CN101748475A - Special processing method for growing large-size high-quality LBO crystals - Google Patents
Special processing method for growing large-size high-quality LBO crystals Download PDFInfo
- Publication number
- CN101748475A CN101748475A CN200810072362A CN200810072362A CN101748475A CN 101748475 A CN101748475 A CN 101748475A CN 200810072362 A CN200810072362 A CN 200810072362A CN 200810072362 A CN200810072362 A CN 200810072362A CN 101748475 A CN101748475 A CN 101748475A
- Authority
- CN
- China
- Prior art keywords
- crystal
- solution
- growing
- lbo
- size high
- 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
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a novel processing technique for growing LBO (LiB3O5, lithium triborate) crystals, in particular to a technique for growing large-size high-quality LBO monocrystals. In order to overcome the problem that the transfer of solutes are difficult in the growing process of a LBO crystal, the invention provides a special forced solution convection technique and improves solution components, thus effectively solving the problem of the difficult transfer of solutes. The invention adds stirring blades (6) in the crystal-growing solution, and as shown in the figure, the stirring blades (6) rotate along with the crystal to drive the whole solution to flow, thus accelerating the transfer of solutes. Besides adding B2O3 as solvent in the solution, the invention also adds a great deal of LiF as cosolvent. Since F- has a bond-breaking effect, F- can effectively destroy the boron-oxygen network structure, consequently, the viscosity of the solution is greatly reduced, impurities can be quickly and effectively discharged in the growing process of the crystal, and the formation of flaw is greatly reduced.
Description
Affiliated technical field
The present invention relates to a kind of growing LBO (LiB
3O
5, three lithium tetraborates) and the crystalline novel technique.Especially technology that can growth of large size high quality LBO monocrystalline.
Background technology
Lbo crystal is the very outstanding non-linear optic crystal of a kind of optical property of Fujian Inst. of Matter Structure, Chinese Academy of Sciences's invention.It has wide scope, high optical homogeneity, relatively large effective two Clock Multiplier Factors and the high laser damage threshold of seeing through.It has important aspect photoelectron technology and uses widely, is widely used in laser frequency and transforms fields such as optical parametric oscillator and optical parameter amplification.
The development of laser technology is now all had higher requirement to lbo crystal size of devices and quality, some device size requires to reach 40 * 30 * 40mm, absorbed inside value (1064nm place) is less than below the 100ppm, and this has proposed very big challenge to lbo crystal growth technique technology.Traditional lbo crystal growth technique relies on the rotation of crystal itself to reach stirred solution more, promote the purpose of solution convection current, under the limited condition of this solution convection current, crystal transports slowly owing to solute in process of growth, solvent and impurity fail in time to discharge, very easily produce a large amount of fine parcels, thereby greatly influenced final size and the quality of crystal.In addition, the traditional solvent of growing LBO crystal is B
2O
3, at high temperature form boron oxygen network structure easily, caused the high viscosity of solution, influence transporting of solute, thereby caused the formation of various defectives.
Summary of the invention
In order to overcome the difficult problem that transports of lbo crystal solute in process of growth, the invention provides a kind of special solution forced convection technology, and improve the solvent composition, solve solute effectively and transported difficult problem.The technical solution used in the present invention is:
The present invention increases by 6 agitating vanes in the solution of crystal growth, as Fig. 1 or shown in Figure 2,6 agitating vanes rotate and rotate along with crystalline, drive flowing of whole solution, thereby accelerate transporting of solute.
The present invention removes in solution and adds B
2O
3Outside flux, also add a large amount of LiF as fusing assistant.Because F
-Have the scission of link effect, it can destroy boron oxygen network structure effectively, has greatly reduced the viscosity of solution, allows crystal can carry out impurities removal rapidly and effectively in process of growth, has greatly reduced the formation of defective.Concrete growth parameter(s) is: B
2O
3With LiF as fusing assistant, cooling rate is 0.5-1 ℃/day; Crystal rotating speed and blade rotational speed are 4.5-9 rev/min.
Description of drawings
Fig. 1 increases agitating vane in the solution bottom of crystal growth.1.LBO crystal wherein; 2. platinum crucible; 3. solution; 4. platinum seed rod; 5. paddle horse; 6. agitating vane.
Fig. 2 increases agitating vane at the solution top of crystal growth.1.LBO crystal wherein; 2. platinum crucible; 3. solution; 4. platinum seed rod; 5. paddle horse; 6. agitating vane.
