CN103225108A - Method for rapid growth of large-size BBO crystal - Google Patents
Method for rapid growth of large-size BBO crystal Download PDFInfo
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- CN103225108A CN103225108A CN2013101151790A CN201310115179A CN103225108A CN 103225108 A CN103225108 A CN 103225108A CN 2013101151790 A CN2013101151790 A CN 2013101151790A CN 201310115179 A CN201310115179 A CN 201310115179A CN 103225108 A CN103225108 A CN 103225108A
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Abstract
The invention provides a method for rapid growth of large-size BBO crystal. The method uses barium carbonate and boric acid as main raw materials, sodium fluoride or sodium oxide as a flux, and a double-layer crucible and a molten salt furnace as growth devices, wherein the double-layer crucible is obtained by adding a bottomless inner crucible into an outer crucible. Melt in the outer crucible is stirred and aerated so as to drive the melt in the inner crucible to flow, thereby improving a growth speed of the crystal and a concentration gradient of solute, shortening the growth period of the crystal, and obtaining the large-size crystal blank. The crystal growth method can effectively solves disadvantages that in traditional growth method, the crystal is grown by temperature, and the melt mainly depends on natural convection during the progress, and thus a crystal growth rate is low, a growth period is long, a risk is large and a cost is high.
Description
Technical field
The present invention designs field of crystal growth, and particularly a kind of large size bbo crystal is the method for growth fast.
Background technology
Low-temperature phase barium metaborate (β-BaB2O4) in non-linear optic crystal, be that a kind of comprehensive advantage is obvious, well behaved crystal, it has extremely wide transparency range, the bigger angle that is complementary, higher optic damage threshold value, the temperature coupling and the good optical homogeneity in broadband, extensively apply to two of Nd:YAG and Nd:YLF laser, three, four, five frequencys multiplication, the frequency multiplication of dye laser, frequency tripling and mixing, two of Ti:Sappire and Alexandrite laser, three, quadruple, optical parameter amplifier (OPA) and optical parametric oscillator (OPO), argon ion, the frequencys multiplication of ruby and Cu vapor laser etc. have a wide range of applications especially for the frequency tripling of Nd:YAG laser apparatus.Yet there are no the over-all properties better material and replace it.
This crystal mainly adopts the top-seeded solution growth growth, utilizes Sodium Fluoride or sodium oxide to be fusing assistant, adopts slow cooling method growth, and growth cycle reaches 7～8 months.Because crystal growth later stage crystal grows to crucible wall, the brilliant commentaries on classics stops simultaneously, and crystal is by the cooling growth, and melt is mainly natural convection in the process.It is low that this method growing crystal has growth velocity, and growth cycle is long, has a big risk characteristics such as cost height.Because melt flow is limited, be difficult to the very thick crystal of growth thickness simultaneously, can't process and obtain large-size device.The present invention adopts the double crucible design, improves crystal growth rate and the solute concentration gradient in the frictional belt, thereby shortens the crystal growth cycle, increases crystal thickness, obtains large-size crystals.
Summary of the invention
The purpose of this invention is to provide a kind of large size bbo crystal method of growth fast, the realization bbo crystal is grown fast, reduces growth cycle, obtains the large size bbo crystal simultaneously.
The present invention realizes in the following way: a kind of large size bbo crystal is the method for growth fast, adopting barium carbonate and boric acid is main raw material, Sodium Fluoride or sodium oxide are fusing assistant, crucible and molten salt furnace are growing apparatus, and described crucible is at the outer crucible the inside interior crucible at a no end of addition, by the outer pot melt is stirred or ventilation, the pot melt flows in driving, thereby improve crystalline growth velocity and solute concentration gradient, shorten the crystal growth cycle, obtain the large-size crystals blank.
Characteristics of the present invention: adopt double-deck crucible design, on the one hand, utilize the outer crucible melt to stir and drive flowing of interior crucible melt, improve crystal growth rate and solute concentration gradient; By double-deck crucible design, increase melt volume simultaneously, help growth and obtain large-size crystals.
Description of drawings
Fig. 1 is the structural representation of crucible of the present invention, and wherein 1 is that interior crucible, 2 is that outer crucible, 3 is that crystal, 4 is seed rod.
Embodiment
Embodiment one: take by weighing a certain amount of barium carbonate, boric acid and Sodium Fluoride, satisfy the BaB2O4:NaF=2:1(mol ratio) mixing in Raw material pail.Mixed material is fused to reacting completely in 1000 ℃ silicon carbide rod furnace.Molten good material is poured in the crucible, placed molten salt furnace, be warming up to 980 ℃, constant temperature 18h is then under more than the temperature of saturation 10 ℃.To be fixed on seed crystal on the seed rod in advance slowly down to molten surface, 4～10r/min rotates, and falls 7 ℃ after half an hour, crystal begins growth, later 1～2 ℃/day cooling when crystal growth during to crucible wall, stops brilliant the commentaries on classics, opening the outer pot stirring rake rotates, rotating speed 10～30r/min, crystal begin 2～5 ℃ of coolings, grow 4～5 months, stop cooling, crystal is come out of the stove.
