CN104651934B - A kind of energy-saving sapphire crystal growing furnace - Google Patents
A kind of energy-saving sapphire crystal growing furnace Download PDFInfo
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- CN104651934B CN104651934B CN201510043615.7A CN201510043615A CN104651934B CN 104651934 B CN104651934 B CN 104651934B CN 201510043615 A CN201510043615 A CN 201510043615A CN 104651934 B CN104651934 B CN 104651934B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
Abstract
A kind of energy-saving sapphire crystal growing furnace, crucible is provided with the furnace chamber of growth furnace and clamps the supporting rod of seed crystal rod, crucible and the seed crystal rod controls it to move up and down by crucible lift device and seed crystal rod lowering or hoisting gear respectively, to ensure that the liquid level of the crucible internal oxidition aluminum melt in crystal growing process remains at an identical position；Demarcation strip is set to be divided into cold air chamber and hot gas room two parts in body of heater, along with seed crystal rod and the part of alumina melt four form four temperature fields, by the temperature in four temperature fields of thermocouple monitoring and it is adjusted, to make it have optimal thermograde, so as to accurately control solid liquid interface temperature, the optimal thermal field mode of crystal growth is improved, and then finds crystal growth optimal path, in favor of improving rate of crystalline growth and crystal growth quality.
Description
Technical field
The present invention relates to the preparation field of sapphire crystal, specifically a kind of energy-saving sapphire crystal growth
Stove.
Background technology
Sapphire composition is aluminum oxide（Al2O3）, it is to be combined by three oxygen atoms and two aluminium atoms with covalent bond pattern
The hexagonal lattice structure formed.Because sapphire has the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, high light transmittance, high-melting-point
（2045℃）The features such as.Because its unique lattice structure, excellent machinery and optical property, sapphire crystal are widely used
In various fields such as large scale integrated circuit, LED substrate material, infrared facility, the radium-shine eyeglasses of high intensity.Semiconductor shines in recent years
The fast development of bright industry, the rapid growth of sapphire demand and the continuous development of crystal technique are promoted.
At present, it is melt method to apply and study in the world widest sapphire crystal growth technology, including flame melt method, is carried
Daraf(reciprocal of farad), heat-exchanging method, kyropoulos, EFG technique, Bridgman-Stockbarger method and vertical-horizontal thermograde cooling method etc..Flame melt method is with pure
Net Al2O3Powder is raw material, using oxyhydrogen flame as thermal source, the Al positioned at device top2O3Powder leads to during being scattered downwards
Cross high-temperature region caused by oxyhydrogen flame and be heated melting, the raw material of melting, which falls on the seed crystal top of lower section and gradually crystallized, grows up to indigo plant
Gem crystal, flame melt method equipment is simple, and rate of crystalline growth is fast, but the Crystalline Quality grown is poor, stress is big, because
This, the sapphire crystal produced in this way is mainly for the manufacture of cheap jewel and wear-resistant element etc.；Lifting
Method be by form crystal raw material be placed in crucible heat fusing, connect seed crystal in bath surface, under controlled conditions, make seed crystal and
Melt constantly carries out rearranging for atom or molecule on interface, with cooling gradually solidification and go out monocrystal, its is main
Advantage is：The growing state of crystal can be easily observed during growth；Crystal grows at bath surface, without with
Crucible is in contact, and can so significantly reduce the stress of crystal, and prevents the parasitic nucleation of sidewall of crucible；Can be easily using fixed
To seed crystal and " necking down " technique, its dislocation density substantially reduces；Crystal has relatively low dislocation density, higher optical-quality homogeneous
Property.Shortcoming is that cost is higher, and crystal diameter is by a definite limitation；Heat-exchanging method is a kind of low-temperature gradient growing method,
Crucible, thermal field and crystal move without any physics, and the growth of crystal fully relies on the thermograde that furnace binding is formed,
Seed crystal is placed in crucible bottom, and by controlling the helium gas flow of crucible bottom to ensure that seed crystal is in low-temperature space, the raw material in crucible is complete
After portion's fusing, it is ensured that seed crystal, by increasing the flow of helium, makes low-temperature space only with melt preferably welding without all being melted
Gradually expand upwards, so that solid liquid interface moves up, heat-exchanging method by controlling heating power except adjusting thermal field temperature
It is outside one's consideration, the cooldown rate of crystal can also be controlled by controlling helium gas flow, the method advantage is：With accurate temperature control
System, can obtain the large-size crystals of high quality, and the defects of crystal and residual stress is relatively low.The weak point of heat-exchanging method is to need
Substantial amounts of helium is consumed, cost is higher, and growth cycle is longer；Kyropoulos are the seed crystal and melt contacts that one is cooled, such as
The temperature at fruit interface is less than freezing point, then seed crystal starts to grow, in order that crystal is constantly grown up, it is necessary to gradually reduces melt
Temperature, while rotating crystal, to improve the Temperature Distribution of melt.Slowly (or stage by stage) crystal can also be above carried, to expand
Big radiating surface.Crystal does not contact in growth course or at the end of growth with sidewall of crucible, and this greatly reduces the stress of crystal.
