CN103339692B - The manufacture method of banded oxide superconducting wire rod and annealing device - Google Patents
The manufacture method of banded oxide superconducting wire rod and annealing device Download PDFInfo
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- CN103339692B CN103339692B CN201280007641.9A CN201280007641A CN103339692B CN 103339692 B CN103339692 B CN 103339692B CN 201280007641 A CN201280007641 A CN 201280007641A CN 103339692 B CN103339692 B CN 103339692B
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- 238000000137 annealing Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000002485 combustion reaction Methods 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 230000007613 environmental effect Effects 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 11
- -1 organic acid salt Chemical class 0.000 claims description 10
- DTQVDTLACAAQTR-UHFFFAOYSA-M Trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-M 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 125000005609 naphthenate group Chemical group 0.000 claims description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-M octanoate Chemical compound CCCCCCCC([O-])=O WWZKQHOCKIZLMA-UHFFFAOYSA-M 0.000 claims description 4
- YPIFGDQKSSMYHQ-UHFFFAOYSA-M 7,7-dimethyloctanoate Chemical compound CC(C)(C)CCCCCC([O-])=O YPIFGDQKSSMYHQ-UHFFFAOYSA-M 0.000 claims description 3
- 150000002902 organometallic compounds Chemical class 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 241000954177 Bangana ariza Species 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 165
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 23
- 229910000040 hydrogen fluoride Inorganic materials 0.000 abstract description 18
- 239000002912 waste gas Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 description 34
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000005245 sintering Methods 0.000 description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 229910052731 fluorine Inorganic materials 0.000 description 7
- 239000011737 fluorine Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 239000002887 superconductor Substances 0.000 description 6
- 238000003618 dip coating Methods 0.000 description 5
- 229910000856 hastalloy Inorganic materials 0.000 description 5
- 229910001026 inconel Inorganic materials 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007735 ion beam assisted deposition Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000007591 painting process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/01—Manufacture or treatment
- H10N60/0268—Manufacture or treatment of devices comprising copper oxide
- H10N60/0296—Processes for depositing or forming superconductor layers
- H10N60/0324—Processes for depositing or forming superconductor layers from a solution
Abstract
The invention provides heat treatment method, it improves the discharge efficiency of hydrogen fluoride gas, has in the longitudinal direction evenly and the banded oxide superconducting wire rod of the superconducting characteristic of excellence to manufacture.In this method, in annealing device (100), in the inside of the cylindric heat treatment space (111) of furnace core tube (110), configure cylindric rotary body (120) in the mode that can rotate relative to combustion chamber axle (C).In rotary body (120), on the surface (121a) being formed with multiple through hole (124), be wound the banded wire rod (20) of the film body of superconduction predecessor.Gas supply pipe (130) is to banded wire rod (20) the supply environment gas (6) be wrapped on rotary body (120).In heat treatment space (111), configure dividing plate (170) in remaining space (111b) between the both ends of rotary body (120) and the combustion chamber flange part (116,118) of furnace core tube (110), avoid reacted gas, i.e. waste gas (6c) with face to flow into remaining space (111b).
Description
Technical field
The present invention relates to manufacture method and the annealing device of banded oxide superconducting wire rod, particularly relate to the technology using MOD (Metal-organicDeposition, metal organic salt deposits) method to form superconducting layer on the directed metal base being formed with intermediate layer.
Background technology
In the past, as YBa
2cu
3o
7-x(YBCO) manufacture method of the banded oxide superconducting wire rod being, is known to the method utilizing metal organic salt coated heat decomposition (MOD:Metal-organicDeposition) method to form superconducting layer (with reference to reference to patent documentation 1, patent documentation 2 and patent documentation 3) on the orientation metal base material being formed with intermediate layer.
In above-mentioned MOD method, first, be impregnated in by the banding substrate being formed with intermediate oxide layer in superconduction material solution, this superconduction material solution is the mol ratio that specifies and comprises each metallic element of forming superconductor and with the mixed solution of the metal organic acid salt of trifluoroacetate (tfa salt) be representative caprylate, naphthenate etc.Then, in superconduction material solution, pull above-mentioned base material (so-called dip coating (dipcoatingmethod)) out, thus, mixed solution is coated the surface of base material.Then, by carrying out presintering and formally sinter forming oxide superconducting layer.
MOD method also forms oxide superconducting layer serially in antivacuum in long strip base material, therefore, with pulsed laser deposition (PulseLaserDeposition, PLD) method or chemical vapour deposition (CVD) (ChemicalVaporDeposition, CVD) vapor phase method such as method is compared, technique is simple and can realize cost degradation, therefore receives publicity.
The annealing device of the batch (batchtype) that base material that effects on surface is attached with superconduction material solution is heat-treated is disclosed in patent documentation 1, patent documentation 2.The annealing device of batch, compared with the annealing device of winding (reel-to-reel) formula such as shown in patent documentation 3, has the advantage being easy to control the environment in stove, therefore can form stable superconducting layer.In addition, the annealing device of batch, compared with the annealing device of coil type, has equipment miniaturization and can complete the advantage of sintering at short notice.In addition, the annealing device of coil type be by wire rod delivering mechanism and wire coil around the two ends of organization establishes at the furnace core tube of tunnel-shaped, wire rod is moved with fixed speed in stove, comes thus to sinter this wire rod.
