CN1482289A - Combined crucible for growing spherical crown-shaped heteromorphic crystals - Google Patents
Combined crucible for growing spherical crown-shaped heteromorphic crystals Download PDFInfo
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- CN1482289A CN1482289A CNA031419011A CN03141901A CN1482289A CN 1482289 A CN1482289 A CN 1482289A CN A031419011 A CNA031419011 A CN A031419011A CN 03141901 A CN03141901 A CN 03141901A CN 1482289 A CN1482289 A CN 1482289A
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- crucible
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- cylinder
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- 239000013078 crystal Substances 0.000 title claims abstract description 39
- 230000007704 transition Effects 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910001182 Mo alloy Inorganic materials 0.000 claims 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 description 18
- 230000012010 growth Effects 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 208000035126 Facies Diseases 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 description 1
- PPTYJKAXVCCBDU-UHFFFAOYSA-N Rohypnol Chemical compound N=1CC(=O)N(C)C2=CC=C([N+]([O-])=O)C=C2C=1C1=CC=CC=C1F PPTYJKAXVCCBDU-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000034655 secondary growth Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
一种生长球冠形异型晶体用组合式坩埚，由外部坩埚、内部坩埚及坩埚内部锥体组成：该外部坩埚的底设有籽晶槽，该籽晶槽以一定弧度平滑过渡地于一半球形弧相接，坩埚顶部开有一定宽度和深度的三个纵向槽，在纵向槽的下部开有相同宽度的横向槽；该内部坩埚的顶部设有三个与外部坩埚三个纵向槽相对应的间距离相等的且带负公差的横向固定块体，内部坩埚半球形弧之上设有三个相间120°的倾斜向下的导流槽；该坩埚内部锥体之顶为锥体，其下是直径与锥体底面直径相等且有一定厚度的圆柱体，圆柱体下面是小直径的圆柱体，该坩埚内部锥体的高度，恰使锥体底边与导流槽在内部坩埚开口的内壁底沿平齐。
A combined crucible for growing spherical crown-shaped special-shaped crystals, which is composed of an external crucible, an internal crucible, and an internal cone of the crucible: the bottom of the external crucible is provided with a seed crystal groove, and the seed crystal groove smoothly transitions in a semi-spherical shape with a certain arc. The arcs are connected, and there are three longitudinal grooves of a certain width and depth on the top of the crucible, and there are horizontal grooves of the same width on the lower part of the longitudinal grooves; the top of the inner crucible is provided with three spaces corresponding to the three longitudinal grooves of the outer crucible. Horizontal fixed blocks with equal distances and negative tolerances, three 120° angled downward diversion grooves are arranged on the hemispherical arc of the inner crucible; the top of the inner cone of the crucible is a cone, and the bottom is a diameter A cylinder with the same diameter as the bottom surface of the cone and a certain thickness. Below the cylinder is a cylinder with a small diameter. The height of the cone inside the crucible is just so that the bottom edge of the cone and the diversion groove are at the bottom edge of the inner wall of the inner crucible opening. flush.
Description
Technical field
The present invention relates to crystal growth, the vertical warm terraced method growing special spherical crown crystal combined type copple of particularly a kind of confession.This combined type copple also goes for heat-exchanging method (HEM) and falling crucible method growing large-size high temperature single crystal such as (Bridgman).
Background technology
Crystal with the common shape of general method growth becomes the loss that the complicated crystal of shape can cause expensive material through cutting, mechanical workout supervisor, in lattice, introduce defective simultaneously and change the crystalline physical and mechanical properties, in order to overcome these shortcomings, the crystallization method that development can be satisfied size, shape and performance requriements just seems extremely important, and promptly direct growth is near the special-shaped crystal of moulding.The moulding crystal growth provides the possibility according to different predetermined cross-sectional parameter growing single-crystals, its geometrical shape that other method is difficult to form of can growing.Different crystal shape such as tabular, special-shaped crystal such as bar-shaped, the tubulose of different cross section, plate-like, spherical crown shape is used in the many aspects in the science and technology, is applied to the involucrum of laser pumping lamp, exterior lighting high-pressure mercury lamp as tubulose; The channelled hollow shaft-like efficient laser aid etc. that can be applicable to.
Special spherical crown crystal has important use in military field, just need spherical or analogous shape as the head bell jar of guided missile.Growing special spherical crown crystal was (referring to Journal of crystal growth with non-kapillary forming technique (NoncapillaryShaping Technique) growth in the past, the 179th volume, 1997, the 175th page), grow (referring to Window andDome Technologies and Materials II with guided mode method (Edge-defined Film-fed Growth), SPIE Proc.1326, nineteen ninety, page 2).
Above-mentioned prior art has significant disadvantages: die design is very complicated, and the accurate control of growth needs is awkward, and raw material availability is not high, the growth cost is higher.
Summary of the invention
Purpose of the present invention just is to provide a kind of combined type copple that is used for growing special spherical crown crystal, to satisfy vertical warm terraced method, heat-exchanging method (HEM) and falling crucible method method growing special spherical crown crystal such as (Bridgman).