But, when crystal and remaining melt depart from, it will usually produce larger thermal shock.Kyropoulos are to apply most indigo plant at present
Jewel growing method, to improve growing efficiency and improving crystal mass, people propose a variety of evolutionary approach to kyropoulos,
The ES2 techniques of such as cold core shouldering micropulling technique and Rubicon companies.Rubicon was grown in 2009 with the method
Go out the 200kg sapphire crystal that weighs.This method and technology is ripe, and cost is relatively low, is adapted to produce in enormous quantities.Major defect is to need
The crystal grown draw cutting, bring certain labor content, and utilization rate of crystal is relatively low；EFG technique, it is
The mould for having slit is put into melt, melt rises to die tip by capillarity by slit, on this mould top
The melt position tripping in seed crystal at end, the shape then limited according to guided mode slit continuously grow crystal.By changing guided mode
Shape, the sapphire crystal of the various special shapes such as piece, rod, pipe, silk can be grown, it is numerous for sapphire crystal so as to eliminate
The procedures such as cutting, shaping, greatly reduce the loss of material, save process time, so that sapphire again
Cost significantly reduces.The outstanding advantages of EFG technique are to save material, can grow the material of various special shapes, but reduce defect
Level is its difficult point, and equipment construction is complicated；Bridgman-Stockbarger method is proposed by Chinese yunnan aquamaine Science and Technology Ltd..This method
Similar vertical Bridgman technique, using molybdenum crucible and induction heating mode, seed crystal is placed in crucible bottom.Raw material all melts
Afterwards, by seed crystal and the good welding of melt, thermograde then is obtained by driving crucible from high-temperature region to low-temperature space movement, is made
Solid liquid interface, which moves up, completes crystal growth.The uniformity of crystal can be improved by adding Melt Stirring device.The method
Major advantage be that crystal perfection is good, it is therefore, big straight in production simultaneously as crucible diameter is exactly obtained crystal diameter
Technique is complex during the crystal of footpath；Vertical-horizontal thermograde cooling method, the method is by South Korea STC (Sapphire
Technology Com) company's proposition.VHGF methods are that VGF techniques are applied to a kind of process of Sapphire Crystal Growth,
Similar to VGF techniques, crystal growth interface is realized by the thermograde of computer control vertically and horizontally both direction
It is mobile, it is not necessary to mechanical driving device.This method makes device structure simpler, improves the stability of crystal growth, can
To obtain the sapphire crystal of high integrality low stress.The crystal diameter of this method growth at present is 50~100mm (2 ~ 4 English
It is very little), length reaches 250mm (10 inches).STC Corporation supplies sapphire crystal since 2000, and VHGF methods are its exclusive patents
Technology, defect concentration is small, and material purity is high, and crystalline size and shape are relatively unrestricted, and comprehensive advantage is more apparent.
At present, the heater of the heating system of domestic and international crystal growing furnace is induction heating type graphite heater, resistance-type
The bar-shaped either netted graphite heater of hot type, resistance-type heating tungsten filament or tungsten plate heater, these heaters do not have cold end
With point in hot junction, energization feature is low-voltage, heavy current, changed power scope is big, conduction time is long, power consumption is big and maximum is born
Lotus is fluctuated.In addition, the crystal sintering furnace of above-mentioned making all can not accurately control solid liquid interface temperature in crystal growth, crystal
Growth course controls by experience completely, and the speed of crystal growth can not realize the accurate control of automation.
