CN101787560A - Special-shaped crucible for adjusting gas-liquid temperature difference of crystal grown by melt pulling method - Google Patents
Special-shaped crucible for adjusting gas-liquid temperature difference of crystal grown by melt pulling method Download PDFInfo
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- CN101787560A CN101787560A CN200910076877A CN200910076877A CN101787560A CN 101787560 A CN101787560 A CN 101787560A CN 200910076877 A CN200910076877 A CN 200910076877A CN 200910076877 A CN200910076877 A CN 200910076877A CN 101787560 A CN101787560 A CN 101787560A
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- CN
- China
- Prior art keywords
- iridium
- iraurite
- crucible
- temperature difference
- sheet
- 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.)
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- 239000013078 crystal Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 title claims abstract description 19
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 33
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 33
- 230000005540 biological transmission Effects 0.000 abstract description 2
- UYVZCGGFTICJMW-UHFFFAOYSA-N [Ir].[Au] Chemical compound [Ir].[Au] UYVZCGGFTICJMW-UHFFFAOYSA-N 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 8
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 238000002050 diffraction method Methods 0.000 description 4
- 238000011081 inoculation Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000006698 induction Effects 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- QWVYNEUUYROOSZ-UHFFFAOYSA-N trioxido(oxo)vanadium;yttrium(3+) Chemical compound [Y+3].[O-][V]([O-])([O-])=O QWVYNEUUYROOSZ-UHFFFAOYSA-N 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000007648 laser printing Methods 0.000 description 1
- PSVBHJWAIYBPRO-UHFFFAOYSA-N lithium;niobium(5+);oxygen(2-) Chemical compound [Li+].[O-2].[O-2].[O-2].[Nb+5] PSVBHJWAIYBPRO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- -1 rare earth yttrium vanadate Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a special-shaped crucible for adjusting gas-liquid temperature difference for crystal growth by a melt pulling method, which is an iridium crucible; it is characterized by also comprising: the iridium support stand column is vertically fixed at the center of the inner bottom surface of the iridium crucible; the iridium sheet is fixed at the upper end of the iridium support stand column and is horizontally placed, and a gap is reserved between the edge of the iridium sheet and the edge of the iridium crucible; the iridium gold sheet is planar, concave or convex; the iridium sheet arranged in the iridium crucible plays a role of a heat source, the gas-liquid temperature difference at the growth interface is effectively changed, the mass transport and heat transmission are enhanced, the grown crystal has no defects of inclusion, growth stripes and the like, and the crystal utilization rate can be greatly improved.
Description
Technical field
The present invention relates to the crucible of field of crystal growth, particularly a kind of special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt.
Technical background
Vanadate crystal is the crystalline material with important value that develops rapidly over past ten years.Vanadic acid yttrium (YVO wherein
4) have favorable mechanical and a physical property, have the 0.4 μ m～transparency range of 5 μ m and bigger degree of birefringence, be comparatively ideal optical birefringence crystalline material, be widely used in the optical passive components such as the shield retaining in optical communication, circulator, beam splitter and intersection wavelength division multiplexer.Doped yttrium vanadate (as: Nd:YVO
4, Nd:GdVO
4) crystal is the laser crystals of excellent property, the Nd:YVO of LD pumping
4, Nd:GdVO
4Crystal laser and frequency multiplier thereof are widely used in the light source of opticmeasurement, transmitter, laser printing, medicine, highdensity optical memory and color monitor etc., use under field and the severe environmental conditions being more suitable for aspect laser communications and the laser ranging, possess military meaning under battle conditions.
As far back as the 60 to 70's, yttrium vanadate crystal has just caused the concern of academia, people attempt with multiple means such as flame method, hydrothermal method, horizontal zone-melting technique, floating zone melting, crystal pulling method growth rare earth yttrium vanadate crystal, but fail to obtain the monocrystalline of sufficient size and higher optical quality.Human LHPG methods such as the investigation of materials chamber S.Erdei of U.S. University of Pennsylvania in 1992 growth YVO
4Single crystal fibre is succeedd.1993, YVO
4, Nd:YVO
4Crystalline Czochralski increment study has been obtained breakthrough progress, and the Czochralski technology has become the major technique means of vanadate serial crystal growth at present.