Technical solution of the present invention is as follows:
A kind of growing special spherical crown crystal combined type copple, it is characterized in that it is made up of outer crucible, interior crucible and crucible interior cone: the end of described outer crucible, be provided with seed slot, this seed slot joins in half globular arc with certain radian with seamlessly transitting, the crucible top has three longitudinal slots of the certain width and the degree of depth,, have the transverse groove of same widths in the bottom of longitudinal slot; Described interior crucible, its top be provided with three with outer crucible between distance equate and be with the crosswise fixed block of minus tolerance, on the interior crucible semisphere arc certain altitude be provided with three alternate 120 ° be tilted under diversion trench; This crucible interior cone places interior crucible, the top of this crucible interior cone is a cone, be diameter and facies basialis pyramidis equal diameters under it and certain thickness right cylinder is arranged, it below the right cylinder right cylinder of minor diameter, the height of this crucible interior cone, when this crucible interior cone is put into interior crucible, just make cone base and diversion trench at the bottom of the inwall of interior crucible opening along concordant.
Alternate 120 ° of described three longitudinal slots.
Described interior crucible, outer crucible and crucible interior cone are made of the same material, and material can be graphite, molybdenum, tungsten and miramint etc., the polishing of outer crucible internal surface, the polishing of interior crucible outside surface, the upper surface polishing of cone.
Compare with technology formerly, the present invention has adopted a kind of combined type copple that is used for growing special spherical crown crystal, and this combined type copple is applicable to the terraced method of vertical temperature, heat-exchanging method (HEM) and falling crucible method growing large-size high temperature single crystal such as (Bridgman).Utilize combined type copple of the present invention in crucible, directly to form the special spherical crown crystal that needs with temperature gradient furnace, or according to the crystal of other shapes of design needs, process of growth is simple to operate, be easy to control, and compare with technology formerly, utilization ratio of raw materials is higher, can effectively reduce cost.
Description of drawings
Fig. 1 is the outer crucible structure iron
Fig. 2 is an interior crucible structure sectional view
Fig. 3 is an interior crucible structure vertical view
Fig. 4 is a crucible interior cone structure iron
Fig. 5 is a crucible combination synoptic diagram
Embodiment
Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5 are the combined type copple most preferred embodiment structure iron of special spherical crown crystal of the present invention, the combined type copple of special spherical crown crystal of the present invention is made up of 3 parts: outer crucible 1, interior crucible 2 and crucible interior cone 3, see Fig. 1, Fig. 2 and Fig. 3 respectively.Overall constitutional diagram is seen Fig. 4.Interior crucible, outer crucible and crucible interior cone are commaterial, and material can be graphite, molybdenum, tungsten and miramint etc., the polishing of outer crucible internal surface, the polishing of interior crucible outside surface, the polishing of cone upper surface.
Outer crucible is seen Fig. 1, has seed slot 11, and seed slot 11 seamlessly transits with certain radian with semisphere arc 12, and the crucible top has alternate 120 ° of 13, three grooves of three longitudinal slots.Have the transverse groove 14 of same widths in the bottom of longitudinal slot 13.
Interior crucible is seen Fig. 2, outside surface from the top begin down be three alternate 120 ° with inside and outside crucible between distance equate and be with the crosswise fixed block 21 of minus tolerance, on the interior crucible semisphere arc on the certain altitude, have and three alternate 120 ° of diversion trenchs 22 under oblique.
The top of this crucible interior cone 3 is a cone 31, be diameter and facies basialis pyramidis equal diameters under it and certain thickness right cylinder 32 is arranged, be the right cylinder 33 of minor diameter below the right cylinder 32, the height of this crucible interior cone 3 just make cone 31 bases and diversion trench 22 at the bottom of the inwall of interior crucible 2 openings along concordant.
The design that forms special spherical crown shape crucible is as follows:
Growth is to be that hemispheric special-shaped crucible constitutes jointly by inside and outside two bottoms with the formation of special spherical crown crucible, and inside and outside crucible is seen Fig. 1 and 2 respectively.Wherein outer crucible bottom has seed slot 11, and seed slot and semisphere arc 12 seamlessly transit with certain radian, and the semisphere arc has certain taper with top.The interior crucible bottom is a semisphere, and its diameter is partly with the tapering the same with outer crucible by the thickness decision of growing crystal more than the semisphere arc.In order to make inside and outside crucible assembling easier, interior crucible is higher than outer crucible semisphere arc with top from the semisphere arc with top.
Fixing means between the inside and outside crucible is:
The outer crucible top has alternate 120 ° of 13, three grooves of three longitudinal slots of the certain width and the degree of depth.Having the transverse groove 14 of same widths in the bottom of longitudinal slot, highly is half of longitudinal slot 13.The interior crucible outside surface begins down to be three alternate 120 ° and equates and be with the crosswise fixed block 21 of minus tolerance with inside and outside crucible spacing distance from the top, block width is greater than the total width of outer crucible fluting, and height is opened the longitudinal slot height greater than outer crucible.On preceding described three horizontal blocks, in the middle of the block bottom, begin to have width to be slightly smaller than three riveted pieces of outer crucible transverse groove.The width of riveted piece is slightly smaller than the outer crucible longitudinal slot, highly is slightly smaller than the outer crucible transverse groove.Outer crucible longitudinal slot bottom is identical with the height that interior crucible riveted piece bottom begins to the semisphere arc to the height that the semisphere arc begins to locate.Three blocks of interior crucible are put into the described groove rotation of outer crucible fixes inside and outside two crucibles.
