CN101465178B - High-performance bismuth series high-temperature superconducting strip and preparation method thereof - Google Patents
High-performance bismuth series high-temperature superconducting strip and preparation method thereof Download PDFInfo
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- CN101465178B CN101465178B CN200910103047XA CN200910103047A CN101465178B CN 101465178 B CN101465178 B CN 101465178B CN 200910103047X A CN200910103047X A CN 200910103047XA CN 200910103047 A CN200910103047 A CN 200910103047A CN 101465178 B CN101465178 B CN 101465178B
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Abstract
The invention relates to a bismuth system high temperature superconducting tape and the preparation method thereof. The tape consists of a metal sheath and a superconducting core positioned in the metal sheath; the main phase of the superconducting core is (Bi, Pb)2Sr2Ca2Cu3Oy; the weight percentage content of the main phase is 75 to 98 percent of the superconducting core; the second phase is anytwo among CuO, (Ca, Sr)2CuO3, (Ca, Sr)14Cu24O41, Bi2Sr2CuO6, Ca2PbO4, SrCaCuO, CaCuO and Pb3Sr2.5Bi0.5Ca2CuOy, or more than two combinations; the weight percentage content of the second phase is 2 to25 percent of the superconducting core; and the material of the metal sheath is silver or silver alloy. By adopting the method, the prepared bismuth system high temperature superconducting tape has the advantages of high performance and relative high critical current density.
Description
Technical field
The present invention relates to a kind of with BSCCO-2223 (promptly (and Bi, Pb)
2Sr
2Ca
2Cu
3O
y) be high-performance bismuth series high-temperature superconducting strip of principal phase and preparation method thereof.
Background technology
Bi-based high-temperature superconductive strip is present unique high temperature superconducting materia that is produced on a large scale.The research and development of products such as the hyperconductive cable that the application Bi-based high-temperature superconductive strip is made, superconducting motor, superconductive current limiter, superconduction magnetic separator, superconductive energy storage system have obtained important breakthrough, and numerous items has entered the model machine trial run stage.But also wherein seldom a part of product just that can coming into the market application.
The preparation method of Bi-based high-temperature superconductive (Bi-2223/Ag) band is filled into the superconducting precursor powder end in silver or the silver alloy sleeve pipe earlier, be processed into the shape (as line or belt etc.) of technological requirement then by a series of mechanical deformation (swage, drawing and rolling etc.), carry out heat treatment or repetitious thermomechanical treatment again, the Bi-based high-temperature superconductive strip that obtains having certain superconductivity at last.Utilize said method, the bismuth that can prepare length at present and be the km level is a multi-core high temperature superconducting tape, and has realized industrialization.
Owing to adopt in the process of tube plug drawing mill of method for preparing Bi-based high-temperature superconductive strip, the superconduction crystal grain of sheet is broken under the effect of pressure in the superconducting precursor powder end, the size of crystal grain diminishes gradually, when finishing to process of tube plug drawing mill, the size of crystal grain is generally below 0.2 micron, and the shape of crystal grain is a column or spherical etc. by the sheet fragmentation.In the operation of rolling subsequently, the orientation of column or spherical crystal grain is at random, and this will have influence on, and the superconduction intergranule connects in the final superconducting tape, has had a strong impact on the raising of the critical current density of Bi-based high-temperature superconductive strip.Therefore at present, the tidemark of other long band critical current density of km level is about 40000A/cm
2, this numerical value is apart from its theoretical value (10
5A/cm
2～10
6A/cm
2) remain the difference on the order of magnitude.
Summary of the invention
The purpose of this invention is to provide a kind of high-performance bismuth series high-temperature superconducting strip and preparation method thereof.Adopt the inventive method can prepare high performance Bi-based high-temperature superconductive strip, described band has higher critical current density.
Technical scheme of the present invention is:
Described band is made up of metallic sheath and the superconducting core that is positioned at metallic sheath, described superconducting core principal phase be (Bi, Pb)
2Sr
2Ca
2Cu
3O
y, its weight percent content be 75～98%, second of superconducting core be mutually CuO, (Ca, Sr)
2CuO
3, (Ca, Sr)
14Cu
24O
41, Bi
2Sr
2CuO
6, Ca
2PbO
4, SrCaCuO, CaCuO, Pb
3Sr
2.5Bi
0.5Ca
2CuO
yIn any two kinds or two or more combinations, its weight percent content is 2～25% of a superconducting core; Described metallic sheath is silver or silver alloy.
