CN1861388A - Method for preparing high-temp. superconductive composite Ni alloy base belt - Google Patents
Method for preparing high-temp. superconductive composite Ni alloy base belt Download PDFInfo
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- CN1861388A CN1861388A CN 200610066447 CN200610066447A CN1861388A CN 1861388 A CN1861388 A CN 1861388A CN 200610066447 CN200610066447 CN 200610066447 CN 200610066447 A CN200610066447 A CN 200610066447A CN 1861388 A CN1861388 A CN 1861388A
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- 239000002131 composite material Substances 0.000 title claims abstract description 72
- 229910000990 Ni alloy Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims description 16
- 238000000137 annealing Methods 0.000 claims abstract description 55
- 239000000843 powder Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 229910001080 W alloy Inorganic materials 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 12
- 239000002887 superconductor Substances 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 28
- 238000001953 recrystallisation Methods 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 22
- 238000003825 pressing Methods 0.000 claims description 16
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 239000011651 chromium Substances 0.000 claims description 10
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 7
- 229910000756 V alloy Inorganic materials 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 5
- 238000004663 powder metallurgy Methods 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 abstract description 89
- 230000005291 magnetic effect Effects 0.000 abstract description 23
- 238000005097 cold rolling Methods 0.000 abstract description 22
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 abstract description 21
- 229910052759 nickel Inorganic materials 0.000 abstract description 8
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 70
- 238000005275 alloying Methods 0.000 description 35
- 239000000463 material Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 13
- 238000005096 rolling process Methods 0.000 description 9
- 238000007599 discharging Methods 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 229910001004 magnetic alloy Inorganic materials 0.000 description 2
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
A composite Ni alloy band used as the substrate for depositing high-temp superconductor YBCO film on it is composed of a low-W surficial Ni-W alloy layer and non-magnetic lower or middle alloy layer. It is prepared through mixing Ni, W, Cr and V powders, sequentially loading in mould, sintering, cold rolling, recrystallizing in the mixture of Ar gas and H2, and annealing.
Description
Technical field
The present invention relates to a kind of preparation method of MULTILAYER COMPOSITE polycrystalline Ni alloy base band, belong to the technical field of high-temperature superconducting coating tenacity strip and superconducting thin film preparation.
Background technology
With Bi is that superconducting tape is compared, YBa
2Cu
3O
7-δBe called for short the ability that the YBCO superconductor possesses the bigger electric current of carrying in magnetic field, boundless in the liquid nitrogen temperature application prospect.It is the important step that realizes its practical application that the fragility high temperature superconducting materia is made line, band.In recent years, the deposition superconducting film had been obtained very big progress with the research of preparation line, band on the employing polycrystalline ductile metal base band, had successfully prepared high performance YBCO coating conductor.But the TEXTURE STATE of base band directly has influence on the TEXTURE STATE of epitaxially grown superconducting film thereon, and influences the electrical property of superconduction, so TEXTURE STATE is extremely important to the base band material.
Pure nickel is a kind of base band material that is widely used.This is because pure nickel has good working performance, drastic deformation and annealing back are very easy to form strong cubic texture (100)＜100 〉, being most nickel crystallites is parallel to the face that rolls of base band with (100) face, again with＜100〉direction is parallel to the rolling direction of base band.But the intensity of pure nickel is not high, and mechanical performance is relatively poor; Be ferromagnetism under the normal temperature, its Curie temperature is 627K, makes the application of YBCO coating conductor in the highfield meet difficulty, such as Magnetic resonance imaging etc.; And because the effect of magnetic hystersis loss, the pure nickel base band can cause energy loss in AC applications.
The alloying of nickel is to solve the not high and ferromagnetic effective way of removal of pure nickel intensity, and wherein nickel tungsten has obtained paying close attention to widely.The Ni-W alloy base band possesses following advantage: strong cubic texture occurs after (1) violent cold rolling and recrystallization annealing; (2) strength of materials improves, and mechanical performance is better; (3) with other Ni alloy phase ratios better non-oxidizability is arranged, such as Ni-Cr, Ni-V, Ni-Fe.Therefore, the Ni-W base band be easier to commercially produce can be in liquid nitrogen temperature 77K and magnetic field the HTS YBCO band of bearing great current.
