CN101323978B - Large size sapphire crystal preparing technology and growing apparatus thereof - Google Patents
Large size sapphire crystal preparing technology and growing apparatus thereof Download PDFInfo
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- CN101323978B CN101323978B CN2008100456663A CN200810045666A CN101323978B CN 101323978 B CN101323978 B CN 101323978B CN 2008100456663 A CN2008100456663 A CN 2008100456663A CN 200810045666 A CN200810045666 A CN 200810045666A CN 101323978 B CN101323978 B CN 101323978B
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Abstract
The invention relates to a preparing technique and a growth device of a large-size sapphire crystal, and the preparing technique of the large-size sapphire crystal comprises the following steps: (1) aluminum sesquioxide with high purity that is weighted is filled into a molybdenum crucible pot, a stove is vacuumized until the atmospheric pressure inside the stove is less than 10<-3> Pa, and then protective gases are filled into the stove, and the stove pressure achieves minus 90 to plus 20 KPa; (2) raw materials are heated until complete melting is achieved, and heat is preserved for 3 to 5 hours; (3) seed crystals are lowered by 15 to 120mm under heat preservation, and then the molybdenum crucible pot is lowered by the height of the molybdenum crucible pot; (4) the temperature in the stove is decreased until 1600 to 1750 DEG C; (5) the molybdenum crucible pot is re-raised to a heating region, and heat is preserved for 100 to 150 hours and then the temperature is decreased slowly until room temperature. The preparing technique of the large-size sapphire crystal of the invention is characterized by simple device structure, low production cost, good preparing technique stability, reliable process, easier bubble elimination and high yield, and can cultivate the single sapphire crystal with large size, small dislocation density and high quality.
Description
Technical field
The present invention relates to a kind of crystal structure technology field.
Background technology
Sapphire is widely used in window material, the high pressure material of substrate material, special optical components and parts, high energy detection and the superpower light laser of GaN substrate material, precision instrument bearing, large-scale integrated circuit SOI and the SOS of high-brightness LED.But the growth method of growing large-size optical grade sapphire crystal mainly contains at present: heat-exchanging method, kyropoulos, the terraced method of resistive heating temperature, falling crucible method.But heat-exchanging method adopts helium to make cooling gas, costs dearly, and can not the axial crystal of direct growth C; The kyropoulos process repeatability is poor, the energy consumption height; The terraced method process repeatability of resistive heating temperature is poor, yield rate is low.Induction heating iridium crucible crystal pulling method has high input, the cost height.Traditional falling crucible method, the thermograde setting range is limited, and the thermograde that provides the growing large-size sapphire crystal required is provided, and causes the ability of crystal impurities removal matter and bubble low simultaneously, and matter crystal internal defect is more, crystal yield rate only about 50%.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of low cost of manufacture, technology controlling and process is simple, yield rate is high, crystal mass is good large size sapphire crystal preparation technology are provided.
A further object of the present invention provides a kind of growing apparatus of realizing large size sapphire crystal preparation technology.
The objective of the invention is to realize by the enforcement following technical proposals:
A kind of large size sapphire crystal preparation technology is characterized in that: comprise the steps:
(1) aluminium sesquioxide of load weighted purity 〉=99.995% is packed in the molybdenum crucible, be evacuated to the stove internal gas pressure less than 10
-3Pa, fill protective atmosphere to furnace pressure and be-90～+ 20KPa;
(2) heat temperature raising, temperature rise rate 500W～1000W/h, after fully melting to raw material, constant temperature 3～5h melts the stage at raw material, and seed crystal is the insulation shutoff crucible through hole of insulation holder down down, guarantees that the heat insulation effect at molybdenum crucible seed crystal place melts seed crystal;
(3) seed crystal in the burner hearth is incubated decline 15-120mm down, molybdenum crucible descends then, dropping distance is the height of crucible, fall off rate 0.5～3.0mm/h, the through hole of insulation holder under the crucible is opened, entering in the hole than freezing air of bottom played the effect of a cooling to the seed crystal in the seed crystal pipe, for crystal growth provides enough thermogrades;
(4) cooling, temperature is reduced to 1600～1750 ℃ in the stove, and rate of temperature fall is 100W～300W/h;
(5) molybdenum crucible gos up to the heating zone, in-situ annealing, 1600～1750 ℃ of constant temperature 100-150h;
(6) slowly be cooled to room temperature, rate of temperature fall 50W～100W/h continues logical recirculated cooling water 24～36h, takes out crystal.
