CN107475772A - A kind of bbo crystal method for fast growing - Google Patents
A kind of bbo crystal method for fast growing Download PDFInfo
- Publication number
- CN107475772A CN107475772A CN201710761767.XA CN201710761767A CN107475772A CN 107475772 A CN107475772 A CN 107475772A CN 201710761767 A CN201710761767 A CN 201710761767A CN 107475772 A CN107475772 A CN 107475772A
- Authority
- CN
- China
- Prior art keywords
- crucible
- crystal
- seed
- seed rod
- bbo
- 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
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
Abstract
The invention discloses a kind of bbo crystal method for fast growing, using crucible rise method, utilized thermograde that cold-zone is big and crucible rotation to strengthen the convection current of melt, and improved rate of crystalline growth.
Description
Technical field
The present invention relates to a kind of artificial crystal growth field, more particularly to a kind of bbo crystal method for fast growing.
Background technology
Low-temperature phase barium metaborate β-BaB2O4 are a kind of very important new nonlinear crystals measureds, have wide printing opacity model
Enclose, big effective Clock Multiplier Factor, big birefringence and high laser damage threshold, be widely used in laser freuqency doubling, at present also
It there are no the more preferable material of performance and substitute it.
The crystal is grown using top-seeded solution growth at present, and crystal growing process uses slow cooling, fluid free convection life
Long, rate of crystalline growth is slow, the problems such as middle percardium.
The content of the invention
The present invention seeks to use crucible rise method, rotated using crucible and strengthen flow of fluid, utilized cooling layer increase temperature
Gradient is spent, realizes rapid growth of crystal.
In order to realize the above object the present invention is as follows using technical scheme：
Using barium carbonate, sodium fluoride, boric acid is raw material.
The growth apparatus of use includes burner hearth, peep hole, rotatable crucible tray, motor.Burner hearth is by three different temperature
District's groups are into temperature raises from top to down, and middle area thermograde is 5 ~ 15 DEG C.Seed rod, which is ined succession, can rise, declines and rotate
Motor, crucible tray in succession can raising and lowering motor.
Crystal growth step is as follows：
1）Pretreatment of raw material：BBO raw materials are fitted into U-shaped crucible by melt stove penetration, crucible is placed in lower heating zone, crucible
Mouth is in lower heating zone and middle area boundary, is warming up to 1100 DEG C, raw material reaches molten condition；
2）Crystal growth：Melt temperature is down to more than saturation temperature seed crystal at 2 DEG C, the seed rod for being fixed with BBO seed crystals is delayed
Slowly sink down into melt liquid level, with 5 revs/min of speed rotary seed crystal rod, crucible does not rotate, when crystal growth soon to sidewall of crucible when,
Crucible starts, with 30 revs/min of rotations, then to adjust seed rod rotating speed, keep crucible seed rod same rotational speed to turn to rotation, simultaneously
Crucible and seed rod start with 0.05 ~ 1mm/h of phase same rate toward rise, by centre cross cold-zone, crystal along sidewall of crucible down
Growth, utilized thermograde that cold-zone is big and crucible rotation to strengthen the convection current of melt, and improved rate of crystalline growth.When crucible liter
When entering upper heating zone and middle area border to crucible bottom, crucible and seed rod stop operating and risen, then by 10 ~ 30 DEG C
Speed be cooled to room temperature, cut off crucible, take out crystal.
Brief description of the drawings
Fig. 1 is crystal growth equipment schematic diagram of the present invention：In figure, 1, seed rod motor, 2, peep hole, 3, seed rod, 4,
Upper heating zone, 5, seed crystal, 6, middle area, 7, crucible, 8, lower heating zone, 9, crucible tray, 10, motor.
Embodiment
The present invention will be further described below in conjunction with the accompanying drawings：
Embodiment one：
In embodiments of the invention, for preparing the growth apparatus of bbo crystal as shown in figure 1, including the bell with peep hole, electricity
Machine, seed rod, burner hearth, crucible composition.Wherein burner hearth is made up of three humidity provinces, respectively upper heating zone, middle area and lower heating
Area.It is made up of around middle area the oxidation aluminium heat insulation material of 20mm thickness, the minimum temperature difference of highest is 10 DEG C, on upper heating zone bell
There are two and the centrosymmetric peep hole of boiler tube in face, and peep hole is covered with quartz plate.
Based on the growth apparatus in above-described embodiment, method that embodiment of the invention prepares bbo crystal, including it is following
Step：
1）Pretreatment of raw material：By BBO oxide spinel barium, boric acid, sodium fluoride mixes using material stove penetration in proportion, loads U-shaped
In crucible, crucible is placed in lower heating zone, mouth of pot is in lower heating zone and middle area boundary, is warming up to 1100 DEG C, raw material
Reach molten condition；
2）Crystal growth：Melt temperature is down to seed crystal at 1000 DEG C, the seed rod for being fixed with BBO seed crystals slowly sunk down into molten
Body fluid face, with 5 revs/min of speed rotary seed crystal rod, crucible does not rotate, when crystal growth soon to sidewall of crucible when, crucible start with
30 revs/min of rotations, then adjust seed rod rotating speed, keep crucible seed rod same rotational speed to turn to rotation, while crucible and seed crystal
Bar starts to rise so that phase same rate 0.05mm/h is past, when crucible bottom enters upper heating zone and middle area border, crucible and seed
Crystalline style stops rising, and is then cooled to room temperature by 10 ~ 30 DEG C of speed, cuts off crucible, takes out crystal.
