CN101635185B - Method for preparing Ni-W alloy base band with non/low magnetic cubic texture - Google Patents
Method for preparing Ni-W alloy base band with non/low magnetic cubic texture Download PDFInfo
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- CN101635185B CN101635185B CN2009100918915A CN200910091891A CN101635185B CN 101635185 B CN101635185 B CN 101635185B CN 2009100918915 A CN2009100918915 A CN 2009100918915A CN 200910091891 A CN200910091891 A CN 200910091891A CN 101635185 B CN101635185 B CN 101635185B
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Abstract
The invention belong to the field of metal base bands with high-temperature super conduction coating conductor textures. The method comprises the following steps: obtaining initial billet ingots by a powder metallurgy method, wherein the W element of initial billet is not uniformly distributed; processing the initial ingots by cold rolling and optimized high-temperature thermal treatment to obtain the metal base band by the diffusion of the W element from an core layer to an outer layer, wherein the obtained metal base band has high strength non/low magnetism and high cubic texture content and the W content of the obtained metal base band is 7-9.3at percent The method is simple and feasible, and the prepared Ni-W alloy base band has favorable surface quality and sharp cubic texture and can be directly used for extensionally growing transitional layers and superconductive layers; and meanwhile, the Ni-W alloy base band has no (low) magnetism in a liquid nitrogen temperature zone and high mechanical strength, and can meet and further improve the requirement of the YBCO coating conductor performance.
Description
Technical field
The present invention relates to the preparation method of a kind of nonmagnetic (or low magnetic) cubic texture nickel tungsten (Ni-W) alloy base band, belong to conductor of high-temperature superconductor coat texture metal base band technical field.
Background technology
Second generation conductor of high-temperature superconductor coat is since finding, because its good performance has been subjected to people and has paid close attention to widely.In the research of practicability, on the ductile metal base band of polycrystalline a kind of effective thinking with its epitaxial growth.The metal base band of preparation texture then is one of key that obtains the high-performance coating conductor.
At present, the material that is applied to coating conductor texture metal base band is mainly pure Ni and Ni alloy, and in the world wide, the Ni-5at.%W of hundred meter levels (Ni5W) alloying metal base band is commercially produced by number company.But because Ni5W alloy curie transition temperature is higher, when using down, 77K (coating conductor operation temperature area) still has ferromagnetism, the loss of can increasing exchanges in carrying the process of alternating current reduced the performance of coating conductor, and the mechanical strength of Ni5W metal base band remains further to be improved.This has all limited the practical application of coating conductor greatly.And the increase of W content can improve the mechanical strength of NiW alloy base band and the curie transition temperature that reduces base band greatly, when W content is 9.3%at.%, its Curie temperature is reduced to below the 77K, makes coating conductor eliminate A.C.power loss when (77K) uses under the temperature of its application.But along with the increase of W content, the stacking fault energy of alloy reduces gradually, makes the formation of cubic texture become very difficult.
Summary of the invention
The purpose of this invention is to provide a kind of preparation high strength, nonmagnetic (low magnetic), that the surface has is high 001}＜100〉and cubic texture, can be used for the method for the NiW alloy base band of subsequently epitaxial growing oxide process layer and superconducting layer.
