CN101857970B - Growing method of large-size flaky sapphire crystals - Google Patents
Growing method of large-size flaky sapphire crystals Download PDFInfo
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Abstract
The invention relates to a manufacture technology of sapphire crystals, in particular to a growing method of large-size flaky sapphire crystals. A crystal growing process of the method is carried out in a single-crystal growing furnace internally provided with a crucible and a guide mould, wherein the crystal growing process sequentially comprises the following steps of: sapphire raw material heating, seeding, shouldering, constant-diameter lifting and cooling. The single-crystal growing furnace is internally provided with a protective gas inlet and outlet system capable of introducing and exhausting protective gas and a pressure control system capable of controlling the pressure in the furnace, wherein the protective gas is introduced into the furnace in the steps of sapphire raw material heating, seeding, shouldering and constant-diameter lifting and is formed into flowing gas in the furnace through the protective gas inlet and outlet system, and the gas inlet flow of the protective gas is 0.1-50slpm; and meanwhile, the pressure in the furnace is controlled to be 100pa-90kpa through the pressure control system. The method can be directly used for growing the flaky sapphire crystals with a larger size and has simple manufacture procedure, high material utilization ratio and low manufacture cost.
Description
Technical field
The present invention relates to the manufacturing technology of sapphire crystal, specifically is a kind of growth method of large-size flaky sapphire crystals.
Background technology
Sapphire (Alpha-alumina) crystalline material is the water white transparency monocrystal material.Because sapphire crystal and gan have analog structure, close with the thermal expansivity of silicon and good anti-ultraviolet property is arranged, so be used widely at aspects such as LED, SOS unicircuit, satellite spatial technology.
Sapphire crystal has the optical window material that good through performance is used to many measurement and analysis instruments at visible light in the 5.6um spectral range.The anisotropy of sapphire crystal is applied to waveguide laser cavity, SAW filter, retarding line, ultrasonic element; The hardness of sapphire crystal (Mohs degree 9) is only second to diamond; Characteristics and chemical property that he has hardness and intensity is high, resistance to wear, heat-resisting ability is strong are stable; Series of characteristics such as acid-alkali-corrosive-resisting are widely used in high power laser light window, high temperature resistant, high pressure, anti-high-speed friction, container or the viewing window of vacuum vessel and the heating panel of optical window and projector etc. such as be able to bear strong corrosion; The sapphire crystal of different shape such as square, arc, trilateral, ellipse are widely used in nonmagnetic bracing frame, high temperature insulating material, isolating frame, scanner panel etc.And use size increasing.Therefore large-sized sapphire crystal material is the material that many industries are badly in need of.
The main method of sapphire crystal growth has at present: flame method, crystal pulling method, kyropoulos, heat-exchanging method and the terraced method of guiding temperature etc.In the aforesaid method, flame method is can't growth diameter because thermograde is excessive higher greater than the monocrystalline of 50mm and crystalline defective and inner-stress value, and range of application has received great restriction.Methods such as crystal pulling method, kyropoulos, heat-exchanging method, the terraced method of guiding temperature can the growing large-size sapphire crystal; But they need be through repeatedly high firmness cutting, and moulding is after a series of heavy mechanical workouts such as grinding; Can process suitable shape and size, operation is complicated; Cost is high and consuming time; The crystalline material utilization ratio is lower, and working efficiency is not high, and cost is high.
Summary of the invention
Technical problem to be solved by this invention is, provides that a kind of flaky sapphire crystals, manufacturing process that can direct growth goes out large-size (width reaches 200mm) is simple, material use efficiency is high, the growth method of the large-size flaky sapphire crystals of low cost of manufacture.
The growth method of large-size flaky sapphire crystals of the present invention is: crystal growing process carries out in monocrystal growing furnace; Crucible and guided mode are set in the stove, and crystal growing process comprises the heating of sapphire raw material, seeding, shouldering, isometrical lifting and cooling step successively; The pressure control system that the shielding gas that can feed and discharge shielding gas passes in and out gas system and may command furnace pressure is set in the said monocrystal growing furnace; In stove, feed shielding gas in the step the heating of sapphire raw material, seeding, shouldering, isometrical lifting; Make shielding gas formation flowing gas in the stove through shielding gas turnover gas system; Its charge flow rate is 0.1-50slpm, and making furnace pressure through pressure control system simultaneously is 100pa-90kpa.
Said monocrystal growing furnace heating unit is the graphite resistance heating unit, and its heating power is 10-50kw;
Said guided mode and crucible material are pure tungsten or pure Mo, perhaps are the miramint material; The size of guided mode is according to the sized of product request for utilization, and the guided mode width is selected in the 80-200mm scope, and guided mode thickness is selected at 0.8-25mm;
Said shielding gas is an argon gas.