Fig. 1 is used to carry out the schematic configuration of batch annealing device disclosed in simple declaration patent documentation 1, patent documentation 2.As shown in Figure 1, surface attachment has the base material 2 of superconduction raw material to be wrapped on the rotary body 3 of cylinder shape by this annealing device 1.The cylindric rotary body 3 being wound with base material 2 is driven in rotation mechanism and drives rotation in furnace core tube 4, and described furnace core tube 4 is formed with the opening that flange (flange) 4b closes two ends in the body 4a of cylindrical shape.Rotary body 3 is formed with multiple not shown through hole.The heater 5 that base material 2 is being wrapped in the surface direction being arranged on base material 2 under the state on rotary body 3 heated.In addition, the environmental gas 6 of inert gas, oxygen and steam etc. is comprised from the surface direction of base material 2 to spraying method, after the superconduction raw material reaction of this environmental gas 6 and base material 2, as reacted gas (waste gas), via the through hole be formed on rotary body 3 and as the shaft portion of rotary body 3 and the blast pipe 7 arranged discharge (representing with arrow 6a).
Prior art document
Patent documentation
Patent documentation 1: Japan Patent No. 4468901 publication
Patent documentation 2: Japanese Patent Laid-Open 2009-48817 publication
Patent documentation 3: Japan Patent No. 4401992 publication
Summary of the invention
Making predecessor on the intermediate layer after film forming, formal sintering is implemented to this predecessor thus is formed in the method (TFA-MOD method) of YBCO film, use steam supply to the environmental gas (reactant gas) of precursor film when formally sintering, above-mentioned predecessor uses patent documentation 1, annealing device disclosed in patent documentation 2, the base material being coated with the mixed solution comprising trifluoroacetate etc. is carried out to the superconduction predecessor of presintering gained, and above-mentioned predecessor contains fluorine (F).
The reaction equation of generation YBCO is now
1/2Y
2Cu
2O
5+2BaF
2+2CuO+2H
2O→YBCO+4HF。
So, due to when formally sintering, using steam to heat-treat precursor film as environmental gas, therefore can produce HF, HF gas can be produced after the reaction as gas after reaction.
In TFA-MOD method, decompose fluoride (BaF
2) time fluorine removal speed become YBCO generate reaction speed limit.Therefore there is the impact of hydrogen fluoride (HF) gas (waste gas) owing to reacting rear generation, the problem of the superconducting characteristic reduction of the YBCO film sintered.
Especially in order to obtain the bar-shape wire rod with the characteristic that critical current density (Jc) is more than 2.0, critical electric current value (Ic) is more than 300A, superconducting layer must be made to be formed as the thickness of more than 1.5 μm.If be formed as above-mentioned thickness, be then difficult to all the more hydrogen fluoride (HF) gas to remove completely, thus above-mentioned characteristic cannot be obtained.
Therefore, in order to make the superconducting characteristic of YBCO film improve, importantly how fluorine contained in predecessor is removed in formal sintering.
But, in the annealing device 1 shown in Fig. 1, in furnace core tube 4, between the flange 4b in the rotary body 3 and furnace core tube 4 of cylinder shape, form remaining space R.
Therefore there is following problems: hydrogen fluoride (HF) gas is not discharged (in figure arrow 6b) via blast pipe 7 in furnace core tube 4, but is trapped in remaining space R.
Thus, hydrogen fluoride (HF) the gas 6b produced by predecessor, cannot form the discharge air-flow of certain orientation, and cannot remove hydrogen fluoride (HF) gas 6b completely.If fluorine cannot be removed completely, then there is the problem cannot with uniform in the longitudinal direction superconducting characteristic.
The object of the present invention is the manufacture method and the annealing device that provide banded oxide superconducting wire rod, it can improve reacted gas purging efficiency in furnace core tube inside, and manufactures and have in the longitudinal direction evenly and the banded oxide superconducting wire rod of the superconducting characteristic of excellence.
The manufacture method of the banded oxide superconducting wire rod of a form of the present invention, the annealing device wherein used comprises: furnace core tube, the closed at both ends possessing the cylindrical body portion of heat treatment space is formed with flange part, cylindric rotary body, is configured in described heat treatment space in the mode that can rotate relative to the combustion chamber axle of described furnace core tube inner, and at the banded wire rod of the surface wrap being formed with multiple through hole, described banded wire rod is formed with the film body of superconduction predecessor, gas supply pipe, for described banded wire rod supply environment gas, and gas outlet pipe, outside for described environmental gas to be expelled to described furnace core tube from described rotary body inside, in the manufacture method of described banded oxide superconducting wire rod, use described annealing device, to the face of the described film body of the described banded wire rod be wrapped on described rotary body, described environmental gas is supplied from the position separated up, wherein, the interval dividing plate of the axial end of rotation of described flange part and described rotary body is separated, and described environmental gas is supplied to the face of the described film body of the described banded wire rod be wrapped on described rotary body.
The annealing device of the banded oxide superconducting wire rod of a form of the present invention, comprising: furnace core tube, the closed at both ends possessing the cylindrical body portion of heat treatment space is formed with flange part; Cylindric rotary body, is configured in described heat treatment space in the mode that can rotate relative to the combustion chamber axle of described furnace core tube inner, and at the banded wire rod of the surface wrap being formed with multiple through hole, described banded wire rod is formed with the film body of superconduction predecessor; Gas supply pipe, is configured in the face relative to the described film body of the described banded wire rod be wrapped on described rotary body and the position separated up, and for described face supply environment gas; And gas outlet pipe, discharged from described rotary body inside by reacted gas, wherein, in described furnace core tube, be equipped with dividing plate, described dividing plate separates for the interval of the axial end of rotation by described flange part and described rotary body.
The effect of invention
According to the present invention, reacted gas purging efficiency can be improved, manufacture and have in the longitudinal direction evenly and the banded oxide superconducting wire rod of the superconducting characteristic of excellence.
Accompanying drawing explanation
Fig. 1 is the summary section of the major part structure representing existing batch annealing device.
Fig. 2 is the summary section of the major part structure of the annealing device of the banded oxide superconducting wire rod represented involved by one of the present invention execution mode.
Fig. 3 is the A-A line profile of the Fig. 2 of the major part structure representing described annealing device.
Fig. 4 is the skeleton diagram of the rotary body representing described annealing device.