A kind of growing apparatus of realizing large size sapphire crystal preparation technology, its bottom is insulation holder under the aluminum oxide, the zirconium white insulating brick is established on insulation holder top under the aluminum oxide, the side insulation is established in zirconium white insulating brick outside, and ruhmkorff coil is established in the outside of side insulation, and the top of side insulation and zirconium white insulating brick is provided with protective guard, following insulation holder and insulating brick surround hollow cavity, described inner chamber bottom is provided with the crucible pole that links to each other with hoisting appliance, it is characterized in that, heating tube is established in the inboard of insulating brick; Molybdenum crucible is incubated holder down by crucible and is connected with crucible pole, and the molybdenum crucible top is provided with on the crucible covers.
Insulation is held in the palm to be divided into from bottom to up and is incubated insulation holder under the holder and second aluminum oxide under first aluminum oxide under the described aluminum oxide, described zirconium white insulating brick is divided into the first zirconium white insulating brick and the second zirconium white insulating brick from bottom to up, and described heating tube is arranged on the top of the first zirconium white insulating brick and the place, inboard of the second zirconium white insulating brick.
The crucible of described molybdenum crucible seed crystal pipe bottom correspondence down insulation holder has through hole, and the seed crystal that is provided with in the through hole is insulation its underpart secondary elevating lever that is connected down, and secondary elevating lever bottom passes with secondary hoisting appliance from the crucible pole bottom and links to each other.
Described large size sapphire crystal preparation technology's growing apparatus also comprises an atmosphere Controlling System, described atmosphere Controlling System comprises PID controller, frequency transformer, pressure transmitter, transmitter and vacuum pump, pressure transmitter links to each other with the PID controller by transmitter, and the PID controller output end is graphite heating pipe or tungsten heating tube or molybdenum heating tube by the frequency transformer described heating tube that links to each other with vacuum pump.
Adopt technical scheme of the present invention, between ruhmkorff coil and the molybdenum crucible heating tube is set, after being heated, heating tube reaches the crystal melting temperature, with the crystal starting material in molybdenum crucible fusings, and the common molybdenum crucible problem serious and that crucible is out of shape of at high temperature volatilizing when having solved conventional induction heating.By in-situ annealing, can fine elimination thermal stresses, avoid crystal cleavage, but therefore direct growth C to sapphire single-crystal.Raw material at crystal growing process melts the stage, the seed crystal that the secondary elevating lever that secondary hoisting appliance links to each other is connected is incubated the shutoff communicating pores of insulation holder down down, the heat insulation effect of guaranteeing molybdenum crucible seed crystal place melts seed crystal, when crystal growth begins, secondary hoisting appliance and hoisting appliance descend, insulation and molybdenum crucible are also descended, the communicating pores of following insulation holder is opened, entering in the hole of bottom than freezing air, play the effect of a cooling to the seed crystal in the seed crystal pipe,, improve crystal impurities removal effect for crystal growth provides enough thermogrades, reduce the defect and impurity of crystals, thereby improve perfection of crystal and quality.In the process of crystal preparation, the protective atmosphere that injects in the stove is owing to the pressure that constantly reacts descends, under the condition of high temperature; cause the crucible voloxidation easily; volatile matter forms impurity after entering crystal, causes crystal quality to descend, and causes crystals impurity more.After adopting the atmosphere Controlling System, when the stove internal gas pressure was higher than set(ting)value, vacuum pump was just started working, and gas unnecessary in the stove is extracted out; When the stove internal gas pressure was lower than set(ting)value, vacuum pump just quit work, and can guarantee that from the shielding gas that aeration aperture enters protective atmosphere meets the requirements in the stove, had avoided the generation of molybdenum crucible volatilization rear impurity.
Description of drawings
Fig. 1 is the structural representation of growing apparatus of the present invention.