As the backing material of YBCO, the Ni-W base band had both required to have very strong cubic texture, required to have alap magnetic at liquid nitrogen temperature again.According to nickel tungsten binary phase diagraml and bibliographical information, during when the atomic percent arrival of W in the Ni-W alloy or above about 9at.%, promptly the Ni-9at%W base band can reach nonmagnetic at liquid nitrogen temperature.But as long as W content in the Ni-W alloy atomic percent above about 5% o'clock, the cubic texture intensity of alloy base band just sharply descends, and the cubic texture intensity on surface is not high, just can not adopt epitaxially grown method preparation to have the YBCO superconducting film of high electrical performance thereon.Can't still not have successfully preparation at present in the world and have the very report of strong cubic texture Ni-9at%W alloy base band, promptly both had very strong cubic texture, nonmagnetic again.
So, just have the scholar to carry out the research of composite baseband.It is lower to allow the superficial layer of base band contain the W amount, thereby makes the surface can form cubic texture; Non-magnetic alloy is adopted in the intermediate layer, reduces the magnetic of whole base band like this.The composite baseband that so obtains, surface have very strong cubic texture, can satisfy the epitaxially grown needs of YBCO superconducting film, and whole magnetic is lower again.Document " V.Subramanya Sarma et.al, Acta Material 51 (2003) 4919-4927 " was once reported: adopt the method for composite baseband to prepare the Ni-W alloy base band.Promptly elder generation prepares long rod of Ni-4.5at%W alloy and the little pole of non-magnetic Ni-15atCr% alloy with the method for melting, in the long rod of Ni-4.5at%W alloy, go out a hole along excellent length direction machining, the little pole of Ni-15atCr% alloy is inserted in the hole, carry out follow-up rolling, heat treatment again, obtaining the surface is three layers of composite strip of non-magnetic Ni-15atCr% for the Ni-4.5at%W of cubic texture, core.This composite baseband surface has cubic texture, can satisfy the epitaxially grown needs of YBCO superconducting film, and magnetic is lower again simultaneously.But the process for preparing composite baseband with the method is very complicated; Because two kinds of alloys are to adopt the way of machinery to be combined with each other, the joint portion separates easily in addition; And the alloy that can only adopt two kinds of percentage elongation to equate substantially carries out compound, otherwise can give the follow-up rolling very big difficulty of bringing.
Summary of the invention
The present invention adopts powder metallurgy process to prepare MULTILAYER COMPOSITE Ni alloy base band, only needs colded pressing powder and high temperature sintering of layering can obtain the blank of composite Ni alloy.Blank is rolled and recrystallization annealing, can obtains meeting the composite strip of plated film requirement.Multilayer Ni alloy sheets can be compound the Ni alloy of two-layer or multilayer, preparation process is comparatively simple, and layer with layer between what form in powder metallurgy process is metallurgical binding, even follow-up rolling reduction reaches 99.9%, can not separate between each layer yet.
