CN101418468A - Apparatus for growing lithium aluminate crystal by czochralski method - Google Patents
Apparatus for growing lithium aluminate crystal by czochralski method Download PDFInfo
- Publication number
- CN101418468A CN101418468A CNA2008102026068A CN200810202606A CN101418468A CN 101418468 A CN101418468 A CN 101418468A CN A2008102026068 A CNA2008102026068 A CN A2008102026068A CN 200810202606 A CN200810202606 A CN 200810202606A CN 101418468 A CN101418468 A CN 101418468A
- Authority
- CN
- China
- Prior art keywords
- stay
- warm case
- lithium aluminate
- crystal
- growing
- 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
Images
Abstract
The invention provides a device for growing lithium aluminate crystals by a pulling method, which comprises a pulling-method single crystal growth furnace. The device is characterized in that the sidewall of a heat preservation cover of the single crystal furnace is intact and is provided with no observation window, and on the furnace wall opposite to an observation window, an observation mirror is erected above the heat preservation cover through a bracket, so as to observe a melt interface in an iridium crucible through the reflection of the observation mirror. The device has the advantages that the device can guarantee the uniformity and symmetry of a temperature field in a cavity of the heat preservation cover, effectively inhibit component volatilization in a process of growing the lithium aluminate crystals by the pulling method, and realize the growth of large-size and high-quality lithium aluminate crystals.
Description
Technical field
The present invention relates to lithium aluminate crystal, particularly a kind of device with growing lithium aluminate crystal by czochralski method.
Background technology
In recent years, lithium aluminate crystal is because of can extension obtaining nonpolar GaN film and device has caused researchist's great interest thereon.But, adopting often to be accompanied by serious bath component volatilization in traditional growing lithium aluminate crystal by czochralski method process, the crystal nonstoichiometry is more serious frequently, makes crystal phenomenons such as devitrification, cracking occur, and crystal mass is affected and is difficult to long; The thermal stresses that produces in the crystal growth temperature-fall period can make crystal burst in temperature-fall period or occur in slice processing that the wafer song sticks up even phenomenon such as cracking in addition.Tradition lifting furnace device is seen Fig. 1, among the figure: 1-furnace wall, 4-stay-warm case loam cake, 5-seed rod, 6-zirconium white stay-warm case, 8-iridium crucible, 9-quartz barrel, 10-zirconium white insulation sand, 11-alumina tray, 12-tray supporter, 13-ruhmkorff coil, 14-furnace wall observation window, 19-stay-warm case sidewall view port.Also have 15-melt, 16-seed crystal, 17-light, 18-human eye among Fig. 1.This is the stay-warm case 6 that hollow circular cylinder is arranged outward because of the crucible that carries out the lithium aluminate crystal growth with traditional lifting furnace device, this stay-warm case is generally made with zirconium white, zirconium white top cover 4 is arranged at the stay-warm case top, there is a little perforate in top cover central authorities, seed rod is by this hole, stretch into stay-warm case inside, from melt, lift out crystal by seed rod 5 lower end fixed seed crystals 16.On the other hand, stay-warm case 6 outsides generally have an aperture, the perforate of the top cover at these stay-warm case 6 outside viewing windows 19 and stay-warm case top forms circulation flow path owing to the temperature difference, but this stay-warm case often can not solve the quality problems of the volatile high temperature crystal growth of component, and how to suppress the volatilization of crystal component when high growth temperature, be the key problem in technology that obtains the high quality crystal material.Therefore, the bath component that exists in a kind of lithium aluminate crystal process that can effectively solve of exploitation with Czochralski grown volatilize and reduce by warm field distribution inequality, thermograde is asymmetric and the growing apparatus of the thermal stresses introduced in crystal just seems important all the more.
Summary of the invention
The objective of the invention is to solve with the most outstanding bath component evaporable problem of running in crystal pulling method (Czochralski method or Cz method) the growing lithium aluminate crystal process, a kind of device with growing lithium aluminate crystal by czochralski method is provided, prevent lithium aluminate crystal component deviation stoichiometric ratio and cause crystal devitrification and cracking phenomena in process of growth, realize the large-size high-quality lithium aluminate crystal crystal growth.
