CN102965723B - A kind of method suppressing the radial too fast growth of bbo crystal - Google Patents
A kind of method suppressing the radial too fast growth of bbo crystal Download PDFInfo
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- CN102965723B CN102965723B CN201210516864.XA CN201210516864A CN102965723B CN 102965723 B CN102965723 B CN 102965723B CN 201210516864 A CN201210516864 A CN 201210516864A CN 102965723 B CN102965723 B CN 102965723B
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Abstract
A kind of method suppressing the radial too fast growth of bbo crystal, core content of the present invention adopts barium carbonate and boric acid to be main raw material, Sodium Fluoride or sodium oxide are fusing assistant, self-control fused salt pulling stove is growing apparatus, adopt the nested crucible of particular design, that in crucible, melt produces different temperature distribution, improve edge melt temperature thus the speed of growth of suppression bbo crystal radial direction, realize the isometrical pulling growth of bbo crystal, the present invention is adopted to carry out the fused salt pulling growth of bbo crystal, solve the radial too fast growth of the crystal existed in growth method in the past and easily encounter the problem that crucible wall twists off, it is simple that the method has structure, convenient and practical feature.
Description
Technical field
The present invention relates to fused salt pulling method field of crystal growth, particularly a kind of method suppressing the radial too fast growth of bbo crystal.
Technical background
Low-temperature phase barium metaborate β-BaB2O4 is a kind of very important new nonlinear crystals measured, there is wide transparency range, large effective Clock Multiplier Factor, large degree of birefringence and high laser damage threshold, be widely used in two of Nd:YAG and Nd:YLF laser, three, four, fifth harmonic, the frequency multiplication of dye laser, frequency tripling and mixing, Ti:Sappire and Alexandrite laser two, three, quadruple, optical parametric amplifier (OPA) and optical parametric oscillator (OPO), the frequency multiplication etc. of argon ion, ruby and Cu vapor laser.Yet there are no the better material of performance and replace it.
Molten-salt growth method (flux method) is a kind of growth method generally applied in artificial crystal growth.It adopts usually by the component fusing assistant of required growing crystal, obtains required crystal by slow cooling.Its feature is that suitability is wide, can find suitable fusing assistant for most crystal.Crystal pulling method is also the growing method of commonplace application, and it adopts after compound melts, and be directly upwards pulled from melt, obtain required crystal, its feature is fast growth.Fused salt pulling rule is a kind of flux growth method of improvement, and its process of growth is similar to flux method, adopts slow cooling, crystal is grown up, and makes crystal long thick in conjunction with lift simultaneously.
What barium metaborate β-BaB2O4 generally adopted is flux method growth, and the method growth cycle is long, has a big risk, and cost is high.Fused salt pulling method, in conjunction with the feature of crystal pulling method and molten-salt growth method, effectively shortens growth cycle, reduces the risk and cost.There is a problem in current employing fused salt pulling method for growing BBO crystal, bbo crystal radial growth speed is greater than longitudinal growth speed, after crystal growth for some time, easily touches crucible wall, occurs twisting off, and is unfavorable for later stage pulling growth.In order to control radial growth speed, we providing a kind of method suppressing the radial growth fast of bbo crystal, adopting special warm field and crucible design, can be good at the radial growth suppressing bbo crystal in fused salt pulling method.
Summary of the invention
The object of this invention is to provide the radial too fast growth of a kind of suppression bbo crystal, realize the method for the isometrical pulling growth of bbo crystal.
In order to suppress the radial too fast growth of bbo crystal, the temperature of crucible preglabellar field melt must be improved, make edge melt temperature a little more than crystal growth point temperature, the present invention realizes in the following way: a kind of fused salt pulling method suppressing the radial too fast growth of bbo crystal, barium carbonate and boric acid is adopted to be main raw material, Sodium Fluoride or sodium oxide are fusing assistant, self-control fused salt pulling stove is growing apparatus, described fused salt pulling stove adopts nested crucible design, crucible cover wall is had at Crucible body overcoat, Crucible body is connected by connecting wall with crucible cover wall, space is left between Crucible body and crucible cover wall, crucible cover wall upper limb is higher than Crucible body upper limb, Crucible body, crucible cover wall and connecting wall are integrated to be cast, described connecting wall can be cast different shapes and form different melt temperatures from the relative position of crucible cover wall distribute to adjust Crucible body.
During crystal growth, heater coil carries out heating to Crucible body makes melt be warming up to crystal growth point, but near the melt edge of boiler port closer to crucible cover wall, and sidewall of crucible cover closer to the temperature at heater coil therefore melt edge higher than the temperature at melt center, so melt lip temperature is higher than vegetative point temperature, thus inhibit the radial growth of bbo crystal, connecting wall simultaneously by processing different radian and shape realizes regulating the relative position of main body and outer wall cover thus regulating the relative temperature of edge melt and central melt to distribute, thus better can control the radial growth speed of bbo crystal, realize isodiametric growth.
Advantage of the present invention is that structure is simple, adopts the nested crucible of particular design, improves near crucible edge melt temperature, inhibits the radial too fast growth of bbo crystal.
