CN1323195C - Cold core shouldering micropulling proparation method of large size sapphire single crystal - Google Patents
Cold core shouldering micropulling proparation method of large size sapphire single crystal Download PDFInfo
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Abstract
The present invention relates to a method for growing sapphire single crystals, particularly to a cold core crystal formation micropulling method for growing sapphire single crystals, which is characterized in that the temperature of cooling water output is stabilized within the range of 15 DEG C to 35 DEG C during the technical process; vacuum pressure is not more than 6*10<-3>Pa during the whole technical process; a sapphire crystal is prepared in a special single crystal furnace by a tungsten heating body, a crucible, a tungsten molybdenum separating shield, and a high temperature component; raw material in the crucible is heated until the raw material is melted, according to the observation of the surface morphology of a liquid surface, the heating value of the heating body in the special single crystal furnace is regulated to ensure that the convection morphology of the liquid surface is stabilized; the heating regulation range of the heating body is 100 w/h to 2500 w/h; the relative deviation of the position of a cold core in a melt and the geometric center of the crucible is not more than phi 20.0mm; in the crystal seeding technical process, a seed crystal is slowly regulated to ensure that the lower end of the seed crystal is preheated at the point 5mm to 20mm above the liquid surface of the melt so that the thermal stress of the seed crystal is eliminated; the traditional crystal pulling method process is utilized to ensure that a crystallizing center is transferred to a cold core after 5 to 15 times of crystal seeding along the departure direction of the cold core and to ensure that a crystallizing end is symmetrical along the central axis of the seed crystal and begins crystal formation by being matched with rotation control of the shape of the crystallizing end, and the rotation speed is 2 round / minute to 16 round / minute.
Description
Technical field:
The present invention relates to the Sapphire Crystal Growth method, be specially a kind of cold core shouldering micropulling proparation method of large-size sapphire single-crystal.
Background technology:
Sapphire (α-Al
2O
3) claim white stone again, be that hardness is only second to adamantine crystalline material.It has, and hardness height (Mohs' hardness 9), high temperature resistant (fusing point reaches 2050 ℃), wear-resisting wiping, corrosion resistance are strong, and chemical property is stable, generally water insoluble, acid and alkali corrosion, series of characteristics such as translucidus energy, electrical insulation capability are good.Sapphire single-crystal can be applicable to the microwave tube medium, the ultrasonic wave transport element, retarding line, waveguide laser cavity and precision instrument bearing, the window of heating panel, obnoxious flavour detector and the fire monitoring instrument of the window material of optical element such as balance edge of a knife and infrared military installation, satellite spatial technology, high intensity laser beam and the viewing window of High Temperature High Pressure or vacuum vessel, LCD projector, optical-fibre communications connector box etc.With the white stone single-chip is that the SOS device of insulating substrate material then has advantages such as high integration, high-speed, reduce power consumption and capability of resistance to radiation are strong; In addition,, therefore can be used as the substrate material of unicircuit, can be widely used in photodiode (LED) and microelectronic circuit, thereby substitute the gallium substrate of high price, make very high speed integrated circuit owing to sapphire electrical isolation, transparent, easy heat conduction, hardness height; Can make optical pickocff and some other optical communication and fiber waveguide device.Unstressedly retain, defective is few, large-sized sapphire single-crystal is the material that a lot of industry of field of photoelectric technology is badly in need of.
At present, the main method of Sapphire Crystal Growth has: flame method, crystal pulling method, zone melting method, reverse mould method, heat-exchanging method, the terraced method of guiding temperature and GOI method etc.In the aforesaid method, the monocrystalline of flame method growth is difficult to low cost, high-quality batch process sapphire goods because the thermograde of monocrystalline is very big, and defective and stress value are all very high; Though crystal pulling method can prepare high-quality monocrystal material, but require to have the rotation of certain speed owing to seed crystal in the process of growth, cause the diameter of monocrystalline less, and crystallographic direction and single crystal pulling direction that monocrystalline uses have certain included angle, so utilization ratio is very low; Though zone melting method can reduce the energy consumption of single crystal growing, can increase the monocrystalline dislocation desity greatly, reduce its end-use performance; The reverse mould method has special advantages to making small-sized sapphire single-crystal member, but if do not adopted because of the defect concentration on the sapphire unit surface is too high with the sapphire method of substrate base as producing microelectronics; The common feature of heat-exchanging method and the warm terraced method of guiding is can the bigger sapphire single-crystal of growth size, and crystal mass is very high, but the utilization ratio of crucible is very low, makes the cost of this method high.