Claims (1)
1. a kind of bbo crystal method for fast growing, using barium carbonate, sodium fluoride, boric acid is raw material；The growth apparatus of use includes
Burner hearth, peep hole, rotatable crucible tray, motor, burner hearth are made up of three different humidity provinces, and temperature raises from top to down, in
Between area's thermograde be 5 ~ 15 DEG C；The motor that seed rod, which is ined succession, can rise, declines and rotate, crucible tray is ined succession can raising and lowering
Motor；Crystal growth step is as follows：1）Pretreatment of raw material：BBO raw materials are fitted into U-shaped crucible by melt stove penetration, will
Crucible is placed in lower heating zone, and mouth of pot is in lower heating zone and middle area boundary, is warming up to 1100 DEG C, raw material reaches molten
State；2）Crystal growth：Melt temperature is down to more than saturation temperature seed crystal at 2 DEG C, the seed rod for being fixed with BBO seed crystals is slow
Sink down into melt liquid level, with 5 revs/min of speed rotary seed crystal rod, crucible does not rotate, when crystal growth soon to sidewall of crucible when, earthenware
Crucible starts, with 30 revs/min of rotations, then to adjust seed rod rotating speed, keeps crucible seed rod same rotational speed to turn to rotation, while earthenware
Crucible and seed rod start with 0.05 ~ 1mm/h of phase same rate toward rising, and cross cold-zone by centre, crystal is down given birth to along sidewall of crucible
Long, when crucible, which rises to crucible bottom, enters upper heating zone and middle area border, crucible and seed rod stop operating and risen, so
Room temperature is cooled to by 10 ~ 30 DEG C of speed afterwards, cuts off crucible, takes out crystal, it is characterised in that after crystal growth to sidewall of crucible,
Crucible and seed rod same rotational speed, identical steering rotation, while crucible and seed rod start past with 0.05 ~ 1mm/h of phase same rate
Rise, cold-zone is crossed by centre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710761767.XA CN107475772A (en) | 2017-08-30 | 2017-08-30 | A kind of bbo crystal method for fast growing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710761767.XA CN107475772A (en) | 2017-08-30 | 2017-08-30 | A kind of bbo crystal method for fast growing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107475772A true CN107475772A (en) | 2017-12-15 |
Family
ID=60604064
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710761767.XA Pending CN107475772A (en) | 2017-08-30 | 2017-08-30 | A kind of bbo crystal method for fast growing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107475772A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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) |
| 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 |
| CN102011186A (en) * | 2010-11-22 | 2011-04-13 | 福建福晶科技股份有限公司 | Middle seed crystal method for growing high-quality (beta-BaB2O4) BBO crystals |
| 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 |
| CN103225108A (en) * | 2013-04-07 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of large-size BBO 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 |
| CN106757341A (en) * | 2017-01-05 | 2017-05-31 | 福建福晶科技股份有限公司 | A kind of special growth technique for reducing bbo crystal envelope |
-
2017
- 2017-08-30 CN CN201710761767.XA patent/CN107475772A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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) |
| 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 |
| CN102011186A (en) * | 2010-11-22 | 2011-04-13 | 福建福晶科技股份有限公司 | Middle seed crystal method for growing high-quality (beta-BaB2O4) BBO crystals |
| 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 |
| CN103225108A (en) * | 2013-04-07 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of large-size BBO 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 |
| CN106757341A (en) * | 2017-01-05 | 2017-05-31 | 福建福晶科技股份有限公司 | A kind of special growth technique for reducing bbo crystal envelope |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107475772A (en) | A kind of bbo crystal method for fast growing | |
| CN103806101A (en) | Growth method and equipment of square sapphire crystal | |
| CN104350186A (en) | Sic single-crystal ingot, sic single crystal, and production method for same | |
| CN102383182A (en) | Molten-salt growth method for reducing central envelope of BBO(Barium Boron Oxide) crystals | |
| CN103225108B (en) | A kind of method of rapid growth of large-size BBO crystal | |
| CN101503819B (en) | Method and apparatus for growth of large size nonlinear optical crystal by copple and inoculating crystal | |
| CN102965723B (en) | A kind of method suppressing the radial too fast growth of bbo crystal | |
| CN202744653U (en) | Graphite crucible for preparing single crystal silicon by adopting Czochralski method | |
| CN104264213A (en) | EFG (edge-defined film-fed growth) device of large-size doped sapphire crystals and growth process thereof | |
| CN100494513C (en) | Fluxing agent growth method for trigallium phosphate crystal | |
| CN102912430B (en) | Sapphire crystal growth equipment and method | |
| CN104499043A (en) | 83kg-grade sapphire crystal furnace crystal-growing structure and crystal-growing method | |
| CN201962418U (en) | Sapphire single crystal furnace | |
| CN205313716U (en) | Independent rotary mechanism of crucible in siC growth of single crystal equipment | |
| CN106757341A (en) | A kind of special growth technique for reducing bbo crystal envelope | |
| CN103290466B (en) | A kind of YAB crystal growth flux and YAB growing method | |
| CN205501448U (en) | Growing device of jumbo size crystal | |
| Bennett | Seeded growth of garnet from molten salts | |
| CN104894637B (en) | The grower and growing method of a kind of crystal | |
| CN103114327B (en) | A kind of molten-salt growth method eliminating low-temperature phase defection barium borate crystal core parcel | |
| CN107475771A (en) | A kind of method of envelope among reduction bbo crystal | |
| CN208776874U (en) | A kind of crucible of lithium niobate crysal near stoichiometric ratio growth | |
| CN208685104U (en) | A kind of multiple crucible crystal growth furnace | |
| CN106958041B (en) | A kind of xTeO2·P2O5(x=2,4) preparation method and preparation facilities of crystal | |
| CN104264222B (en) | Crucible used by the growth of a kind of large scale borate crystal and method used |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171215 |
|
| WD01 | Invention patent application deemed withdrawn after publication |