CN105624787A - Melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. - Google Patents
Melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. Download PDFInfo
- Publication number
- CN105624787A CN105624787A CN201610087431.5A CN201610087431A CN105624787A CN 105624787 A CN105624787 A CN 105624787A CN 201610087431 A CN201610087431 A CN 201610087431A CN 105624787 A CN105624787 A CN 105624787A
- Authority
- CN
- China
- Prior art keywords
- crystal
- growth
- yag
- diameter
- sapphire
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. Diameter of obtained large-size YAG or sapphire crystals can reach 90% of diameter of a crucible. Shouldering is realized through two stages, and lifting and rotating of the crystals are stopped after reaching equal-diameter growing; control on crystal growing rate is realized through PID (proportion integration differentiation), so that control on crystal crystallizing speed is realized. The melt-process crystal growing method has the advantages of controllable growing speed, large growing size and high repeatability and is suitable for industrialized production of large-size YAG crystals or sapphire crystals.
Description
Technical field
The present invention relates to laser crystal and substrate crystal technical field, particularly relate to the crystal growth method by melt method of a kind of large scale YAG or sapphire crystal.
Background technology
YAG crystal has good luminescence because of it, mechanically and thermally leads performance, and doping Nd then becomes excellent crystal growth performance, is front combination property working-laser material the most excellent, the most widely used. Existing numerous units are engaged in Nd:YAG production at present both at home and abroad, domestic such as Beijing Lei Shi Johson & Johnson, Chengdu Dong Jun laser company etc., abroad there are NorthropGrummanSynoptics, Saint-GobainCrystals&Defectors, II-VI optics VLOC subsidiary laboratory, MTI, ULTI Crystal Is Inc.. What these companies adopted is all method of crystal growth by crystal pulling technology.
Superlaser technology and photoelectronic industry field all need large-sized YAG crystal and sapphire crystal. Due to current large scale YAG crystal all adopt iridium crucible as heater sensing heat czochralski method prepare, crystalline size is generally less than or equal to about 1/2 size of crucible diameter, size-constrained; For Nd:YAG, greatest diametrical dimension only has �� 125mm both at home and abroad at present. And sapphire crystal can adopt czochralski method, kyropoulos and heat-exchanging method etc. to grow. For kyropoulos, though large-size crystals can be obtained, but due in isometrical crystal growing process, dependence is the temperature control growth of manual intervention, and repeatability is poor, and the empirical dependence of people is very big, is unfavorable for the concordance of growth batch.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes the crystal growth method by melt method of a kind of large scale YAG or sapphire crystal, the present invention has possessed the controllability of czochralski method, reproducible Automatic Control feature, also possessed the feature of kyropoulos growing large-size crystal, it is a kind of novel large scale YAG crystal and sapphire crystal growth method, at home and abroad there is no report.
A kind of large scale YAG of present invention proposition or the crystal growth method by melt method of sapphire crystal, adopt czochralski method seed crystal oriented growth, including: shouldering, isodiametric growth, cooling.
The present invention is with general heating czochralski method single crystal growing furnace for equipment, iridium crucible, tungsten crucible and molybdenum crucible is adopted to be used as sensing calandria and melt reservoirs, mode of heating includes: the eddy current 1. produced by changing currents with time inductive crucible melt is heated, 2. by graphite, the heating of tungsten silk screen resistance heating.
Preferably, the cylinder seed crystal of seed crystal to be cross section be �� 5��20mm or cross section are (5��20mm) �� (5��20mm) cuboid seed crystal.
Preferably, in shouldering process, crystal diameter d progressively grows into the 90% of crucible diameter D from �� 5��20mm, and the diameter of crystal does linear change with length, wherein 100mm��D��200mm.
Preferably, the concrete steps of shouldering include:
A, upwards to be lifted by 0.1��2.5mm/h by crystal to crystal diameter d be the 70% of crucible diameter D, is rotated by the speed of 0.5��30rpm by crystal in upwards lift process; Feedback according to crystal weight and detection, by controlling heating power to realize crystal growth;
B, the crystal growth obtained by step a are the 90% of crucible diameter D to crystal diameter d; Wherein in growth course, upwards pull rate is progressively down to 0mm/h by 0.1��2.5mm/h, and rotary speed is progressively down to 0rpm by 0.5��30rpm.