Fig. 5 A ~ Fig. 5 E is the skeleton diagram of the manufacture method representing the YBCO superconducting wire utilizing MOD method to carry out.
Reference numeral:
6,6a, 6c: environmental gas
100: annealing device
110: furnace core tube
111: heat treatment space
111b: remaining space
114: combustion chamber body (cylindrical body portion)
116,118: combustion chamber flange part (flange part)
120: rotary body
121: cylinder
121a: surface
122,123: lid (end of rotary body)
130: gas supply pipe
132: gas squit hole
140: gas outlet pipe
170: dividing plate
20: banded wire rod
Embodiment
Below, the execution mode that present invention will be described in detail with reference to the accompanying.
< utilizes MOD legal system to make the summary > of banded oxide superconducting wire rod
Fig. 5 A ~ Fig. 5 E represents the outline of the manufacture method of the banded oxide superconducting wire rod (YBCO superconducting wire) possessing superconducting layer (YBCO superconducting layer) utilizing MOD method to carry out.
First, on the Ni alloy substrate (base material) of band shape, utilize ion beam assisted depositing (IonBeamAssistedDeposition, IBAD) method to form Gd
2zr
2o
7intermediate layer as template (template), then, at this Gd
2zr
2o
7intermediate layer utilize sputtering method (sputteringmethod) form CeO
2intermediate layer and obtain composite base plate, and in painting process (with reference to Fig. 5 A), dip coating is utilized to be coated on this composite base plate by mixed solution (superconduction material solution) 8, above-mentioned mixed solution (superconduction material solution) 8 is the ratios with Y:Ba:Cu=1:1.5:3, Y-TFA salt (trifluoroacetate), Ba-TFA salt and Cu-naphthenate is dissolved in organic solvent and forms.After coating mixed solution 8, in presintering operation (with reference to Fig. 5 B), carry out presintering.Above-mentioned painting process (with reference to Fig. 5 A) and presintering operation (with reference to Fig. 5 B) are repeated by stipulated number, the intermediate layer of banded wire rod 20 is formed the film body as superconduction predecessor.Then, in formal sintering circuit (with reference to Fig. 5 C), crystallization heat process is implemented to the film body of the superconduction predecessor of banded wire rod 20, that is, implements the heat treatment producing YBCO superconductor.Then, in operation (with reference to Fig. 5 D), utilize sputtering method and after form Ag stabilized zone on the YBCO superconductor produced, heat treated after implementing in operation (with reference to Fig. 5 E), thus manufacture YBCO superconducting wire.
The annealing device of embodiments of the present invention is used to the crystallization heat process of operation (with reference to Fig. 5 C), and this annealing device implements heat treatment to the predecessor of the superconductor formed in banded wire rod, thus produces YBCO superconductor.Moreover annealing device is also applicable to and forms intermediate layer.
Ni alloy substrate can be the substrate with biaxially oriented property, also can be the substrate being formed on the metal substrate of astaticism and have the intermediate layer of biaxially oriented property.In addition, one or more layers intermediate layer is formed.Except above-mentioned dip coating, also ink-jet method (inkjetmethod), spray-on process (spraymethod) etc. can be used as coating process, substantially, as long as serially mixed solution to be coated the technique on composite base plate, then not by the restriction of above-mentioned example.Once be coated with thickness is 0.01 μm ~ 2.0 μm, is preferably 0.1 μm ~ 1.0 μm.
Moreover superconduction material solution as used herein is the mixed solution metal organic acid salt or organo-metallic compound that comprise Y, Ba and Cu with the mol ratio of regulation are dissolved in organic solvent.Use when molal quantity is set to Y:Ba:Cu=1:a:3, Ba mol ratio is less than the material solution in the scope of 2.When this situation, in order to obtain high Jc value and Ic value, Ba mole in material solution is preferably in the scope of 1.0≤a≤1.8, and the Ba mol ratio be more preferably in material solution is in the scope of 1.3≤a≤1.7.Thus, can suppress the segregation (segregation) of Ba, result, the precipitation of the impurity based on Ba in crystal boundary is suppressed.Thus, suppress the generation of slight crack, and the electric coupling (electriccouplingproperty) between crystal grain improves, by utilizing MOD method to form superconducting film, can manufacture at a high speed and easily and there is uniform thick film and the banded oxide superconductor of superconducting characteristic excellence.In addition, as metal organic acid salt, the caprylate of each element, naphthenate, neodecanoate and trifluoroacetate etc. can be enumerated, as long as but the above-mentioned salt of more than one in these salt can be dissolved in organic solvent equably and be coated on composite base plate, then all can use.
The structure > of < annealing device
Annealing device 100 shown in Fig. 2 and Fig. 3 is the sintering carrying out the mixed solution (the superconduction material solution 8 shown in Fig. 5 A) be coated with as the film body of the superconduction predecessor in banded wire rod 20 using batch.Annealing device 100 possesses: have the furnace core tube 110 of cylindric heat treatment space 111, cylindric rotary body 120, gas supply pipe 130, gas outlet pipe 140 and dividing plate (reflecting plate) 170.
Furnace core tube 110 is formed as hollow cylindrical.Furnace core tube 110 possesses: combustion chamber flange part 116, the combustion chamber flange part 118 of cylindric combustion chamber body (cylindrical body portion) 114 and the respectively opening at the two ends of closed combustion chamber body 114.Combustion chamber flange part 116, combustion chamber flange part 118 form two end faces of furnace core tube 110.
The heat treatment space 111 of furnace core tube 110 delimited by combustion chamber body 114 and combustion chamber flange part 116, combustion chamber flange part 118.Heat treatment space 111 utilizes combustion chamber body 114 and combustion chamber flange part 116, combustion chamber flange part 118, can keep the reduced pressure atmosphere in stove or vacuum.
