CN104264222A - Crucible and method for large-size borate crystal growth - Google Patents
Crucible and method for large-size borate crystal growth Download PDFInfo
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- CN104264222A CN104264222A CN201410455749.5A CN201410455749A CN104264222A CN 104264222 A CN104264222 A CN 104264222A CN 201410455749 A CN201410455749 A CN 201410455749A CN 104264222 A CN104264222 A CN 104264222A
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- crucible
- crystal
- growth
- special
- large size
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- 239000013078 crystal Substances 0.000 title claims abstract description 119
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000007373 indentation Methods 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 238000010583 slow cooling Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000002109 crystal growth method Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 230000026267 regulation of growth Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000003203 everyday effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a special-shaped crucible capable of adjusting the appearance of a crystal for large-size borate crystal growth, wherein a notch for adjusting the temperature field in the crucible is arranged on the wall of the special-shaped crucible. The invention also discloses a large-size borate crystal growth method, and the special-shaped crucible is adopted for crystal growth. The special-shaped crucible provided by the invention has the advantages of simple structure, convenience in manufacturing and lower cost. The special-shaped crucible capable of adjusting the crystal morphology for the growth of the large-size borate crystal and the method for growing the large-size borate crystal can effectively adjust the morphology of the grown crystal, obviously improve the utilization rate of the crystal and are beneficial to cutting devices with larger sizes.
Description
Technical field
The present invention relates to technical field of crystal growth, more specifically relate to a kind of large size borate crystal and grow crucible used and method used.
Background technology
Three lithium tetraborate (LiB
3o
5, being called for short LBO) and crystal has the advantages such as damage threshold is large, optical homogeneity good, nonlinear factor is large, physical and chemical performance is stable, is widely used in the field such as fixed laser frequency conversion, optical parameter concussion.Its growth method is generally top-seeded flux method, top seeded solvent growth etc.
Along with the continuous breakthrough of large size lbo crystal growing technology, large size lbo crystal is widely used in various ultra high power laser aid.These application propose more and more higher requirement to the size of quartz crystal device.When making quartz crystal device, must cut along special angle, usually also requiring that the logical light face of device is for square.But the large size lbo crystal pattern of growth is at present difficult to control, and this just causes when making devices, and the utilization ratio of crystal is not high, is difficult to cut out larger sized LBO device.
Summary of the invention
(1) technical problem that will solve
The technical problem to be solved in the present invention overcomes exactly in prior art and is difficult to obtain large size LBO device, the not high difficult problem of the utilization ratio of crystal when making devices, for the demand of specific direction large size LBO device, provide a kind of special-shaped crucible and growing method of the regulate crystal pattern for the growth of large size borate crystal.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of special-shaped crucible for the growth of large size borate crystal, described crucible diameter is 80-400mm, is 40-300mm deeply, along being provided with the breach regulating warm field in crucible on sidewall of crucible.
Preferably, on described sidewall of crucible, the breach number on edge is 1-6.
Preferably, on described sidewall of crucible, the breach on edge is symmetrical.
Preferably, the material of described crucible is platinum, iraurite or pottery.
Preferably, on described sidewall of crucible, the notch geometry on edge is rectangle, is of a size of 5-30mm × 10-40mm.
Preferably, on described sidewall of crucible, the notch geometry on edge is V-arrangement, and breach is long is 5-50mm, is 5-25mm deeply.
Preferably, on described sidewall of crucible, the notch geometry on edge is semicircle, and diameter is 5-50mm.
Present invention also offers the method for a kind of large size borate crystal growth, the method adopts above-mentioned special-shaped crucible, and the method comprising the steps of:
Step one: for the preparation of the raw material of crystal growth from f lux, is placed in described special-shaped crucible, and raw material height must lower than crucible indentation, there, is warming up to described raw material and melts obtain pyrosol completely;
Step 2: introduce seed crystal, cooling starts growing crystal;
Step 3: after crystal growth terminates, slow cooling, to room temperature, takes out crystal.
Preferably, in step 2: by described solution warms to the above 0.5-5 DEG C of saturation point, slow introducing seed crystal is to described solution surface or wherein, be incubated after 0.5-2 hour, lowering the temperature with the speed of 0.02-2 DEG C/day starts growing crystal.
Preferably, described seed crystal non rotating, described crucible rotation or static, seed face to the crystal face of breach as the crystal face of crystal development.