Preferably, in isodiametric growth process, according to the mass change situation that crystal grows within the unit interval, by pid algorithm, heating power is carried out feedback control, it is achieved the active of rate of crystalline growth is controlled, make crystal weight more than the 80% of raw material weight.
Preferably, the concretely comprising the following steps of cooling: the crystal obtained by isodiametric growth is down to room temperature in 48��140h and is obtained large scale YAG or sapphire crystal.
The present invention growth characteristic according to large scale YAG crystal and sapphire crystal, pulling rate and rotating speed is gradually reduced at shouldering stage leading portion, when shouldering terminates crystal rotation and upwards pull rate reduce to 0, hereafter the growing method not lifting and rotating is taked, it is achieved thereby that large scale YAG and sapphire crystal growth. The advantage that the method combines the controllability of czochralski method, reproducible full-automatic control, also the feature of kyropoulos growing large-size crystal is combined, it is a kind of novel large scale YAG crystal and sapphire crystal growth method, is suitable for industrialized mass production large scale YAG, sapphire crystal etc.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
The YAG crystal of growth �� 200mm:
Adopt the tungsten crucible of �� 230mm �� 230mm, with Zhong electricity section 26 the JGD1000 pulling single crystal furnace system being furnished with diffusion pump high vacuum system long for next life, wherein YAG raw material charged material weight is 34.5kg, and seed crystal is<111>direction, is of a size of the cylinder YAG crystal of �� 18mm �� 100mm.
After raw material is fully melted in single crystal growing furnace, the temperature at melt center is dropped to 1980 DEG C, YAG seed crystal is added in melt, growth is started from diameter �� 18mm with the speed of 2mm/h, initial speed is 20rpm, crystal shouldering angle is set to 45 ��, and isometrical diameter is set to 206.9mm, is set to 140mm etc. electrical path length. In shouldering part, machinery pull rate progressively becomes 0 from 1.984mm/h. By the feedback regulation of heating power so that crystal keeps the growth rate of 2mm/h in whole growth course. Growth time is 4.9 days, and temperature fall time is 5 days, namely within 10 days, can complete the YAG crystal growth of the �� 200mm of 30kg.
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; it is equal to replacement according to technical scheme and inventive concept thereof or is changed, all should be encompassed within protection scope of the present invention.
Claims (6)
1. the crystal growth method by melt method of a large scale YAG or sapphire crystal, it is characterised in that adopt czochralski method seed crystal oriented growth, including: shouldering, isodiametric growth, cooling.
2. the crystal growth method by melt method of large scale YAG or sapphire crystal according to claim 1, it is characterized in that, seed crystal is cross section is the cylinder seed crystal of �� 5��20mm or cross section is (5��20mm) �� (5��20mm) cuboid seed crystal.
3. the crystal growth method by melt method of large scale YAG according to claim 1 or claim 2 or sapphire crystal, it is characterized in that, in shouldering process, crystal diameter d progressively grows into the 90% of crucible diameter D from �� 5��20mm, the diameter of crystal does linear change with length, wherein 100mm��D��200mm.
4. the crystal growth method by melt method of large scale YAG or sapphire crystal according to any one of claim 1-3, it is characterised in that the concrete steps of shouldering include:
A, upwards to be lifted by 0.1��2.5mm/h by crystal to crystal diameter d be the 70% of crucible diameter D, is rotated by the speed of 0.5��30rpm by crystal in upwards lift process;
B, the crystal growth obtained by step a are the 90% of crucible diameter D to crystal diameter d; Wherein in growth course, upwards pull rate is progressively down to 0mm/h by 0.1��2.5mm/h, and rotary speed is progressively down to 0rpm by 0.5��30rpm.
5. the crystal growth method by melt method of large scale YAG or sapphire crystal according to any one of claim 1-4, it is characterized in that, in isodiametric growth process, according to the mass change situation that crystal grows within the unit interval, by pid algorithm, heating power is carried out feedback control, realize the active of rate of crystalline growth is controlled, make crystal weight more than the 80% of raw material weight.