The invention provides a kind of preparation method who is used for the composite Ni alloy base band of high-temperature superconductor, it is characterized in that it may further comprise the steps successively:
1) structure of elder generation's design composite band: the number of plies of composite band is two-layer or multilayer; For having only two-layer composite band, upper strata up and down altogether is the nickel tungsten of tungstenic 3～7at.%; Lower floor is that W content is the Ni-W alloy of 9～20at.%, the Ni-Cr alloy of chromium content 8～20at.% or the Ni-V alloy thrin of content of vanadium 8～20at.%; The composition of three layers of composite band and structure are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, intermediate layer are that W content is Ni-W alloy or the Ni-Cr alloy of chromium content 8～20at.% or the Ni-V alloy thrin of content of vanadium 8～20at.% of 9～20at.%; The composition and the structure that surpass three layers composite band are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, innermost layer is that W content is the Ni-W alloy of 9～20at.%, the intermediate layer is the nickel tungsten composition transition zone of tungstenic 6～12at.%, be that desurfacing and innermost layer intermediate layer in addition is the composition transition zone, reduce gradually from innermost layer toward superficial layer direction W content;
2) use Ni powder, W powder, Cr powder and V powder to be raw material, purity is weight percentage more than 99.9%, and granularity is 1～10 micron; Nickel powder is evenly mixed with alloy powder, then set by step 1) structure of the composite band of the design powder of different proportionings of in mould, packing into successively in, carry out adopting powder metallurgy sintered method to sinter the composite Ni alloy plate into behind the layering pressing mold, sintering temperature is 800 ℃～1400 ℃, is incubated 3 minutes～30 hours;
3) at room temperature above-mentioned composite Ni alloy plate is carried out cold rollingly, pass deformation is 5～15%, and total deformation is greater than 96%;
4) adopt H
2Percent by volume be 4～7% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 800～1400 ℃ of annealing temperatures, and annealing time is 0.5～3 hour.
The present invention prepares MULTILAYER COMPOSITE Ni alloy blank by powder metallurgy process, has the advantages that composition is even, each interfacial bonding strength is high, makes preparation process simplification and rapid simultaneously.For adopting this method to prepare MULTILAYER COMPOSITE Ni alloy blank both at home and abroad first.
The structural design of composite band is two-layer or the composite band of multilayer.The simplest for having only two-layer composite tape structure up and down altogether, the upper strata is the nickel tungsten of tungstenic 3～7at.%, and the content of W is lower, is strong cubic texture to guarantee what obtain through deformation and annealing in process rear surface; Lower floor is for being the Ni-W alloy of 9～20at.%, the Ni-Cr alloy of chromium content 8～20at.% or the Ni-V alloy of content of vanadium 8～20at.% at the non-magnetic W content of liquid nitrogen temperature, to reduce the magnetic of whole base band.The composition of three layers of composite band and structure are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, intermediate layer are that the non-magnetic W content of liquid nitrogen temperature is a kind of among the Ni-V alloy three of the Ni-Cr alloy of Ni-W alloy, chromium content 8～20at.% of 9～20at.% and content of vanadium 8～20at.%.The composition and the structure that surpass three layers composite band are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, innermost layer is that the non-magnetic W content of liquid nitrogen temperature is the Ni-W alloy of 9～20at.%, intermediate layer beyond desurfacing and the innermost layer is the composition transition zone, reduces gradually from innermost layer toward superficial layer direction W content.
The compound process that adopts among the present invention is two-layer or multilayer, and its central idea all is to contain the lower nickel tungsten of W amount in order to use at superficial layer, thereby guarantees that the surface can form cubic texture; Non-magnetic alloy is adopted in lower floor or intermediate layer, reduces the magnetic of whole base band like this.The composite baseband that so obtains, surface have very strong cubic texture, can satisfy the epitaxially grown needs of YBCO superconducting film, and whole magnetic is lower again.The number of plies is many more, and the preparation formality of base band is complicated more, but because the composition transition between each layer comparatively delays, so interlayer is tightr in conjunction with meeting, even rolling mill practice is not too accurate in follow-up rolling deformation process, also can not cause consequences such as cracking.Certainly for the simplification of both considering the base band preparation, consider that again base band has low magnetic, three layers is only.More careful in the time of two-layer base band rolling deformation, guarantee rolling reduction＜10% of per pass, but the magnetic of two-layer base band is minimum.
To control its deformation and recrystallization annealing process to the Ni-W composite alloy blank that adopts the powder research method to make, obtain certain deformation texture comprising controlled rolling total deformation and every time deflection.Wherein, pass deformation forms twin too greatly easily in the Ni-W band, be unfavorable for the acquisition of single-orientated texture.Through our research, pass deformation is 5～15% suitable.And total deformation need be greater than 96%, otherwise texture is concentrated inadequately.