Furnace core tube 110, is configured with heater 150 around it, utilizes heater 150 to heat inside as heat treatment space 111.
Have rotary body 120 in furnace core tube 110 internal configurations, rotary body 120 can rotate centered by the combustion chamber axle C of the axis as furnace core tube 110.In addition, in furnace core tube 110, at least one in combustion chamber flange part 116, combustion chamber flange part 118 is freely to load and unload relative to combustion chamber body 114 or the form of freely openable is installed.Thereby, it is possible to freely take off rotary body 120 in heat treatment space 111.
In furnace core tube 110, rotary body 120 is configured in the position of substantial middle separating combustion chamber flange part 116, combustion chamber flange part 118 both sides, i.e. the space (being called central space 111a) of the substantial middle of heat treatment space 111.
Rotary body 120 has cylinder 121, and the surperficial 121a of this cylinder 121 is wound the banded wire rod 20 of predecessor.In addition, banded wire rod 20, as being described in use Fig. 5 A, implements presintering afterwards by coating mixed solution (being equivalent to the superconduction material solution 8 shown in Fig. 5 A), base material is formed the predecessor that YBCO superconduction generates body.
This banded wire rod 20 exposes the face of the predecessor formed by mixed solution, is spirally wrapped around the surperficial 121a (surface of rotary body 120) of cylinder 121.
As shown in Figure 4, the cylinder 121 of rotary body 120 is formed with multiple through hole 124.The internal diameter of this through hole 124 is preferably identical with the bandwidth of banded wire rod 20.In addition, its percent opening is set to 20% ~ 95%, particularly preferably the percent opening of scope of 89% ~ 91%.Rotary body 120 utilizes not shown rotating mechanism to rotate with fixed speed in heat treatment.Rotary body 120 is made up of the pottery such as quartz glass, aluminium oxide (ceramics) or the high temperature resistant and not oxidizable materials such as metal such as Hastelloy (Hastelloy), inconel (inconel).
Rotary body 120 is fixed on gas outlet pipe 140, and described gas outlet pipe 140 is inserted in the inside of cylinder 121 with one heart with the combustion chamber axle C as the axis of furnace core tube 110.In addition, gas outlet pipe 140 plays the effect of the rotating shaft of rotary body 120.
The two ends of cylinder 121 are inserted through the lid 122 of gas outlet pipe 140, lid 123 is closed.The position that lid 122, lid 123 are formed in beyond the gas outlet pipe 140 that is exported together with cylinder 121 is airtight inner space.At the position of tubular gas outlet pipe 140 being positioned at this inner space, that be formed with the inner space that is communicated with rotary body 120 and gas outlet pipe 140 inside, not shown interconnecting part.
In addition, as shown in Figures 2 and 3, in the central space 111a in the heat treatment space 111 of furnace core tube 110, separate the surperficial 121a of cylinder 121 and be configured with multiple gas supply pipe 130.Multiple gas supply pipe 130 is parallel to combustion chamber axle C and configures, and balanced configuration in the section vertical with combustion chamber axle C.Here, in furnace core tube 140, symmetrical and be equipped with 4 gas supply pipes 130 in parallel with each other relative to combustion chamber axle C.That is, in furnace core tube 110, many gas supply pipes 130, centered by combustion chamber axle C, along the circumferential direction configure with the pitch of 90 °.
Each gas supply pipe 130 has multiple gas squit hole 132 spraying environmental gas 6 to rotary body 120.
Gas squit hole 132 in gas supply pipe 130 is similarly formed in the body part of gas supply pipe 130 along its length with fixed intervals.Each gas squit hole 132 is circular port, sprays environmental gas 6 equably.In order to evenly spray environmental gas and remove fluorine gas further, preferably, the flow velocity of supply environment gas, flow velocity when specifically contacting with the face of the above-mentioned film body be wrapped on above-mentioned rotary body are in more than 200m/s and below 500m/s.If above-mentioned flow velocity is less than 200m/s, then not only to superconduction predecessor supply environment gas equably, also cannot cannot remove the waste gas (HF gas) on the surface of the face being stranded in above-mentioned film body.Therefore, desired superconducting characteristic cannot be obtained.In addition, if flow velocity is more than 500m/s, although then really can spray environmental gas equably, crystallization reaction carries out rapidly, so be difficult to control epitaxial growth (epitaxialgrowth) speed.Therefore, desired superconducting characteristic cannot be obtained.
As shown in Figures 2 and 3, the position that each gas supply pipe 130 is configured to make gas squit hole 132 to be located at top relative to the surperficial 121a of cylinder 121 to separate, with the surperficial 121a supply environment gas 6 from vertical direction to cylinder 121.
In furnace core tube 110, gas supply pipe 130 is configured to make that the surperficial 121a's of gas squit hole 132 and rotary body 120 reach 10mm ~ 150mm separated by a distance.Above-mentioned preferable range is separated by a distance 50m ~ 100mm.If be in above-mentioned scope separated by a distance, then can spray environmental gas equably to superconduction predecessor, therefore can remove fluorine gas further.If be less than above-mentioned scope separated by a distance, then the environmental gas sprayed only contacts with a part of face of the above-mentioned film body of the banded wire rod 20 be wrapped on rotary body 120, so cannot obtain uniform superconducting characteristic on the length direction of superconducting wire.In addition, if exceed above-mentioned scope separated by a distance, then gas flow increases, and not only production cost improves, and crystallization reaction carries out rapidly, so be difficult to control epitaxial growth speed.Therefore, desired superconducting characteristic cannot be obtained.
Therefore, in order to obtain the bar-shape wire rod superconducting layer of the thick film with more than 1.5 μm, must with above-mentioned scope separated by a distance, utilize suitable gas flow that environmental gas is ejected to superconduction predecessor, thus, the superconducting wire with the characteristic that thickness critical current density (Jc) is more than 2.0, critical electric current value (Ic) is more than 300A can be obtained.