Summary of the invention:
The object of the invention is to provide a kind of cold core shouldering micropulling proparation method of large-size sapphire single-crystal.The object of the present invention is achieved like this: heating raw in specific single crystal growing furnace and under the vacuum condition, carry out seeding, shouldering subsequently, isometrically lift, cooling and annealing process procedure.Be specially: it comprises places the high purity aluminium oxide raw material in tungsten thermoscreen and the high temperature member, under vacuum condition, adopt the heating element of tungsten heating raw, after treating its fusing, by seeding, shouldering, isometrically lift, cooling, annealing process procedure prepare sapphire crystal.Cooling water outlet temperature is stabilized in 25 ± 10 ℃ of scopes in the technological process, and vacuum pressure is not more than 6 * 10 in the whole technological process
-3Pa.Utilize heating element of tungsten and crucible, tungsten thermoscreen and thermal structure spare prepare sapphire crystal in special-purpose single crystal growing furnace.After raw material in the crucible is heated to fusing,, regulate stove internal heating body thermal value, make liquid level convection current form stable by observing the liquid level configuration of surface; Add heat regulation range 100-2500W/h; Cold heart position and crucible geometric centre relative deviation are not more than Φ 20.0mm in the melt.In the seeding technological process, slowly regulate seed crystal and make its lower end to the above 5-20mm of melt liquid level place's preheating, eliminate thermal stresses; Utilize traditional crystal pulling method technology, make nucleus of crystal be transferred to the cold heart behind 5-15 the seeding of direction that departs from along the cold heart, cooperate rotation, the crystallization control end shape makes it along seed crystal central shaft symmetry and begin self cooling heart shouldering, wherein speed of rotation 2-16r/min; Pull rate is 0.3-6mm/h in the shouldering process, shouldering stage power lowering speed 0.1-25.5w/h.Lift isometrical that the speed with 0.5-6.8mm/h lifts seed rod in the process, reduce heating power, make the single crystal shoulder outside near sidewall of crucible, but do not contact with the speed of 12-25w/h; The monocrystalline quality evenly increases; 20-170g/h gathers way.After meter to be weighed shows that the monocrystalline quality no longer increases, regulate the speed 20-40w/h that heating power descends, after temperature in the stove was reduced to 1700 ℃, the speed of regulating power decline once more was 10-18w/h, temperature in the growth furnace is slowly descended, monocrystalline is carried out anneal; When temperature in the stove drops to below 500 ℃, the heating power lowering speed is adjusted to 30-60w/h once more, reduce to 100 ℃ until temperature.
What cold core shouldering micropulling method growing sapphire single crystal technology was primarily aimed at is that monocrystalline very easily grows up to plow-shape generation eccentric growth in the existing method for monocrystal growth, after the monocrystalline shouldering, can't realize isodiametric growth, cause monocrystalline to contact with crucible, destroy the homogeneity of the thermograde of single crystal, cause monocrystalline to break, and the eccentric growth of monocrystalline also can cause the solid-liquid interface shape disorder, is unfavorable for the discharge of volatile matter and the minimizing of defective.
Under the perfect condition, the geometric centre of crucible should overlap with the center of seed rod, but in the real work, seed rod is difficult to aim at the geometric centre of crucible, and this just causes, and solid-liquid interface does not overlap with the seed rod center foremost in the single crystal growth process.This situation exists in the practice of crystal pulling method always, and for avoiding single crystal direction one side excess growth, crystal pulling method seed rod in crystal growing process needs rotation continuously, and the single crystal growing size is restricted, and its radius and crucible radius differ greatly.
In addition, after raw material is inserted in the crucible, be heated to the fusion that (is about 2050 ℃) under the certain temperature through heating member, there is the error that to eliminate because of body of heater processing simultaneously, as throughout density difference of crucible material, heating member structure not as the ununiformity of the ideal of design, thermoscreen and crucible distance and thermoscreen inside multilayered structure etc., all cause the inner melt temperature skewness of crucible, promptly " cold spot " of the inner melt of crucible is scarcely at the center.Try one's best near crucible internal diameter (but not contacting) for the monocrystalline size that makes growth, must progressively " cold heart position " be adjusted to the geometric centre place of crucible in the seeding process, the measure of taking is located shouldering at melt " the cold heart ".