Adopt certain recrystallization annealing temperature, annealing atmosphere and annealing time then, can obtain the surface and have very strong (100)＜100 crystallization cubic texture and whole base band have the polycrystalline composite Ni alloy base band of low magnetic again.
Through system research, we have obtained two-layer and composite Ni alloy base band multilayer, and the surface all has very strong cubic texture, and magnetic is lower again, can be used to deposit the YBCO high temperature superconducting film.
Description of drawings:
The structure chart of two-layer composite Ni alloy blank Ni-3at.%W/Ni-9at.%W among Fig. 1: the embodiment 1;
Among Fig. 2: the embodiment 1 annealed state composite Ni alloy base band Ni-3at.%W/Ni-9at.%W (111) (a), (200) (b) utmost point figure;
The M-H loop of annealed state composite Ni alloy base band Ni-3at.%W/Ni-9at.%W and Ni-5at.%W base band among Fig. 3: the embodiment 1;
The structure chart of three layers of composite Ni alloy blank Ni-5at.%W/Ni-10at.%W/Ni-5at.%W among Fig. 4: the embodiment 2;
Among Fig. 5: the embodiment 2 annealed state composite Ni alloy base band Ni-5at.%W/Ni-10at.%W/Ni-5at.%W (111) (a), (200) (b) utmost point figure;
The M-H loop of annealed state composite Ni alloy base band Ni-5at.%W/Ni-10at.%W/Ni-5at.%W and Ni-5at.%W base band among Fig. 6: the embodiment 2;
Among Fig. 7: the embodiment 3 three layers of composite Ni alloy base band of annealed state Ni-5at.%W/Ni-8at.%Cr/Ni-5at.%W (111) (a), (200) (b) utmost point figure;
Among Fig. 8: the embodiment 4 three layers of composite Ni alloy base band of annealed state Ni-5at.%W/Ni-20at.%Cr/Ni-5at.%W (111) (a), (200) (b) utmost point figure;
The M-H loop of annealed state composite Ni alloy base band Ni-5at.%W/Ni-20at.%Cr/Ni-5at.%W and Ni-5at.%W base band among Fig. 9: the embodiment 4;
Among Figure 10: the embodiment 5 three layers of composite Ni alloy base band of annealed state Ni-5at.%W/Ni-8at.%V/Ni-5at.%W (111) (a), (200) (b) utmost point figure;
Among Figure 11: the embodiment 6 three layers of composite Ni alloy base band of annealed state Ni-7at.%W/Ni-20at.%V/Ni-7at.%W (111) (a), (200) (b) utmost point figure;
Five layers of composite Ni alloy base Ni-5at.%W/Ni-12at.%W/Ni-20at.%W/Ni-12at.%W/Ni-5at.%W structure chart among Figure 12: the embodiment 7;
Among Figure 13: the embodiment 7 (111) of five layers of composite Ni alloy Ni-5at.%W/Ni-10at.%W/Ni-20at.%W/Ni-10at.%W/Ni-5at.%W of annealed state base band (a), (200) (b) utmost point figure;
The structure chart of seven layers of composite Ni alloy blank Ni-3at.%W/Ni-6at.%W/Ni-12at.%W/Ni-20at.%W/Ni-12at.%W/Ni-6at.%W/Ni-3at.%W among Figure 14: the embodiment 8;
Among Figure 15: the embodiment 8 seven layers of composite Ni alloy base band of annealed state Ni-3at.%W/Ni-6at.%W/Ni-12at.%W/Ni-20at.%W/Ni-12at.%W/Ni-6at.%W/Ni-3at.%W (111) (a), (200) (b) utmost point figure;
Among Figure 16: the embodiment 9 annealed state composite Ni alloy base band Ni-7at.%W/Ni-20at.%W (111) (a), (200) (b) utmost point figure;
Among Figure 17: the embodiment 10 annealed state composite Ni alloy base band Ni-3at.%W/Ni-10at.%W/Ni-3at.%W (111) (a), (200) (b) utmost point figure;
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Example 1. as shown in Figure 1, this Ni alloy sheets structure is divided into two-layer, the alloying component on upper strata is Ni-3at.%W, the alloying component of lower floor is Ni-9at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.The powder of pressing Ni-3at.%W and two kinds of alloying component proportionings of Ni-9at.%W evenly after, the mould of packing into successively carries out pressing mold.Obtain the powder green compact of design shown in Figure 1 after the demoulding.Green compact are put into H
2Percent by volume be 7% Ar mixing H
2Carry out sintering in the stove of the atmosphere that flows, sintering temperature is 1400 ℃, is incubated 20 hours.Prepared density behind the sintering and be 97.8% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 96%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 900 ℃ of annealing temperatures, and annealing time is 1 hour.Fig. 2 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.Fig. 3 is the hysteresis loop M-H figure of this base band and Ni-5at.%W base band, as seen from the figure, compares with the Ni-5at.%W base band, and the magnetic of this composite baseband has significantly decline.
