A kind of energy-saving sapphire crystal growing furnace
Technical field
The present invention relates to the preparation field of sapphire crystal, specifically a kind of energy-saving sapphire crystal growing furnace.
Background technology
Sapphirely consist of aluminum oxide (Al
2o
3), be the hexagonal lattice structure be combined into covalent linkage pattern by three Sauerstoffatoms and two aluminium atoms.Because sapphire has the high velocity of sound, high temperature resistant, anticorrosive, the feature such as high rigidity, high light transmittance, high-melting-point (2045 DEG C).Due to the crystalline network of its uniqueness, excellent machinery and optical property, sapphire crystal is widely used in the various fields such as large-scale integrated circuit, LED substrate material, infrared facility, the radium-shine eyeglass of high strength.The fast development of semiconductor lighting industry in recent years, has promoted the quick growth of sapphire demand and the development of crystal technique.
At present, in the world application and research the most widely sapphire crystal growth technology be melting method, comprise flame melt method, crystal pulling method, heat-exchanging method, kyropoulos, EFG technique, falling crucible method and vertical-horizontal thermograde method of cooling etc.Flame melt method is with pure Al
2o
3powder is raw material, is thermal source, is positioned at the Al on device top with oxyhydrogen flame
2o
3the high-temperature zone produced by oxyhydrogen flame in the process that powder scatters downwards by heating and melting, the raw material of melting drop on below seed crystal top and gradually crystallization grow up to sapphire crystal, flame melt method equipment is simple, crystalline growth velocity is fast, but the Crystalline Quality grown is poor, stress is large, therefore, the sapphire crystal produced in this way is mainly for the manufacture of the jewel and wear-resistant element etc. of cheapness; Crystal pulling method is that the raw material forming crystal is placed on heat fused in crucible, seed crystal is connect at bath surface, under controlled conditions, make seed crystal and melt on interface, constantly carry out rearranging of atom or molecule, solidify gradually with cooling and go out single crystal, its major advantage is: can observe the growing state of crystal easily in the process of growth; Crystal in the growth of bath surface place, and does not contact with crucible, can reduce the stress of crystal so significantly, and prevent the parasitic nucleation of sidewall of crucible; Can use oriented seed and " necking down " technique easily, its dislocation desity reduces greatly; Crystal has lower dislocation desity, higher optical homogeneity.Shortcoming is that cost is higher, and crystal diameter is subject to a definite limitation, heat-exchanging method is a kind of low-temperature gradient growing method, crucible, thermal field and crystal all move without the need to any physics, the thermograde that the growth of crystal relies on furnace binding to be formed completely, seed crystal is placed in crucible bottom, ensure that seed crystal is in cold zone by the helium gas flow controlling crucible bottom, after raw material in crucible all melts, guarantee seed crystal only with melt welding preferably and all not melted, by strengthening the flow of helium, cold zone is upwards expanded gradually, thus solid-liquid interface is moved up, heat-exchanging method is except regulating temperature of thermal field by control heating power, the rate of cooling of crystal can also be controlled by controlling helium gas flow, this method advantage is: have temperature accurately and control, high-quality large-size crystals can be obtained, defect and the residual stress of crystal are lower.The weak point of heat-exchanging method needs to consume a large amount of helium, and cost is higher, and growth cycle is longer; Kyropoulos is the seed crystal and melt contacts of catching a cold one, if the temperature at interface is lower than zero pour, then seed crystal starts growth, in order to make crystal constantly grow up, just needs the temperature reducing melt gradually, simultaneously rotating crystal, to improve the temperature distribution of melt.Also slowly (or stage by stage) can carry crystal, to expand radiating surface.Crystal does not contact with sidewall of crucible in process of growth or at the end of growth, this greatly reduces the stress of crystal.But, when crystal and remaining melt depart from, usually larger thermal shocking can be produced.Kyropoulos is the sapphire growth method that at present application is maximum, is improve growing efficiency and improve crystal mass, and people propose multiple evolutionary approach to kyropoulos, as the ES2 technique etc. of cold core shouldering micropulling technique and Rubicon company.Rubicon grew the sapphire crystal of the 200kg that weighs in 2009 by this method.This method and technology is ripe, and cost is lower, is applicable to producing in enormous quantities.Main drawback needs to draw the crystal grown to cut, and bring certain labor content, and crystal utilization ratio is lower; EFG technique, be to have the mould of slit to put in melt, melt rises to die tip by capillary phenomenon by slit, under the melt position of this die tip, enter seed crystal, then according to the continuous growing crystal of shape that guided mode slit limits.By changing the shape of guided mode, the sapphire crystal of the various special shapes such as