To the face of the predecessor in the banded wire rod 20 be wrapped on the surperficial 121a of cylinder 121, gas supply pipe 130 from the position separated up, vertically supply environment gas 6.Uniform mode must be become to make air pressure and gas flow, the diameter of gas squit hole 20 is designed.
Via the not shown tube connector be connected on gas supply pipe 130, by the not shown environmental gas feedway supply environment gas 6 of outside being configured in furnace core tube 110.In addition, in gas supply device, generate the environmental gas 6 comprising inert gas, oxygen or steam etc., spray this environmental gas 6 from gas supply pipe 130.Above-mentioned environmental gas 6 reacts with superconduction precursor film, gas (waste gas) after forming reactions, i.e. HF gas, described superconduction precursor film is that presintering is coated with the base material of the mixed solution comprising trifluoroacetate etc. and the superconduction precursor film of fluorine-containing (F) that obtain.
In addition, here, the length of the axis of gas supply pipe 130 is the length with the same length of the axis of rotary body 120, but preferably long than the length of rotary body 120.That is, when the length when between the gas squit hole 132 at two ends being positioned at gas supply pipe 130 is longer than the length of rotary body 120, all more effectively can react uniformly throughout the total length of the banded wire rod 20 be wrapped on cylindric rotary body 120.Gas supply pipe 130 is made up of high temperature resistant and not oxidizable materials such as the pottery such as quartz glass, aluminium oxide or the metals such as Hastelloy, inconel.
Gas outlet pipe 140 is inserting the center of combustion chamber flange part 116, combustion chamber flange part 118 from lid 122, the outward extending both end sides of lid 123.Thus, gas outlet pipe 140 at both ends 141, end 142 rotatably supports by combustion chamber flange part 116, combustion chamber flange part 118.In addition, the two ends of gas outlet pipe 140 are configured in the outside of furnace core tube 110.Thus, the inside of rotary body 120 is formed via the state of gas outlet pipe 140 with the ft connection of furnace core tube 110.
Gas outlet pipe 140 be connected with the inner space of cylinder 121 and as the rotating shaft of cylinder 121 a part and formed.Here, gas outlet pipe 140 is inserted through the inside of cylinder 121, on the rotating shaft (being equivalent to combustion chamber axle C) of cylinder 121, as the axle portion of cylinder 121, i.e. rotary body 120 rotating shaft and formed.In gas outlet pipe 140, in the periphery of middle body of inside being configured at cylinder 121, be formed with multiple not shown through hole.The inside of the inside of cylinder 121, i.e. rotary body 120 becomes via these through holes the state be communicated with the inside of gas outlet pipe 140.Here, gas outlet pipe 140 forms following structure: close between the opening of a side, end 141 and the middle body being configured in cylinder 121 inside, only the opening of side, the other end 142 is connected with the inside of cylinder 121, discharges HF gas from the opening of side, the other end 142.In addition, gas outlet pipe 140 can also form following structure: an end 141 is also connected with the position of cylinder 121 inside, thus from both ends 141, the opening of side, end 142 all discharges HF gas.In addition, also can with rotating shaft split gas outlet pipe 140 is set.
Here, gas outlet pipe 140 inserts via from side, the other end 142 position that lid 123 exports to the outside of furnace core tube 110, discharges reacted gas (this refers to HF gas).Like this, the gas (environmental gas 6 and reacted gas) of cylinder 121 inside is discharged to the outside of furnace core tube 110 by gas outlet pipe 140.Here, gas outlet pipe 140 is formed on cylinder 121.In addition, gas outlet pipe 140 is made up of high temperature resistant and not oxidizable materials such as the pottery such as quartz glass, aluminium oxide or the metals such as Hastelloy, inconel.
As mentioned above, in the heat treatment space 111 of furnace core tube 110, be configured with gas supply pipe 130 and rotary body 120 at central space 111a, HF gas is discharged to the outside of furnace core tube 110 by described rotary body 120 via gas outlet pipe 140.Dividing plate 170 is configured in the heat treatment space 111 in furnace core tube 110, to separate this central space 111a.
Dividing plate 170 is positioned in the plane orthogonal with combustion chamber axle C, and separates the interval of the end (lid 122, lid 123) in the rotating shaft direction in combustion chamber flange part 116, combustion chamber flange part 118 and rotary body 120.Here, dividing plate 170 is configured in space, the i.e. so-called remaining space 111b (being equivalent to the remaining space R in past case) between each combustion chamber flange part 116 of rotary body 120 and furnace core tube 110, combustion chamber flange part 118.Specifically, dividing plate 170 separates the central space 111a and remaining space 111b that are configured with rotary body 120.
Here, the space (remaining space 111b) between an end (lid 122) of the axis of combustion chamber flange part 116 and rotary body 120 is configured with polylith dividing plate 170.In addition, the space (remaining space 111b) between the other end (lid 123) of the axis of combustion chamber flange part 118 and rotary body 120 is configured with polylith dividing plate 170.
Preferably, the dividing plate 170-1 be oppositely disposed with the both ends (position of the outside of lid 122, lid 123) of the axis of rotary body 120 is configured at respectively as far as possible close to the position of the end (position of the outside of lid 122, lid 123) of rotary body 120.
Here, the position of dividing plate 170-1 compared with the both ends of the heater 150 longer than rotary body 120 closer to rotary body 120 side, and respectively with the end of gas supply pipe 130 close to and relative.