At Cz method lithium aluminate crystal growth phase, cause lithium aluminate melt evaporable mechanism more complicated.Our a large amount of experiment find the iridium crucible and on it small variations of stay-warm case system just might make and almost not have volatileness and become serious volatileness.We think thus, and suppressing the evaporable key is by regulating warm, suppressing melt top stay-warm case inner chamber and cover outer gaseous exchange.One of them main strong gaseous exchange is exactly to cause the asymmetric caused of temperature field and temperature gradient distribution by being positioned at the lateral view port of stay-warm case, thereby have a strong impact on the stability, uniformity of temperature field, cause lithium aluminate crystal in process of growth, to have serious component volatilization phenomenon.
Technical solution of the present invention is as follows:
A kind of device with growing lithium aluminate crystal by czochralski method, comprise a Czochralski grown single crystal growing furnace, its characteristics are: the stay-warm case sidewall of this single crystal growing furnace is complete, do not establish viewing window, on the furnace wall relative, set up a sight glass above described stay-warm case, so that the reflection by described sight glass realizes the observation to melt interface in the described iridium crucible by support with view port.
A kind of device with growing lithium aluminate crystal by czochralski method, comprise a Czochralski grown single crystal growing furnace, in the burner hearth that the furnace wall constitutes, tray supporter is arranged, on this tray supporter, be alumina tray, quartz barrel and iridium crucible are set on this alumina tray, round shape iridium after-heater is housed on described iridium crucible, round shape oxidation zirconium stay-warm case is set outside this iridium after-heater, at described quartz barrel and iridium crucible, fill zirconium white insulation sand between the round shape oxidation zirconium stay-warm case, outside described quartz barrel, be ruhmkorff coil, there is the furnace wall observation window described furnace wall, its characteristics are: described round shape oxidation zirconium stay-warm case sidewall is complete, do not establish viewing window, setting up a sight glass above described round shape oxidation zirconium stay-warm case by the sight glass support on the furnace wall relative, so that the reflection by described sight glass realizes the observation to melt interface in the described iridium crucible with described furnace wall observation window.
Described round shape oxidation zirconium stay-warm case also has the stay-warm case loam cake.
Described stay-warm case loam cake is the circular disc of being made by transparent material or opaque material with center through hole, and this through hole supplier observes just that seed crystal is sowed, crystal growth situation and seed crystal is sowed, crystalline lifting etc.
The quartzy disk of the sapphire disk that described stay-warm case loam cake is twin polishing, the magnesium-aluminium spinel disk of twin polishing, twin polishing or the yttrium aluminum garnet disk of twin polishing.
Described sight glass is the silver-plated plane mirror of polishing copper sheet, the silver-plated plane mirror of silica glass, K9 glass silvering plane mirror, the silver-plated dimpling minute surface of polishing copper sheet, the silver-plated dimpling minute surface of silica glass, or K9 glass silvering dimpling minute surface.
Technique effect of the present invention:
This device is because described round shape oxidation zirconium stay-warm case sidewall is complete, do not establish viewing window and can effectively improve warm field uniformity, symmetry in the traditional method of crystal growth by crystal pulling system, suppress in the growing lithium aluminate crystal by czochralski method process because the bath component that the convection current of intensive lateral gas causes volatilization, prevent lithium aluminate crystal substantial deviation stoichiometric ratio in process of growth, significantly improved the quality of crystal growth, the available large-size high-quality lithium aluminate crystal crystal that grows;
Apparatus of the present invention also are applicable to the non-volatile crystalloid of growth, and this device also can effectively improve temperature field in the lifting furnace system and thermograde homogeneity, symmetry, helps improving crystal mass and yield rate, and has advantages such as with low cost, easy handling.