Special-shaped crucible raw material and melt fill method are:
Raw material is the big raw material of the bigger material of particle and growing crystal thickness when being easy to fill, and raw material can directly be filled between the inside and outside crucible.When raw material is the powder material, carry out filling behind the binder with interior crucible in.Interior crucible is at the alternate 120 ° of diversion trenchs 22 under oblique of certain altitude on the semisphere arc and three in this case.To put into a cone 3 in the interior crucible simultaneously.There is diameter etc. cone 31 bottoms with the facies basialis pyramidis equal diameters and certain thickness right cylinder 32 is arranged, be the littler small cylinder 33 that contacts with the interior crucible bottom of diameter below the right cylinder 32, height should make above-mentioned cone base concordant with the diversion trench 22 bottom opening places of interior sidewall of crucible.Raw material is joined cone 31 tops, and the raw material fusing is after diversion trench 22 flows into the hemisphere portion between the interior outer crucible, and this design can make raw material make full use of.
The crucible design of a plurality of special spherical crown crystal of one secondary growth is as follows:
One time growth population needs N+1 crucible to be used greater than the individual crystal of N (N＞2), and the fixing means between the crucible is the same described identical, and difference is that except that outside crucible all there is the little foramen primum of same diameter all crucible bottom centers.Raw material directly is filled within the penetralia crucible, raw material fusing after the circular hole of crucible bottom be filled in the semisphere between each crucible.
Embodiment 1:
Carry out the growth of special spherical crown calcium fluoride crystal with above-mentioned illustrated combined type copple
Used combined type copple material of the present invention adopts high purity graphite in the present embodiment.Outer crucible is fixed on the zirconium white seat of temperature gradient furnace, interior crucible is fixing with it with preceding method, and cone is put into interior crucible, with reserve to seed crystal put into seed slot, calcium fluoride raw material through binder is filled on the cone, installs stove, is evacuated to 10
-4Pa charges into high-purity argon gas protective atmosphere to 1 normal atmosphere again, is warming up to melt temperature～1430 ℃ then, and constant temperature 2 hours is with 2 ℃/hr speed cooling growing crystal.Reduce to room temperature with 20 ℃ of/hour speed after crystallization is finished, the growth whole process finishes.
Take out combined type copple from gradient furnace, built-up type interior crucible and outer crucible, crucible interior cone are separated, the special spherical crown calcium fluoride crystal that will be positioned between interior crucible and outer crucible takes out.Crystal is transparent, complete.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03141901 CN1273652C (en) | 2003-07-29 | 2003-07-29 | Combined crucible for growing spherical special-shaped crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03141901 CN1273652C (en) | 2003-07-29 | 2003-07-29 | Combined crucible for growing spherical special-shaped crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1482289A true CN1482289A (en) | 2004-03-17 |
| CN1273652C CN1273652C (en) | 2006-09-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03141901 Expired - Fee Related CN1273652C (en) | 2003-07-29 | 2003-07-29 | Combined crucible for growing spherical special-shaped crystal |
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| Country | Link |
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| CN (1) | CN1273652C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586891A (en) * | 2012-02-28 | 2012-07-18 | 浙江上城科技有限公司 | Lining combined type high-temperature resisting crucible |
| CN104219806A (en) * | 2014-07-01 | 2014-12-17 | 长安大学 | Liquid-interlayer ceramic-metal composite bushing for immersion heater and manufacturing method of bushing |
| CN105921192A (en) * | 2016-07-19 | 2016-09-07 | 苏州普京真空技术有限公司 | Anti-skid crucible |
-
2003
- 2003-07-29 CN CN 03141901 patent/CN1273652C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586891A (en) * | 2012-02-28 | 2012-07-18 | 浙江上城科技有限公司 | Lining combined type high-temperature resisting crucible |
| CN102586891B (en) * | 2012-02-28 | 2015-09-30 | 浙江上城科技有限公司 | A kind of lining combined type high-temperature resisting crucible |
| CN104219806A (en) * | 2014-07-01 | 2014-12-17 | 长安大学 | Liquid-interlayer ceramic-metal composite bushing for immersion heater and manufacturing method of bushing |
| CN104219806B (en) * | 2014-07-01 | 2016-01-06 | 长安大学 | A kind of immersion heater liquid intermediate layer ceramic-metal cladding sleeve pipe and manufacture method thereof |
| CN105921192A (en) * | 2016-07-19 | 2016-09-07 | 苏州普京真空技术有限公司 | Anti-skid crucible |
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| Publication number | Publication date |
|---|---|
| CN1273652C (en) | 2006-09-06 |
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Granted publication date: 20060906 Termination date: 20090831 |