With the development of science and technology, market is more urgent to higher quality and the demand of larger sized sapphire crystal
Cut, therefore, how to produce high-quality, large size sapphire crystal simultaneously, reduce the cost of raw material, shorten the process time, save
Power cost turns into the urgent task that current Chang Jing enterprises face.
The content of the invention
For solve in the prior art high energy consumption, crystal growth temperature existing for sapphire production technology can not accuracy controlling lead
The problems such as crystal growth of cause is slow, of poor quality, the invention provides a kind of energy-saving sapphire crystal growing furnace.
The present invention be solve the technical scheme that uses of above-mentioned technical problem for：A kind of energy-saving sapphire crystal growing furnace,
Crucible is provided with the furnace chamber of growth furnace and clamps the supporting rod of seed crystal rod, crucible and the seed crystal rod is filled by crucible lifting respectively
Put and control it to move up and down with seed crystal rod lowering or hoisting gear, and seed crystal rod keeps the rotation of certain speed during moving up and down,
The demarcation strip of molybdenum system or tungsten, the earthenware are provided with the position of alumina melt liquid level flush in crucible in furnace chamber
Crucible is through the through hole on demarcation strip, so as to which relative motion occur with demarcation strip under the control of crucible lift device, with ensure with
While the lifting of seed crystal rod, the liquid level flush of demarcation strip and crucible internal oxidition aluminum melt is remained；The demarcation strip will
The cold air chamber on top and the hot gas room of bottom are separated into furnace chamber, be provided with cold air chamber cold air field thermocouple, cold air inlet and
Cold air outlet, cold air indoor temperature is determined by cold air field thermocouple, and input is cold into it from cold air inlet and cold air outlet
Gas is circulated to adjust the temperature of cold air chamber, seed crystal rod and alumina melt liquid level；In the upper surface of demarcation strip and hot gas
It is indoor to set thermocouple to be monitored with the temperature to both respectively；Press close at the outer wall of crucible bottom to be provided with female fan-shaped chamber
Room, the thermocouple for measuring the chamber indoor temperature is provided with it, its testing result is equivalent to the temperature of alumina melt.
Temperature adjustment is realized in the hot gas room by the heater set in it, and heater is U-shaped ZrB2Ceramics-graphite
Heater is combined, the combination heater is made up of the hot junction of two cold ends and a connection cold end, and cold end is by ZrB2Ceramics system
Into hot junction is made up of graphite, and cold end wiring water cooling plant is provided with cold end wiring, to reduce the temperature at cold end wiring.
Cooling water circulation pipeline is provided with the supporting rod, to carry out temperature control to supporting rod and seed crystal rod.
The observation window of observation crucible and seed crystal rod is offered on the growth furnace furnace wall.
Cold air field of the present invention thermocouple is superhigh temperature special alloy thermocouple（0-1800 DEG C of temperature-measuring range）, hot gas
Indoor thermocouple is superhigh temperature composite ceramics thermocouple（0-2200 DEG C of temperature-measuring range）, the thermocouple on demarcation strip answers for high temperature
Close ceramic electric thermo-couple（0-2200 DEG C of temperature-measuring range）, the thermocouple in female sector-shaped compartments is high temperature composite ceramics thermocouple（Survey
Warm 0-2200 DEG C of scope）.