Fig. 2 is an atmosphere Controlling System block diagram of the present invention.
Mark among the figure: stay-warm case on 1, cover 3 second zirconium white insulating bricks on 2 crucibles, 4 heating tubes, the insulation of 5 sides, 6 ruhmkorff coils, 7 molybdenum crucibles, 8 first zirconium white insulating bricks, the insulation holder down of 9 seed crystal pipes, 10 crucibles, insulation holder under 11 second aluminum oxide, 12 crucible poles, insulation holder under 13 first aluminum oxide, the insulation down of 14 seed crystals, 15 secondary elevating levers
Embodiment
Adopt following steps to prepare large size sapphire crystal:
(1) with load weighted high purity aluminium oxide (Al
2O
3) purity 〉=99.995% packs in the molybdenum crucible, is evacuated to the stove internal gas pressure less than 10
-3During Pa, fill protective atmosphere Ar or N
2Or He or H
2Or Ar+2%H
2, to furnace pressure be-90～+ 20KPa (normal atmosphere is 0 relatively), protective atmosphere is taked immobilising mode.
(2) induction heating, temperature rise rate 500W～1000W/h, after fully melting to raw material, constant temperature 3～5h melts the stage at raw material, and seed crystal is the insulation shutoff crucible through hole of insulation holder down down, guarantees that the heat insulation effect at molybdenum crucible seed crystal place melts seed crystal;
(3) seed crystal in the burner hearth is incubated decline 15-120mm down, molybdenum crucible descends then, dropping distance is the height of crucible, fall off rate 0.5～3.0mm/h, the through hole of insulation holder under the crucible is opened, entering in the hole than freezing air of bottom played the effect of a cooling to the seed crystal in the seed crystal pipe, for crystal growth provides enough thermogrades;
(4) cooling, temperature is reduced to 1600～1750 ℃ in the stove, and rate of temperature fall is 100W～300W/h;
(5) molybdenum crucible gos up to the heating zone in-situ annealing, 1600～1750 ℃ of constant temperature 100-150h;
(6) slowly be cooled to room temperature, rate of temperature fall 50W～100W/h continues logical recirculated cooling water 24～36h, takes out crystal.
The growing apparatus for preparing above-mentioned large size sapphire crystal as shown in Figure 1, comprise insulation holder 11 under insulation holder 13 and second aluminum oxide under first aluminum oxide of furnace bottom successively, insulation holder top is established the first zirconium white insulating brick 8 and the second zirconium white insulating brick 3 successively under second aluminum oxide, the place, inboard of the top of the first zirconium white insulating brick 8 and the second zirconium white insulating brick 3 establishes graphite heating pipe 4, and heating tube also can be tungsten heating tube or molybdenum heating tube.First, second zirconium white insulating brick the outside establish side insulation 5, ruhmkorff coil 6 is established in the outside of side insulation 5; The top of side insulation 5 and second insulating brick 3 is provided with protective guard 1; Insulation holder and first, second zirconium white insulating brick surround the hollow cavity bottom and are provided with crucible pole 7 under first, second aluminum oxide, molybdenum crucible 7 by crucible down insulation holder 10 be connected with crucible pole 12, be provided with above the molybdenum crucible and cover 2 on the crucible; The crucible pole bottom links to each other with hoisting appliance, be provided with seed crystal in the seed crystal pipe 9 of molybdenum crucible, the crucible of molybdenum crucible seed crystal pipe bottom correspondence insulation holder down has through hole, the seed crystal that is provided with in the through hole is insulation 14 its underparts secondary elevating lever 15 that is connected down, and secondary elevating lever bottom passes with secondary hoisting appliance from the crucible pole bottom and links to each other.Hoisting appliance that the control molybdenum crucible moves up and down and control seed crystal are incubated the secondary hoisting appliance that moves up and down down and can relatively independently move each other.
The present invention is provided with the formed thermal field of heating tube between ruhmkorff coil and molybdenum crucible, and under the crucible of seed crystal pipe bottom correspondence, be provided with under the seed crystal moving up and down in the insulation holder and be incubated, and the suitable processing step of employing, for crystal growth provides enough temperature and thermogrades, improve crystal impurities removal effect, reduce the defect and impurity of crystals, thereby improve perfection of crystal and quality.