Description of drawings
Fig. 1 is the synoptic diagram of traditional pulling crystal stove,
Fig. 2 is the structural representation of the present invention with an embodiment of device of growing lithium aluminate crystal by czochralski method
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
See also Fig. 2 earlier, Fig. 2 is the structural representation of the present invention with an embodiment of device of growing lithium aluminate crystal by czochralski method, as seen from the figure, the present invention's device of growing lithium aluminate crystal by czochralski method, comprise a Czochralski grown single crystal growing furnace, in the burner hearth that furnace wall 1 constitutes, tray supporter 12 is arranged, on this tray supporter 12, be alumina tray 11, quartz barrel 9 and iridium crucible 8 are set on this alumina tray 11, round shape iridium after-heater 7 is housed on described iridium crucible 8, round shape oxidation zirconium stay-warm case 6 is set outside this iridium after-heater 7, at described quartz barrel 9 and iridium crucible 8, fill zirconium white insulation sand 10 between the round shape oxidation zirconium stay-warm case 6, outside described quartz barrel 9, be ruhmkorff coil 13, there is furnace wall observation window 14 described furnace wall 1, described round shape oxidation zirconium stay-warm case 6 sidewalls are complete, do not establish viewing window, with the furnace wall 1 of described furnace wall observation window 14 opposite faces on set up a sight glass 2 above round shape oxidation zirconium stay-warm case 6 by sight glass support 3 so that the reflection by described sight glass 2 realizes the observation to melt interfaces in the described iridium crucible 8.Described in the present embodiment round shape oxidation zirconium stay-warm case 6 also has stay-warm case loam cake 4.Described stay-warm case loam cake 4 is circular discs with central openings of being made by zirconia material.
Described stay-warm case loam cake 4 can be made by transparent material or opaque material, is the sapphire disk of twin polishing, the magnesium-aluminium spinel disk of twin polishing, the quartzy disk of twin polishing or the yttrium aluminum garnet disk of twin polishing.
Described sight glass 2 is the silver-plated plane mirror of polishing copper sheet, the silver-plated plane mirror of silica glass, K9 glass silvering plane mirror, the silver-plated dimpling minute surface of polishing copper sheet, the silver-plated dimpling minute surface of silica glass, or K9 glass silvering dimpling minute surface.
Utilize the present embodiment device to carry out the growth of lithium aluminate crystal, situation is as follows:
According to mol ratio Al2O3: Li2CO3=1: 1 to take by weighing purity be 99.999% exsiccant raw material, mixes, and depresses to the material cake of Φ 78 * 30mm3 at the pressure of 1GPa, synthetic 10 hours of 1100 ℃ of pre-burnings; During the agglomerate material packed in the Iridium Crucible 8 of Φ 110 * 80mm3, and in the lifting furnace of packing into, as shown in Figure 2, among the figure: 1-furnace wall, 2-sight glass, 3-sight glass support, 4-stay-warm case loam cake, 5-seed rod, 6-zirconium white stay-warm case, 7-iridium after-heater, 8-iridium crucible, 9-quartz barrel, 10-zirconium white insulation sand, 11-alumina tray, 12-tray supporter, 13-ruhmkorff coil, 14-furnace wall observation window, 15-melt, 16-seed crystal, 17-light, 18-human eye.Fill in zirconium white insulation sand 10 around the Iridium Crucible 8, after-heater 7 is put in the Iridium Crucible top, after-heater 7 outsides put zirconium white stay-warm case 6, cover zirconium white loam cake 4 again, the silver-plated plane mirror of adopting quartz glass is as sight glass 2 and regulate the position and sow and the crystal growth situation with the convenient seed crystal of observing in the angle of inclination.Seal burner hearth then and vacuumize (being better than 0.1Pa), after charge into high-purity N 2 gas, temperature increasing for melting materials; Wait to expect to become melt 15 after all fusings, the light that this melt 15 sends is received observation, constant temperature 2 hours by described furnace wall observation window 14 by human eye 18 after sight glass 2 reflections; Adopt the γ-LiAlO2 seed crystal of [100] direction, pull rate be the 1-3 millimeter/hour, 15-30 rev/min of crystal rotating speed.In crystal growing process, do not observe tangible volatilization flue gas, show that the component volatilization of melt has obtained good restraining, took out crystal after slowly lowering the temperature 40-60 hour, grown the transparent complete γ of Φ 52 * 130mm-LiAlO2 crystal.
We have also done corresponding experiment, adopt polishing copper sheet silvered mirror or other high temperature resistant material plane or little convex mirror to make sight glass 2, do not use stay-warm case loam cake 4, or the two sapphire discs of throwing of use, two throwing magnesium-aluminium spinel discs, two jackstone English discs, stay-warm case loam cakes 4 such as two throwing yttrium aluminum garnet discs, according to the opening shape that whether uses the stay-warm case loam cake or the stay-warm case loam cake that uses and aperture position and the position of corresponding adjusting sight glass, shape and angle of inclination are observed the seed crystal of lithium aluminate crystal and are sowed and the crystal growth situation, other processing condition are constant, grow transparent complete γ-LiAlO2 crystal equally.