In the present invention, demarcation strip will be separated into cold air chamber and hot gas room in stove, now, have four temperature fields in stove, the
One temperature field is the cold air chamber on top, and second temperature field is for the interface of growth crystal and melt contacts on seed crystal rod, the
Three temperature fields are the hot gas room of bottom, and the 4th temperature field is the alumina melt in crucible, and the temperature in four temperature fields is equal
Differ.In order to determine the temperature in four temperature fields, superhigh temperature special alloy thermocouple is set in cold air chamber（Temperature-measuring range 0-
1800℃）, superhigh temperature composite ceramics thermocouple is set in hot gas room（0-2200 DEG C of temperature-measuring range）, in the upper plane of demarcation strip
One high temperature composite ceramics thermocouple is set（0-2200 DEG C of temperature-measuring range）, press close to crucible in crucible liquid part outer wall（From earthenware
Crucible 1-3mm）Place sets a female fan cavity, and female fan cavity connects a metal tube, and metal tube is fixed on furnace wall,
One high temperature composite ceramics thermocouple is set in female fan cavity（0-2200 DEG C of temperature-measuring range）, for determining liquid in crucible
With the temperature between hot gas field, this temperature can determine the temperature of liquid in crucible indirectly.Pass through four temperature fields of measure
Temperature, the optimal thermal field mode of crystal growth with relatively accurate control solid liquid interface temperature, can be improved, so as to improve crystal growth
Optimal path.
The thermocouple uses ZrB2Composite ceramic temperature sensor either ZrC composite ceramic temperature sensors, it has
There is temperature measurement accuracy height, accurately and reliably.Sensor temperature measuring point is the cold air on crucible top, the middle part of crucible（That is solid liquid interface
Outside）, the outer hot gas of crucible bottom wall and crucible lower liquid crystal outside it is convex it is fan-shaped it is empty it is small between, after amendment, warp
The temperature of four key positions in whole thermal field can be determined by crossing demarcation.By determining the temperature in four temperature fields, Ke Yixiang
To accurately controlling solid liquid interface temperature, the optimal thermal field mode of crystal growth is improved, so as to improve crystal growth optimal path, with
Beneficial to raising rate of crystalline growth and crystal growth quality.
The heater used in the present invention is U-shaped ZrB2Ceramics-graphite combination heater, U-shaped ZrB2Ceramics-graphite heating
Element can be arranged on around crucible and bottom, can effectively improve the temperature homogeneity of high temperature thermal field, can be accurately
The temperature of high temperature thermal field is controlled, improves the sintering quality of product；ZrB2Ceramics-graphite combines heater by two cold ends and one
The hot junction for connecting cold end is formed, and cold end is by electric conductivity is preferable, resistant to elevated temperatures ZrB2Ceramics are prepared, and hot junction is made up of graphite,
The resistance of isometrical graphite is ZrB2More than 100 times of ceramic resistor, after energization, graphite is easy to generate heat, and it has control accuracy
Height, heater heating efficiency is higher, and energy consumption is small, energy saving.According to Conventional wisdom, different heat body resistivity, energy loss
It is that different, different principle of heating heating efficiency is also different with heating efficiency.The cold end of heater and hot junction electricity
Resistance difference is bigger, and heating power is bigger, and electrothermal calefactive rate is faster, and practical experience is learnt, ZrB2Ceramics-graphite combining structure heating
Element is compared with the induction furnace, traditional graphite heater resistance furnace and molybdenum wire furnace of same specification, energy-conservation more than 50%.
In U-shaped ZrB2The cold end of ceramics-graphite combination heater is provided with cold end wiring hydrologic cycle cooling system, is used for
Reduce the temperature of cold end terminals.
Crucible lift device of the present invention can be such that crucible constantly rises, and remain at liquid interface in crucible
Fixed position, during crystalline growth, seed crystal increase liquid interface declines, and passes through the crucible lift device and seed set outside body of heater
Crystal bar lowering or hoisting gear lifts crucible and draws high crystal bar, so that the alumina melt liquid level in crucible remains at and demarcation strip water
Flat position.
It is first that 99.995% high purity aluminium oxide raw material pre-processes to content, warp during sapphire produces
The alpha-alumina crystals block and oriented seed crystal for crossing pretreatment are put into crucible, are then moved in crystal growing furnace, start startup power supply,
Vacuum pump set is first opened, is evacuated to 10-3Pa, keep under vacuum state, start to warm up to 500-600 DEG C, pour inertia protection
Gas, 2100-2150 DEG C is continuously heating to, is incubated 4-6 hours, the accurate temperature of thermal field that adjusts makes crystal bar and liquid crystal contact surface
Just part is melted, and crystal starts slowly to grow.