sheet, rod, pipe, silk can be grown, thus eliminate for the heavy cutting of sapphire crystal, the work program such as shaping, greatly reduce the loss of material, save process period, thus sapphire cost is significantly reduced.The outstanding advantages of EFG technique saves material, can grow the material of various special shape, but reduction defect level is its difficult point, and equipment complex structure; Falling crucible method is proposed by Chinese yunnan aquamaine Science and Technology Ltd..The similar vertical Bridgman technique of the method, adopt molybdenum crucible and induction heating mode, seed crystal is placed in crucible bottom.After raw material all melts, by seed crystal and the good welding of melt, then obtain thermograde by driving crucible to move from high-temperature zone to cold zone, solid-liquid interface has been moved up crystal growth.The homogeneity of crystal can be improved by adding Melt Stirring device.The major advantage of this method is that perfection of crystal is good, and meanwhile, because crucible diameter is exactly the crystal diameter obtained, therefore, when production major diameter crystal, technique is comparatively complicated; Vertical-horizontal thermograde method of cooling, this method is proposed by Korea S STC (Sapphire Technology Com) company.VHGF method is by a kind of processing method of VGF process application in Sapphire Crystal Growth, and be similar to VGF technique, thermograde that is vertical by computer control and horizontal both direction realizes the movement of crystal growth interface, does not need mechanical drive.This method makes device structure more simple, improves the stability of crystal growth, can obtain the sapphire crystal of high integrality low-stress.The crystal diameter of current the method growth is 50 ~ 100mm (2 ~ 4 inches), and length reaches 250mm (10 inches).STC Corporation started to supply sapphire crystal from 2000, and VHGF method is its exclusive patented technology, and defect concentration is little, and material purity is high, and crystalline size and shape relatively unrestricted, comprehensive advantage is more obvious.
At present, the heating element of the heating system of domestic and international crystal growing furnace is induction heating type graphite heater, resistance-type hot type bar-shaped or netted graphite heater, resistance-type heating tungsten filament or tungsten plate heating element, these heating elements do not have cold junction and hot junction point, energising feature is low voltage, strong current, variable power scope is large, conduction time is long, current consumption is large and maximum load is fluctuated.In addition, the crystal sintering oven of above-mentioned making all accurately cannot control solid-liquid interface temperature in crystal growth, and crystal growing process controls by experience completely, and the speed of crystal growth cannot realize automatization and accurately control.
Along with the development of science and technology, the demand of market to more high-quality and larger sized sapphire crystal is more urgent, therefore, simultaneously, reduction material cost, shortening process time, conservation of power cost become the urgent task that current Chang Jing enterprise faces for how production high-quality, large size sapphire crystal.
Summary of the invention
In order to solve, the energy consumption that sapphire production technique exists in prior art is high, crystal growth temperature cannot the problems such as the crystal growth that causes of accuracy controlling is slow, of poor quality, the invention provides a kind of energy-saving sapphire crystal growing furnace.
The present invention is the technical scheme solving the problems of the technologies described above employing: a kind of energy-saving sapphire crystal growing furnace, the supporting rod of crucible and clamping seed crystal rod is provided with in the furnace chamber of growth furnace, described crucible and seed crystal rod control it by crucible lift device and seed crystal rod lifting device respectively and move up and down, and seed crystal rod is moving up and down in process the rotation keeping certain speed, position mutually concordant with alumina melt liquid level in crucible in furnace chamber is provided with the division plate of molybdenum system or tungsten, described crucible is through the through hole on division plate, thus under the control of crucible lift device with division plate generation relative movement, to ensure along with while the lifting of seed crystal rod, remain that division plate is mutually concordant with the liquid level of crucible internal oxidition molten aluminium, described division plate is by the hot gas room of the cold air chamber and bottom that are separated into top in furnace chamber, cold air field thermopair, cold air inlet and cold air outlet is provided with in cold air chamber, by cold air field thermocouple measurement cold air room temp, and by cold air inlet and cold air outlet to the temperature inputting cold air in it and carry out circulating to regulate cold air chamber, seed crystal rod and alumina melt liquid level, at the upper surface of division plate and hot gas indoor, thermopair is set respectively to monitor both temperature, the outer wall place pressing close to crucible bottom is provided with female sector-shaped compartments, is provided with the thermopair measuring this chamber room temp, its detected result to be equivalent to the temperature of alumina melt in it.
