CN103849926A - Method and equipment for pulling high-activity metal monocrystalline - Google Patents
Method and equipment for pulling high-activity metal monocrystalline Download PDFInfo
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- CN103849926A CN103849926A CN201410121375.3A CN201410121375A CN103849926A CN 103849926 A CN103849926 A CN 103849926A CN 201410121375 A CN201410121375 A CN 201410121375A CN 103849926 A CN103849926 A CN 103849926A
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- crucible
- metal
- high activity
- lifts
- lifting head
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- 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
- C30B29/52—Alloys
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- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- 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 provides a technical scheme of a method and equipment for pulling high-activity metal monocrystalline. The method is a general method of multiple high-activity metals of transition metals, a rare earth metals and alloys thereof. Compared with a conventional crucible pulling method and a mould casting method, the method has the advantages of preventing pollution of a crucible or mould to a melt and erosion of the melt to the crucible, being high in purity of a grown crystal, being capable of melting a high-melting point metal, and the like. Compared with a magnetic suspension cold crucible technology, the equipment has the advantages of preventing from a complicated design and a customized processing of the crucible and an induction coil, being good in universality, low in equipment energy consumption, high in heating and warming speed, simple and convenient to operate, easy to maintain and repair, and the like.
Description
Technical field
What the present invention relates to is that metal single crystal lifts field, especially a kind of method and apparatus that lifts high activity metal monocrystalline.
Background technology
In the prior art, known technology is to utilize quartz crucible to lift single crystal silicon semiconductor.The single crystal pulling technology of this routine in semicon industry tool have been widely used, and be progressively generalized in the research and development of other type materials, as metallurgical and special type function material are prepared related high activity metal material, but also run into the restriction of a lot of technical barriers simultaneously.First, conventional crucible or fusion casting die can pollute the melt of high activity metal, and self are subject to the erosion of melt and cause work-ing life very short.Secondly, the material of crucible has seriously limited the melting of refractory metal, is difficult to choose suitable crucible material for dystectic metal.In recent years, for these highly active metallic substance, a kind of technology that lifts of magnetic levitation cold crucible is developed.Magnetic levitation cold crucible technology adopts radio-frequency current to produce the magnetic field of alternation in space by coil, and the surface of raw metal produces induced current under the action of a magnetic field, and then due to the direct impedance fusing of generating heat.Meanwhile, magnetic field suspends melt or half suspension to the repulsion of melt, thereby realizes the effect that melt separates with crucible.But, the core that magnetic levitation cold crucible lifts technology relates to the cold crucible that catchments, ruhmkorff coil, shift mechanism etc. in the somewhat complex design of one and customization processing, waste time and energy, and versatility is poor, use inconvenience, often need change design just can be applied to different metal systems.This is the existing weak point of prior art.
Summary of the invention
Object of the present invention, be exactly for the existing deficiency of prior art, and provide a kind of technical scheme of the method and apparatus that lifts high activity metal monocrystalline, this scheme is used ortho-water cold crucible, lift technology in conjunction with arc melting and Czochralski, can solve that crucible pollutes melt and the technical problem of restriction to refractory metal, also there is somewhat complex design and the customization processing of avoiding crucible etc., versatility is good, equipment energy consumption is lower, heat temperature raising is fast, easy and simple to handle, and is easy to the features such as maintenance and repair.
This programme is achieved by the following technical measures: a kind of equipment that lifts high activity metal monocrystalline, includes crucible, arc gum, rotary pulling mechanism, atmosphere Controlling System, vacuum chamber; Crucible is arranged on the bottom of vacuum chamber; Rotary pulling mechanism is fixed on directly over crucible; Arc gum is symmetrically fixed on rotary pulling mechanism both sides and electric arc transmitting terminal is positioned at crucible top; Atmosphere Controlling System is communicated with vacuum chamber; Atmosphere Controlling System comprises and vacuumizes assembly and argon gas source of the gas; Choosing dress shift mechanism is the lifting head that can be moved up and down and rotate by motor-driven.
As this programme preferably: crucible is the cold-crucible of oxygen free copper material.
A method that lifts high activity metal monocrystalline, comprises the following steps:
A, after having been configured by required composition, raw metal puts into crucible;
The space in vacuum chamber is vacuumized rear injection argon gas by b, use atmosphere Controlling System;
C, use arc gum heat crucible burner hearth;
D, after raw metal fusing, fall the lifting head of rotary pulling mechanism, until lifting head promotes lifting head after immersing liquid metal again, complete the operation that lifts metal single crystal rod.