In heat treatment space 111, dividing plate 170 is reflected in the central space 111a being configured with gas supply pipe 130 and rotary body 120 the reacted gas, i.e. the HF gas 6c that produce, prevents HF gas 6c from flowing into remaining space 111b.That is, dividing plate 170 prevents the HF gas that produces in central space 111a from flowing into from end (position of the outside of lid 122, lid 123) the combustion chamber flange part 116 to furnace core tube 110 of rotary body 120, the space of combustion chamber flange part 118.In addition, dividing plate 170 also prevents the gas before reacting, and namely environmental gas 6 flows in remaining space 111b, and environmental gas 6 can be made more effectively to react with superconducting layer in central space 111a.In addition, preferably, in above-mentioned remaining space 111b, polylith dividing plate 170 is configured.By configuration polylith dividing plate 170, can prevent HF gas 6c from flowing into remaining space 111b, therefore, it is possible to obtain desired superconducting characteristic further.
On these dividing plates 170, the rotating shaft of rotary body 120, i.e. gas outlet pipe 140 are inserted.
Here, these dividing plates 170 are fixed on gas outlet pipe 140.In other words, dividing plate 170 is inserted the axle portion (rotating shaft of cylinder 121) of rotary body 120, and this axle portion is fixed on dividing plate 170, here, dividing plate 170 and rotating shaft (rotating shaft of the cylinder 121) direction of rotary body 120 end noncontact and relatively near configuring.
Specifically, in the present embodiment, in furnace core tube 110, polylith dividing plate 170 is fixed on the position of the gas outlet pipe 140 in each combustion chamber flange part 116 of furnace core tube 110, remaining space 111b between combustion chamber flange part 118 and rotary body 120 respectively.Thus, in furnace core tube 110, dividing plate 170 and rotary body 120 together rotate freely.And when taking off rotary body 120 from furnace core tube 110, dividing plate 170 can take off in the lump with gas outlet pipe 140 and rotary body 120.Thereby, it is possible to easily take off banded wire rod 20 to winding of band-type wire rod 20 on rotary body 120 or from rotary body 120.In addition, dividing plate 170 is the same with gas supply pipe 130, gas outlet pipe 140 etc., is made up of high temperature resistant and not oxidizable materials such as the pottery such as quartz glass, aluminium oxide or the metals such as Hastelloy, inconel.In addition, although define aforementioned barriers 170 to be fixed on structure on gas outlet pipe 140, being not limited to this, can also be the structure in aforementioned barriers 170 is fixed in furnace core tube 110 remaining space 111b.In addition, as long as dividing plate 170 separates at least one in the interval of the interval of the axial end of rotation (lid 122) of combustion chamber flange part 116 and rotary body 120 and the axial end of rotation (lid 123) of combustion chamber flange part 118 and rotary body 120, then can form by any way.
As mentioned above, annealing device 100 possesses furnace core tube 110, and furnace core tube 110 closes with combustion chamber flange part 116, combustion chamber flange part 118 two ends that possess the combustion chamber body 114 of heat treatment space 111 and formed.In addition, cylindric rotary body 120 is had in heat treatment space 111 internal configurations, this rotary body 120 configures in the mode that can rotate relative to the combustion chamber axle of furnace core tube 110, and is being formed with the surface of multiple through hole, is wound the banded wire rod of the film body of superconduction predecessor.And, annealing device 100 also possesses gas supply pipe 130, described gas supply pipe 130 is configured in the position separated up relative to the face of the film body of the banded wire rod be wrapped on rotary body 120 in heat treatment space 111, and it is to face supply environment gas.Further, annealing device 100 also possesses gas outlet pipe 140, and described gas outlet pipe 140 discharges reacted gas from the inside of rotary body 120.In furnace core tube 110, arrange dividing plate 170, described dividing plate 170 separates the interval of the end in the rotating shaft direction in combustion chamber flange part 116, combustion chamber flange part 118 and rotary body 120.
In above-mentioned annealing device 100, the cylindric rotary body 120 being wound with banded wire rod 20 is rotated with fixed speed.And, utilizing heater 150 to remain in the heat treatment space 111 of heating environment, the environmental gas supplied by gas supply device (not shown) is ejected into the face of banded wire rod 20 equably via multiple gas squit holes 132 of gas supply pipe 130.The environmental gas 6 and the face that sprayed react and generate HF gas, and the multiple through holes 124 via the cylinder 121 in rotary body 120 enter the inside of cylinder 121.
Now, owing to being configured with polylith dividing plate 170 in furnace core tube 110, so waste gas (specifically referring to HF gas) can not flow to combustion chamber flange part 116, combustion chamber flange part 118 side of furnace core tube 110 from the end of rotary body 120 (cylinder 121) (lid 122, lid 123).Thus, waste gas can not be trapped in remaining space 111b, but as shown in the arrow 6c of Fig. 2, enters in cylinder 121.Afterwards, the waste gas of cylinder 121 inside via the gas outlet pipe 140 connected in the other end of cylinder 121 discharged to outside stove.
In the manufacture method using above-mentioned annealing device 100, separate the interval of the end in rotating shaft (the combustion chamber axle C) direction of combustion chamber flange part 116, combustion chamber flange part 118 and rotary body 120 with dividing plate 170.Separate this interval, and the face of film body to the superconduction predecessor be wrapped on rotary body 120, from the position supply environment gas separated up.In addition, the film body of superconduction predecessor is, substrate forms intermediate layer, is coated with on the intermediate layer and the metal organic acid salt or organo-metallic compound that comprise metallic element are dissolved in the mixed solution obtained in organic solvent, utilize presintering afterwards and the film body formed.Further, the metal organic acid salt comprising metallic element in mixed solution is made up of more than one being selected from caprylate, naphthenate, neodecanoate or trifluoroacetate.Manufactured oxide superconducting wire rod possesses: be formed in the intermediate layer on substrate, formation REBa on the intermediate layer
ycu
3o
zthe stabilized zone being superconducting layer and being formed on superconducting layer, RE is made up of more than one the element being selected from Y, Nd, Sm, Eu, Gd and Ho.