The present invention obtains the initial billet of W element uneven distribution by adopting powder metallurgic method, through cold rolling and optimization high-temperature heat treatment, by the W element by sandwich layer to the skin diffusion high strength that to obtain surperficial W content be 7～9.3at.%, do not have the metal base band of (low) magnetic and high cubic texture content, specifically may further comprise the steps:
1) in protective atmosphere, be 99.9% Ni powder and purity after to be 99.9% W powder according to the W atom account for 9%～12% of Ni atom and W total atom number and mix with purity, ball milling 2～4h obtains high W alloy powder; In protective atmosphere, be 99.9 Ni powder and purity after to be 99.9 W powder according to the W atom account for 5%～7% of Ni atom and W total atom number and mix with purity, ball milling 2～4h obtains low W alloy powder; High W alloy powder and low W alloy powder packed into according to the order of low W alloy powder-Gao W alloy powder-low W alloy powder suppress in the mould, the volume ratio of low W alloy powder-Gao W alloy powder-low W alloy powder is 1: 1～3: 1, and after discharge plasma sintering prepares initial billet, sintering temperature is 800-1000 ℃, sintering time 3-8min;
2) initial billet is carried out cold rolling, pass deformation is less than 5%, and total deformation finally obtains the cold rolling base band that 50 μ m～100 μ m are thick greater than 99%;
3) cold rolling base band is carried out stepped thermal treatment in protective atmosphere; the low temperature forming core heat treatment of at first carrying out 30min between 650 ℃～750 ℃ preferentially forms a cube nucleus; rising to the cubic grain that carries out 30min～60min between 1100 ℃～1200 ℃ then grows up and temperature is risen to the solute DIFFUSION TREATMENT of carrying out 60min～240min between 1300 ℃～1450 ℃ after the heat treatment; the W atom is fully spread, the N-Wi alloy base band of Ni-W alloy, high strength, nothing (low) magnetic and sharp keen cubic texture that to obtain outer W atomic percentage conc be 7～9.3at.%.
Wherein, described protective atmosphere is Ar and H
2Mist, H in the mist
2Volume fraction be 4%.
Core technology of the present invention is that the characteristics of at first utilizing the outer NiW alloy that hangs down W content to form cubic texture easily at first form sharp keen cubic texture in heat treatment process, thereby by the method for solute diffusion the W atom diffusion in the interior floor height W layer to skin being hanged down the W layer through the high-temperature heat treatment of higher temperature or long period then increases outer W content, reduce the magnetic property of base band integral body, and guarantee outer field cubic texture content.Another core technology of the present invention is the volume ratio of control ectonexine alloy powder, and the thickness of outer layer alloys directly influences the technology of internal layer W elemental diffusion efficient and follow-up solute diffusion heat treatments.Skin is too thick, and solute diffuses to skin needs heat treatment temperature higher or the time is longer, and the base band surface is formed hot corrosion, is unfavorable for the growth of follow-up extension transition zone; Skin is too thin, can influence the formation of outer cubic texture in the grow up diffusion of internal layer W atom in period of outer cubic texture forming core.Therefore should take into account initial billet ectonexine ratio and solute diffusion heat treatments technology simultaneously.
The present invention has following beneficial effect:
With the high W content of existing employing warm-rolling prepared (＞7at.%) Ni-W alloy base band technology is compared, the Ni-W alloy base band of the inventive method preparation has favorable surface quality and sharp keen cubic texture, directly epitaxial growth transition zone and superconducting layer.Simultaneously, can satisfy further raising YBCO coating conductor performance demands because this kind Ni-W alloy base band has does not have (low) magnetic at liquid nitrogen temperature and have very high mechanical strength; Compare with warm-rolling simultaneously and adopt cold rolling rolling mode, can simplify rolling mill practice and realize industrialization easily.
Description of drawings
Cold rolling base band cross section back scattering figure among Fig. 1, the embodiment 1.
(111) utmost point figure of base band among Fig. 2, the embodiment 1.
Cold rolling base band cross section back scattering figure among Fig. 3, the embodiment 2,3.
(111) utmost point figure of base band among Fig. 4, the embodiment 2.
(111) utmost point figure of base band among Fig. 5, the embodiment 3.
The present invention will be further described below in conjunction with the drawings and the specific embodiments.
Embodiment
Embodiment 1
1) at protective atmosphere (Ar-4%H
2) in, be that 99.9 Ni powder and purity be 99.9 W powder according to Ni atom and W atomic ratio are 95: 5 and 91: 9 ball milling 3h respectively with purity, obtain high W alloy powder and low W alloy powder; High W alloy powder and low W alloy powder packed into according to the order of the low W of the low high W-of W-suppress in the mould, the volume ratio of low W alloy powder-Gao W alloy powder-low W alloy powder is 1: 3: 1, then adopt discharge plasma sintering technique at 800 ℃ of sintering 5min, obtain preparing initial billet;
2) initial billet is carried out cold rolling, pass deformation is 5%, and total deformation is 99%, finally obtains the thick cold rolling base band (see figure 1) of 75 μ m;
3) with cold rolling base band at protective atmosphere (Ar-4%H
2) in carry out stepped thermal treatment, at first 650 ℃ the insulation 30min, be warming up to then 1100 ℃ the insulation 30min after with temperature rise to 1450 ℃ the insulation 60min, obtain Ni-W alloy base band with non/low magnetic cubic texture.