The principle of growing method of the present invention is: along the breach arranging specified shape on the sidewall of crucible of conventional crucible, is aided with multistage crystal growing furnace and regulates the temperature being positioned at crucible top position, can play the effect regulating warm field in crucible.If the temperature of crucible top position is lower in crystal growing furnace, then because indentation, there convection current is comparatively strong, the temperature of indentation, there solution is lower, and degree of supersaturation is comparatively large, and crystal is very fast along this direction speed of growth.The direction of adjustment seed crystal, makes the crystal face towards indentation, there be the crystal face of wishing crystal development, the pattern of the crystal that energy growth regulation goes out.Be conducive to improving crystal utilization ratio, cut out the crystal for more large-size device.
(3) beneficial effect
The invention provides a kind of special-shaped crucible and growing method of the regulate crystal pattern for the growth of large size borate crystal, adopt special-shaped crucible of the present invention and growing method, the pattern of the crystal that energy growth regulation goes out.Be conducive to improving crystal utilization ratio, cut out the crystal for more large-size device.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the special-shaped crucible schematic diagram of the regulate crystal pattern grown for large size borate crystal for the present invention;
Fig. 2 is the lbo crystal schematic diagram that growth method according to the present invention generates;
Mark in figure: 1, crucible, 2, breach.
Embodiment
Below in conjunction with drawings and Examples, embodiments of the present invention are described in further detail.Following examples for illustration of the present invention, but can not be used for limiting the scope of the invention.
As shown in Figure 1, the special-shaped crucible of the present embodiment is the cylindrical crucible of upper end open, closed bottom, be provided with on the upper edge of sidewall of crucible for regulate warm field in crucible breach.Described crucible diameter is 80-400mm, is 40-300mm deeply.The breach number of described sidewall of crucible is 1-6.
As optional technical scheme, the breach of sidewall of crucible is symmetrical or mal-distribution.
As optional technical scheme, the notch geometry of described sidewall of crucible is rectangle, is of a size of 5-30mm × 10-40mm.
As optional technical scheme, the notch geometry of described sidewall of crucible is V-arrangement, and breach is long is 5-50mm, is 5-25mm deeply.
As optional technical scheme, the notch geometry of described sidewall of crucible is semicircle, and diameter is 5-50mm.
As optional technical scheme, the material of described crucible is platinum, iraurite or pottery.
When adopting the special-shaped crucible growing LBO crystal of the present embodiment, process is as follows: be first placed in crucible by the LBO growth raw material of preparation, after ensureing fusing, liquid level is no more than the indentation, there of crucible, crucible is placed in growth furnace and is heated to fusing formation pyrosol and is incubated for some time, solution temperature is down to 0.5-5 DEG C on saturation point, to solution surface or wherein introduce seed crystal, after insulation appropriate time, with specific cooling rate slow cooling.Seed crystal is motionless, is aided with multistage crystal growing furnace and regulates the temperature being positioned at crucible top position, can play the effect regulating warm field in crucible.Make the temperature of crucible top position in crystal growing furnace lower, then because indentation, there convection current is comparatively strong, the temperature of indentation, there solution is lower, and degree of supersaturation is comparatively large, and crystal is very fast along this direction speed of growth.The direction of adjustment seed crystal, makes the crystal face towards indentation, there be the crystal face of wishing crystal development, the pattern of the crystal that energy growth regulation goes out.Be conducive to improving crystal utilization ratio, cut out the crystal for more large-size device.
Embodiment 1
By the LiCO of analytically pure 2329 grams
3, 3896 grams of H
3bO
3with 3026 grams of MoO
3after grinding, Homogeneous phase mixing loads in special-shaped crucible.Crucible material is platinum, is of a size of Φ 200 × 180mm, along symmetrical two rectangular indentation on sidewall of crucible, is of a size of 20mm × 35mm.Crucible is put into syllogic Resistant heating monocrystal growing furnace, crucible top position is positioned at resistance wire place topmost.Be heated to 900 DEG C with the temperature rise rate of 80 DEG C/about h, the heating power of adjustment three sections of resistance wires, forms upper and lower two ends temperature lower, the warm field that medium temperature is high.Be incubated 24 hours, then slowly cool to 710 DEG C.Trial seed-grain method is adopted to measure saturation point temperature accurately.Then more than saturation point 3 DEG C introduce seed crystals to solution surface.Adjustment seed crystal direction, make the crystal face towards indentation, there be the crystal face of wishing crystal development, constant temperature 2 as a child after, start slow cooling.Seed crystal non rotating, rate of temperature fall is every day 0.02 DEG C-0.5 DEG C.Terminate through 80 days crystal growth, crystal is slowly proposed liquid level, be cooled to room temperature with the speed of 8 DEG C per hour, finally obtain and be of a size of 170 × 165 × 78mm
3lbo crystal.