As mentioned above, in furnace core tube 110, during to the face of the film body of the banded wire rod 20 be wrapped on rotary body 120 from the position supply environment gas 6 separated up, in the central space 111a separated by dividing plate 170, from gas squit hole 132 (with reference to Fig. 2 ~ Fig. 4) the supply environment gas 6 of gas supply pipe 130 being configured in the total length spreading all over rotary body 120.Thus, can to the entirety of the banded wire rod 20 on the surperficial 121a of the cylinder 121 be wrapped in rotary body 120 supply environment gas 6 well.Thereby, it is possible to improve the reacted gas that discharges and HF gas purging efficiency, and can manufacture and have in the longitudinal direction evenly and the banded oxide superconducting wire rod of the superconducting characteristic of excellence.
Embodiment
In annealing device 100, gas supply pipe 130 is formed with the internal diameter of the length of 2m and 20mm, in this gas supply pipe 130, on the length direction of gas supply pipe 130, form gas squit hole 132 with the spacing of 30mm, the respective diameter (nozzle diameter) of this gas squit hole 132 is 1.0mm.Pressure in the furnace pressure of furnace core tube 11 now, i.e. heat treatment space 111 is set to 50torr to 200torr, gas flow is set to 250L/min to 1000L/min (scaled value under normal temperature, normal pressure).And, gas squit hole 132 in annealing device 100 to be sprayed and the flow velocity being supplied to the environmental gas of the surperficial 121a of rotary body 120 is set to 300m/s, gas squit hole 132 and the S separated by a distance of the surperficial 121a being configured at the rotary body 120 in annealing device 100 are set to 80mm.Moreover the film body being wound in the banded wire rod 20 of rotary body 120 is following film body, that is, the Ni alloy substrate (base material) of band shape utilize IBAD method to form Gd
2zr
2o
7intermediate layer as template, then at this Gd
2zr
2o
7on intermediate layer, sputtering method is utilized to form CeO
2intermediate layer and obtain composite base plate, and in painting process, utilize after mixed solution (superconduction material solution) coats on this composite base plate by dip coating, in presintering operation, carry out the film body of presintering, above-mentioned mixed solution (superconduction material solution) Y-TFA salt (trifluoroacetate), Ba-TFA salt and Cu-naphthenate to be dissolved in organic solvent with the ratio of Y:Ba:Cu=1:1.5:3 to form.Utilize the in-furnace temperature of 750 DEG C to carry out the heat treatment of formal sintering circuit to above-mentioned film body, obtain the superconducting layer of 1.5 μm.And, the structure being respectively provided with three pieces of dividing plates using the both end sides at rotary body 120 as embodiment 1, not establish the structure of dividing plate as comparative example 1.
The characteristic of the superconducting wire using the annealing device of above-described embodiment 1 to make is as follows: Jc is 2.2, Ic is 330A, and the characteristic of the superconducting wire utilizing comparative example 1 to make is as follows: Jc is 1.5, Ic is 225A.
Compared with the superconducting wire utilizing comparative example 1 to make, the excellent of the superconducting wire utilizing embodiment 1 to make.
As mentioned above, compared with the manufacture method of the banded oxide superconducting wire rod of the annealing device of use comparative example, use the manufacture method of banded oxide superconducting wire rod of the annealing device of embodiment can improve the discharge efficiency of HF gas (hydrogen fluoride gas), and can manufacture and have in the longitudinal direction evenly and the banded oxide superconducting wire rod of the superconducting characteristic of excellence.
Further, be the sintering of batch due to what carry out, with carry out volume to volume mode sintering situation compared with, easily control furnace inner environment, so stable superconducting layer can be formed, and oxide superconducting wire rod can be manufactured at short notice.
In addition, furnace core tube 110 by cylindrical shape combustion chamber body 114 and close the combustion chamber flange part 116 of both ends open of combustion chamber body 114 respectively, combustion chamber flange part 118 forms, at least one in combustion chamber flange part 116, combustion chamber flange part 118 can freely openable or freely load and unload relative to combustion chamber body 114, but is not limited to this.As long as inner rotary body 120 freely can be loaded and unloaded and easily carry out winding and the removal operation of banded wire rod 20, then can form in any way.Also can adopt in the furnace core tube 110 of hollow cylindrical, combustion chamber body 114 is divided into the structure of semicircle shape.
In addition, about the invention described above, only otherwise depart from the spirit of the present invention, then can carry out various change, certainly, the present invention contain carry out this change after invention.
The disclosure of the specification, accompanying drawing and the specification digest that comprise in the Japanese publication of the Japan Patent Patent 2011-022116 that on February 3rd, 2011 files an application all is referred in the application.
Industrial applicibility
In sum, the manufacture method of banded oxide superconducting wire rod involved in the present invention and annealing device can be widely used in improving reacted gas purging efficiency and be formed and have in the longitudinal direction evenly and the situation of the banded oxide superconducting wire rod of the superconducting characteristic of excellence.
Claims (9)
1. a manufacture method for banded oxide superconducting wire rod, the annealing device wherein used comprises:
Furnace core tube, is formed the closed at both ends possessing the cylindrical body portion of heat treatment space with flange part;
Cylindric rotary body, is configured in described heat treatment space in the mode that can rotate relative to the combustion chamber axle of described furnace core tube inner, and at the banded wire rod of the surface wrap being formed with multiple through hole, described banded wire rod is formed with the film body of superconduction predecessor;
Gas supply pipe, for described banded wire rod supply environment gas; And
Gas outlet pipe, outside for described environmental gas to be expelled to described furnace core tube from described rotary body inside,
In the manufacture method of described banded oxide superconducting wire rod, use described annealing device, to the face of the described film body of the described banded wire rod be wrapped on described rotary body, supply described environmental gas from the position separated up,
Wherein, the interval dividing plate of the axial end of rotation of described flange part and described rotary body is separated, and described environmental gas is supplied to the face of the described film body of the described banded wire rod be wrapped on described rotary body.