Adopt following steps to prepare large size sapphire crystal:
(1) with load weighted high purity aluminium oxide (Al
2O
3) purity 〉=99.995% packs in the molybdenum crucible, is evacuated to the stove internal gas pressure less than 10
-3During Pa, fill protective atmosphere Ar to furnace pressure be-90～+ 20KPa (normal atmosphere is 0 relatively), atmosphere is taked not flow pattern;
(2) induction heating, temperature rise rate 1000W/h, after fully melting to raw material, constant temperature 3～5h melts the stage at raw material, and seed crystal is the insulation shutoff crucible through hole of insulation holder down down, guarantees that the heat insulation effect at molybdenum crucible seed crystal place melts seed crystal;
(3) seed crystal in the burner hearth is incubated decline 15-120mm down, molybdenum crucible descends then, dropping distance is the height of crucible, fall off rate 3.0mm/h, the through hole of insulation holder under the crucible is opened, entering in the hole than freezing air of bottom played the effect of a cooling to the seed crystal in the seed crystal pipe, for crystal growth provides enough thermogrades;
(4) cooling, temperature is reduced to 1600 ℃ in the stove, and rate of temperature fall is 100WW/h;
(5) molybdenum crucible gos up to the heating zone, in-situ annealing, 1600 ℃ of constant temperature 150h;
(6) slowly be cooled to room temperature, rate of temperature fall 100W/h continues logical recirculated cooling water 24～36h, takes out crystal.
The growing apparatus that the present invention adopts is with embodiment 1.
Adopt following steps to prepare large size sapphire crystal:
(1) with load weighted high purity aluminium oxide (Al
2O
3) purity 〉=99.995% packs in the molybdenum crucible, is evacuated to the stove internal gas pressure less than 10
-3During Pa, filling protective atmosphere is that Ar adds 2%H
2To furnace pressure be-90～+ 20KPa (normal atmosphere is 0 relatively), atmosphere is taked the mobile mode, guarantees that the stove internal gas pressure meets processing requirement.
(2) induction heating, temperature rise rate 500W/h, after fully melting to raw material, constant temperature 3～5h melts the stage at raw material, and seed crystal is the insulation shutoff crucible through hole of insulation holder down down, guarantees that the heat insulation effect at molybdenum crucible seed crystal place melts seed crystal;
(3) seed crystal in the burner hearth is incubated decline 15-120mm down, molybdenum crucible descends then, dropping distance is the height of crucible, fall off rate 0.5mm/h, the through hole of insulation holder under the crucible is opened, entering in the hole than freezing air of bottom played the effect of a cooling to the seed crystal in the seed crystal pipe, for crystal growth provides enough thermogrades;
(4) cooling, temperature is reduced to 1750 ℃ in the stove, and rate of temperature fall is 300W/h;
(5) molybdenum crucible gos up to the heating zone, in-situ annealing, 1750 ℃ of constant temperature 100h;
(6) slowly be cooled to room temperature, rate of temperature fall 50W/h continues logical recirculated cooling water 24～36h, takes out crystal.
The growing apparatus that present embodiment adopts is except the part identical with embodiment 1, also comprise the atmosphere Controlling System of forming by PID controller, frequency transformer, pressure transmitter and transmitter, as shown in Figure 2, pressure transmitter is sent into the PID controller with the pressure signal that the stove internal gas pressure value that monitors produces through transmitter, and with controller in set(ting)value compare, its difference via controller after computing exports the frequency transformer that joins with vacuum pump to.The protective atmosphere inflation system is opened all the time, and when the stove internal gas pressure was higher than set(ting)value, vacuum pump was just started working, and gas unnecessary in the stove is extracted out; When the stove internal gas pressure was lower than set(ting)value, vacuum pump quit work, and shielding gas enters in the stove from aeration aperture.The atmosphere Controlling System guarantees that furnace atmosphere is always protective atmosphere, thereby has avoided the oxidation of crucible and the generation of impurity.