Accompanying drawing explanation
Fig. 1 is a kind of nested crucible structure schematic diagram suppressing the radial too fast growth method of bbo crystal of the present invention
Wherein 11 is Crucible body, and 12 is crucible cover wall, and 13 is connecting wall
Fig. 2 is a kind of crystal growth schematic diagram suppressing the radial too fast growth method of bbo crystal of the present invention
Wherein 21 is nested crucible, and 22 is melt, and 23 is crystal growing furnace, and 24 is crystal, and 25 is heater coil, and 26 is seed rod
Fig. 3 is a kind of temperature subregion schematic diagram suppressing the radial too fast growth method of bbo crystal of the present invention
Wherein 31 is melt central section, 32 melt marginariums, and 33 is crystal growth district
Embodiment
Embodiment one: take a certain amount of barium carbonate, boric acid and Sodium Fluoride, meets BaB2O4:NaF=2:1(mol ratio) mix in Raw material pail.Mixed material is melted to reacting completely in the silicon carbide rod furnace of 1000 DEG C.The nested crucible of the platinum material melted being poured into particular design is placed in fused salt pulling stove, is warming up to 980 DEG C, constant temperature 18h, then more than temperature of saturation at 10 DEG C.By the seed crystal that is fixed in advance on seed rod slowly down to molten surface, 4 ~ 10r/min rotates, 7 DEG C are fallen after half an hour, crystal growth began, later 1 ~ 2 DEG C DEG C/day lowers the temperature, and 0.5 ~ 1.0mm/day lifts, grow 2 months, mention crystal, be annealed to room temperature with 50 DEG C/h, obtain the crystal boule of isodiametric growth.
Embodiment two: take a certain amount of barium carbonate, boric acid and Sodium Fluoride, meets BaB2O4:NaO=3.5:1(mol ratio) mix in Raw material pail.Mixed material is melted to reacting completely in the silicon carbide rod furnace of 1000 DEG C.The nested crucible of the platinum material melted being poured into particular design is placed in fused salt pulling stove, is warming up to 980 DEG C, constant temperature 18h, then more than temperature of saturation at 10 DEG C.By the seed crystal that is fixed in advance on seed rod slowly down to molten surface, 4 ~ 10r/min rotates, 8 DEG C are fallen after half an hour, crystal growth began, later 1 ~ 2 DEG C DEG C/day lowers the temperature, and 0.5 ~ 1.0mm/day lifts, grow 2 months, mention crystal, be annealed to room temperature with 50 DEG C/h, obtain the crystal boule of isodiametric growth.
Claims (2)
1. one kind is suppressed the method for the radial too fast growth of bbo crystal, barium carbonate and boric acid is adopted to be main raw material, Sodium Fluoride is fusing assistant, self-control fused salt pulling stove is that growing apparatus carries out fused salt pulling method for growing, it is characterized in that: adopt nested crucible design, crucible cover wall is had at Crucible body overcoat, Crucible body is connected by connecting wall with crucible cover wall, certain space is left between Crucible body and crucible cover wall, Crucible body, crucible cover wall and connecting wall are integrated to be cast, and connecting arm makes near the melt edge of boiler port closer to crucible cover wall.
2. a kind of method suppressing the radial too fast growth of bbo crystal as claimed in claim 1, is characterized in that: described connecting wall can be cast as different shapes and form different melt temperatures to adjust Crucible body and the relative position of crucible cover wall and distribute.
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| CN201210516864.XA CN102965723B (en) | 2012-12-06 | 2012-12-06 | A kind of method suppressing the radial too fast growth of bbo crystal |
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| CN201210516864.XA CN102965723B (en) | 2012-12-06 | 2012-12-06 | A kind of method suppressing the radial too fast growth of bbo crystal |
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| CN102965723A CN102965723A (en) | 2013-03-13 |
| CN102965723B true CN102965723B (en) | 2016-03-09 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112626A (en) * | 2018-10-25 | 2019-01-01 | 莱芜职业技术学院 | Non-linear optical crystal material β-BaB2O4Growing 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 |
| CN115233286A (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 oxide as fluxing agent |
| 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 |
| CN115652407A (en) * | 2022-11-16 | 2023-01-31 | 福建福晶科技股份有限公司 | Preparation method of BIBO crystal with high utilization rate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1118023A (en) * | 1994-08-30 | 1996-03-06 | 中国科学院上海硅酸盐研究所 | Method for pulling growth of beta-barium metaborate from solvent constant level |
| 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 |
| CN101760785A (en) * | 2010-02-08 | 2010-06-30 | 中国科学院理化技术研究所 | Device for adjusting radial temperature gradient in crucible in crystal growth furnace |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01241529A (en) * | 1988-03-24 | 1989-09-26 | Toshiba Corp | Nonlinear optical crystal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1118023A (en) * | 1994-08-30 | 1996-03-06 | 中国科学院上海硅酸盐研究所 | Method for pulling growth of beta-barium metaborate from solvent constant level |
| 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 |
| CN101760785A (en) * | 2010-02-08 | 2010-06-30 | 中国科学院理化技术研究所 | Device for adjusting radial temperature gradient in crucible in crystal growth furnace |
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