CN101414497A - Method for continuously preparing two-sided texture high-temperature superconduction bibasic strip transition layer - Google Patents

Method for continuously preparing two-sided texture high-temperature superconduction bibasic strip transition layer Download PDF

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CN101414497A
CN101414497A CNA2008100465605A CN200810046560A CN101414497A CN 101414497 A CN101414497 A CN 101414497A CN A2008100465605 A CNA2008100465605 A CN A2008100465605A CN 200810046560 A CN200810046560 A CN 200810046560A CN 101414497 A CN101414497 A CN 101414497A
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colloid
temperature
base band
transition layer
preparing
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雷鸣
赵勇
蒲明华
张红
李果
程翠华
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Southwest Jiaotong University
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Abstract

The invention discloses a method for continuously preparing a second generation high-temperature superconducting tape transition layer with double-side texture. The method comprises the following steps: cerous nitrate or rare-earth nitrate is dissolved in N,N-dimethylformamide (DMF) to obtain precursor solution; polyacrylic acid (PPA) or polymethacrylic acid is added to the precursor solution to prepare colloid; Ni alloy base band is wound to pass through the prepared colloid, and after the base band is taken out, the colloid is evenly dipped and coated on the surface of the base band and then dried; and finally, the base band is placed in a sintering furnace for molding. The method helps realize the continuous preparation and the high preparation efficiency of the high-temperature superconducting transition layer, and is suitable for mass industrialized production; meanwhile, the prepared double-side tape transition layer film has the advantages of good consistency, good evenness, high degree of orientation and high surface smoothness; and the critical thickness of the transition layer is thick.

Description

A kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer
Technical field
The present invention relates to high-temperature superconductor two generations band preparing technical field, especially the technology of preparing of high-temperature superconductor two bibasic strip transition layers.
Background technology
Superconductor technology will become the core technology in this century as the environmental protection characteristic of energy-conservation ultimate technology and height.And high performance superconducting tape will be the key point that superconductor technology realizes large-scale application.Bi in 1986 2Sr 2Ca 2Cu 3O 10(Bi2223) discovery of system first generation belt material of high temperature superconduct has caused the upsurge of research in the world wide, and has realized commercially producing, and has promoted the development of superconduction forceful electric power application technology.But Bi series superconducting material intrinsic property physically limits its range of application greatly, and secondly owing to need a large amount of silver as sheath material, cost is limited.Therefore, development in recent years is slow, is abroad abandoning substantially aspect research, the production.REBa 2Cu 3O xThe second generation belt material of high temperature superconduct of (be called for short REBCO, RE is yttrium or lanthanide series) system, because the advantage of self, irreversible high (7T), high current capacity (10 5～10 7Acm -2), low A.C.power losss etc. have caused people's very big interest.
The superconducting layer composition of high-temperature superconductor two generations band is REBa 2Cu 3O x(being called for short REBCO).This high-temperature superconductor layer material is because the layer structure of itself causes extremely strong anisotropy, and the load current ability on the ab face of lattice is higher than the c direction of principal axis far away.The current-carrying performance of REBCO high temperature superconducting materia is also very responsive to the lattice mismatch on a, the b direction, and big lattice mismatch angle will form weak connection, has a strong impact on its current capacity.Studies show that the current capacity of REBCO is exponential damping with the increase at lattice mismatch angle on a, the b direction.Reduce lattice mismatch angle on a, the b direction, reduce weak joint efficiency, guarantee the current capacity of REBCO, extension has been configured to indispensable technical process in its technology of preparing.For practical application area such as superconducting tape, superconducting magnets, the REBCO high-temperature oxide superconducting material of fragility must be coated in could reduce on the good metal substrate of mechanical performance (intensity, toughness) avoid processing or use in mechanical damage.In addition, this backing material also need have good electrical conductivity and thermal conductivity, to avoid in the use because thrashing and collapse that local quench causes.Up to now, the best backing material of generally acknowledging both at home and abroad is the Ni base alloy material.Because there is certain lattice mismatch in the ab face of Ni base alloy and REBCO high temperature superconducting materia, directly epitaxial growth REBCO high temperature superconducting materia almost is impossible on the Ni base alloy baseband.Moreover, in the one-tenth phase heat treatment process of REBCO, having stronger counterdiffusion mutually and chemical reaction between Ni base alloy and the REBCO, this has just had a strong impact on the superconductivity of REBCO.Therefore, between Ni base alloy substrate and REBCO, must increase one deck buffer layer material, should serve as from Ni base alloy to the epitaxially grown intermediate die plate of REBCO, stop the phase counterdiffusion of two kinds of materials again, mainly be Ni with REBCO in the counterdiffusion mutually of Cu, could guarantee to prepare the REBCO conductor of high-temperature superconductor coat of function admirable like this.Therefore, belt material of high temperature superconduct all has substrate, transition zone (one deck at least) and REBCO superconducting coating three-decker.