Experiment shows, apparatus of the present invention can effectively be improved homogeneity, stability and the symmetry that tradition lifts the furnace temperature field, cut off the intensive gaseous exchange that stay-warm case causes because of the lateral observation window, effectively suppressed the volatilization of bath component in the lithium aluminate crystal process of growth, and need not original lifting furnace is done big change, avoid influencing the resistance to air loss of whole burner hearth.This device also is suitable for other non-volatile crystalline growth, improves its crystal mass, yield rate with the improvement by the temperature field, and has advantages such as with low cost, easy handling, has good practical value.
Claims (6)
1, a kind of device with growing lithium aluminate crystal by czochralski method, comprise a Czochralski grown single crystal growing furnace, it is characterized in that: the stay-warm case of this single crystal growing furnace (6) sidewall is complete, do not establish viewing window, on the furnace wall relative, set up a sight glass (2) in the top of described stay-warm case (6), so that the reflection by described sight glass realizes the observation to melt interface in the described iridium crucible by support with view port.
2, device with growing lithium aluminate crystal by czochralski method according to claim 1, it is characterized in that: this device comprises a Czochralski grown single crystal growing furnace, in the burner hearth that furnace wall (1) constitutes, tray supporter (12) is arranged, on this tray supporter (12) alumina tray (11), quartz barrel (9) and iridium crucible (8) are set on this alumina tray (11), round shape iridium after-heater (7) is housed on described iridium crucible (8), outside this iridium after-heater (7), round shape oxidation zirconium stay-warm case (6) is set, at described quartz barrel (9) and iridium crucible (8), fill zirconium white insulation sand (10) between the round shape oxidation zirconium stay-warm case (6), outside described quartz barrel (9) ruhmkorff coil (13), there is furnace wall observation window (14) described furnace wall (1), it is characterized in that: described round shape oxidation zirconium stay-warm case (6) sidewall is complete, do not establish viewing window, go up in the furnace wall (1) relative and to set up the top of a sight glass (2), so that the reflection realization by described sight glass (2) is to the observation of the interior melt interface of described iridium crucible (8) in round shape oxidation zirconium stay-warm case (6) by sight glass support (3) with described furnace wall observation window (14).
3, the device with growing lithium aluminate crystal by czochralski method according to claim 2, it is characterized in that: described round shape oxidation zirconium stay-warm case (6) also has stay-warm case loam cake (4).
4, the device with growing lithium aluminate crystal by czochralski method according to claim 3 is characterized in that: described stay-warm case loam cake (4) is the circular disc of the central openings made by transparent material.
5, the device with growing lithium aluminate crystal by czochralski method according to claim 4, it is characterized in that: described stay-warm case loam cake (4) is the magnesium-aluminium spinel disk of the sapphire disk of twin polishing, twin polishing, the quartzy disk of twin polishing or the yttrium aluminum garnet disk of twin polishing.