As this programme preferably: the composition of the raw metal described in step a is high pure metal raw material, and its purity is not less than 99.9%.
As this programme preferably: the purity of argon injecting in the vacuum chamber described in step b is not less than 99.999%, argon pressure is 0.98-1.15atm.
As this programme preferably: the top temperature of the crucible burner hearth described in step c is not higher than 3000 DEG C.
As this programme preferably: the travelling speed up and down of the lifting head described in steps d is 0.01-39mm/min; The rotating speed of described lifting head is 0-10r/min.
The beneficial effect of this programme can be learnt according to the narration to such scheme, due to this scheme to cold crucible etc. without particular design requirement, device simple structure, easy and simple to handle, be easy to maintenance and repair, and allow user's adjusting process parameter in the light of actual conditions easily, the pulling growth of realizing high activity metal monocrystalline that can be reliable and stable.
As can be seen here, the present invention compared with prior art, has outstanding substantive distinguishing features and progressive significantly, and the beneficial effect of its enforcement is also apparent.
Brief description of the drawings
Fig. 1 is the structural representation of a kind of equipment that lifts high activity metal monocrystalline of the present invention.
In figure, 1 is atmosphere Controlling System, and 2 is vacuum chamber, and 3 is arc chamber, and 4 is rotary pulling mechanism, 5 single crystal rod that are pulling growth, and 6 is metal melt, 7 is crucible.
Embodiment
For clearly demonstrating the technical characterstic of this programme, below by an embodiment, and in conjunction with its accompanying drawing, this programme is set forth.
Can find out by accompanying drawing, this programme is a kind of method that lifts high activity metal monocrystalline with electric arc cold crucible, is on the basis of the synthetic master alloy ingot of melting, to lift technology in conjunction with arc melting and Czochralski and the novel method that forms.Master alloy ingot adopts high pure metal raw material (purity is not less than 99.9%) by required one-tenth assignment system, is the homogeneity of ingredients of guarantee master alloy ingot, can melt back repeatedly.Master alloy ingot is positioned in cold crucible, and then closed furnace control atmosphere are wherein the high-purity argon gas of 1 atm left and right.Open electric arc, progressively increase flame current, master alloy ingot is all melted, and then start shift mechanism.Lifting head is immersed after melt, set pull rate and rotating speed, just the direct monocrystalline of pulling growth high activity metal.
The single crystal pulling method of the electric arc cold crucible that this programme provides, is applicable to the multiple high activity metal materials such as transition metal, rare earth metal and their alloy.
This programme is without cold crucible etc. is carried out to particular design, and device simple structure is easy and simple to handle, is easy to maintenance and repair, and allows user's adjusting process parameter in the light of actual conditions easily, the pulling growth of realizing high activity metal monocrystalline that can be reliable and stable.
This programme adopts the mode of electric-arc heating, compares with magnetic levitation cold crucible technology, and energy consumption is lower, and the speed of heat temperature raising is faster.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. an equipment that lifts high activity metal monocrystalline, is characterized in that: include crucible, arc gum, rotary pulling mechanism, atmosphere Controlling System, vacuum chamber; Described crucible is arranged on the bottom of vacuum chamber; Described rotary pulling mechanism is fixed on directly over crucible; Described arc gum is symmetrically fixed on rotary pulling mechanism both sides and electric arc transmitting terminal is positioned at crucible top; Described atmosphere Controlling System is communicated with vacuum chamber; Described atmosphere Controlling System comprises and vacuumizes assembly and argon gas source of the gas; Described choosing dress shift mechanism is the lifting head that can be moved up and down and rotate by motor-driven.
2. a kind of equipment that lifts high activity metal monocrystalline according to claim 1, is characterized in that: described crucible is the cold-crucible of oxygen free copper material.
3. a method that lifts high activity metal monocrystalline, is characterized in that: comprise the following steps:
A, after having been configured by required composition, raw metal puts into crucible;
The space in vacuum chamber is vacuumized rear injection argon gas by b, use atmosphere Controlling System;
C, use arc gum heat crucible burner hearth;
D, after raw metal fusing, fall the lifting head of rotary pulling mechanism, until lifting head promotes lifting head after immersing liquid metal again, complete the operation that lifts metal single crystal rod.
4. a kind of method that lifts high activity metal monocrystalline according to claim 3, is characterized in that: the composition of the raw metal described in described step a is high pure metal raw material, and its purity is not less than 99.9%.
5. a kind of method that lifts high activity metal monocrystalline according to claim 3, is characterized in that: the purity of argon injecting in the vacuum chamber described in described step b is not less than 99.999%, argon pressure is 0.98-1.15atm.