Current, two generation superconducting tape research and development in, lacking reliable, cost performance band technology of preparing high, that be easy to promote is the bottleneck of restriction large-scale application.The longer the better for the second generation superconducting tape of requirement preparation on the one hand, simultaneously, in order to carry bigger current strength, the dual-face superconducting strip that just needs preparation two sides high conformity, and for industrialized demand, how preparing two-sided oxide transition zone on long base band fast continuously becomes the technical problem that urgent need solves.
Summary of the invention
The object of the present invention is to provide a kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer.This method can realize continuous preparation, the preparation efficiency height of high-temperature superconductor transition zone, is applicable to large-scale industrial production; The transition layer film consistency of the two-sided band of preparing simultaneously, good uniformity, degree of orientation height, surface smoothness height; The critical thickness of transition zone is thick.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of chemical solution deposition prepares the method for the transition zone of conductor of high-temperature superconductor coat, is made of following steps successively:
A, preparation of precursor solution: rare earth nitrades and cerous nitrate are pressed cation ratio M:Ce=x:1-x, the ratio of 0≤x≤0.5, be dissolved in N, in the dinethylformamide (DMF), form precursor aqueous solution, wherein M is a kind of among Y (yttrium), La (lanthanum), Pr (praseodymium), Nd (neodymium), Sm (samarium), Eu (europium), Gd (gadolinium), Tb (terbium), Dy (dysprosium), Ho (holmium), Er (erbium), Tm (thulium), Yb (ytterbium), Lu (lutetium), the Zr (zirconium);
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA) or polymethylacrylic acid (PMAA), form the colloid of good film-forming property;
C, film preparation and drying: go on foot Ni alloy base band coiling in the colloid that makes by b, vertically go out band with the pull rate of 5mm～100mm/min going out band edge, and to make the Ni alloy base band be 10 seconds～1 minute by the time of colloid, make the even dip-coating of colloid on the base band surface after going out band, carry out drying again;
D, sinter phase into: dried base band is put into sintering furnace sinter phase into, promptly make pure or doping of cerium oxide M xCe 1-xO y, the belt material of high temperature superconduct transition zone that constitutes of 0≤x≤0.5,1.75≤y≤2 wherein.
Compared with prior art, the invention has the beneficial effects as follows:
When adopting above technical scheme to prepare the belt material of high temperature superconduct transition zone, owing to apply the mode of colloid is to adopt to lift out band, and the base band continuous reeling had both made preparation process continuous by the impregnation method that lifts of colloid, the preparation efficiency height is applicable to large-scale industrial production; The base band of selecting for use simultaneously can be endless in theory, therefore can prepare the very long superconducting tape transition zone of length; In lifting the process of dipping, the two-sided of base band all can be realized two-sided deposition simultaneously by colloid in the dip-coating simultaneously; Baseband section by colloid during dip-coating is soaked in the colloid fully, has guaranteed the two-sided consistency and the single face uniformity of deposit film, surfacing, the degree of orientation height of transition layer film;
Secondly, the colloid that will contain rare earth nitrades is coated on base band, can form doping of cerium oxide M by sintering xCe 1-xO yTransition zone.In preparation process, control rare earth nitric acid and cerous nitrate salt additional proportion, can make things convenient for the cerium oxide M of controlled doping xCe 1-xO yThe cation proportioning of dopant ion in the transition zone and cerium.And the doping of cerium oxide M that makes xCe 1-xO yTransition zone texture is good, the surfacing densification.The doping of rare earth element makes cerium oxide M xCe 1-xO yThe critical thickness of transition zone reaches 150-200nm, can serve as the transition zone of belt material of high temperature superconduct.