Positively effect of the present invention: 1. grow that size is low greater than Φ 220 * 200mm, defect concentration, designated band scope iuuminting rate height, sapphire single-crystal body that substrate base process redundancy is few.The technical characterstic of cold core shouldering micropulling method is that the technology cost is low, crystalline physical and chemical performance excellence.2. locate the seeding shouldering at " the cold heart ", avoided crystal to contact crucible too early, greatly improved raw material availability, reduced the single crystal scrap rate.3. locate shouldering in conjunction with micropulling with at " the cold heart ", may enter into intracrystalline defective when having reduced shouldering.Improved the quality of monocrystalline greatly.4. cold core shouldering can make the later use rate that single crystal diameter reasonably maximizes, the filler of the interior crucible of single crystal growing furnace compares increase, monocrystal material increase in conjunction with the micropulling process.5. monocrystalline can be realized in-situ annealing in temperature-fall period, reduces the oxygen vacancy that forms in the process of growth in the crystal, has simplified program with other growth method ratios, has saved a large amount of energy.To sum up, adopt cold core shouldering micropulling method growing sapphire monocrystalline, outstanding advantage such as have that size is big, quality is high, cost is low, production efficiency and material use efficiency height, power consumption are low, technology has a extensive future, and the promotion and application of this technology will have obvious economic benefit and social benefit.
Utilize embodiment further to set forth technical solution of the present invention below.
In following examples, single crystal growing furnace adopts the heating of heating element of tungsten resistance mode, and heat-insulation system adopts the tungsten thermoscreen, and constant pressure source pattern, the total power 60kw of system are adopted in power control.Variable power is varied to direct ratio with electric power output voltage.Describing power index electric power output voltage value commonly used in an embodiment replaces.
Embodiment 1: the present invention adopts resistance-type heating, with the pretreated aluminium sesquioxide 25.5kg pure tungsten system crucible of packing into.Open water coolant, flow velocity is 6m
3/ h; With the speed of 2.5w per hour power is risen to 55kw, vacuum tightness was once dropping to 1.0 * 10 therebetween
-2Pa due to organism volatilization in the stove, returns to 6.0 * 10 after 40 minutes
-3Pa.When arriving target voltage, observe liquid level and find have a small amount of bubble to overflow, judge that temperature is too high in the crucible,, make the solid-liquid translated image that just has ordered pair stream on the liquid level with the speed setting power of 250w per hour from liquid level.After stablizing 4 hours with this understanding, beginning is " cold heart position " seeding 8 times,, seed rod pull rate 5mm/h, the power speed of regulating that descends is 2.5w/h.Treat to begin shouldering after said process is finished, the seed rod pull rate is 1.5mm/h, and the speed of regulating power decline is 3w/h.Isometrical stage seed rod pull rate is 5mm/h, and the speed of regulating power decline is 5w/h.After crystallisation process finishes, rate adaptation power with 22w/h drops to 1700 ℃, the back drops to 500 ℃ with the rate adaptation power of 11w/h, and the rate adaptation power with 22w/h drops to 100 ℃ again, stops power, continued to keep vacuum and water coolant 24 hours, crystal is taken out in last blow-on, and partly there is a small amount of bubble in the sapphire crystal of this technology growth in the crystallization final stage after testing, rest part is good, and single crystal is of a size of Φ 225 * 205mm.
Embodiment 2: with the pretreated aluminium sesquioxide 27.5kg pure tungsten system crucible of packing into.Open water coolant, flow velocity is 6.2m
3/ h.With the speed of 70mV per hour voltage is risen to 9700mV, vacuum tightness once descended therebetween, returned to 6.0 * 10 after 35 minutes
-3Pa.When arriving target voltage, observe liquid level and find have a large amount of bubbles to overflow from liquid level, it is very high to judge that the interior temperature of crucible exceeds Tc, with the speed setting voltage of every 75mV/h, makes the solid-liquid translated image that just has ordered pair stream on the liquid level.After stablizing 8 hours with this understanding, begin at " cold heart position " seeding, seed rod pull rate 4.5mm/h, the speed that voltage decline is regulated is 7mV/h.Treat to begin shouldering after said process is finished, the seed rod pull rate is 3mm/h, and the speed that voltage decline is regulated is 10mV/h.Isometrical stage seed rod pull rate is 4.5mm/h, and the speed that voltage descends is 10mV/h.After crystallisation process finishes, descended 17 hours with the rate adaptation voltage of 15mV/h, the rate adaptation voltage with 6mV/h descended 24 hours then, when circuit voltage is 0.2878V, fed high-purity argon gas at last, made the vacuum tightness in the single crystal growing furnace drop to 10
-2Pa, when circuit voltage stops ventilation during for 0.158V, vacuum tightness rises thereupon.Circuit voltage drops to 0V subsequently, continues to keep vacuum and water coolant 24 hours.Only partly there is the metal fragment of forming crucible in the sapphire crystal of this technology growth in the crystallization final stage after testing, and rest part is good, and single crystal is of a size of Φ 245 * 218mm.