Embodiment
Weighing Li
2CO
3347.19g, LiF69.93g, H
3BO
33240g (53.35%B
2O
3And LiF),, and repeatedly join in the platinum crucible of Φ a 120 * 110mm after the fusion, be warming up to 900 ℃ through thorough mixing, constant temperature 24 hours, and slowly be cooled to 820 ℃, introduce the seed crystal of 3 * 3 * 8mm and grow.Start Crystal Rotation, velocity of rotation is 9 rev/mins.First all constant temperature growths begin later on 1 ℃ of/day cooling, through about growth more than 2 months, obtain the monocrystalline of 70 * 70 * 68mm.The device that cuts out, measuring its absorption value at the 1064nm place is 30ppm.
Claims (4)
1. the special process method of a growth of large size high quality lbo crystal is characterized in that in crystal growing process, adds agitating vane in solution, uses B
2O
3Make fusing assistant with LiF.
2. the special process method of a kind of growth of large size high quality lbo crystal as claimed in claim 1 is characterized in that crystal and agitating vane rotating speed are 4.5-9 rev/min.
3. the special process method of a kind of growth of large size high quality lbo crystal as claimed in claim 1 is characterized in that using B
2O
3Making the fusing assistant add-on with LiF is 40-60mol%.
4. the special process method of a growth of large size high quality lbo crystal is characterized in that in crystal growing process, and crystal and agitating vane rotating speed are 4.5-9 rev/min; Cooling rate is 0.5-1 ℃/day.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810072362A CN101748475A (en) | 2008-12-15 | 2008-12-15 | Special processing method for growing large-size high-quality LBO crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810072362A CN101748475A (en) | 2008-12-15 | 2008-12-15 | Special processing method for growing large-size high-quality LBO crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101748475A true CN101748475A (en) | 2010-06-23 |
Family
ID=42476072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810072362A Pending CN101748475A (en) | 2008-12-15 | 2008-12-15 | Special processing method for growing large-size high-quality LBO crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101748475A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102839422A (en) * | 2012-09-28 | 2012-12-26 | 中国科学院新疆理化技术研究所 | Preparation method for large-size dihydroxy lithium pentaborate crystal |
| CN103114327A (en) * | 2012-12-24 | 2013-05-22 | 福建福晶科技股份有限公司 | Molten-salt growth method for eliminating core package of low-temperature phase barium metaborate crystalloid |
| CN103820856A (en) * | 2014-01-24 | 2014-05-28 | 中国科学院理化技术研究所 | Method for synthesizing LBO (Lithium Triborate) crystal growing raw material and method for preparing LBO crystal |
| CN105624781A (en) * | 2016-01-14 | 2016-06-01 | 福建福晶科技股份有限公司 | Lithium tetraborate crystal preparation method and growth device |
| CN106012007A (en) * | 2016-07-22 | 2016-10-12 | 常州天合光能有限公司 | Method and device for growing crystalline silicone by aid of forced convection |
| CN108774748A (en) * | 2018-07-06 | 2018-11-09 | 福建福晶科技股份有限公司 | A kind of special process method of growth of large size high quality lbo crystal |
| CN110042463A (en) * | 2019-05-27 | 2019-07-23 | 福建福晶科技股份有限公司 | A kind of growing method that bbo crystal thickens |
| CN111020688A (en) * | 2019-11-08 | 2020-04-17 | 中国科学院福建物质结构研究所 | Method for preparing lanthanum fluoride single crystal and rare earth ion doped lanthanum fluoride single crystal by molten salt growth method |
-
2008
- 2008-12-15 CN CN200810072362A patent/CN101748475A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102839422A (en) * | 2012-09-28 | 2012-12-26 | 中国科学院新疆理化技术研究所 | Preparation method for large-size dihydroxy lithium pentaborate crystal |
| CN102839422B (en) * | 2012-09-28 | 2015-04-22 | 中国科学院新疆理化技术研究所 | Preparation method for large-size dihydroxy lithium pentaborate crystal |
| CN103114327A (en) * | 2012-12-24 | 2013-05-22 | 福建福晶科技股份有限公司 | Molten-salt growth method for eliminating core package of low-temperature phase barium metaborate crystalloid |
| CN103114327B (en) * | 2012-12-24 | 2016-06-08 | 福建福晶科技股份有限公司 | A kind of molten-salt growth method eliminating low-temperature phase defection barium borate crystal core parcel |