Described hot gas room relies on the heating element arranged in it to realize temperature and regulates, and heating element is U-shaped ZrB
2pottery-graphite combination heating element, this combination heating element is made up of with a hot junction being connected cold junction two cold junctions, and cold junction is by ZrB
2pottery is made, and hot junction is made up of graphite, and cold junction wiring place is provided with cold junction wiring water cooling plant, to reduce the temperature of cold junction wiring place.
Cooling water circulation pipeline is provided with, to carry out temperature control to supporting rod and seed crystal rod in described supporting rod.
Described growth furnace furnace wall offers the viewing window observing crucible and seed crystal rod.
Cold air field of the present invention thermopair is ultrahigh-temperature special alloy thermopair (temperature-measuring range 0-1800 DEG C), the thermopair of hot gas indoor is ultrahigh-temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C), thermopair on division plate is high temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C), and the thermopair in female sector-shaped compartments is high temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C).
In the present invention, division plate will be separated into cold air chamber and hot gas room in stove, now, there are in stove four temperature fields, first temperature field is the cold air chamber on top, the interface that second temperature field is institute's growing crystal and melt contacts on seed crystal rod, and the 3rd temperature field is the hot gas room of bottom, 4th temperature field is the alumina melt in crucible, and the temperature in four temperature fields is all not identical.In order to measure the temperature in four temperature fields, at cold air chamber, ultrahigh-temperature special alloy thermopair (temperature-measuring range 0-1800 DEG C) is set, ultrahigh-temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C) is set in hot gas indoor, in the upper plane of division plate, a high temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C) is set, press close to crucible (from crucible 1-3mm) place at crucible liquid part outer wall and a female fan cavity is set, female fan cavity connects a metal tube, metal tube is fixed on furnace wall, a high temperature composite ceramics thermopair (temperature-measuring range 0-2200 DEG C) is set in female fan cavity, for measuring the temperature between liquid in crucible and hot gas field, this temperature can measure temperature liquid in crucible indirectly.By measuring the temperature in four temperature fields, can relatively accurate control solid-liquid interface temperature, improve the optimal heat field type of crystal growth, thus improve crystal growth optimal path.
Described thermopair adopts ZrB
2composite ceramic temperature sensor or ZrC composite ceramic temperature sensor, it is high that it has temperature measurement accuracy, accurately and reliably.Sensor point for measuring temperature be the cold air on crucible top, the middle part (i.e. the outside of solid-liquid interface) of crucible, the outer hot gas of crucible bottom wall and crucible the convex fan-shaped sky in outside of lower liquid crystal little between, after revising, through demarcating the temperature that can determine four key positions in whole thermal field.By measuring the temperature in four temperature fields, can relatively accurate control solid-liquid interface temperature, improve the optimal heat field type of crystal growth, thus improve crystal growth optimal path, be beneficial to improve crystalline growth velocity and crystal growth quality.
The heating element adopted in the present invention is U-shaped ZrB
2pottery-graphite combination heating element, U-shaped ZrB
2pottery-graphite heating component can be arranged on surrounding and the bottom of crucible, effectively can improve the temperature homogeneity of high temperature thermal field, accurately can control the temperature of high temperature thermal field, improves the sintering quality of product; ZrB
2pottery-graphite combination heating element is made up of with a hot junction being connected cold junction two cold junctions, better by electroconductibility, the resistant to elevated temperatures ZrB of cold junction
2ceramic preparation forms, and hot junction is made up of graphite, and the resistance of isometrical graphite is ZrB
2more than 100 times of ceramic resistor, after energising, graphite is easy to heating, and it is high that it has control accuracy, and heating element heating efficiency is higher, and energy consumption is little, energy saving.According to Conventional wisdom, different heat body resistivity, energy waste and heating efficiency are different, and different principle of heating heating efficiencies is also different.Cold junction and the hot junction resistance value difference of heating element are larger, and heating power is larger, and electrothermal calefactive rate is faster, and practical experience is learnt, ZrB
2pottery-graphite unitized construction Heating element is compared with molybdenum wire furnace with the induction furnace of same specification, traditional graphite heater resistance furnace, and energy-conservation more than 50%.
At U-shaped ZrB
2the cold junction of pottery-graphite combination heating element is provided with cold junction wiring hydrologic cycle cooling system, for reducing the temperature of cold junction terminals.
Crucible lift device of the present invention can make crucible constantly rise, liquid interface in crucible is made to remain at fixed position, in crystalline growth process, seed crystal increases liquid interface and declines, the crucible lift device arranged outward by body of heater and seed crystal rod lifting device are promoted crucible and draw high crystal bar, remain at the position with division plate level to make the alumina melt liquid level in crucible.