Example 2. as shown in Figure 4, this Ni alloy sheets structure is divided into three layers, the alloying component of levels is all Ni-5at.%W, the alloying component in intermediate layer is Ni-10at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold.Obtain powder green compact after the demoulding.Green compact are put into H
2Percent by volume be 7% Ar mixing H
2Carry out sintering in the stove of the mobile atmosphere of atmosphere, sintering temperature is 1200 ℃, is incubated 30 hours.Prepared density behind the sintering and be 98.3% composite Ni alloy base.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 97.2%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1100 ℃ of annealing temperatures, and annealing time is 2 hours.Fig. 5 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.Fig. 6 is the M-H figure of this base band and Ni-5at.%W base band, as seen from the figure, compares with the Ni-5at.%W base band, and the magnetic of this composite baseband has significantly decline.
Example 3. these Ni alloy sheets structures are divided into three layers, and the alloying component of levels is all Ni-5at.%W, and the alloying component in intermediate layer is Ni-8at.%Cr.Adopting Ni powder and Cr powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 900 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 98.1% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 99%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1200 ℃ of annealing temperatures, and annealing time is 1 hour.Fig. 7 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 4. these Ni alloy sheets structures are divided into three layers, and the alloying component of levels is all Ni-5at.%W, and the alloying component in intermediate layer is Ni-20at.%Cr.Adopting Ni powder and Cr powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 950 ℃, is incubated 5 minutes.Prepared density behind the sintering and be 98.3% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 98%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1400 ℃ of annealing temperatures, and annealing time is 0.5 hour.Fig. 8 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.Fig. 9 is the M-H figure of this base band and Ni-5at.%W base band, as seen from the figure, compares with the Ni-5at.%W base band, and the magnetic of this composite baseband has significantly decline.
Example 5. these Ni alloy sheets structures are divided into three layers, and the alloying component of levels is all Ni-5at.%W, and the alloying component in intermediate layer is Ni-8at.%V.Adopting Ni powder and V powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 920 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 98.2% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 98.5%; Adopt H
2Percent by volume be 5% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1200 ℃ of annealing temperatures, and annealing time is 2 hours.Figure 10 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 6. these Ni alloy sheets structures are divided into three layers, and the alloying component of levels is all Ni-7at.%W, and the alloying component in intermediate layer is Ni-20at.%V.Adopting Ni powder and V powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 970 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 98.4% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 98%; Adopt H
2Percent by volume be 5% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1300 ℃ of annealing temperatures, and annealing time is 3 hours.Figure 11 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had stronger (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 7. as shown in figure 12, this Ni alloy sheets structure is divided into five layers, the alloying component of levels is all Ni-5at.%W, the alloying component of innermost layer is Ni-20at.%W, the alloying component in intermediate layer is Ni-10at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 970 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 98.3% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 97.5%; Adopt H
2Percent by volume be 7% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1200 ℃ of annealing temperatures, and annealing time is 2 hours.Figure 13 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 8. as shown in figure 14, this Ni alloy sheets structure is divided into seven layers, the alloying component of levels is all Ni-3at.%W, the alloying component of innermost layer is Ni-20at.%W, the alloying component in intermediate layer is respectively Ni-6at.%W and Ni-12at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 970 ℃, is incubated 5 minutes.Prepared density behind the sintering and be 97.4% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 97%; Adopt H