Said sapphire raw material heating steps is: in crucible, put into the Alpha-alumina raw material, close the growth fire door, the opening device cooling water system; Be evacuated to 3.0 * 10 in the stove
-2Open the heating slope heating raw of heating power supply behind the pa with 4.5-450w/min; During to 2-20kw or before not opening heating, open shielding gas turnover gas system at heating power, regulating its flow is 0.1-50slpm; Opening pressure system again, making system pressure is 100pa-90kpa; Heating slope heating raw with above-mentioned melts until raw material; Fusing back raw material rises to the guided mode mouth through guided mode.
Said seeding step is: seed crystal is displaced downwardly to the guided mode mouth, seed crystal is contacted with the guided mode mouth, form growing film, observe its growing film thickness and regulate heating power, making growing film thickness is 0.1-2mm;
Said shouldering step is: open pulling apparatus, the control pull rate is 0.1-9mm/min, and guided mode mouth growing film begins expansion until covering whole guided mode mouth;
The said isometrical step that lifts is: the speed with 0.5-16mm/min lifts seed rod, and crystal is in the first-class width growth of guided mode mouth ready-formed size; Its radial symmetry gradient keeps 0.025-0.9 ℃/mm; Have been found that its radial symmetry gradient surpasses the integrity that 0.9 ℃/mm will influence crystalline structure; Axial-temperature gradient upwards is being 3-50 ℃/cm apart from the guided mode mouth; Have been found that axial-temperature gradient surpasses the integrity that 50 ℃/cm will influence crystalline structure; Crystal to be grown breaks away from the guided mode mouth, accomplishes the flaky sapphire crystals process of growth;
Said cooling step is: regulate heating power and lower the temperature with 4.5-400w/min, when heating power is reduced to 5Kw, close heating system, the closing presure automatic control system is closed shielding gas turnover gas system when treating system's internal pressure to 100KPa again; Room temperature is reduced in the temperature natural cooling in the stove; The closing device cooling water system, the flaky sapphire crystals growth ending.
Positively effect of the present invention is embodied in:
1. generally, because the size of flaky sapphire crystals is big more, radiation surface area S is just big more; Flaky sapphire crystals thickness is thinner relatively; Volume is less, and radiation surface area S is just high more with the ratio e=S/V plane of crystal radiation capacity value of crystal volume V, is easy to generate bigger stress in the process of growth; Crystal just is easy to generate a large amount of dislocations and the polycrystalline crystal boundary causes crystal to break when the crystal width dimensions is too big, so the width of growing crystal is restricted.Method of the present invention is through the reasonable disposition of processing parameter, and it is wide to grow size 80-200mm, thick 0.8-25mm, visible light and infrared light transmitance height, no polycrystalline, the optical grade sapphire crystal that defect concentration is low.
2. in the inventive method; Flow and the shielding gas of tool certain pressure value can the attemperation field distribution; Improved the uneven situation of crystal surrounding temperature; Solved unstable temperature phenomenon on the crystal growth direction, make crystal when growth radial temperature distribute rationally with axial temperature, the length and width of making a living size does not have the polycrystalline crystal boundary, crystal that dislocation desity is low has been created condition.
3. when using the graphite charcoal as well heater, high temperature with have that the graphite charcoal is easy to volatilization and has polluted furnace atmosphere under the trace oxygen condition, charcoal can make the defect concentration on the crystal unit area too high with crystal combination, thereby can influence the crystalline transparency.The inventive method adopts the shielding gas with certain pressure value of directed flow; Can remove the pollution that graphite volatilizes, remove charcoal and be penetrated into the phenomenon in the crystalline structure, the crystalline transparency is increased; The integrity of crystalline structure is improved, and has also reduced the crystalline dislocation desity simultaneously.
4. the present invention has abandoned traditional induction furnace type of heating and has used the resistance furnace type of heating; Removed the energy efficiency loss that is brought by twice conversion of induction heating electric energy and the conversion of heat energy secondary; Practiced thrift 2/3rds the energy than induction heating mode, energy-conservation very obvious.Make the large-size flaky sapphire crystals cost further reduce.In addition, also make in the crystal growing process can be through to the control of heating power control growing temperature more accurately in the use of resistance furnace.
5. owing to adopted the guided mode growth method, the width of size and thickness can be made in advance, thus can grow directly meet request for utilization and tolerance+/-the sapphire sheet crystal of 0.2mm.Directly removed the back road manufacturing procedure of heavy, high firmness, with high costs repeatedly excision forming.Thereby its crystal utilization ratio is high, and production efficiency is high, and cost is low, less energy consumption.