Embodiment 3: with the pretreated aluminium sesquioxide 26kg crucible of packing into.Open water coolant, flow velocity is 5m
3/ h.With the speed of 100mV per hour voltage is risen to 9600mV, when arriving target voltage,, make the solid-liquid translated image that just has ordered pair stream on the liquid level with the speed setting voltage of 75mV per hour.After stablizing 10 hours with this understanding, begin in " the cold heart " position shouldering, seed rod pull rate 6mm/h, the speed that voltage decline is regulated is 10mV/h; Treat to begin shouldering after said process is finished, the seed rod pull rate is 4mm/h, and the voltage fall off rate is 8mV/h; Isometrical stage seed rod pull rate is 5.5mm/h, and the speed that voltage decline is regulated is 8mV/h.After crystallisation process finishes, descended 12 hours with the rate adaptation voltage of 12mV/h, the speed with 5mV/h reduces voltage then, when circuit voltage is 0.2575V, feeds high-purity argon gas at last, makes the interior vacuum tightness of single crystal growing furnace drop to 10
-2Pa stops ventilation when remaining to circuit voltage for 0.160V, vacuum tightness rises thereupon.When circuit voltage drops to 0V, continued to keep vacuum and water coolant 24 hours.The sapphire crystal fat light of this technology growth is good after testing, and no naked eyes visible bubble in bubble and crackle exist, and single crystal is of a size of Φ 230 * 210mm.
Claims (5)
1. the cold core shouldering micropulling proparation method of a large-size sapphire single-crystal, it is included in heating aluminium sesquioxide raw material under the vacuum condition, after treating its fusing, by seeding, shouldering, isometrically lift, cooling, annealing process procedure prepare sapphire crystal, it is characterized in that: cooling water outlet temperature is stabilized in 25 ± 10 ℃ of scopes in the technological process, and vacuum pressure is not more than 6 * 10 in the whole technological process
-3Pa.
2. the cold core shouldering micropulling proparation method of a kind of large-size sapphire single-crystal according to claim 1, it is characterized in that: utilize heating element of tungsten and crucible, tungsten thermoscreen and thermal structure spare prepare sapphire crystal in special-purpose single crystal growing furnace.
3. the cold core shouldering micropulling proparation method of a kind of large-size sapphire single-crystal according to claim 1 and 2, it is characterized in that: after the raw material in the crucible is heated to fusing, by observing the liquid level configuration of surface, regulate stove internal heating body thermal value, make liquid level convection current form stable; Add heat regulation range 100-2500W/h; Cold heart position and crucible geometric centre relative deviation are not more than Φ 20.0mm in the melt.
4. according to the cold core shouldering micropulling proparation method that utilizes claim 1 or 2 described a kind of large-size sapphire single-crystals, it is characterized in that: in the seeding technological process, slowly regulate seed crystal and make its lower end, eliminate thermal stresses to the above 5-20mm of melt liquid level place's preheating; Utilize traditional crystal pulling method technology, make nucleus of crystal be transferred to the cold heart behind 5-15 the seeding of direction that departs from along the cold heart, cooperate rotation, the crystallization control end shape makes it along seed crystal central shaft symmetry and begin self cooling heart shouldering, wherein speed of rotation 2-16r/min; Shouldering process pull rate is 0.3-6mm/h, shouldering stage power lowering speed 0.1-25.5w/h.
5. according to the cold core shouldering micropulling proparation method that utilizes claim 1 or 2 described a kind of large-size sapphire single-crystals, it is characterized in that: lift isometrical that the speed with 0.5-6.8mm/h lifts seed rod in the process, speed with 12-25w/h reduces heating power, make the single crystal shoulder outside near sidewall of crucible, but do not contact; The monocrystalline quality evenly increases; 20-170g/h gathers way.
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