In Czochralski pulling growth vanadate series monocrystal process, the general design acquisition institute suitable temperature gradient of passing through the relative position and the top stay-warm case of adjusting crucible and induction coil, but only whereby, be difficult to reach some crystal (as: Nd:YVO sometimes
4) the needed thermograde of growing.
Summary of the invention
The object of the present invention is to provide a kind of simple in structurely, easily manufactured, can effectively regulate the special-shaped crucible of the adjusting gas-liquid temperature difference that is used for crystal grown by Czochralski method from melt of interface gas-liquid temperature difference.
Technical scheme of the present invention is as follows:
The special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt provided by the invention comprises the Iridium Crucible body; It is characterized in that, also comprise:
The vertical iraurite support post that is fixed in described Iridium Crucible body inner bottom surface center; With
Be fixed in the iraurite sheet that described iraurite support post upper end is horizontal positioned;
Described iraurite sheet edge and Iridium Crucible body edges keep the space.
Described Iridium Crucible body internal diameter is 60-80mm, is 35-75mm deeply.
Described iraurite support post height is 15-40mm.
Described iraurite sheet is plate, its thickness 2-5mm.
Described iraurite sheet is a concave type, and its concave surface radian is 10-30 °, its thickness 2-5mm.
Described iraurite sheet is a convex-surface type, 10-30 ° of its convex surface radian, its thickness 2-5mm.
The space is 8-20mm between iraurite sheet edge and the Iridium Crucible body edges.
Use the special-shaped crucible growth vanadate crystal that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of the present invention, step is: synthetic vanadate raw material is fused in the special-shaped Iridium Crucible of the present invention in batches, the abnormity Iridium Crucible places quartz tube, on every side with ZrO
2Sand is filled, and behind the seed crystal position fixing process, medium-frequency induction furnace is evacuated to pressure is-0.095MPa, with high-purity N
2Or Ar gas makes protection atmosphere, to pressure be 0.03MPa, heat up raw material is dissolved after, carry out crystal growth according to steps such as inoculation, shouldering, isometrical, annealing; It is 1-3mm/h that shouldering finishes the back isodiametric growth stage rate of pulling, and rotating speed is 8-20rpm, and the seed crystal direction is crystallography a or c axle, and the crystalline size that obtains of growing generally is that diameter is 20-30mm, long for about 30-40mm, Nd
3+Concentration is between 0.1at%-3at%.
Use the effect of growing crystal of the special-shaped crucible of the adjusting gas-liquid temperature difference that is used for crystal grown by Czochralski method from melt of the present invention to show: owing to use special-shaped crucible of the present invention, the iraurite sheet plays the effect of thermal source, can effectively regulate the gas-liquid temperature difference at growth interface place, only overcome in the traditional C zochralski technology and regulated unfavorable that gas-liquid temperature difference brought by the relative position of crucible and induction coil, strengthened the transmission of mass transport and heat, the crystal that grows does not have defectives such as inclusion and striation, and the crystal utilization ratio is increased substantially.The special-shaped crucible of this invention is suitable for Lithium niobium trioxide, lithium tantalate, and particularly vanadate crystal is (as YVO
4, Nd:YVO
4, Nd:GdVO
4) growth.
Description of drawings
Fig. 1 is the special-shaped crucible sectional view of flush type for the iraurite sheet;
Fig. 2 is the special-shaped crucible sectional view of concave type for the iraurite sheet;
Fig. 3 is the special-shaped crucible sectional view of convex-surface type for the iraurite sheet.
Embodiment
Further describe the present invention below in conjunction with drawings and Examples:
Embodiment 1: the iraurite sheet be flush type special-shaped crucible structure as shown in Figure 1:
Iridium Crucible body 1 internal diameter is 80mm, in high (deeply) be 50mm (degree of depth be 35-75mm all can), welding one diameter in Iridium Crucible body 1 bottom centre place is that 4mm, length are the iraurite support post 2 of 30mm (top diameter 3mm), iraurite sheet 3 is the flush type iraurite sheet of thickness 5mm (thickness be 2-5mm all can), its diameter is 56mm, it is the 3.5mm circular hole that there is a diameter its center, lower surface, this circle hole sleeve is contained in iraurite support post 2 tops, keeps the 12mm gap between iraurite sheet 3 edges and Iridium Crucible body 1 edge.