Temperature when the above-mentioned c step is dry is 100 ℃-200 ℃.Under this temperature conditions, can be so that the N in the colloid, dinethylformamide (DMF) can be more, vapor away quickly.
After carrying out the drying in c step, also carry out the thermal decomposition process before the sintering, the substrate that is about to be coated with colloid places sintering furnace, makes furnace temperature slowly rise to 200 ℃-230 ℃ from room temperature, and rises at 280 ℃-400 ℃ with the speed of 0.1-1 ℃/min, is incubated 15 minutes; Subsequently, carry out the phase that sinters in d step again.Handle through the predecomposition before such sintering, the transition zone that can make sintering form is more smooth finer and close.
The concrete practice that sinters phase in above-mentioned d step is: the sintering furnace furnace temperature is risen to 850 ℃-1150 ℃ with the speed of 5-100 ℃/min fast, be incubated 15 minutes to 2 hours, subsequently furnace temperature is slowly reduced to room temperature.
Below in conjunction with the drawings and specific embodiments the present invention is done a step explanation.
Description of drawings
Fig. 1 is the pure CeO of the embodiment of the invention one 2The X ray diffracting spectrum of two-sided individual layer transition zone.
Fig. 2 is the pure CeO of the embodiment of the invention one 25000 times of scanning electron microscopy (SEM) photo of two-sided individual layer transition zone.
Fig. 3 is the samarium Sm doping of cerium oxide Sm of the embodiment of the invention two 0.2Ce 0.8O 1.9The X ray diffracting spectrum of the two-sided individual layer transition zone of coating conductor.
Fig. 4 is the samarium Sm doping of cerium oxide Sm of the embodiment of the invention two 0.2Ce 0.8O 1.91000 times of scanning electron microscopy (SEM) photo of the two-sided individual layer transition zone of coating conductor.
Fig. 5 is the samarium Sm doping of cerium oxide Sm of the embodiment of the invention two 0.2Ce 0.8O 1.9The electron spectrum (EDS) of the two-sided individual layer transition zone of coating conductor.
Fig. 6 is the gadolinium Gd doping of cerium oxide Gd of the embodiment of the invention three 0.5Ce 0.5O 1.75The X ray diffracting spectrum of the two-sided individual layer transition zone of coating conductor.
Fig. 7 is the gadolinium Gd doping of cerium oxide Gd of the embodiment of the invention three 0.5Ce 0.5O 1.755000 times of scanning electron microscopy (SEM) photo of the two-sided individual layer transition zone of coating conductor.
Fig. 8 is the gadolinium Gd doping of cerium oxide Gd of the embodiment of the invention three 0.5Ce 0.5O 1.75The electron spectrum (EDS) of the two-sided individual layer transition zone of coating conductor.
Fig. 9 is the europium Eu doping of cerium oxide Eu of the embodiment of the invention four 0.2Ce 0.8O 1.9The X ray diffracting spectrum of the two-sided individual layer transition zone of coating conductor.
Figure 10 is the europium Eu doping of cerium oxide Eu of the embodiment of the invention four 0.2Ce 0.8O 1.910000 times of scanning electron microscopy (SEM) photo of the two-sided individual layer transition zone of coating conductor.
Figure 11 is the europium Eu doping of cerium oxide Eu of the embodiment of the invention four 0.2Ce 0.8O 1.9The electron spectrum (EDS) of the two-sided individual layer transition zone of coating conductor.