Outer W atomic percentage conc in base band is 7%, its (111) face utmost point figure sees Fig. 2, and cubic texture content is 99%, because base band makes top layer W content bring up to 7% from 5% through DIFFUSION TREATMENT, greatly reduce the magnetic property of base band integral body, guaranteed higher cubic texture content simultaneously.
Embodiment 2
1) at protective atmosphere (Ar-4%H
2) in, be that 99.9 Ni powder and purity be 99.9 W powder according to Ni atom and W atomic ratio are 93: 7 and 89: 11 ball milling 2h respectively with purity, obtain high W alloy powder and low W alloy powder; High W alloy powder and low W alloy powder packed into according to the order of the low W of the low high W-of W-suppress in the mould, the volume ratio of low W alloy powder-Gao W alloy powder-low W alloy powder is 1: 1: 1, then adopt discharge plasma sintering technique at 800 ℃ of sintering 5min, obtain preparing initial billet;
2) initial billet is carried out cold rolling, pass deformation is 5%, and total deformation is 99%, finally obtains the thick cold rolling base band (see figure 3) of 75 μ m;
3) with cold rolling base band at protective atmosphere (Ar-4%H
2) in carry out stepped thermal treatment, at first 700 ℃ the insulation 30min, be warming up to then 1200 ℃ the insulation 60min after with temperature rise to 1400 ℃ the insulation 180min, obtain Ni-W alloy base band with non/low magnetic cubic texture.
The outer W atomic percentage conc of this base band is 8%, its (111) face utmost point figure sees Fig. 4, and cubic texture content is 99%, because base band makes top layer W content bring up to 8.7% from 7% through DIFFUSION TREATMENT, greatly reduce the magnetic property of base band integral body, guaranteed higher cubic texture content simultaneously.
Embodiment 3
1) at protective atmosphere (Ar-4%H
2) in, be that 99.9 Ni powder and purity be 99.9 W powder according to Ni atom and W atomic ratio are 93: 7 and 88: 12 ball milling 4h respectively with purity, obtain high W alloy powder and low W alloy powder; High W alloy powder and low W alloy powder packed into according to the order of the low W of the low high W-of W-suppress in the mould, the volume ratio of low W alloy powder-Gao W alloy powder-low W alloy powder is 1: 1: 1, then adopt discharge plasma sintering technique at 800 ℃ of sintering 5min, obtain preparing initial billet;
2) initial billet is carried out cold rolling, pass deformation is 5%, and total deformation is 99%, finally obtains the thick cold rolling base band (see figure 3) of 75 μ m;
3) with cold rolling base band at protective atmosphere (Ar-4%H
2) in carry out stepped thermal treatment, at first 700 ℃ the insulation 30min, be warming up to then 1200 ℃ the insulation 60min after with temperature rise to 1400 ℃ the insulation 180min, obtain Ni-W alloy base band with non/low magnetic cubic texture.
The outer W atomic percentage conc of this base band is 9%, its (111) face utmost point figure sees Fig. 5, as seen formed sharp keen cubic texture on its surface, because base band makes top layer W content bring up to 9% from 7% through DIFFUSION TREATMENT, the curie transition temperature of base band has been dropped to below the 77K, eliminate the A.C.power loss of coating conductor in the transmission of electricity process, guaranteed higher cubic texture content simultaneously, helped the growth of follow-up epitaxial film.