Embodiment
Instance 1: adopt the resistive heating single crystal growing furnace, heating power 20kw, type of heating are the graphite resistance heating, and heating is controlled to be the constant current source mode, and single crystal growing furnace is equipped with shielding gas inlet and outlet device and automatic pressure control device.Prefabricated wide 110mm, the thick 5mm of being of a size of of guided mode mouth.700g is packed in the crucible that pure tungsten makes through pretreated Alpha-alumina, and it is 1.5m that the opening device water cooling system makes system's water outlet flow
3/ h.Be evacuated to 3.2 * 10 in the stove
-2Open heating power supply behind the Pa, with the heating slope heating raw of 200w/min, vacuum tightness descends midway, and the final vacuum degree rose to 3.2 * 10 again gradually in 20 minutes
-2Pa.When heating power rises to 18Kw, open high-purity argon gas turnover gas system, regulate flow at 0.1-50slpm, the opening pressure system makes furnace pressure at 100Pa-90Kpa again.Continuation is heated to the raw material fusing with above-mentioned heating slope.Seed crystal moved down apart from guided mode mouth 3-15mm place kept 3-60 minute, move down seed crystal again seed crystal is contacted with the guided mode mouth, observe its growing film thickness; Find that its growing film is very thin, regulate heating power and improve 180w, observe growing film thickness at 0.1-2mm; Open the seed rod pulling apparatus; The control pull rate is 0.1-9mm/min, and crystal expansion adjustment pull rate when covering whole guided mode mouth is 0.5-16mm/min, improves heating power 270w simultaneously; The seed rod pulling apparatus continued to lift 3 minutes again after crystal breaks away from from the guided mode mouth, closed the seed rod pulling apparatus.Regulate the slope cooling of heating power with 20-300w/min, during heating power 5kw, close heating system, the closing presure automatic control system is closed the high-purity argon gas in-out apparatus during system pressure 101Kpa.Naturally cool to closing device cooling water system after the room temperature in the stove.Crystal is taken out in blow-on, and through check, there is a small amount of bubble in the shouldering part, near some bubbles of end part existence in crystal at middle portion.Crystal mass is good.
Instance 2: adopt the resistive heating single crystal growing furnace, heating power 45kw, type of heating are the graphite resistance heating, and heating is controlled to be the constant current source mode, and single crystal growing furnace is equipped with shielding gas inlet and outlet device and automatic pressure control device.Prefabricated wide 150mm, the thick 12mm of being of a size of of guided mode mouth.1200g is packed in the crucible that pure molybdenum makes through pretreated Alpha-alumina, the opening device water cooling system, system's water outlet flow is 1.4m
3/ h.Be evacuated to 3.5 * 10 in the stove
-2Pa opens heating unit, with the rate of heating heating raw of 9.5w/min, when 19.5kw, opens high-purity argon gas turnover gas system, regulates flow at 0.2-40slpm, opening pressure system again, and pressure is at 400Pa-70Kpa.Continue to be warming up to the raw material fusing.Seed crystal is with after the guided mode mouth contacts; Observe its growing film thickness greater than 2mm, regulate power decline 120w, open the seed rod pulling apparatus; Pull rate 0.1-8mm/min; The adjustment pull rate was 0.5-15mm/min when the crystal expansion covered whole guided mode mouth edge, improved heating power 120w simultaneously, finished until process of growth.Seed rod continues to lift after 5 minutes again closes the seed crystal pulling apparatus.Regulate heating power with the cooling of 20-250w/min speed, when heating power was reduced to 9kw, the closing presure automatic control system had been closed the high-purity argon gas in-out apparatus during system pressure 98Kpa.Close heating system when continuation is cooled to 4kw with above-mentioned cooling rate, system naturally cools to room temperature, closes cooling water system.There is a small amount of bubble in flaky sapphire crystals through the growth of this technology of check near closing position; There is seldom bubble at middle portion.Other part crystal mass is good.
