CN102628184B - Method for growing gem crystals by way of vacuum induction heating and device realizing method - Google Patents
Method for growing gem crystals by way of vacuum induction heating and device realizing method Download PDFInfo
- Publication number
- CN102628184B CN102628184B CN 201210138298 CN201210138298A CN102628184B CN 102628184 B CN102628184 B CN 102628184B CN 201210138298 CN201210138298 CN 201210138298 CN 201210138298 A CN201210138298 A CN 201210138298A CN 102628184 B CN102628184 B CN 102628184B
- Authority
- CN
- China
- Prior art keywords
- tungsten
- molybdenum
- crystal
- crucible
- miramint
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention provides a method for growing gem crystals by way of vacuum induction heating and a device realizing the method. The method includes the following steps: an inductive tungsten, molybdenum or tungsten-molybdenum alloy heating body is utilized to heat alumina material in a crucible until the alumina material is melted, the convection of the melt and the linear velocity of flow are observed, an appropriate seeding temperature is chosen by adjusting the relative positional relation between the inductive tungsten, molybdenum or tungsten-molybdenum alloy heating body and the crucible, and after seeding, crystallization, equal-diameter growth and separation between crystals and the crucible, crystal growth is finished. An adjustable gap exists between the inductive tungsten, molybdenum or tungsten-molybdenum alloy heating body (7) and the tungsten, molybdenum or tungsten-molybdenum alloy crucible of the device (13), so that the relative positional relation between the inductive tungsten, molybdenum or tungsten-molybdenum alloy heating body (7) and the tungsten, molybdenum or tungsten-molybdenum alloy crucible of the device (13) can be adjusted. The method and the device can be adopted to produce large-dimension sapphires, the process can be conveniently and automatically controlled, energy consumption is reduced, and the cost is saved.
Description
Technical field
The present invention relates to a kind of method of vacuum induction heat growth sapphire crystal, be included on the basis of induction heating Czochralski grown crystal, mode by induction tungsten, molybdenum or miramint heating member heats, alumina raw material is to fusing in the heating crucible, observe melt convection situation and liquid stream linear velocities, select the suitable temperature of sowing by regulating tungsten, molybdenum or miramint heating member and crucible relative position relation, through sowing, shouldering, isodiametric growth and crystal and crucible detach procedure, finish crystal and grow.
The invention still further relates to a kind of equipment of vacuum induction heat growth sapphire crystal, comprise that graphite felt is as thermal insulation layer, tungsten, molybdenum or miramint crucible, also comprise induction tungsten, molybdenum or miramint heating member, between induction tungsten, molybdenum or miramint heating member and tungsten, molybdenum or the miramint crucible adjustable gap is arranged, can regulate induction tungsten, molybdenum or miramint heating member and tungsten, molybdenum or miramint crucible relative position relation.
Background technology
Sapphire crystal has stable chemical property, good mechanical property, good heat conductivity and electric insulating quality have unique mechanics, optical property, and resistance to chemical attack, high temperature resistant, heat conduction good, hardness is high, can work under mal-condition, be a kind of desirable optics starting material.Sapphire crystal have near ultraviolet to the infrared very wide scope that sees through, be widely used in the GaN substrate material of high-brightness LED, the substrate material of large-scale integrated circuit, special optical components and parts, high energy are surveyed and the window material of high power laser light.In recent years because the increasing rapidly of the market requirements such as LED illumination, LED TV, its technology of preparing is widely studied, and large size sapphire crystal prepares common method kyropoulos, heat-exchanging method and warm terraced method etc. are arranged.