Embodiment two: take by weighing a certain amount of barium carbonate, boric acid and sodium oxide, satisfy the BaB2O4:NaO=3.5:1(mol ratio) mixing in Raw material pail.Mixed material is fused to reacting completely in 1000 ℃ silicon carbide rod furnace.Molten good material is poured in the crucible, placed molten salt furnace, be warming up to 980 ℃, constant temperature 18h is then under more than the temperature of saturation 10 ℃.To be fixed on seed crystal on the seed rod in advance slowly down to molten surface, 4～10r/min rotates, and falls 7 ℃ after half an hour, crystal begins growth, later 1～2 ℃/day cooling when crystal growth during to crucible wall, stops brilliant the commentaries on classics, opening the outer pot stirring rake rotates, rotating speed 10～30r/min, crystal begin 2～5 ℃ of coolings, grow 4～5 months, stop cooling, crystal is come out of the stove.
Claims (2)
1. the large size bbo crystal method of growth fast, adopting barium carbonate and boric acid is main raw material, Sodium Fluoride or sodium oxide are fusing assistant, and crucible and molten salt furnace are growing apparatus, it is characterized in that: described crucible is the interior crucible at a no end of addition inside outer crucible.
2. a kind of large size bbo crystal according to claim 1 is the method for growth fast, it is characterized in that: the mobile of the interior crucible melt of drive stirs between described outer crucible and the interior crucible or ventilates.
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| CN201310115179.0A CN103225108B (en) | 2013-04-07 | 2013-04-07 | A kind of method of rapid growth of large-size BBO crystal |
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| CN201310115179.0A CN103225108B (en) | 2013-04-07 | 2013-04-07 | A kind of method of rapid growth of large-size BBO crystal |
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| CN103225108A true CN103225108A (en) | 2013-07-31 |
| CN103225108B CN103225108B (en) | 2016-04-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475772A (en) * | 2017-08-30 | 2017-12-15 | 福建福晶科技股份有限公司 | A kind of bbo crystal method for fast growing |
| CN110616455A (en) * | 2018-06-20 | 2019-12-27 | 福州高意光学有限公司 | Crystal pulling and growing device |
| CN112176395A (en) * | 2020-10-13 | 2021-01-05 | 福建福晶科技股份有限公司 | Device and method for growing high-quality large-size BiBO crystal by molten salt growth method |
| CN115233287A (en) * | 2022-08-11 | 2022-10-25 | 山东重山光电材料股份有限公司 | beta-BBO crystal growth method using cesium fluoride as fluxing agent |
| CN115467010A (en) * | 2022-09-26 | 2022-12-13 | 福建福晶科技股份有限公司 | Low-temperature phase BBO crystal growth device and growth method |
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| CN1057868A (en) * | 1990-07-06 | 1992-01-15 | 中国科学院上海硅酸盐研究所 | Barium metaborate (the constant level Czochralski grown of monocrystalline of β-BBO) |
| CN1086552A (en) * | 1992-11-04 | 1994-05-11 | 中国科学院福建物质结构研究所 | Improved growing low temperature phase-deviation barium borate monocrystal by smelting salt crystal method |
| JPH085741B2 (en) * | 1989-04-19 | 1996-01-24 | 日本電気株式会社 | Single crystal growth method |
| CN1160779A (en) * | 1996-01-12 | 1997-10-01 | 三菱麻铁里亚尔硅材料株式会社 | Single crystal fulling apparatus |
| CN1443879A (en) * | 2002-03-08 | 2003-09-24 | 中国科学院福建物质结构研究所 | Fused salt pulling method for growing BBO crystal |
| CN101748476A (en) * | 2008-12-15 | 2010-06-23 | 福建福晶科技股份有限公司 | Special processing method for growing large-size high-quality BBO crystals |
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2013
- 2013-04-07 CN CN201310115179.0A patent/CN103225108B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1045282A (en) * | 1985-04-01 | 1990-09-12 | 中国科学院福建物质结构研究所 | Growing low temperature phase-deviation barium borate monocrystal by smelting salt crystal method |
| JPH085741B2 (en) * | 1989-04-19 | 1996-01-24 | 日本電気株式会社 | Single crystal growth method |
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| CN101748476A (en) * | 2008-12-15 | 2010-06-23 | 福建福晶科技股份有限公司 | Special processing method for growing large-size high-quality BBO crystals |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475772A (en) * | 2017-08-30 | 2017-12-15 | 福建福晶科技股份有限公司 | A kind of bbo crystal method for fast growing |
| CN110616455A (en) * | 2018-06-20 | 2019-12-27 | 福州高意光学有限公司 | Crystal pulling and growing device |
| CN112176395A (en) * | 2020-10-13 | 2021-01-05 | 福建福晶科技股份有限公司 | Device and method for growing high-quality large-size BiBO crystal by molten salt growth method |
| CN115233287A (en) * | 2022-08-11 | 2022-10-25 | 山东重山光电材料股份有限公司 | beta-BBO crystal growth method using cesium fluoride as fluxing agent |
| CN115467010A (en) * | 2022-09-26 | 2022-12-13 | 福建福晶科技股份有限公司 | Low-temperature phase BBO crystal growth device and growth method |
| CN115467010B (en) * | 2022-09-26 | 2023-11-14 | 福建福晶科技股份有限公司 | Low-temperature phase BBO crystal growth device and growth method |
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| CN103225108B (en) | 2016-04-06 |
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