Embodiment 2: the iraurite sheet be concave type special-shaped crucible structure as shown in Figure 2:
Iridium Crucible body 1 internal diameter is 70mm, in high (deeply) be 45mm (degree of depth be 35-75mm all can), welding one diameter in Iridium Crucible body 1 bottom centre place is that 4mm, length are the iraurite support post 2 of 25mm (top diameter 3mm), iraurite sheet 3 is the concave type iraurite sheet of thickness 3mm (thickness be 2-5mm all can) (concave surface radian be concave surface all can), its diameter is 40mm, it is the 3.5mm circular hole that there is a diameter its center, lower surface, this circle hole sleeve is contained in iraurite support post 2 tops, keeps the 15mm gap between iraurite sheet 3 edges and Iridium Crucible body 1 edge.
Embodiment 3: the iraurite sheet be convex-surface type special-shaped crucible structure as shown in Figure 3:
Iridium Crucible body 1 internal diameter is 60mm, in high (deeply) be 40mm (degree of depth be 35-75mm all can), welding one diameter in Iridium Crucible body 1 bottom centre place is that 4mm, length are the iraurite support post 2 of 20mm (top diameter 3mm), iraurite sheet 3 is the convex-surface type iraurite sheet of thickness 2mm (thickness be 2-5mm all can) (convex surface radian be concave surface all can), its diameter is 40mm, it is the 3.5mm circular hole that there is a diameter its center, lower surface, this circle hole sleeve is contained in iraurite support post 2 tops, keeps the 10mm gap between iraurite sheet 3 edges and Iridium Crucible body 1 edge.
Embodiment 4:YVO
4Crystal growth
With synthetic good 500gYVO
4Raw material is fused in the embodiment 1 described flush type abnormity Iridium Crucible in batches, and crucible places quartz tube, on every side with ZrO
2Sand is filled, and after finishing the seed crystal position fixing process, is evacuated to pressure and is-0.095MPa, with high-purity N
2Gas is made protection atmosphere, to pressure be 0.08MPa, heat up raw material is dissolved after, carry out crystal growth according to steps such as inoculation, shouldering, isometrical, annealing; It is 2mm/h that shouldering finishes the back isodiametric growth stage rate of pulling, and rotating speed is 15rpm, and the seed crystal direction is a crystallography c axle, the crystalline size φ 33 * 50mm that grows and obtain, and weight reaches 192g; This crystal does not have defectives such as inclusion, striation and low angle boundary.
Embodiment 5:Nd (0.2at%): YVO
4Crystal growth
With synthetic good 450g Nd (3at%): YVO
4Raw material is fused in the embodiment 2 described concave type abnormity Iridium Crucible in batches, and crucible places quartz tube, on every side with ZrO
2Sand is filled, and behind the seed crystal position fixing process, is evacuated to pressure and is-0.095MPa, then with high-purity N
2Gas is made protection atmosphere, to pressure be 0.08MPa, heat up raw material is dissolved after, carry out crystal growth according to steps such as inoculation, shouldering, isometrical, annealing.It is 1.0mm/h that shouldering finishes the back isodiametric growth stage rate of pulling, rotating speed is 12rpm, the seed crystal direction is crystallography a, after the growth ending crystal is carried and being taken off, be cooled to 1100 ℃ by 10 ℃/h, 15 ℃/h is cooled to 900 ℃, and 25 ℃/h is cooled to 700 ℃, 50 ℃/h is cooled to 400 ℃, and 100 ℃/h is cooled to room temperature; The crystalline size that obtains of growing is: 28 * (29-34) * 26mm, this crystal weight is 98g.Crystal does not have defectives such as inclusion, striation and low angle boundary.