Wherein warm terraced method contacts with crucible because of the crystal that grows, because crucible is different from the thermal expansivity of crystal, crucible can produce stress to the crystal that grows and increase the probability of crystal cleavage in temperature-fall period, and yield rate is difficult to raising.Heat-exchanging method technique is relatively ripe, generally can prepare the above sapphire crystal of 300 mm diameter, but equipment cost is very high.Kyropoulos can the relatively large sapphire crystal of growth size because of it, suitable equipment cost and being adopted in a large number gradually.But traditional kyropoulos heats and heat-insulation system adopts tungsten and molybdenum material to make, and tungsten and molybdenum material is at high temperature yielding, can cause the temperature field asymmetric after repeatedly using, and is unfavorable for sapphire growth.Chinese invention patent 200510010116.4 discloses a kind of " cold core shouldering micropulling proparation method of large-size sapphire single-crystal ", the method is by the mode of resistive heating, adopt the insulation of tungsten radiation shield, under vacuum condition through heating raw, seeding, shouldering, isometrically lift, cooling and annealing process procedure, but thermograde is very little in this method technological process, technological process control is very difficult, needs very high peopleware, and level of automation is difficult to improve.Chinese patent 200910053206.X relates to a kind of " method of growing crystal by reducing atmosphere Kyropoulos method " in addition; the method is owing to carbon containing in the lagging material; at high temperature with system in a small amount of oxygen reaction form carbon monoxide reducing atmosphere be provided; and be filled with high-purity N 2 or Ar as protective gas; because the kyropoulos crystal growing process cycle is very long; can increase energy consumption; thereby increased the crystal growth cost; under non-vacuum condition, adopt simultaneously the kyropoulos growing crystal, very easily cause parcel bubble, of low quality in the crystal.
[0005] however aforesaid method has only solved the problems such as sapphire crystal growth atmosphere surrounding in the sapphire crystal growth process, induction tungsten calorifier, the insulation of tungsten radiation shield.Existing sapphire crystal growth method is not equipped with tungsten, molybdenum or miramint crucible temperature setting device, can not regulate the rate of temperature fall after can finishing with growth in the crystal growing process, can not energy-saving and emission-reduction.Therefore, the technology of existing growing sapphire crystal can not solve the following problem that present stage occurs: tungsten, molybdenum or miramint crucible temperature gradient are less, crystal growth intensification temperature reduction technology process control difficulty can't be carried and do level of automation, and energy consumption is huge etc.
Summary of the invention
The deficiency that exists for overcoming above-mentioned sapphire crystal growth technology, technical problem to be solved by this invention provide a kind of sapphire crystal growth process and are convenient to control, and the sapphire crystal growth method of energy-conserving and environment-protective more.
Corresponding therewith, another technical problem that will solve of the present invention provides a kind of sapphire crystal growth process and is convenient to control and the equipment of the sapphire crystal growth of energy-conserving and environment-protective more.
With regard to the sapphire crystal making method, the method that the present invention solves the problems of the technologies described above is as follows: on the basis of induction heating Czochralski grown crystal, mode by induction tungsten, molybdenum or miramint heating member heats, alumina raw material is to fusing in the heating crucible, observe melt convection situation and liquid stream linear velocities, select the suitable temperature of sowing by regulating tungsten, molybdenum or miramint heating member and crucible relative position relation: when sowing, if temperature is then on the low side, produce easily polycrystalline and cause crystal cleavage, and in crystal, form the defective such as bubble; , temperature drift, seed crystal carry out nothing but normal crystal growth if can being melted.Through sowing, shouldering, isodiametric growth and crystal and crucible detach procedure, finish crystal and grow.
As the improvement of vacuum induction heat growth sapphire crystal method of the present invention, vacuum pressure in the crystal growing process can be kept being not more than 6 * 10
-3Pa; thermal conduction reduces greatly under this vacuum condition; adopt the growth conditions of protection of inert gas to compare with tradition; has the advantage that reduces energy consumption, saves cost; simultaneously under vacuum condition in the melt dissolved gases evaporate easily; reduce the defective of the wraps such as bubble in the crystal, improved crystal mass.
As the improvement of vacuum induction heat growth sapphire crystal method of the present invention, process of growth lifts pulling rate in the 0.05-0.6mm/h scope with the mode growing crystal of slow crystal pulling method.Adopt the mode slowly lift in the process of growth, can avoid in the kyropoulos that tradition do not lift crystal easily sticking crucible and the speed of growth wait slowly problem, improved greatly efficient and the controllability of crystal growth.
As the improvement of vacuum induction heat growth sapphire crystal method of the present invention, the crystal growing process rate of temperature fall is 5-500 watt/hour, and rate of temperature fall was 100-2000 watt/hour after growth finished.
With regard to vacuum induction heat growth sapphire crystal method, the present invention is that the equipment of the employing that solve the technical problem comprises that graphite felt (4) is as thermal insulation layer, tungsten, molybdenum or miramint crucible (13), vacuum induction adds and also comprises induction tungsten, molybdenum or miramint heating member (7), between induction tungsten, molybdenum or miramint heating member (7) and tungsten, molybdenum or the miramint crucible (13) adjustable gap is arranged, can regulate induction tungsten, molybdenum or miramint heating member (7) and tungsten, molybdenum or miramint crucible (13) relative position relation.