6, according to each described device of claim 2 to 5 with growing lithium aluminate crystal by czochralski method, it is characterized in that: described sight glass (2) is the silver-plated plane mirror of polishing copper sheet, the silver-plated plane mirror of silica glass, K9 glass silvering plane mirror, the silver-plated dimpling minute surface of polishing copper sheet, the silver-plated dimpling minute surface of silica glass, or K9 glass silvering dimpling minute surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102026068A CN101418468A (en) | 2008-11-12 | 2008-11-12 | Apparatus for growing lithium aluminate crystal by czochralski method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102026068A CN101418468A (en) | 2008-11-12 | 2008-11-12 | Apparatus for growing lithium aluminate crystal by czochralski method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101418468A true CN101418468A (en) | 2009-04-29 |
Family
ID=40629462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102026068A Pending CN101418468A (en) | 2008-11-12 | 2008-11-12 | Apparatus for growing lithium aluminate crystal by czochralski method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101418468A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103541008A (en) * | 2013-11-12 | 2014-01-29 | 上海硅酸盐研究所中试基地 | Growth method and growth device of large-size gallium oxide single crystal |
| CN105696068A (en) * | 2016-04-12 | 2016-06-22 | 盐城市振弘电子材料厂 | Lithium tantalate monocrystal growth apparatus |
| CN108486647A (en) * | 2018-05-24 | 2018-09-04 | 蔡凡 | Czochralski method CeAlO3Crystal growing apparatus and its control method |
| CN110284187A (en) * | 2018-03-19 | 2019-09-27 | 夕心科技（上海）有限公司 | Incude kyropoulos crystal growing apparatus and its control method |
| WO2021008159A1 (en) * | 2019-07-12 | 2021-01-21 | 中国电子科技集团公司第二十六研究所 | Coil-movable temperature field structure suitable for czochralski method, and single crystal growth method |
-
2008
- 2008-11-12 CN CNA2008102026068A patent/CN101418468A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103541008A (en) * | 2013-11-12 | 2014-01-29 | 上海硅酸盐研究所中试基地 | Growth method and growth device of large-size gallium oxide single crystal |
| CN103541008B (en) * | 2013-11-12 | 2016-01-06 | 上海硅酸盐研究所中试基地 | A kind of growth method of large size gallium oxide single crystal and growing apparatus |
| CN105696068A (en) * | 2016-04-12 | 2016-06-22 | 盐城市振弘电子材料厂 | Lithium tantalate monocrystal growth apparatus |
| CN110284187A (en) * | 2018-03-19 | 2019-09-27 | 夕心科技（上海）有限公司 | Incude kyropoulos crystal growing apparatus and its control method |
| CN108486647A (en) * | 2018-05-24 | 2018-09-04 | 蔡凡 | Czochralski method CeAlO3Crystal growing apparatus and its control method |
| WO2021008159A1 (en) * | 2019-07-12 | 2021-01-21 | 中国电子科技集团公司第二十六研究所 | Coil-movable temperature field structure suitable for czochralski method, and single crystal growth method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101580961A (en) | Method for growing crystal by reducing atmosphere Kyropoulos method | |
| CN101418468A (en) | Apparatus for growing lithium aluminate crystal by czochralski method | |
| CN102758249A (en) | Method for preparing colorless corundum monocrystal | |
| CN201321505Y (en) | Device for growing lithium aluminate crystal by Czochralski method | |
| CN104109904A (en) | Seeding method of sapphire crystal growth kyropoulos method | |
| CN108203844B (en) | Magnesium tantalate series crystal and its preparing process | |
| CN101348939B (en) | Growth method improving gallium arsenide single crystal utilization ratio | |
| JP2002293693A (en) | Terbium-aluminum-garnet single crystal and method of manufacturing for the same | |
| CN102534758A (en) | Growth method and growth device for bar-shaped sapphire crystals | |
| CN102560631A (en) | Growth method and equipment of sapphire crystal | |
| CN111575795A (en) | Preparation method of blue morusite | |
| CN103215646A (en) | Novel production method of c-orientation sapphire single crystal | |
| CN109868501A (en) | A kind of quartz boat and utilize the quartz boat for the method for primary completion gallium selenide polycrystal synthesis and crystal growth | |
| JP6053018B2 (en) | Crystal growth method | |
| TWI580827B (en) | Sapphire single crystal nucleus and its manufacturing method | |
| JP4844429B2 (en) | Method for producing sapphire single crystal | |
| CN100422393C (en) | Temperature gradient method rotary multiple crucible crystal growth system | |
| CN108221052B (en) | Preparation of large-size Zn4B6O13Method for single crystal | |
| Wood et al. | Growth stoichiometric magnesium aluminate spinel crystals by flux evaporation | |
| CN105586638A (en) | Preparation method of potassium and lead niobate piezoelectric monocrystal | |
| CN110685006A (en) | Intermediate infrared nonlinear optical crystal POC and preparation method thereof | |
| CN102691103B (en) | Method for growing sapphire crystals by double control technology | |
| CN1259461C (en) | Composite crucible used for growing high temperature oxide crystal | |
| CN107541779A (en) | A kind of growing method of colored spinelle jewel monocrystalline | |
| JP2013049607A (en) | Method of manufacturing sapphire single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090429 |