2. the manufacture method of banded oxide superconducting wire rod as claimed in claim 1, wherein,
Be configured with dividing plate described in polylith.
3. the manufacture method of banded oxide superconducting wire rod as claimed in claim 1 or 2, wherein,
The film body of described superconduction predecessor is, substrate forms intermediate layer, and after mixed solution being coated on described intermediate layer, the film body formed by presintering, described mixed solution is that the metal organic acid salt or organo-metallic compound that comprise metallic element are dissolved in the mixed solution obtained in organic solvent.
4. the manufacture method of banded oxide superconducting wire rod as claimed in claim 3, wherein,
The described metal organic acid salt comprising metallic element in described mixed solution is made up of more than one the salt being selected from caprylate, naphthenate, neodecanoate or trifluoroacetate.
5. the manufacture method of banded oxide superconducting wire rod as claimed in claim 1, wherein,
Described oxide superconducting wire rod comprises:
Be formed in the intermediate layer on substrate;
Be formed in the REBa on described intermediate layer
ycu
3o
zit is superconducting layer; And
Be formed in the stabilized zone on described superconducting layer,
Described RE is made up of more than one the element being selected from Y, Nd, Sm, Eu, Gd and Ho.
6. an annealing device for banded oxide superconducting wire rod, comprising:
Furnace core tube, is formed the closed at both ends possessing the cylindrical body portion of heat treatment space with flange part;
Cylindric rotary body, is configured in described heat treatment space in the mode that can rotate relative to the combustion chamber axle of described furnace core tube inner, and at the banded wire rod of the surface wrap being formed with multiple through hole, described banded wire rod is formed with the film body of superconduction predecessor;
Gas supply pipe, is configured in the face relative to the described film body of the described banded wire rod be wrapped on described rotary body and the position separated up, and for described face supply environment gas; And
Gas outlet pipe, discharges reacted gas from described rotary body inside,
Wherein, in described furnace core tube, be equipped with dividing plate, described dividing plate is for the interval of the axial end of rotation that separates described flange part and described rotary body.
7. the annealing device of banded oxide superconducting wire rod as claimed in claim 6, wherein,
Be configured with dividing plate described in polylith.
8. the annealing device of banded oxide superconducting wire rod as claimed in claims 6 or 7, wherein,
Described dividing plate is inserted the axle portion of described rotary body, and described dividing plate is fixed on described axle portion.
9. the annealing device of banded oxide superconducting wire rod as claimed in claim 6, wherein,
The rotation axial end noncontact of described dividing plate and described rotary body and relatively near configuring.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011022116A JP5837751B2 (en) | 2011-02-03 | 2011-02-03 | Tape-like oxide superconducting wire manufacturing method and heat treatment apparatus |
| JP2011-022116 | 2011-02-03 | ||
| PCT/JP2012/000652 WO2012105244A1 (en) | 2011-02-03 | 2012-02-01 | Method of producing tape-form oxide superconducting wire, and heat treatment device |
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| CN103339692A CN103339692A (en) | 2013-10-02 |
| CN103339692B true CN103339692B (en) | 2016-01-20 |
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| CN201280007641.9A Active CN103339692B (en) | 2011-02-03 | 2012-02-01 | The manufacture method of banded oxide superconducting wire rod and annealing device |
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| JP (1) | JP5837751B2 (en) |
| CN (1) | CN103339692B (en) |
| TW (1) | TWI509635B (en) |
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| JP7286032B1 (en) | 2022-05-24 | 2023-06-02 | 三菱電機株式会社 | Rotating electric machine |
| KR102593634B1 (en) * | 2023-07-07 | 2023-10-26 | 주식회사 마루엘앤씨 | Wire rod deposition system |
| KR102591747B1 (en) * | 2023-07-07 | 2023-10-23 | 주식회사 마루엘앤씨 | Wire rod deposition system |
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| JPH02208209A (en) * | 1989-02-08 | 1990-08-17 | Furukawa Electric Co Ltd:The | Production of oxide superconductor precursor |
| JP2511320Y2 (en) * | 1989-12-11 | 1996-09-25 | 横河電機株式会社 | Oxide high temperature superconductor manufacturing equipment |
| JP3789341B2 (en) * | 2001-10-12 | 2006-06-21 | 財団法人国際超電導産業技術研究センター | Atmosphere controlled heat treatment furnace |
| CN1296943C (en) * | 2002-05-24 | 2007-01-24 | 住友电气工业株式会社 | Oxide superconducting wire producing method |
| JP4401992B2 (en) * | 2005-03-25 | 2010-01-20 | 財団法人国際超電導産業技術研究センター | Tape-like oxide superconducting wire manufacturing method and manufacturing apparatus thereof |
| CN100372140C (en) * | 2005-03-29 | 2008-02-27 | 清华大学 | Method for making large area uniform film or long superconducting wire and its apparatus |
| JP4468901B2 (en) * | 2006-01-13 | 2010-05-26 | 財団法人国際超電導産業技術研究センター | Heat treatment equipment for oxide superconducting wire. |
| CN100575540C (en) * | 2006-08-28 | 2009-12-30 | 北京有色金属研究总院 | Batch preparation of double-faced high-temperature superconducting film device |
| JP4876044B2 (en) * | 2007-08-16 | 2012-02-15 | 財団法人国際超電導産業技術研究センター | Heat treatment apparatus for oxide superconducting wire and method for manufacturing the same |
| CN101471161B (en) * | 2007-12-28 | 2010-12-08 | 北京有色金属研究总院 | Method for producing high-temperature superconducting thin film by tri-fluorate |
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| CN103339692A (en) | 2013-10-02 |
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| JP2012164443A (en) | 2012-08-30 |
| TWI509635B (en) | 2015-11-21 |
| TW201237889A (en) | 2012-09-16 |
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