Induction tungsten, molybdenum or miramint heating member (7) adopt the equipment of said structure, owing to can be regulated with tungsten, molybdenum or miramint crucible (13) gap size.When seeding growth process excessive velocities occurring, restive, namely thermograde too hour can tune up induction tungsten, molybdenum or miramint heating member (7) and tungsten, molybdenum or miramint crucible (13) gap, thereby improves the controllability of crystal growth.When ftractureing easily after the crystal growth, can turn induction tungsten, molybdenum or miramint heating member (7) and tungsten, molybdenum or miramint crucible (13) gap down, thereby reduce the thermograde of system, the stress that reduces crystal forms.
The equipment of realizing vacuum induction heat growth sapphire crystal method as the present invention further improves, the outer zirconium white bucket (6) that uses of induction tungsten, molybdenum or miramint heating member (7) is as thermal insulation layer, and zirconium white bucket (6) skin uses graphite felt (4) parcel.The nexine of lagging material adopts the zirconium white bucket as thermal insulation layer, the outer graphite felt of using is as thermal insulation layer, at high temperature outer graphite felt can be removed oxygen a small amount of in the system, internal layer uses the zirconium white bucket can avoid crucible to contact with graphite simultaneously, carbon and crucible reaction produce the probability of carbide in the reduction graphite felt, thereby prolong pot life.
The equipment of realizing vacuum induction heat growth sapphire crystal method as the present invention further improves, adopt the zirconium white stay-warm case as thermal insulation layer (9) at tungsten, molybdenum or miramint crucible (13) top nexine, outer graphite felt (4) parcel that uses is as thermal insulation layer.The nexine of lagging material adopts the zirconium white bucket as thermal insulation layer, the outer graphite felt of using is as thermal insulation layer, at high temperature outer graphite felt can be removed oxygen a small amount of in the system, internal layer uses the zirconium white bucket can avoid crucible to contact with graphite simultaneously, carbon and crucible reaction produce the probability of carbide in the reduction graphite felt, thereby prolong pot life.
Description of drawings
Fig. 1: the synoptic diagram of vacuum induction heat growth sapphire crystal equipment of the present invention.
Among the figure: 1-eye-observation position, 2-viewing window, 3-seed rod, 4-graphite felt, 5-seed crystal, 6-zirconium white bucket, 7-induction tungsten, molybdenum or miramint heating member, the holder of 8-zirconium white, 9-zirconium white stay-warm case, 10-crystal, 11-ruhmkorff coil, 12-melt, 13-tungsten, molybdenum or miramint crucible, 14-body of heater.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Embodiment 1: adopt method growth Φ 100 sapphire crystals of the present invention
Alumina raw material is packed in tungsten, molybdenum or the miramint crucible 13, and by the induction heater that installs shown in Figure 1, among the figure: 1-eye-observation position, 2-viewing window, 3-seed rod, 4-graphite felt, 5-seed crystal, 6-zirconium white bucket, 7-induction tungsten, molybdenum or miramint heating member, the holder of 8-zirconium white, 9-zirconium white stay-warm case, 10-crystal, 11-ruhmkorff coil, 12-melt, 13-tungsten, molybdenum or miramint crucible, 14-body of heater.Be evacuated to vacuum tightness and be higher than 6 * 10
-3Pa, after begin to heat up with the raw material fusing, the seed crystal direction be a to, adopt traditional kyropoulos crystal growth technique, observe the charge level situation by viewing window 2, according to seeded growth speed, behind seed crystal contact liquid level 5-10 minute, the 1-2mm that grows around the seed crystal was the suitable temp temperature of sowing, afterwards with 60 watts/hour cooling rate cooling growing crystal, be down to power as 0 take 150 watts/hour cooling rate after the crystal growth finishes, powered-down cools to room temperature with the furnace, takes out crystal.Growing crystalline size is Φ 100 * 150mm
3Sapphire crystal.