6. a kind of method that lifts high activity metal monocrystalline according to claim 3, is characterized in that: the top temperature of the crucible burner hearth described in described step c is not higher than 3000 DEG C.
7. a kind of method that lifts high activity metal monocrystalline according to claim 3, is characterized in that: the travelling speed up and down of the lifting head described in described steps d is 0.01-39mm/min; The rotating speed of described lifting head is 0-10r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410121375.3A CN103849926A (en) | 2014-03-28 | 2014-03-28 | Method and equipment for pulling high-activity metal monocrystalline |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410121375.3A CN103849926A (en) | 2014-03-28 | 2014-03-28 | Method and equipment for pulling high-activity metal monocrystalline |
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| CN103849926A true CN103849926A (en) | 2014-06-11 |
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| CN201410121375.3A Pending CN103849926A (en) | 2014-03-28 | 2014-03-28 | Method and equipment for pulling high-activity metal monocrystalline |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110629280A (en) * | 2019-10-29 | 2019-12-31 | 合肥科晶材料技术有限公司 | Crystal growth suspension pulling furnace |
| CN110644044A (en) * | 2019-11-05 | 2020-01-03 | 中国工程物理研究院材料研究所 | CeRu2Si2Four-arc pulling growth method of single crystal |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4087313A (en) * | 1975-11-28 | 1978-05-02 | Joseph Beril Milstein | Process and apparatus for preparation of single crystals and textured polycrystals |
| CN1060318A (en) * | 1991-10-30 | 1992-04-15 | 武汉工业大学 | Lift the method for rare-earth-iron monocrystalline with magnetic levitation cold crucible |
| CN2129766Y (en) * | 1991-09-27 | 1993-04-14 | 冶金工业部包头稀土研究院 | Smelting furnace for preparing lanthanum hexaborane single crystal zone |
| CN1267751A (en) * | 2000-03-30 | 2000-09-27 | 天津市半导体材料厂 | Vertical pulling and zone melting process of producing monocrystalline silicon |
| JP2006347834A (en) * | 2005-06-17 | 2006-12-28 | Tokuyama Corp | Method for producing metal fluoride single crystal |
| CN101469940A (en) * | 2007-12-26 | 2009-07-01 | 北京有色金属研究总院 | Annular region smelting furnace |
| CN101826385A (en) * | 2010-04-30 | 2010-09-08 | 中国科学院物理研究所 | Magnetic material with exchange bias effect and preparation method thereof |
| CN102168919A (en) * | 2011-04-14 | 2011-08-31 | 张森 | Induction cold crucible zone-refining equipment and method for preparing high-purity and hyperpure materials |
-
2014
- 2014-03-28 CN CN201410121375.3A patent/CN103849926A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4087313A (en) * | 1975-11-28 | 1978-05-02 | Joseph Beril Milstein | Process and apparatus for preparation of single crystals and textured polycrystals |
| CN2129766Y (en) * | 1991-09-27 | 1993-04-14 | 冶金工业部包头稀土研究院 | Smelting furnace for preparing lanthanum hexaborane single crystal zone |
| CN1060318A (en) * | 1991-10-30 | 1992-04-15 | 武汉工业大学 | Lift the method for rare-earth-iron monocrystalline with magnetic levitation cold crucible |
| CN1267751A (en) * | 2000-03-30 | 2000-09-27 | 天津市半导体材料厂 | Vertical pulling and zone melting process of producing monocrystalline silicon |
| JP2006347834A (en) * | 2005-06-17 | 2006-12-28 | Tokuyama Corp | Method for producing metal fluoride single crystal |
| CN101469940A (en) * | 2007-12-26 | 2009-07-01 | 北京有色金属研究总院 | Annular region smelting furnace |
| CN101826385A (en) * | 2010-04-30 | 2010-09-08 | 中国科学院物理研究所 | Magnetic material with exchange bias effect and preparation method thereof |
| CN102168919A (en) * | 2011-04-14 | 2011-08-31 | 张森 | Induction cold crucible zone-refining equipment and method for preparing high-purity and hyperpure materials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110629280A (en) * | 2019-10-29 | 2019-12-31 | 合肥科晶材料技术有限公司 | Crystal growth suspension pulling furnace |
| CN110644044A (en) * | 2019-11-05 | 2020-01-03 | 中国工程物理研究院材料研究所 | CeRu2Si2Four-arc pulling growth method of single crystal |
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Application publication date: 20140611 |
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