Instance 3: adopt the resistive heating single crystal growing furnace, heating power 10kw, type of heating are the graphite resistance heating, and heating is controlled to be the constant current source mode, and single crystal growing furnace is equipped with shielding gas inlet and outlet device and automatic pressure control device.Prefabricated wide 80mm, the thick 0.8mm of being of a size of of guided mode mouth.150g is packed in the crucible that pure molybdenum makes through pretreated Alpha-alumina, the opening device water cooling system, system's water outlet flow is 1.4m
3/ h.Vacuumize 3.5 * 10 in the stove
-2Pa opens high-purity argon gas turnover gas system, regulates flow at 0.2-40slpm, opening pressure system again, and pressure is at 400Pa-70Kpa.Open heating unit, the rate of heating heating raw with 130w/min melts until raw material.Seed crystal is with after the guided mode mouth contacts; Observing its growing film thickness is 0.1-2mm; Open the shouldering of seed rod pulling apparatus, pull rate 0.1-6mm/min, to be that 0.5-15mm/min is isometrical lifted the adjustment pull rate when crystal expansion covered whole guided mode mouth edge; Lift intensification 50w when soon finishing isometrical, finish until process of growth.Close the seed crystal pulling apparatus.Regulate heating power with the cooling of 20-350w/min speed, when heating power was reduced to 0kw, the closing presure automatic control system had been closed the high-purity argon gas in-out apparatus during 101Kpa.System cools is closed cooling water system to room temperature.There is a small amount of bubble through this flaky sapphire crystals of check at the shouldering position; At middle portion 2 bubbles less than the 0.2mm diameter are arranged.Other part crystal mass is good.
Claims (9)
1. the growth method of a large-size flaky sapphire crystals, its crystal growing process carries out in monocrystal growing furnace, and crucible and guided mode are set in the stove; Crystal growing process comprises the heating of sapphire raw material, seeding, shouldering, isometrical lifting and cooling step successively; It is characterized in that: the pressure control system that the shielding gas that can feed and discharge shielding gas passes in and out gas system and may command furnace pressure is set in the said monocrystal growing furnace; In stove, feed shielding gas in the step the heating of sapphire raw material, seeding, shouldering, isometrical lifting; Make shielding gas formation flowing gas in the stove through shielding gas turnover gas system; Its charge flow rate is 0.1-50slpm, makes through pressure control system simultaneously that pressure pressure is 100pa-90kpa in the stove.
2. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: the heating unit of said monocrystal growing furnace is the graphite resistance heating unit, its heating power is 5-50kw.
3. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: said guided mode and crucible material are pure tungsten or pure Mo, perhaps are the miramint material; The size of guided mode is according to the sized of product request for utilization, and the guided mode width is selected in the 80-200mm scope, and guided mode thickness is selected at 0.8-25mm.
4. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: said shielding gas is an argon gas.
5. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: said sapphire raw material heating steps is: in crucible, put into the Alpha-alumina raw material, close the growth fire door, the opening device cooling water system; Open the heating slope heating raw of heating power supply after being evacuated to 3.0x10-2pa in the stove with 4.5-450w/min; During to 2-20kw or before not opening heating, open shielding gas turnover gas system at heating power, regulating its flow is 0.1-50slpm; Opening pressure system again, making system pressure is 100pa-90kpa; Heating slope heating raw with above-mentioned melts until raw material; Fusing back raw material rises to the guided mode mouth through guided mode.
6. the growth method of large-size flaky sapphire crystals according to claim 1; It is characterized in that: said seeding step is: seed crystal is displaced downwardly to the guided mode mouth; Seed crystal is contacted with the guided mode mouth; Form growing film, observe its growing film thickness and regulate heating power, making growing film thickness is 0.1-2mm.
7. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: said shouldering step is: open pulling apparatus, control pull rate is 0.1-9mm/min, guided mode mouth growing film begins expansion until the whole guided mode mouth of covering.
8. the growth method of large-size flaky sapphire crystals according to claim 1, it is characterized in that: the said isometrical step that lifts is: the speed with 0.5-16mm/min lifts seed rod, and crystal is in the first-class width growth of guided mode mouth ready-formed size; Its radial symmetry gradient keeps 0.025-0.9 ℃/mm; Axial-temperature gradient upwards is being 3-50 ℃/cm apart from the guided mode mouth; Crystal to be grown breaks away from the guided mode mouth, accomplishes the flaky sapphire crystals process of growth.
9. the growth method of large-size flaky sapphire crystals according to claim 1; It is characterized in that: said cooling step is: regulate heating power and lower the temperature with 4.5-400w/min; When heating power is reduced to 5Kw; Close heating system, the closing presure automatic control system is closed shielding gas turnover gas system when treating system's internal pressure to 100KPa again; Room temperature is reduced in the temperature natural cooling in the stove; The closing device cooling water system, the flaky sapphire crystals growth ending.
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| CN114737253B (en) * | 2022-06-10 | 2022-11-04 | 太原彩源新材料科技有限公司 | Single crystal furnace thermal field structure and method for growing large-size sapphire single crystal plate |
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