises the sapphire crystallization furnace thermal field described in any one of claims 1 to 3.
5. sapphire crystallization furnace according to claim 4, is characterized in that, is provided with well heater, thermal insulation layer, body of heater inner casing and body of heater shell outside the described stainless steel cask of described sapphire crystallization furnace thermal field successively.
6. sapphire crystallization furnace according to claim 5, is characterized in that, described thermal insulation layer selects zirconium white material.
7. sapphire crystallization furnace according to claim 5, it is characterized in that, also comprise intelligent control system, described intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with described CPU module, described CPU module is also electrically connected with the described heating basket assembly of described well heater and described sapphire crystallization furnace respectively, described power module is electrically connected with electrical network, it is characterized in that, described intelligent control system also comprises photovoltaic cell component, described photovoltaic cell component is electrically connected with described power module by photovoltaic processing module.
8. sapphire crystallization furnace according to claim 5, also comprise intelligent control system, described intelligent control system comprises CPU module and the power module of electrical connection, also comprise the control panel be electrically connected with described CPU module, described CPU module is also electrically connected with the described heating basket assembly of described well heater and described sapphire crystallization furnace respectively, described power module is electrically connected with electrical network, it is characterized in that, described intelligent control system also comprises wind energy system, and described wind energy system is electrically connected with described power module by inverter.
9. the sapphire crystallization furnace according to claim 7 or 8, is characterized in that, also comprises the seed chuck Component driver portion be electrically connected with described CPU module, and described seed chuck Component driver portion and described seed chuck assembly are in transmission connection.
10. the brilliant technique of the length of sapphire crystallization furnace according to claim 4, comprises step: get the raw materials ready, and prepares three pure dichlorine monoxides as raw material, it is characterized in that, further comprising the steps of:
S (5), filler and frame are brilliant, are packed into by described aluminium sesquioxide in the described crucible of described sapphire crystallization furnace thermal field, and are clipped in by crystal seed on the described seed rod of described seed chuck assembly of described sapphire crystallization furnace thermal field;
S (10), to vacuumize, vacuum in the described stainless steel cask making described sapphire crystallization furnace thermal field;
S (15), heating, start described sapphire crystallization furnace to described sapphire crystallization furnace thermal field heating;
S (20), melting sources, when the power in described sapphire crystallization furnace thermal field is in 501 ~ 505KW power range, described aluminium sesquioxide be melted into liquid; When temperature in the described tungsten cylinder of described sapphire crystallization furnace thermal field falls into 2030 ° ~ 2050 ° of scopes, carry out seeding;
S (25), welding crystal seed, the described seed chuck assembly of described sapphire crystallization furnace thermal field makes seed crystal decline close to described aluminium sesquioxide liquid level, then contacts described aluminium sesquioxide liquid level, then mentions seed crystal; Repetition aforesaid operations completes washes crystalline substance; After washing crystalline substance, under seed crystal being dropped to described aluminium sesquioxide liquid level, carry out welding crystal seed; When carrying out described welding crystal seed, the power range in described sapphire crystallization furnace thermal field is 500 ~ 504KW;
S (30), brilliant Diameter growth, after welding crystal seed, the described seed chuck assembly of described sapphire crystallization furnace thermal field continues lift, makes the diameter of crystal become large, until crystal weight is in 5 ~ 10KG weight range;
S (35), crystal growth, crystal enters the production phase from growth phase, according to the pace of change of crystal weight in process of growth, adjusts the power in described sapphire crystallization furnace thermal field; Crystal weight continues constant production and completes;
S (40), brilliant footpath are separated with crucible, make the described seed chuck assembly pull-up of described sapphire crystallization furnace thermal field, are separated in brilliant footpath with crucible;
Crystal is taken out in S (50), cooling, when the described stainless steel cask internal pressure of described sapphire crystallization furnace thermal field is normal atmosphere, opens the described stainless steel cask naturally cooling of described sapphire crystallization furnace thermal field, after 36 hours, takes out crystal.
CN201510676049.3A 2015-10-16 2015-10-16 Sapphire crystal growing furnace heat field, crystal growing furnace with heat field and crystal growing process of crystal growing furnace Pending CN105177711A (en)

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CN113584572B (en) * 2019-08-21 2022-05-10 眉山博雅新材料股份有限公司 Crystal preparation device
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CN116949557B (en) * 2023-09-18 2024-02-13 内蒙古晶环电子材料有限公司 Thermal insulation structure and sapphire crystal growth furnace

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