Specific implementation method:
Embodiment one
A kind of embodiment of the present invention is:
A kind of chemical solution deposition prepares the method for double-faced high-temperature superconducting band transition zone, is made of following steps successively:
A, preparation of precursor solution: cerous nitrate is dissolved in N, in the dinethylformamide (DMF), forms precursor aqueous solution (ion ratio that also is this routine rare earth ion and cerium is 0:1);
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA), form the colloid of good film-forming property;
C, film preparation and drying: the Ni alloy base band reeled (promptly in colloid, establish a runner in the colloid that makes by the b step, base band is walked around this runner from the below, and go out band edge and give band edge all above colloid), vertically go out band (promptly going out band edge) with the pull rate of 5mm/min going out band edge vertically upward base band is pulled out, and make the time of Ni alloy base band by colloid (be base band a bit when entering colloid to leave colloid the time total time) be 1 minute, make the even dip-coating of colloid on the base band surface after going out band, carry out temperature again and be 100 ℃ drying;
After carrying out the drying in c step, also carry out the thermal decomposition process before the sintering, the base band that is about to be coated with colloid places sintering furnace, makes furnace temperature slowly rise to 200 ℃ from room temperature, and rises at 280 ℃ with the speed of 0.1 ℃/min, is incubated 15 minutes; Subsequently, carry out the phase that sinters in following d step again.
D, sinter phase into: place sintering furnace to put into sintering furnace the base band after the thermal decomposition, with furnace temperature fast with rise to 1150 ℃ of 50 ℃/min, be incubated 1 hour subsequently furnace temperature slowly reduce to room temperature, the M that finally makes xCe 1-xO yX in the transition zone equals 0, and y equals 2, promptly makes the transition zone of the high-temperature superconductor two generations band of the two-sided individual layer of pure ceria (one deck is two-layer altogether).
Embodiment two
This routine preparation method is made of following steps successively:
A, preparation of precursor solution: samaric nitrate and cerous nitrate in the ratio of cation ratio Sm:Ce=0.2:0.8, are dissolved in N, in the dinethylformamide (DMF), form precursor aqueous solution; Also be that the doped chemical M that adopts in this example is samarium Sm, the M that finally makes xCe 1-xO yX in the transition zone equals 0.2, and y equals 1.9, and promptly the material of the transition zone that makes of this example is specially Sm 0.2Ce 0.8O 1.9
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA), form the colloid of good film-forming property;
C, film preparation and drying: go on foot Ni alloy base band coiling in the colloid that makes by b, vertically go out band with the pull rate of 100mm/min going out band edge, and to make the Ni alloy base band be 10 seconds by the time of colloid, make the even dip-coating of colloid on the base band surface after going out band, carry out temperature again and be 150 ℃ drying;
After carrying out the drying in c step, also carry out the thermal decomposition process before the sintering, the base band that is about to be coated with colloid places sintering furnace, makes furnace temperature slowly rise to 210 ℃ from room temperature, and rises at 320 ℃ with the speed of 0.15 ℃/min, is incubated 15 minutes; Subsequently, carry out the phase that sinters in d step again.
D, sinter phase into: place sintering furnace to put into sintering furnace the base band after the thermal decomposition, with furnace temperature fast with rise to 1000 ℃ of 5 ℃/min, be incubated 2 hours subsequently furnace temperature slowly reduce to room temperature, promptly make Sm 0.2Ce 0.8O 1.9The transition zone of the high-temperature superconductor two generations band of the formation of (mixing the samarium ceria).