Claims (2)
1. the preparation method of a Ni-W alloy base band with non/low magnetic cubic texture is characterized in that, may further comprise the steps:
1) in protective atmosphere, be 99.9% Ni powder and purity after to be 99.9% W powder according to the W atom account for 9%～12% of Ni atom and W total atom number and mix with purity, ball milling 2～4h obtains high W alloy powder; In protective atmosphere, be 99.9 Ni powder and purity after to be 99.9 W powder according to the W atom account for 5%～7% of Ni atom and W total atom number and mix with purity, ball milling 2～4h obtains low W alloy powder; High W alloy powder and low W alloy powder packed into according to the order of low W alloy powder-Gao W alloy powder-low W alloy powder suppress in the mould, the volume ratio of low W alloy powder-Gao W alloy powder-low W alloy powder is 1: 1～3: 1, and after discharge plasma sintering prepares initial billet, sintering temperature is 800-1000 ℃, sintering time 3-8min;
2) initial billet is carried out cold rolling, pass deformation is less than 5%, and total deformation finally obtains the cold rolling base band that 50 μ m～100 μ m are thick greater than 99%;
3) cold rolling base band is carried out stepped thermal treatment in protective atmosphere; at first at 650 ℃～750 ℃ insulation 30min; after being warming up to 1100 ℃～1200 ℃ insulation 30min～60min then temperature is risen to 1300 ℃～1450 ℃ insulation 60min～240min, obtain Ni-W alloy base band with non/low magnetic cubic texture.
2. method according to claim 1 is characterized in that, described protective atmosphere is Ar and H
2Mist, in the mist, H
2Percent by volume be 4%.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101850422B (en) * | 2010-04-30 | 2011-11-16 | 北京工业大学 | Ni-base alloy composite base band prepared by hot isostatic pressing method |
| CN102329973B (en) * | 2011-09-21 | 2013-04-17 | 西安理工大学 | Preparation method for Ni-W alloy by using smelting method |
| CN102500638B (en) * | 2011-11-24 | 2014-07-23 | 北京工业大学 | Method for producing high-cube-texture high-tungsten-content NI (nickel)-W (tungsten) alloy substrate bands |
| CN103496205B (en) * | 2013-09-17 | 2015-12-09 | 河南师范大学 | A kind of nonmagnetic, strength texture Cu base alloy composite baseband and preparation method thereof |
| CN103639200B (en) * | 2013-11-17 | 2015-12-02 | 北京工业大学 | A kind of milling method of NiW alloy base belt for coated conductor |
| CN103658172B (en) * | 2013-12-09 | 2015-05-13 | 北京工业大学 | Rolling method of hectometer-level Ni-5at.%W alloy base band used for coated conductor |
| CN105200258A (en) * | 2015-08-11 | 2015-12-30 | 无锡桥阳机械制造有限公司 | Method for preparing sintered nickel alloy material |
| CN106180742B (en) * | 2016-07-16 | 2017-11-07 | 北京工业大学 | A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders |
| CN106077642B (en) * | 2016-07-16 | 2018-10-12 | 北京工业大学 | A kind of method of alloy nano-powder prepares coating conductor high-tungsten alloy base band billet |
| CN106111987B (en) * | 2016-07-16 | 2018-10-12 | 北京工业大学 | A kind of method of alloy powder prepares coating conductor NiW alloy base band billets |
| CN106399756B (en) * | 2016-08-31 | 2018-05-08 | 河南师范大学 | A kind of preparation method of high-performance cubic texture nickel-base alloy base band |
| CN109536907B (en) * | 2018-12-27 | 2020-09-22 | 河南城建学院 | High-strength strong-cube-texture layered composite baseband and preparation method thereof |
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Inventor after: Suo Hongli Inventor after: Gao Mangmang Inventor after: Gao Peikuo Inventor after: Zhao Yue Inventor after: Ma Lin Inventor after: Wang Jianhong Inventor after: Liu Min Inventor after: Qiu Huoqin Inventor before: Gao Mangmang Inventor before: Suo Hongli Inventor before: Gao Peikuo Inventor before: Zhao Yue Inventor before: Ma Lin Inventor before: Wang Jianhong Inventor before: Liu Min Inventor before: Qiu Huoqin |
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Free format text: CORRECT: INVENTOR; FROM: GAO MANGMANG SUO HONGLI GAO PEIKUO ZHAO YUE MA LIN WANG JIANHONG LIU MIN QIU HUOQIN TO: SUO HONGLI GAO MANGMANG GAO PEIKUO ZHAO YUE MA LIN WANG JIANHONG LIU MIN QIU HUOQIN |
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Granted publication date: 20110112 Termination date: 20160828 |