Embodiment 2
By the LiCO of analytically pure 563 grams
3, 953 grams of H
3bO
3with 726 grams of MoO
3after grinding, Homogeneous phase mixing loads in special-shaped crucible.Crucible material is platinum, is of a size of Φ 120 × 80mm, and along symmetrical two V-notch on sidewall of crucible, breach is long is 30mm, is 15mm deeply.Crucible is put into syllogic Resistant heating monocrystal growing furnace, crucible top position is positioned at resistance wire place topmost.Be heated to 880 DEG C with the temperature rise rate of 50 DEG C/about h, the heating power of adjustment three sections of resistance wires, forms upper and lower two ends temperature lower, the warm field that medium temperature is high.Be incubated 36 hours, then slowly cool to 730 DEG C.Trial seed-grain method is adopted to measure saturation point temperature accurately.Then more than saturation point 1.5 DEG C introduce seed crystals to solution surface.Adjustment seed crystal direction, make the crystal face towards indentation, there be the crystal face of wishing crystal development, constant temperature 1 as a child after, start slow cooling.Seed crystal non rotating, rate of temperature fall is every day 0.05 DEG C-1 DEG C.Terminate through 55 days crystal growth, crystal is slowly proposed liquid level, be cooled to room temperature with the speed of 15 DEG C per hour, finally obtain and be of a size of 115 × 108 × 63mm
3lbo crystal.
Embodiment 3
By the LiCO of analytically pure 2056 grams
3, 2173 grams of H
3bO
3with 5235 grams of MoO
3after grinding, Homogeneous phase mixing loads in special-shaped crucible.Crucible material is platinum, is of a size of Φ 310 × 180mm, and along symmetrical two semicircular indentations on sidewall of crucible, diameter is 50mm.Crucible is put into five-part form Resistant heating monocrystal growing furnace, crucible top position is positioned at resistance wire place topmost.Be heated to 860 DEG C with the temperature rise rate of 30 DEG C/about h, the heating power of adjustment five sections of resistance wires, forms tip temperature lower, middle part and the higher warm field of temperature of lower.Be incubated 30 hours, then slowly cool to 715 DEG C.Trial seed-grain method is adopted to measure saturation point temperature accurately.Then more than saturation point 2 DEG C introduce seed crystals to solution surface.Adjustment seed crystal direction, make the crystal face towards indentation, there be the crystal face of wishing crystal development, constant temperature 1.5 as a child after, start slow cooling.Seed crystal non rotating, rate of temperature fall is every day 0.03 DEG C-1.5 DEG C.Terminate through 98 days crystal growth, crystal is slowly proposed liquid level, be cooled to room temperature with the speed of 7-15 per hour DEG C, finally obtain and be of a size of 225 × 208 × 123mm
3lbo crystal.
The invention provides a kind of special-shaped crucible and growing method of the regulate crystal pattern for the growth of large size borate crystal, adopt special-shaped crucible of the present invention and growing method, the pattern of the crystal that energy growth regulation goes out.Be conducive to improving crystal utilization ratio, cut out the crystal for more large-size device.
Above embodiment is only for illustration of the present invention, but not limitation of the present invention.Although with reference to embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, various combination, amendment or equivalent replacement are carried out to technical scheme of the present invention, do not depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of right of the present invention.
Claims (10)
1. for a special-shaped crucible for large size borate crystal growth, it is characterized in that, described crucible diameter is 80-400mm, is 40-300mm deeply, along being provided with the breach regulating warm field in crucible on sidewall of crucible.
2. the special-shaped crucible for the growth of large size borate crystal according to claim 1, is characterized in that, on described sidewall of crucible, the breach number on edge is 1-6.