Embodiment three
This routine preparation method is made of following steps successively:
A, preparation of precursor solution: gadolinium nitrate and cerous nitrate in the ratio of cation ratio Gd:Ce=0.5:0.5, are dissolved in N, in the dinethylformamide (DMF), form precursor aqueous solution; Also be that the doped chemical M that adopts in this example is gadolinium Gd, the M that finally makes xCe 1-xO yX in the transition zone equals 0.5, and y equals 1.75, and promptly the material of the transition zone that makes of this example is specially Gd 0.5Ce 0.5O 1.75
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA), form the colloid of good film-forming property;
C, film preparation and drying: go on foot Ni alloy base band coiling in the colloid that makes by b, vertically go out band with the pull rate of 50mm/min going out band edge, and to make the Ni alloy base band be 20 seconds by the time of colloid, make the even dip-coating of colloid on the base band surface after going out band, carry out temperature again and be 200 ℃ drying;
After carrying out the drying in c step, also carry out the thermal decomposition process before the sintering, the base band that is about to be coated with colloid places sintering furnace, makes furnace temperature slowly rise to 230 ℃ from room temperature, and rises at 400 ℃ with the speed of 1 ℃/min, is incubated 15 minutes; Subsequently, carry out the phase that sinters in d step again.
D, sinter phase into: place sintering furnace to put into sintering furnace the base band after the thermal decomposition, with furnace temperature fast with rise to 1100 ℃ of 100 ℃/min, be incubated 15 minutes subsequently furnace temperature slowly reduce to room temperature, promptly make by Gd 0.5Ce 0.5O 1.75The transition zone of the high-temperature superconductor two generations band that (mixing the gadolinium ceria) constitutes.
Embodiment four
This routine preparation method is made of following steps successively:
A, preparation of precursor solution: europium nitrate and cerous nitrate in the ratio of cation ratio Eu:Ce=0.1:0.9, are dissolved in N, in the dinethylformamide (DMF), form precursor aqueous solution; Also be that the doped chemical M that adopts in this example is europium Eu, the M that finally makes xCe 1-xO yX in the transition zone equals 0.1, and y equals 1.95, and promptly the material of the transition zone that makes of this example is specially Eu 0.1Ce 0.9O 1.95
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA), form the colloid of good film-forming property;
C, film preparation and drying: go on foot Ni alloy base band coiling in the colloid that makes by b, vertically go out band with the pull rate of 20mm/min going out band edge, and to make the Ni alloy base band be 30 seconds by the time of colloid, makes the even dip-coating of colloid on the base band surface after going out band, carries out drying again;
After carrying out the drying in c step, also carry out the thermal decomposition process before the sintering, the base band that is about to be coated with colloid places sintering furnace, makes furnace temperature slowly rise to 210 ℃ from room temperature, and rises at 290 ℃ with the speed of 0.5 ℃/min, is incubated 15 minutes; Subsequently, carry out the phase that sinters in d step again.
D, sinter phase into: place sintering furnace to put into sintering furnace the base band after the thermal decomposition, with furnace temperature fast with rise to 850 ℃ of 50 ℃/min, be incubated 1 hour subsequently furnace temperature slowly reduce to room temperature, promptly make by Eu 0.1Ce 0.9O 1.95The transition zone of the high-temperature superconductor two generations band that (mixing the europium ceria) constitutes.
Fig. 1,3,6,9 is respectively the X ray diffracting spectrum of the transition zone that embodiment one, two, three, four makes, and as seen from the figure, the transition zone that the ownership gets is cubic structure, has good C axle texture.The electron micrograph of Fig. 2,4,7,10 transition zones that make for embodiment one, two, three, four, as seen from the figure, all smooth densification in all transition zone surfaces does not have tangible crackle and hole.Fig. 5,8,11 is electron spectrum (EDS) figure of the transition zone of embodiment two, three, four, and rare earth ion all shows as seen from the figure, shows that rare earth ion all mixes well to have entered transition zone.
Utilizing the inventive method to prepare in the process of transition zone in two generations of high-temperature superconductor, in the b colloid for preparing process in step, also can directly not add polyacrylic acid or polymethylacrylic acid, but add acrylic monomers or methacrylic acid monomer toward the precursor aqueous solution in a step, and adding azodiisobutyronitrile (ABIN) as catalyst, polymerization generates polymer in precursor aqueous solution.