Embodiment 2: adopt method growth Φ 150 sapphire crystals of the present invention
Alumina raw material is packed in the tungsten crucible, and by the induction heater that installs shown in Figure 1, among the figure: 1-eye-observation position, 2-viewing window, 3-lifting rod, 4-graphite felt, 5-seed crystal, 6-zirconium white bucket, 7-tungsten heating member, the holder of 8-zirconium white, 9-zirconium white stay-warm case, 10-crystal, 11-ruhmkorff coil, 12-melt, 13-tungsten crucible, 14-body of heater.Be evacuated to vacuum tightness and be higher than 6 * 10
-3Behind the Pa, begin to heat up raw material is melted, the seed crystal direction be c to, observe the charge level situations by viewing window 2, according to seeded growth speed, behind seed crystal contact liquid level 5-10 minute, the 1-2mm that grows around the seed crystal is the suitable temp temperature of sowing, and with 5 watts/hour cooling rate cooling growing crystal, is down to power as 0 take 200 watts/hour cooling rate after the crystal growth finishes afterwards, powered-down cools to room temperature with the furnace, takes out crystal.Growing crystalline size is Φ 150 * 200mm
3Sapphire crystal.
Claims (2)
1. the method for a vacuum induction heat growth sapphire crystal, it is characterized in that: on the basis of induction heating Czochralski grown crystal, mode by induction tungsten, molybdenum or miramint heating member heats, alumina raw material is to fusing in the heating crucible, observe melt convection situation and liquid stream linear velocities, select the suitable temperature of sowing by regulating tungsten, molybdenum or miramint heating member and crucible relative position relation, through sowing, shouldering, isodiametric growth and crystal and crucible detach procedure, finish crystal and grow; Wherein, vacuum pressure is not more than 6 * 10 in the crystal growing process
-3Pa; Process of growth lifts pulling rate in the 0.05-0.6mm/h scope with the mode growing crystal of slow crystal pulling method; The crystal growing process rate of temperature fall is 5-500 watt/hour, and rate of temperature fall was 100-2000 watt/hour after growth finished.
2. equipment of be used for realizing the described vacuum induction heat growth of claim 1 sapphire crystal method, comprise that graphite felt (4) is as thermal insulation layer, tungsten, molybdenum or miramint crucible (13), the equipment that it is characterized in that described vacuum induction heat growth sapphire crystal method also comprises induction tungsten, molybdenum or miramint heating member (7), induction tungsten, molybdenum or miramint heating member (7) and tungsten, between molybdenum or the miramint crucible (13) adjustable gap is arranged, can regulate induction tungsten, molybdenum or miramint heating member (7) and tungsten, molybdenum or miramint crucible (13) relative position relation; The outer zirconium white bucket (6) that uses of induction tungsten, molybdenum or miramint heating member (7) is as thermal insulation layer, and zirconium white bucket (6) skin uses graphite felt (4) parcel; Adopt zirconium white stay-warm case (9) as thermal insulation layer at tungsten, molybdenum or miramint crucible (13) top nexine, outer graphite felt (4) parcel that uses is as thermal insulation layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210138298 CN102628184B (en) | 2012-05-07 | 2012-05-07 | Method for growing gem crystals by way of vacuum induction heating and device realizing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210138298 CN102628184B (en) | 2012-05-07 | 2012-05-07 | Method for growing gem crystals by way of vacuum induction heating and device realizing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102628184A CN102628184A (en) | 2012-08-08 |
| CN102628184B true CN102628184B (en) | 2013-03-13 |
Family
ID=46586567
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210138298 Active CN102628184B (en) | 2012-05-07 | 2012-05-07 | Method for growing gem crystals by way of vacuum induction heating and device realizing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102628184B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9457405B2 (en) * | 2012-05-29 | 2016-10-04 | H.C. Starck, Inc. | Metallic crucibles and methods of forming the same |
| KR101676213B1 (en) | 2012-09-28 | 2016-11-14 | 가부시끼가이샤 아라이도 마테리아루 | Crucible for growing sapphire single crystal, and method for producing crucible for growing sapphire single crystal |
| KR101439380B1 (en) * | 2012-10-31 | 2014-09-11 | 주식회사 사파이어테크놀로지 | Heat Treatment Method and Apparatus for Sapphier Single Crystal |
| CN103806102B (en) * | 2014-02-14 | 2017-01-11 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN105135883B (en) * | 2015-08-27 | 2018-03-23 | 北京矿冶研究总院 | Intermediate frequency furnace high temperature sintering is with thermal-insulated frock |