3. the special-shaped crucible for the growth of large size borate crystal according to claim 1, it is characterized in that, on described sidewall of crucible, the breach on edge is symmetrical.
4. the special-shaped crucible for the growth of large size borate crystal according to claim 1, it is characterized in that, the material of described crucible is platinum, iraurite or pottery.
5. the special-shaped crucible for the growth of large size borate crystal according to any one of Claims 1-4, it is characterized in that, on described sidewall of crucible, the notch geometry on edge is rectangle, is of a size of 5-30mm × 10-40mm.
6. the special-shaped crucible for the growth of large size borate crystal according to any one of Claims 1-4, it is characterized in that, on described sidewall of crucible, the notch geometry on edge is V-arrangement, and breach is long is 5-50mm, is 5-25mm deeply.
7. the special-shaped crucible for the growth of large size borate crystal according to any one of Claims 1-4, is characterized in that, on described sidewall of crucible, the notch geometry on edge is semicircle, and diameter is 5-50mm.
8. a method for large size borate crystal growth, is characterized in that, adopt special-shaped crucible described in claim 1-7, the method comprising the steps of:
Step one: for the preparation of the raw material of crystal growth from f lux, is placed in described special-shaped crucible, and raw material height must lower than crucible indentation, there, is warming up to described raw material and melts obtain pyrosol completely;
Step 2: introduce seed crystal, cooling starts growing crystal;
Step 3: after crystal growth terminates, slow cooling, to room temperature, takes out crystal.
9. the method for large size borate crystal growth according to claim 8, it is characterized in that, in step 2: by described solution warms to the above 0.5-5 DEG C of saturation point, slow introducing seed crystal is to described solution surface or wherein, be incubated after 0.5-2 hour, start growing crystal with the speed of 0.02-2 DEG C of/day cooling.
10. the method for large size borate crystal growth according to claim 8 or claim 9, is characterized in that, described seed crystal non rotating, described crucible rotation or static, seed face to the crystal face of breach as the crystal face of crystal development.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410455749.5A CN104264222B (en) | 2014-09-09 | Crucible and method for large-size borate crystal growth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410455749.5A CN104264222B (en) | 2014-09-09 | Crucible and method for large-size borate crystal growth |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104264222A true CN104264222A (en) | 2015-01-07 |
| CN104264222B CN104264222B (en) | 2017-01-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115522258A (en) * | 2022-10-08 | 2022-12-27 | 宇泽半导体(云南)有限公司 | Special-shaped silicon single crystal rod, quartz crucible for drawing same and growth method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1422993A (en) * | 2001-11-30 | 2003-06-11 | 中国科学院福建物质结构研究所 | Growth of LiB3O5 nonlinear optical crystal by integrating rotary crucible and molten salt Czochralski growth method |
| CN1443878A (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 LBO crystal |
| JP2009215112A (en) * | 2008-03-11 | 2009-09-24 | Hitachi Cable Ltd | Crucible for crystal growth, and semiconductor single crystal grown using the same |
| CN102383182A (en) * | 2011-10-23 | 2012-03-21 | 福建福晶科技股份有限公司 | Molten-salt growth method for reducing central envelope of BBO(Barium Boron Oxide) crystals |
| CN203613302U (en) * | 2013-10-24 | 2014-05-28 | 江苏大学 | Argon guide system for polycrystalline silicon ingot furnace |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1422993A (en) * | 2001-11-30 | 2003-06-11 | 中国科学院福建物质结构研究所 | Growth of LiB3O5 nonlinear optical crystal by integrating rotary crucible and molten salt Czochralski growth method |
| CN1443878A (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 LBO crystal |
| JP2009215112A (en) * | 2008-03-11 | 2009-09-24 | Hitachi Cable Ltd | Crucible for crystal growth, and semiconductor single crystal grown using the same |
| CN102383182A (en) * | 2011-10-23 | 2012-03-21 | 福建福晶科技股份有限公司 | Molten-salt growth method for reducing central envelope of BBO(Barium Boron Oxide) crystals |
| CN203613302U (en) * | 2013-10-24 | 2014-05-28 | 江苏大学 | Argon guide system for polycrystalline silicon ingot furnace |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115522258A (en) * | 2022-10-08 | 2022-12-27 | 宇泽半导体(云南)有限公司 | Special-shaped silicon single crystal rod, quartz crucible for drawing same and growth method |
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