2Percent by volume be 7% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1100 ℃ of annealing temperatures, and annealing time is 2 hours.Figure 15 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 9. these Ni alloy sheets structures are divided into two-layer, and the alloying component on upper strata is Ni-7at.%W, and the alloying component of lower floor is Ni-20at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.The powder of pressing Ni-7at.%W and two kinds of alloying component proportionings of Ni-20at.%W evenly after, by alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 1000 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 98.2% composite Ni alloy billet.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 96%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1300 ℃ of annealing temperatures, and annealing time is 1 hour.Figure 16 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Example 10. these Ni alloy sheets structures are divided into three layers, and the alloying component of levels is all Ni-3at.%W, and the alloying component in intermediate layer is Ni-10at.%W.Adopting Ni powder and W powder is raw material, and purity is weight percentage 99.9%, and granularity is 1～10 micron.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold.By alloying component prepare powder evenly after, the mould of packing into successively carries out pressing mold, puts into discharging plasma sintering equipment then and carries out sintering, sintering temperature is 900 ℃, is incubated 3 minutes.Prepared density behind the sintering and be 97.9% composite Ni alloy base.At room temperature alloy block is carried out cold rolling and recrystallization annealing, cold rolling pass deformation is 5～10%, and total deformation is 96.8%; Adopt H
2Percent by volume be 4% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 1000 ℃ of annealing temperatures, and annealing time is 3 hours.Figure 17 is its upper surface (111) and (200) utmost point figure.Obtained upper surface and had very strong (100)＜100 strip of texture, can be used for the preparation of follow-up YBCO coating superconducting material.
Claims (1)
1, a kind of preparation method who is used for the composite Ni alloy base band of high-temperature superconductor is characterized in that it may further comprise the steps successively:
1) structure of elder generation's design composite band: the number of plies of composite band is two-layer or multilayer; For having only two-layer composite band, upper strata up and down altogether is the nickel tungsten of tungstenic 3～7at.%; Lower floor is that W content is the Ni-W alloy of 9～20at.%, the Ni-Cr alloy of chromium content 8～20at.% or the Ni-V alloy thrin of content of vanadium 8～20at.%; The composition of three layers of composite band and structure are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, intermediate layer are that W content is Ni-W alloy or the Ni-Cr alloy of chromium content 8～20at.% or the Ni-V alloy thrin of content of vanadium 8～20at.% of 9～20at.%; The composition and the structure that surpass three layers composite band are: the two-layer up and down nickel tungsten that is all tungstenic 3～7at.%, innermost layer is that W content is the Ni-W alloy of 9～20at.%, the intermediate layer is the nickel tungsten composition transition zone of tungstenic 6～12at.%, be that desurfacing and innermost layer intermediate layer in addition is the composition transition zone, reduce gradually from innermost layer toward superficial layer direction W content;
2) use Ni powder, W powder, Cr powder and V powder to be raw material, purity is weight percentage more than 99.9%, and granularity is 1～10 micron; Nickel powder is evenly mixed with alloy powder, then set by step 1) structure of the composite band of the design powder of different proportionings of in mould, packing into successively in, carry out adopting powder metallurgy sintered method to sinter the composite Ni alloy plate into behind the layering pressing mold, sintering temperature is 800 ℃～1400 ℃, is incubated 3 minutes～30 hours;
3) at room temperature above-mentioned composite Ni alloy plate is carried out cold rollingly, pass deformation is 5～15%, and total deformation is greater than 96%;
4) adopt H
2Percent by volume be 4～7% Ar mixing H
2Atmosphere is carried out recrystallization annealing, 800～1400 ℃ of annealing temperatures, and annealing time is 0.5～3 hour.
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