| CN103820856A (en) * | 2014-01-24 | 2014-05-28 | 中国科学院理化技术研究所 | Method for synthesizing LBO (Lithium Triborate) crystal growing raw material and method for preparing LBO crystal |
| CN103820856B (en) * | 2014-01-24 | 2016-08-17 | 中国科学院理化技术研究所 | The synthetic method of lbo crystal growth raw material and the method preparing lbo crystal |
| CN105624781A (en) * | 2016-01-14 | 2016-06-01 | 福建福晶科技股份有限公司 | Lithium tetraborate crystal preparation method and growth device |
| CN106012007A (en) * | 2016-07-22 | 2016-10-12 | 常州天合光能有限公司 | Method and device for growing crystalline silicone by aid of forced convection |
| CN106012007B (en) * | 2016-07-22 | 2018-03-13 | 天合光能股份有限公司 | A kind of method and its device of forced convertion growth crystalline silicon |
| CN108774748A (en) * | 2018-07-06 | 2018-11-09 | 福建福晶科技股份有限公司 | A kind of special process method of growth of large size high quality lbo crystal |
| CN110042463A (en) * | 2019-05-27 | 2019-07-23 | 福建福晶科技股份有限公司 | A kind of growing method that bbo crystal thickens |
| CN111020688A (en) * | 2019-11-08 | 2020-04-17 | 中国科学院福建物质结构研究所 | Method for preparing lanthanum fluoride single crystal and rare earth ion doped lanthanum fluoride single crystal by molten salt growth method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101748475A (en) | Special processing method for growing large-size high-quality LBO crystals | |
| CN101748476B (en) | Special processing method for growing large-size high-quality BBO crystals | |
| CN102976287B (en) | BaGa2GeSe6 compound, BaGa2GeSe6 non-linear optical crystal and their preparation methods and use | |
| EP3620555A1 (en) | Compound cesium fluoroborate, non-linear optical crystal of cesium fluoroborate, preparation method therefor and use thereof | |
| CN108588833B (en) | Compound fluoboric acid calcium and fluoroboric acid calcium non-linear optical crystal and preparation method and purposes | |
| CN102838093B (en) | LiGaGe2Se6 compound, LiGaGe2Se6 nonlinear optical crystals, and preparation method and application thereof | |
| CN106948003B (en) | Compound potassium fluoborate and potassium fluoborate nonlinear optical crystal and preparation method and purposes | |
| CN111334858B (en) | Compound barium fluoborate, barium fluoborate nonlinear optical crystal, preparation method and application | |
| CN101435109B (en) | Growth method for fluxing medium of boron phosphate single crystal | |
| CN103288058B (en) | Li2In2GeSe6 compound and Li2In2GeSe6 nonlinear optical crystal as well as preparation methods and applications thereof | |
| CN103225108B (en) | A kind of method of rapid growth of large-size BBO crystal | |
| Nikolov et al. | Growth and morphology of large LiB3O5 single crystals | |
| CN106835262B (en) | A method of growth aluminium tetraborate salt crystal | |
| Nishioka et al. | Growth of CsLiB6O10 crystals with high laser-damage tolerance | |
| CN1254568C (en) | Growth of LiB3O5 nonlinear optical crystal by integrating rotary crucible and molten salt Czochralski growth method | |
| CN105350082B (en) | A kind of Na2In2GeSe6Nonlinear optical crystal and preparation method and purposes | |
| CN114262932A (en) | Cesium lithium borate crystal fluxing agent and crystal growth method | |
| CN104371560A (en) | Aluminum-base high-temperature adhesive for AlN seed crystal bonding and preparation method thereof | |
| CN1254566C (en) | Fused salt pulling method for growing LBO crystal | |
| CN101787558B (en) | Fluxing agent growing method of K2Al2B2O7 crystal | |
| CN103114327B (en) | A kind of molten-salt growth method eliminating low-temperature phase defection barium borate crystal core parcel | |
| CN101363131B (en) | Top seed solution growth reentrance technology in fluxing agent growth method | |
| CN108774748A (en) | A kind of special process method of growth of large size high quality lbo crystal | |
| CN109056064A (en) | A kind of Rb2Ba(PO3)5The fluxing agent of crystal growth and the growing method for utilizing the fluxing agent | |
| CN213266784U (en) | Seed crystal rod capable of reducing intermediate envelope of BBO 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 |
Application publication date: 20100623 |