The present invention has given full play to the advantage of traditional induction heating iridium crucible crystal pulling method and resistive heating molybdenum crucible descent method, has overcome the having high input of induction heating iridium crucible, shortcoming that cost is high and traditional limited deficiency of falling crucible method thermograde setting range.Can grow size greater than Φ 170X130mm, dislocation desity less than 10
-3/ cm
2High-quality sapphire single-crystal body.But growing sapphire (α-Al
2O
3), Nd:YAG, (Nd, Ce): YAG, (Nd, Ce, Tb): the crystal of high-melting-points such as YAG, Ce:YAG, Yb:YAG.Simple, the low cost of manufacture of growth cell configuration of the present invention, technology of preparing good stability, process are reliable, bubble is easily got rid of, and have effectively improved the crystal growth quality, grow the good crystal of regular columniform large size, and its crystalline yield rate is greater than 80%.
Need to prove: though the foregoing description has been described structure of the present invention in detail; but the present invention is not limited to the foregoing description; the replacement structure that every those skilled in the art just can expect without creative work from the foregoing description all belongs to protection scope of the present invention.
Claims (6)
1. a large size sapphire crystal preparation technology is characterized in that: comprise the steps:
(1) aluminium sesquioxide of load weighted purity 〉=99.995% is packed in the molybdenum crucible, be evacuated to the stove internal gas pressure less than 10
-3Pa, fill protective atmosphere to furnace pressure and be-90～+ 20KPa;
(2) heat temperature raising, temperature rise rate 500W～1000W/h, after fully melting to raw material, constant temperature 3～5h melts the stage at raw material, and seed crystal is the insulation shutoff crucible through hole of insulation holder down down, guarantees that the heat insulation effect at molybdenum crucible seed crystal place melts seed crystal;
(3) seed crystal in the burner hearth is incubated decline 15-120mm down, molybdenum crucible descends then, dropping distance is the height of crucible, fall off rate 0.5～3.0mm/h, the through hole of insulation holder under the crucible is opened, entering in the hole than freezing air of bottom played the effect of a cooling to the seed crystal in the seed crystal pipe, for crystal growth provides enough thermogrades;
(4) cooling, temperature is reduced to 1600～1750 ℃ in the stove, and rate of temperature fall is 100W～300W/h;
(5) molybdenum crucible gos up to the heating zone, in-situ annealing, 1600～1750 ℃ of constant temperature 100-150h;
(6) slowly be cooled to room temperature, rate of temperature fall 50W～100W/h continues logical recirculated cooling water 24～36h, takes out crystal.
2. growing apparatus of realizing the described large size sapphire crystal preparation technology of claim 1, its bottom is insulation holder under the aluminum oxide, the zirconium white insulating brick is established on insulation holder top under the aluminum oxide, side insulation (5) is established in zirconium white insulating brick outside, ruhmkorff coil (6) is established in the outside of side insulation, the top of side insulation and zirconium white insulating brick is provided with protective guard (1), insulation holder and insulating brick surround hollow cavity under the aluminum oxide, described inner chamber bottom is provided with the crucible pole (12) that links to each other with hoisting appliance, it is characterized in that heating tube (4) is established in the inboard of insulating brick; Molybdenum crucible (7) is incubated holder (10) down by crucible and is connected with crucible pole (12), and the molybdenum crucible top is provided with cover (2) on the crucible.
3. large size sapphire crystal preparation technology's as claimed in claim 2 growing apparatus, insulation is held in the palm to be divided into from bottom to up and is incubated insulation holder (11) under the holder (13) and second aluminum oxide under first aluminum oxide under the described aluminum oxide, described zirconium white insulating brick is divided into the first zirconium white insulating brick (8) and the second zirconium white insulating brick (3) from bottom to up, and described heating tube (4) is arranged on the top of the first zirconium white insulating brick and the place, inboard of the second zirconium white insulating brick.
4. as claim 2 or 3 described large size sapphire crystal preparation technologies' growing apparatus, it is characterized in that: the crucible of seed crystal pipe (9) the bottom correspondence of molybdenum crucible (7) insulation holder down has through hole, the seed crystal that is provided with in the through hole is insulation (14) its underpart secondary elevating lever (15) that is connected down, and secondary elevating lever bottom passes with secondary hoisting appliance from the crucible pole bottom and links to each other.