Because yttrium (Y), lanthanum (La), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) that the present invention uses, these elements all belong to rare earth element, they are at chemical property such as ionic valence condition, extremely close on the ionic radius, replace each other easily and intersolubility fine, the oxide of its formation all belongs to cubic system, and lattice parameter all mates with REBCO or Ni alloy phase.Therefore, be not limited to the element among the above embodiment, and adopt any one element in the rare earth element or the mixing of more than one elements, all can prepare the two-sided transition zone of rare earth doped cerium oxide of function admirable.
When the present invention was dissolved in organic solvent formation precursor aqueous solution at nitrate, the amount of organic solvent can fully be dissolved nitrate with it and be got final product.Be generally the part by weight 1:3-8 of nitrate and organic solvent.The addition of polyacrylic acid or polymethylacrylic acid is not strict with yet in b goes on foot, as long as can make anhydrous solution be formed into the good colloid of film properties.

Claims (4)

1, a kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer is made of following steps successively:
A, preparation of precursor solution: rare earth nitrades and cerous nitrate are pressed cation ratio M:Ce=x:1-x, the ratio of 0≤x≤0.5, be dissolved in N, in the dinethylformamide (DMF), form precursor aqueous solution, wherein M is a kind of among Y (yttrium), La (lanthanum), Pr (praseodymium), Nd (neodymium), Sm (samarium), Eu (europium), Gd (gadolinium), Tb (terbium), Dy (dysprosium), Ho (holmium), Er (erbium), Tm (thulium), Yb (ytterbium), Lu (lutetium), the Zr (zirconium);
B, colloid for preparing: in a precursor aqueous solution in step, add polyacrylic acid (PAA) or polymethylacrylic acid (PMAA), form the colloid of good film-forming property;
C, film preparation and drying: go on foot Ni alloy base band coiling in the colloid that makes by b, vertically go out band with the pull rate of 5mm～100mm/min going out band edge, and to make the Ni alloy base band be 10 seconds～1 minute by the time of colloid, make the even dip-coating of colloid on the base band surface after going out band, carry out drying again;
D, sinter phase into: dried base band is put into sintering furnace sinter phase into, promptly make pure or doping of cerium oxide M xCe 1-xO y, the belt material of high temperature superconduct transition zone that constitutes of 0≤x≤0.5,1.75≤y≤2 wherein.
2, a kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer as claimed in claim 1 is characterized in that: the temperature when the described c step is dry is 100 ℃-200 ℃.
3, a kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer as claimed in claim 1, it is characterized in that: after carrying out the c drying in step, also carry out the preceding thermal decomposition process of sintering, the substrate that is about to be coated with colloid places sintering furnace, make furnace temperature slowly rise to 200 ℃-230 ℃ from room temperature, and rise at 280 ℃-400 ℃ with the speed of 0.1-1 ℃/min, be incubated 15 minutes; Subsequently, carry out the phase that sinters in d step again.
4, a kind of continuous method for preparing two-sided texture high-temperature superconduction bibasic strip transition layer as claimed in claim 1, it is characterized in that: the concrete practice that sinters phase in described d step is: the sintering furnace furnace temperature is risen to 850 ℃-1150 ℃ with the speed of 5-100 ℃/min fast, be incubated 15 minutes by 2 hours, subsequently furnace temperature naturally cooled to room temperature.
CNA2008100465605A 2008-11-14 2008-11-14 Method for continuously preparing two-sided texture high-temperature superconduction bibasic strip transition layer Pending CN101414497A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102222761A (en) * 2011-04-12 2011-10-19 西南交通大学 Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film
CN102677030A (en) * 2011-11-02 2012-09-19 西南交通大学 Method for preparing high-temperature superconducting coating conductor CeO2 buffer layer film on biaxial texture NiW alloy substrate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102222761A (en) * 2011-04-12 2011-10-19 西南交通大学 Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film
CN102677030A (en) * 2011-11-02 2012-09-19 西南交通大学 Method for preparing high-temperature superconducting coating conductor CeO2 buffer layer film on biaxial texture NiW alloy substrate

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Open date: 20090422