In the process that sapphire is produced, be first that 99.995% high purity aluminium oxide raw material carries out pre-treatment to content, through pretreated alpha-alumina crystals block with put into crucible through oriented seed, move to again in crystal growing furnace, start to start power supply, first open vacuum pump set, be evacuated to 10
-3pa, under keeping vacuum state, starts to be warming up to 500-600 DEG C, pours inert protective gas, continue to be warming up to 2100-2150 DEG C, insulation 4-6 hour, and accurately regulate temperature of thermal field to make crystal bar and liquid crystal contact surface just partial melting, crystal starts slow growth.
Beneficial effect: the present invention has the following advantages compared with the crystal growing furnace of prior art:
1) ZrB is adopted
2pottery-graphite combination heating element, compares with molybdenum wire furnace with traditional graphite heater resistance furnace, energy-conservation more than 50%;
2) thermopair adopts ZrB
2composite ceramic temperature sensor or ZrC composite ceramic temperature sensor, the precision that improve thermometric is high;
3) four temperature fields are separated in body of heater, regulated by the temperature in thermocouple monitoring four temperature fields, to make it have best thermograde, thus accurately control solid-liquid interface temperature, improve the optimal heat field type of crystal growth, and then find crystal growth optimal path, be beneficial to improve crystalline growth velocity and crystal growth quality;
4) coordinated by crucible lift device and seed crystal rod lifting device, make the liquid level of crucible internal oxidition molten aluminium (i.e. crystal growth position) remain at a position, so that accurately control its temperature, thus be beneficial to the growth of crystal.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Reference numeral: 1, growth furnace, 2, crucible, 3, seed crystal rod, 4, supporting rod, 401, cooling water circulation pipeline, 5, crucible lift device, 6, seed crystal rod lifting device, 7, division plate, 8, cold air chamber, 801, cold air field thermopair, 802, cold air inlet, 803, cold air outlet, 9, hot gas room, 901, chamber, 902, heating element, 10, alumina melt, 11, viewing window.
Embodiment
As shown in the figure, a kind of energy-saving sapphire crystal growing furnace, the supporting rod 4 of crucible 2 and clamping seed crystal rod 3 is provided with in the furnace chamber of growth furnace 1, described crucible 2 and seed crystal rod 3 control it by crucible lift device 5 and seed crystal rod lifting device 6 respectively and move up and down, and seed crystal rod 3 is moving up and down in process the rotation keeping certain speed, position mutually concordant with alumina melt 10 liquid level in crucible 2 in furnace chamber is provided with the division plate 7 of molybdenum system or tungsten, described crucible 2 is through the through hole on division plate 7, thus relative movement is there is with division plate 7 under the control of crucible lift device 5, to ensure along with while seed crystal rod 3 lifting, remain that division plate 7 is mutually concordant with the liquid level of crucible 2 internal oxidition molten aluminium 10, described division plate 7 is by the hot gas room 9 of the cold air chamber 8 and bottom that are separated into top in furnace chamber, cold air field thermopair 801, cold air inlet 802 and cold air outlet 803 is provided with in cold air chamber 8, measure temperature in cold air chamber 8 by cold air field thermopair 801, and by cold air inlet 802 and cold air outlet 803 to its in input the temperature that cold air carries out circulating to regulate cold air chamber 8, seed crystal rod 3 and alumina melt 10 liquid level, thermopair is set respectively in the upper surface and hot gas room 9 of division plate 7 to monitor both temperature, the outer wall place pressed close to bottom crucible 2 is provided with female sector-shaped compartments 901, is provided with the thermopair measuring temperature in this chamber 901, its detected result to be equivalent to the temperature of alumina melt 10 in it,
Described hot gas room 9 relies on the heating element 902 arranged in it to realize temperature and regulates, and heating element 902 is U-shaped ZrB
2pottery-graphite combination heating element, this combination heating element is made up of with a hot junction being connected cold junction two cold junctions, and cold junction is by ZrB
2pottery is made, and hot junction is made up of graphite, and cold junction wiring place is provided with cold junction wiring water cooling plant, to reduce the temperature of cold junction wiring place;
Cooling water circulation pipeline 401 is provided with, to carry out temperature control to supporting rod 4 and seed crystal rod 3 in described supporting rod 4;
Described growth furnace 1 furnace wall offers the viewing window 11 observing crucible 2 and seed crystal rod 3.