Beneficial effect：The present invention has advantages below compared with the crystal growing furnace of prior art：
1）Using ZrB2Ceramics-graphite combination heater, compared with traditional graphite heater resistance furnace and molybdenum wire furnace, section
Energy more than 50%；
2）Thermocouple uses ZrB2Composite ceramic temperature sensor either ZrC composite ceramic temperature sensors, are improved
The precision of thermometric is high；
3）Four temperature fields are separated into body of heater, by the temperature in four temperature fields of thermocouple monitoring and are adjusted, with
Optimal thermograde is made it have, so as to accurately control solid liquid interface temperature, the optimal thermal field mode of crystal growth is improved, enters
And crystal growth optimal path is found, in favor of improving rate of crystalline growth and crystal growth quality；
4）Coordinated by crucible lift device and seed crystal rod lowering or hoisting gear so that the liquid level of crucible internal oxidition aluminum melt（I.e.
Crystal growth position）A position is remained at, in order to accurately control its temperature, so as to the growth beneficial to crystal.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention；
Reference：1st, growth furnace, 2, crucible, 3, seed crystal rod, 4, supporting rod, 401, cooling water circulation pipeline, 5, crucible
Lowering or hoisting gear, 6, seed crystal rod lowering or hoisting gear, 7, demarcation strip, 8, cold air chamber, 801, cold air field thermocouple, 802, cold air inlet,
803rd, cold air outlet, 9, hot gas room, 901, chamber, 902, heater, 10, alumina melt, 11, observation window.
Embodiment
As illustrated, a kind of energy-saving sapphire crystal growing furnace, crucible 2 and clamping are provided with the furnace chamber of growth furnace 1
The supporting rod 4 of seed crystal rod 3, the crucible 2 and seed crystal rod 3 control it by crucible lift device 5 and seed crystal rod lowering or hoisting gear 6 respectively
Move up and down, and seed crystal rod 3 keeps the rotation of certain speed during moving up and down, in furnace chamber with aluminum oxide in crucible 2
The opening position of the liquid level flush of melt 10 is provided with the demarcation strip 7 of molybdenum system or tungsten, and the crucible 2 is passed through on demarcation strip 7
Through hole, so as to which relative motion occur with demarcation strip 7 under the control of crucible lift device 5, to ensure to be lifted with seed crystal rod 3
While, remain the liquid level flush of demarcation strip 7 and the internal oxidition aluminum melt 10 of crucible 2；The demarcation strip 7 is by furnace chamber points
The cold air chamber 8 on top and the hot gas room 9 of bottom are divided into, cold air field thermocouple 801, the and of cold air inlet 802 are provided with cold air chamber 8
Cold air outlet 803, temperature in cold air chamber 8 is determined by cold air field thermocouple 801, and by cold air inlet 802 and cold air outlet 803
Input cold air is circulated to adjust the temperature of cold air chamber 8, seed crystal rod 3 and the liquid level of alumina melt 10 in it；Separating
The upper surface of plate 7 with setting thermocouple to be monitored with the temperature to both respectively in hot gas room 9；Press close to the outer of the bottom of crucible 2
Female sector-shaped compartments 901 are provided with wall, the thermocouple for measuring temperature in the chamber 901 is provided with it, is detected knot
Fruit is equivalent to the temperature of alumina melt 10；
Temperature adjustment is realized in the hot gas room 9 by the heater 902 set in it, and heater 902 is U-shaped ZrB2Pottery
Porcelain-graphite combination heater, the combination heater is made up of the hot junction of two cold ends and a connection cold end, and cold end is by ZrB2
Ceramics are made, and hot junction is made up of graphite, and cold end wiring water cooling plant is provided with cold end wiring, to reduce at cold end wiring
Temperature；
Cooling water circulation pipeline 401 is provided with the supporting rod 4, to enter trip temperature control to supporting rod 4 and seed crystal rod 3
System；
The observation window 11 of observation crucible 2 and seed crystal rod 3 is offered on the furnace wall of growth furnace 1.