5. large size sapphire crystal preparation technology's as claimed in claim 4 growing apparatus, it is characterized in that: also comprise an atmosphere Controlling System, described atmosphere Controlling System comprises PID controller, frequency transformer, pressure transmitter, transmitter and vacuum pump, pressure transmitter links to each other with the PID controller by transmitter, and the PID controller output end links to each other with vacuum pump by frequency transformer.
6. large size sapphire crystal preparation technology's as claimed in claim 5 growing apparatus is characterized in that: described heating tube is graphite heating pipe or tungsten heating tube or molybdenum heating tube.
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| CN101323978B true CN101323978B (en) | 2011-03-23 |
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| KR101136143B1 (en) * | 2009-09-05 | 2012-04-17 | 주식회사 크리스텍 | Method and Apparatus for Growing Sapphire Single Crystal |
| JP5526666B2 (en) * | 2009-09-08 | 2014-06-18 | 国立大学法人信州大学 | Sapphire single crystal manufacturing equipment |
| CN101913636B (en) * | 2010-08-20 | 2011-12-21 | 李振亚 | Method for producing high-purity high-density alumina block material for sapphire single crystals |
| CN102154698B (en) * | 2011-03-24 | 2013-01-23 | 哈尔滨奥瑞德光电技术股份有限公司 | Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method |
| CN102212871A (en) * | 2011-05-23 | 2011-10-12 | 无锡斯达新能源科技有限公司 | Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals |
| CN102418144B (en) * | 2011-11-28 | 2014-06-18 | 天通控股股份有限公司 | Manufacturing method of 4-inch C-directional sapphire crystal |
| CN102560637B (en) * | 2011-12-29 | 2014-11-19 | 中国科学院上海硅酸盐研究所 | Controllable reducing atmosphere Kyropoulos furnace |
| CN103320857B (en) * | 2012-03-20 | 2016-05-18 | 江苏中电振华晶体技术有限公司 | A kind of growing method of sapphire crystal and equipment |
| CN102628184B (en) * | 2012-05-07 | 2013-03-13 | 江苏浩瀚蓝宝石科技有限公司 | Method for growing gem crystals by way of vacuum induction heating and device realizing method |
| CN102644113A (en) * | 2012-05-14 | 2012-08-22 | 苏州海铂晶体有限公司 | Production method and equipment of c-oriented sapphire single crystal |
| CN103215632B (en) * | 2013-04-02 | 2016-02-24 | 苏州海铂晶体有限公司 | A kind of growth method of large size c orientation sapphire single-crystal |
| CN103215635B (en) * | 2013-04-27 | 2016-03-16 | 哈尔滨奥瑞德光电技术有限公司 | A kind of Heat insulation structure of sapphire single crystal furnace |
| CN104120487A (en) * | 2013-08-23 | 2014-10-29 | 江苏中电振华晶体技术有限公司 | Growth method and growth equipment of platelike sapphire crystals |
| CN104451892A (en) * | 2014-12-10 | 2015-03-25 | 上海汇淬光学科技有限公司 | Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system |
| CN105401215B (en) * | 2015-12-03 | 2017-09-29 | 河南西格马晶体科技有限公司 | A kind of device and method for being used to prepare big sheet 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 |
| CN105970292B (en) * | 2016-06-22 | 2018-03-16 | 大连晶达德光电技术有限公司 | A kind of method using cycle lifting and lowering method growing sapphire monocrystalline |
| CN109576788A (en) * | 2018-12-28 | 2019-04-05 | 中国科学院福建物质结构研究所 | A kind of Dy3+/Nd3+Double-doped LaF3The application of middle Tunable Infrared Laser crystal |
| US11674239B2 (en) * | 2020-02-27 | 2023-06-13 | Fujikoshi Machinery Corp. | Gallium oxide crystal manufacturing device |
| CN111455463A (en) * | 2020-04-28 | 2020-07-28 | 天通银厦新材料有限公司 | Manufacturing method of large-size doped sapphire crystal |
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