Embodiment 6:Nd (3at%): YVO
4Crystal growth
With synthetic good 340g Nd (3at%): YVO
4Raw material is fused in the embodiment 3 described convex-surface type abnormity Iridium Crucible in batches, and crucible places quartz tube, on every side with ZrO
2Sand is filled, and behind the seed crystal position fixing process, is evacuated to pressure and is-0.095MPa, then with high-purity N
2Gas is made protection atmosphere, to pressure be 0.08MPa, heat up raw material is dissolved after, carry out crystal growth according to steps such as inoculation, shouldering, isometrical, annealing.It is 1.0mm/h that shouldering finishes the back isodiametric growth stage rate of pulling, rotating speed is 12rpm, the seed crystal direction is crystallography a, after the growth ending crystal is carried and being taken off, be cooled to 1100 ℃ by 10 ℃/h, 15 ℃/h is cooled to 900 ℃, and 25 ℃/h is cooled to 700 ℃, 50 ℃/h is cooled to 400 ℃, and 100 ℃/h is cooled to room temperature; The crystalline size that obtains of growing is: 24 * (25-30) * 22mm, this crystal weight is 61g.Crystal does not have defectives such as inclusion, striation and low angle boundary.
Claims (7)
1. a special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt comprises the Iridium Crucible body; It is characterized in that, also comprise:
The vertical iraurite support post that is fixed in described Iridium Crucible body inner bottom surface center; With
Be fixed in the iraurite sheet that described iraurite support post upper end is horizontal positioned;
Described iraurite sheet edge and Iridium Crucible body edges keep the space.
2. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that described Iridium Crucible body internal diameter is 60-80mm, is 35-75mm deeply.
3. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that described iraurite support post height is 15-40mm.
4. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that described iraurite sheet is plate, its thickness 2-5mm.
5. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that described iraurite sheet is a concave type, its concave surface radian is 10-30 °, its thickness 2-5mm.
6. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that described iraurite sheet is a convex-surface type, 10-30 ° of its convex surface radian, its thickness 2-5mm.
7. by the described special-shaped crucible that is used for the adjusting gas-liquid temperature difference of crystal grown by Czochralski method from melt of claim 1, it is characterized in that the space is 8-20mm between iraurite sheet edge and the Iridium Crucible body edges.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100768778A CN101787560B (en) | 2009-01-23 | 2009-01-23 | Special-shaped crucible for adjusting gas-liquid temperature difference of crystal grown by melt pulling method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100768778A CN101787560B (en) | 2009-01-23 | 2009-01-23 | Special-shaped crucible for adjusting gas-liquid temperature difference of crystal grown by melt pulling method |
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| Publication Number | Publication Date |
|---|---|
| CN101787560A true CN101787560A (en) | 2010-07-28 |
| CN101787560B CN101787560B (en) | 2012-06-13 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877116A (en) * | 2011-07-13 | 2013-01-16 | 中国科学院理化技术研究所 | Closed single crystal growth furnace for crystal growth by molten salt method |
| CN113774483A (en) * | 2021-10-13 | 2021-12-10 | 上海德硅凯氟光电科技有限公司 | Preparation device and method of central special-shaped fluoride optical crystal |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100588425B1 (en) * | 2003-03-27 | 2006-06-12 | 실트로닉 아게 | Method for the Production of a Silicon Single Crystal, Silicon Single Crystal and Silicon Semiconductor Wafers with determined Defect Distributions |
| JP4597619B2 (en) * | 2003-12-26 | 2010-12-15 | シルトロニック・ジャパン株式会社 | Crucible for growing silicon crystal and method for growing silicon crystal |
-
2009
- 2009-01-23 CN CN2009100768778A patent/CN101787560B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877116A (en) * | 2011-07-13 | 2013-01-16 | 中国科学院理化技术研究所 | Closed single crystal growth furnace for crystal growth by molten salt method |
| CN102877116B (en) * | 2011-07-13 | 2014-12-31 | 中国科学院理化技术研究所 | Closed single crystal growth furnace for crystal growth by molten salt method |
| CN113774483A (en) * | 2021-10-13 | 2021-12-10 | 上海德硅凯氟光电科技有限公司 | Preparation device and method of central special-shaped fluoride optical crystal |
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| Publication number | Publication date |
|---|---|
| CN101787560B (en) | 2012-06-13 |
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