Claims (3)
1. a kind of energy-saving sapphire crystal growing furnace, growth furnace（1）Furnace chamber in be provided with crucible（2）With clamping seed crystal rod
（3）Supporting rod（4）, the crucible（2）With seed crystal rod（3）Respectively by crucible lift device（5）With seed crystal rod lowering or hoisting gear（6）
It is controlled to move up and down, and seed crystal rod（3）The rotation of certain speed, growth furnace are kept during moving up and down（1）On furnace wall
Offer observation crucible（2）And seed crystal rod（3）Observation window（11）, it is characterised in that：The supporting rod（4）Inside it is provided with cooling
Water circulating pipe（401）, with to supporting rod（4）With seed crystal rod（3）Carry out temperature control；In furnace chamber and crucible（2）Middle oxidation
Aluminum melt（10）The opening position of liquid level flush is provided with the demarcation strip of molybdenum system or tungsten（7）, the crucible（2）Through point
Dividing plate（7）On through hole, so as in crucible lift device（5）Control under and demarcation strip（7）Generation relative motion, with ensure with
Seed crystal rod（3）While lifting, demarcation strip is remained（7）With crucible（2）Internal oxidition aluminum melt（10）Liquid level flush；
The demarcation strip（7）The cold air chamber on top will be separated into furnace chamber（8）With the hot gas room of bottom（9）, now, there are four in stove
Temperature field, first temperature field are the cold air chamber on top（8）, second temperature field is seed crystal rod（3）Upper grown crystal is with melting
The interface of body contact, the 3rd temperature field are the hot gas room of bottom（9）, the 4th temperature field is crucible（2）Interior aluminum oxide melts
Body（10）, cold air chamber（8）Inside it is provided with cold air field thermocouple（801）, cold air inlet（802）And cold air outlet（803）, by cold
Gas field thermocouple（801）Determine cold air chamber（8）Interior temperature, and by cold air inlet（802）And cold air outlet（803）Inputted in it
Cold air is circulated to adjust cold air chamber（8）, seed crystal rod（3）And alumina melt（10）The temperature of liquid level；In demarcation strip（7）
Upper surface and hot gas room（9）Inside thermocouple is set to be monitored with the temperature to both respectively；Press close to crucible（2）Outside bottom
Female sector-shaped compartments are provided with wall（901）, it is provided with it and measures the chamber（901）The thermocouple of interior temperature, is examined
Survey result and be equivalent to alumina melt（10）Temperature, by determine four temperature fields temperature, accurately to control solid liquid interface
Temperature, so as to improve rate of crystalline growth.
A kind of 2. energy-saving sapphire crystal growing furnace according to claim 1, it is characterised in that：The hot gas room（9）
By the heater set in it（902）Realize temperature adjustment, and heater（902）For U-shaped ZrB2Ceramics-graphite combination heating
Body, the combination heater is made up of the hot junction of two cold ends and a connection cold end, and cold end is by ZrB2Ceramics are made, hot junction by
Graphite is made, and cold end wiring water cooling plant is provided with cold end wiring, to reduce the temperature at cold end wiring.
A kind of 3. energy-saving sapphire crystal growing furnace according to claim 1, it is characterised in that：Cold air field thermoelectricity
It is even（801）For 0-1800 DEG C of superhigh temperature special alloy thermocouple of temperature-measuring range, demarcation strip（7）The thermocouple set on upper surface
For 0-2200 DEG C of high temperature composite ceramics thermocouple of temperature-measuring range, hot gas room（9）The thermocouple of interior setting is temperature-measuring range 0-
2200 DEG C of superhigh temperature composite ceramics thermocouple, female sector-shaped compartments（901）The thermocouple of interior setting is temperature-measuring range 0-2200
DEG C high temperature composite ceramics thermocouple.
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| CN201510043615.7A CN104651934B (en) | 2014-10-17 | 2015-01-29 | A kind of energy-saving sapphire crystal growing furnace |
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| CN201410551530 | 2014-10-17 | ||
| CN201510043615.7A CN104651934B (en) | 2014-10-17 | 2015-01-29 | A kind of energy-saving sapphire crystal growing furnace |
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| CN104651934B true CN104651934B (en) | 2017-12-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386125A (en) * | 2015-12-03 | 2016-03-09 | 河南西格马晶体科技有限公司 | Control method for preparation of sapphire monocrystal |
| CN105401213A (en) * | 2015-12-03 | 2016-03-16 | 河南西格马晶体科技有限公司 | Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method |
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