| CN106119962A (en) * | 2016-02-03 | 2016-11-16 | 江苏浩瀚蓝宝石科技有限公司 | The Performance comparision analysis of kyropoulos sapphire crystal furnace difference heat protection screen material |
| CN108441937A (en) * | 2018-03-06 | 2018-08-24 | 同济大学 | The crystal growing apparatus of included melt agitating function |
| CN108441938A (en) * | 2018-03-06 | 2018-08-24 | 同济大学 | Special-shaped thermal-field device suitable for crystal growth |
| CN108950676A (en) * | 2018-07-16 | 2018-12-07 | 苏州四海常晶光电材料有限公司 | A kind of double induction molybdenum crucible method of crystal growth by crystal pulling device and methods of reducing atmosphere |
| CN108754430A (en) * | 2018-09-04 | 2018-11-06 | 宝鸡市创信金属材料有限公司 | A kind of adjustable tungsten thin-walled evaporation boat of disengagement area |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1228477C (en) * | 2002-06-21 | 2005-11-23 | 深圳市淼浩高新科技开发有限公司 | Using induction heating molybdenium crucible in hydrogen atmosphere to make Czochralski grown sapphire crystal |
| CN1323195C (en) * | 2005-06-24 | 2007-06-27 | 哈尔滨工业大学 | Cold core shouldering micropulling proparation method of large size sapphire single crystal |
| CN101323978B (en) * | 2008-07-29 | 2011-03-23 | 成都东骏激光股份有限公司 | Large size sapphire crystal preparing technology and growing apparatus thereof |
| JP2010052993A (en) * | 2008-08-29 | 2010-03-11 | Kyocera Corp | Crucible for apparatus for growing single crystal, method for growing single crystal, and apparatus for growing single crystal |
-
2012
- 2012-05-07 CN CN 201210138298 patent/CN102628184B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102628184A (en) | 2012-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102628184B (en) | Method for growing gem crystals by way of vacuum induction heating and device realizing method | |
| CN101323978B (en) | Large size sapphire crystal preparing technology and growing apparatus thereof | |
| CN101580963B (en) | SAPMAC method for preparing sapphire single-crystal with size above 300mm | |
| CN100513652C (en) | Process and device for growing low dislocation germanium single crystal by crucible lowering Czochralski method | |
| CN100564615C (en) | The preparation method of multi-element compounds semiconductor single-crystal and growing apparatus | |
| CN102732953B (en) | Technology and apparatus for growing single silicon carbide crystals through double seed crystal-assisted vapor transport method | |
| CN110983429A (en) | Single crystal furnace and monocrystalline silicon preparation method | |
| CN107541776A (en) | A kind of growth apparatus and method of large scale gallium oxide single crystal | |
| CN102154698B (en) | Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method | |
| CN103060901B (en) | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method | |
| CN104109904A (en) | Seeding method of sapphire crystal growth kyropoulos method | |
| CN102758249A (en) | Method for preparing colorless corundum monocrystal | |
| CN104451892A (en) | Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system | |
| CN104651935B (en) | A kind of method that crucible rise method prepares high-quality sapphire crystal | |
| CN102732944A (en) | Crystal growth technology and crystal growth furnace | |
| CN107130289A (en) | A kind of growing method for improving heat exchange large size sapphire crystal | |
| CN102534758A (en) | Growth method and growth device for bar-shaped sapphire crystals | |
| CN103305903B (en) | A kind of high nitrogen pressure fusing assistant-falling crucible method prepares the method for GaN crystal | |
| CN103060913A (en) | Growth method of large-scale sapphire crystal | |
| CN103614765A (en) | Method of heating graphite to grow sapphire crystal | |
| CN102560631A (en) | Growth method and equipment of sapphire crystal | |
| TW201243114A (en) | Resistance heated sapphire single crystal ingot grower, method of manufacturing resistance heated sapphire single crystal ingot, sapphire single crystal ingot, and sapphire wafer | |
| CN103205799A (en) | Method for growing C-oriented white stone crystals | |
| CN103422163A (en) | Device and method for growing sapphire single crystals | |
| CN203530480U (en) | Equipment for growing sapphire single crystals |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20120808 Assignee: JIANGSU NENGJIAN ELECTROMECHANICAL INDUSTRIAL CO., LTD. Assignor: Jiangsu Haohan Lanbaoshi Technology Co., Ltd. Contract record no.: 2013320000172 Denomination of invention: Method for growing gem crystals by way of vacuum induction heating and device realizing method Granted publication date: 20130313 License type: Exclusive License Record date: 20130320 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model |