6. the crystal growth method by melt method of large scale YAG or sapphire crystal according to any one of claim 1-5, it is characterized in that, concretely comprising the following steps of cooling: the crystal obtained by isodiametric growth is down to room temperature in 48��140h and is obtained large scale YAG or sapphire crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610087431.5A CN105624787A (en) | 2016-02-16 | 2016-02-16 | Melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610087431.5A CN105624787A (en) | 2016-02-16 | 2016-02-16 | Melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105624787A true CN105624787A (en) | 2016-06-01 |
Family
ID=56040116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610087431.5A Pending CN105624787A (en) | 2016-02-16 | 2016-02-16 | Melt-process crystal growing method of large-size YAG (yttrium aluminum garnet) or sapphire crystals. |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105624787A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403679A (en) * | 2021-03-15 | 2021-09-17 | 青岛海泰光电技术有限公司 | Method for growing emerald gem crystal by Czochralski method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544712A (en) * | 2003-11-18 | 2004-11-10 | 陈迎春 | Integrated melt method for crystal growth |
| CN102758249A (en) * | 2012-08-13 | 2012-10-31 | 登封市蓝天石化光伏电力装备有限公司 | Method for preparing colorless corundum monocrystal |
| CN103014842A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Rotary shoulder technique for growing sapphire crystal by kyropoulos method |
| CN103710745A (en) * | 2013-12-26 | 2014-04-09 | 南京晶升能源设备有限公司 | Method for automatically controlling growth of 85-120kg sapphire crystals |
-
2016
- 2016-02-16 CN CN201610087431.5A patent/CN105624787A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544712A (en) * | 2003-11-18 | 2004-11-10 | 陈迎春 | Integrated melt method for crystal growth |
| CN102758249A (en) * | 2012-08-13 | 2012-10-31 | 登封市蓝天石化光伏电力装备有限公司 | Method for preparing colorless corundum monocrystal |
| CN103014842A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Rotary shoulder technique for growing sapphire crystal by kyropoulos method |
| CN103710745A (en) * | 2013-12-26 | 2014-04-09 | 南京晶升能源设备有限公司 | Method for automatically controlling growth of 85-120kg sapphire crystals |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403679A (en) * | 2021-03-15 | 2021-09-17 | 青岛海泰光电技术有限公司 | Method for growing emerald gem crystal by Czochralski method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101348940B (en) | Improved Bridgman growth method for compound semiconductor GaAs single crystal | |
| CN103541008B (en) | A kind of growth method of large size gallium oxide single crystal and growing apparatus | |
| CN102758249B (en) | A kind of preparation method of colourless boule monocrystal | |
| CN2885891Y (en) | Temperature control furnace for growth of arsenide gallium monocrystal | |
| CN104962994B (en) | The method that EFG technique grows the rear-earth-doped serial crystal containing Ga garnet of specific dimensions | |
| CN103938270A (en) | Growth method of gallium heavily doped low-dislocation germanium single crystal | |
| CN101323978A (en) | Large size sapphire crystal preparing technology and growing apparatus thereof | |
| CN101580961A (en) | Method for growing crystal by reducing atmosphere Kyropoulos method | |
| CN1844487A (en) | Method for growth of gallium arsenide monocrystal by gradient freeze method in horizontal three-temperature-zone furnace | |
| CN103789835A (en) | Improved gradient freeze GaAs single crystal growing method | |
| US7211142B2 (en) | CdTe single crystal and CdTe polycrystal, and method for preparation thereof | |
| CN101481821B (en) | Novel technology for growth of yttrium-aluminum garnet crystal and equipment thereof | |
| CN102154698A (en) | Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method | |
| CN101280456B (en) | Growing method by Ti3O5 by bridgman method | |
| TWI699464B (en) | Compound semiconductor and compound semiconductor single crystal manufacturing method | |
| CN104313693A (en) | Yttrium aluminum garnet laser crystal doped growth device, crystal growth furnace and preparation method thereof | |
| CN101338453A (en) | Growth device of large size non-core YAG series laser crystal and growth process thereof | |
| CN101348939B (en) | Growth method improving gallium arsenide single crystal utilization ratio | |
| CN104562183A (en) | Method for growing large-sized rare-earth-doped barium yttrium fluoride single crystals | |
| CN107794563A (en) | A kind of vertical pulling method prepares the processing technology of monocrystalline silicon | |
| CN102168307A (en) | Method for growing cerium-yttrium-aluminum garnet crystal | |
| CN102534758A (en) | Growth method and growth device for bar-shaped sapphire crystals | |
| CN102560631A (en) | Growth method and equipment of sapphire crystal | |
| CN103215640A (en) | Method for growing large-size fluoride crystals through top seed crystal kyropoulos method | |
| CN104674340A (en) | Rotary necking and seeding control method used in large-size sapphire crystal growth through kyropoulos method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160601 |