The preparation method of high-performance bismuth series high-temperature superconducting strip has the following steps:
1) the described superconducting precursor powder end with superconducting core composition of claim 1 is pressed into column, pack in silver or the silver alloy sleeve pipe, through obtaining single core circle line behind the draw of multi-pass, divide round wire rod again equally for plurality of sections, pack in another metal sleeve, obtain multicore circle line behind the process draw of multi-pass;
2) the multicore circle wire rod of step 1) preparation is 600～840 ℃ in temperature, the partial pressure of oxygen is to carry out the heat treatment first time under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～30 hour, and the crystallite dimension that makes the superconducting phase in the wire rod is greater than 1 micron;
3) step 2) Zhi Bei multicore wire rod is rolled into 15～80% the band that thickness is gauge or diameter of wire; the band of gained carries out the heat treatment second time; heat treated holding temperature is 600～840 ℃, and the partial pressure of oxygen is 0.01～0.21atm in the protective atmosphere, and the heat treatment temperature retention time is 1～30 hour
4) rolling step 3) gained band obtains thickness and is 0.2～0.4 millimeter multi-core superconducting wire rod;
5) the multi-core superconducting wire rod of step 4) preparation is 800～850 ℃ in temperature, the partial pressure of oxygen is to carry out heat treatment for the third time under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～20 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the wire rod is 30～80%;
6) machine work;
7) the multicore band of step 6) preparation is 800～850 ℃ in temperature, the partial pressure of oxygen is to carry out the 4th heat treatment under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～80 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the wire rod is 75～98%;
8) the multicore band of step 7) preparation carries out the after annealing processing; the temperature that after annealing is handled is 600～840 ℃; the partial pressure of oxygen is 0.01～0.21atm in the protective atmosphere, and heat treatment time is 1～20 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the wire rod is 75～98%.
Phase content of the present invention is measured with X-ray diffraction method.
Protective gas of the present invention is argon gas and oxygen or nitrogen and oxygen.
Adopt preparation method of the present invention, in the band machining process,, improve the arrangement situation of superconduction crystal grain and the connection state of superconduction intergranule, thereby reach the purpose of the critical current density that improves superconducting tape by control to superconduction crystal grain.By the first time and heat treatment for the second time, make the BSCCO-2212 grain growth in the superconducting core, making it the column when draw finishes, spherical equigranular is the lamella size greater than 1 micron bigger crystal grain less than 0.2 micron grain growth, in twice operation of rolling subsequently, the superconduction crystal grain of sheet rotates, the crystal grain of sheet tends to and is arranged in parallel in the face of rolling, and having improved bismuth is the texture degree of superconduction crystal grain.With the 4th heat treatment, in superconducting core, produce a certain amount of BSCCO-2223 superconducting phase for the third time.And after annealing heat treatment reduces the amorphous content in the superconducting core, adjusts the oxygen content in the superconducting phase, further improves the switching performance of superconduction intergranule.Therefore, adopting the bismuth of the inventive method preparation is that superconducting tape has improved critical current density.
In a word, utilize that superconduction crystal grain has higher texture degree in the Bi-based high-temperature superconductive strip that the present invention prepares, intergranule has connection state preferably, thereby the Bi-based high-temperature superconductive strip of preparation has higher critical current density.
Description of drawings
Fig. 1 is a high-performance bismuth series superconducting tape preparation technology schematic diagram;
The schematic diagram that Fig. 2 adopts band of the present invention (line) material cross section to change.
Among the figure, 1 for bismuth is the superconducting precursor powder end, and 2 is silver-colored sleeve pipe.
Embodiment
Embodiment 1
Referring to Fig. 1.With single-core line (band) material is example, and getting principal phase is BSCCO-2212 forerunner's powder 15g, and forerunner's powder 1 is pressed into column, pack in the silver-colored sleeve pipe 2, then through the draw distortion of multi-pass (referring to Ueyama M, Hikata T, Kato K, et al.Microstructures and J
c-BCharacteristics of Ag-Sheathed Bi-Based Superconducting Wires.Jpn.J.Appl.Phys.1991,30:L1384-L1386) become the wire rod that single core is justified line, pack into after the wire rod of gained is divided into 37 sections in the silver alloy sleeve pipe, obtaining diameter through the draw of multi-pass again is 1.5 millimeters multicore wire rod.Referring to Fig. 2, this multicore wire rod is carried out the heat treatment first time (HT1) at 650 ℃, argon gas and oxygen or nitrogen and oxygen are done protective gas, and partial pressure of oxygen is 0.02atm, and heat treatment time is 10 hours.Then, wire rod rolling is become the band of 0.6mm (thick) * 2.5mm (wide).This band is carried out the heat treatment second time under 650 ℃, the time is 10 hours (HT2), and wherein argon gas and oxygen or nitrogen and oxygen are done protective gas, and partial pressure of oxygen is 0.02atm.Then wire rod rolling is become the band of size 0.25mm (thick) * 4.0mm (wide).The superconducting tape intercepted length of above-mentioned preparation is that the short sample of 5 about 4.5cm carries out heat treatment for the third time (HT3) in atmosphere control stove; do protective gas at argon gas and oxygen or nitrogen and oxygen; 0.10atm the partial pressure of oxygen condition under; be warming up to 800 ℃, 810 ℃, 820 ℃, 830 ℃, 840 ℃ respectively by room temperature, heating rate is 150 ℃/hour.After insulation 20 hours, reduce to room temperature with 100 ℃/hour speed.Then the sample after the above-mentioned heat treatment is suppressed under the pressure of 1.5GPa.Sample is carried out the 4th heat treatment, and the technological parameter of each sample is identical with HT3 among the HT4.At last, all samples is carried out after annealing at 780 ℃ handle under the partial pressure of oxygen of 0.1atm, temperature retention time is 20 hours.With the critical current (77K, self-fields) of standard four leads method measuring samples, five sample critical electric currents are respectively 80A, 88A, 95A, 80A, 76A.
Embodiment 2
With principal phase is that forerunner's powder 20 gram of BSCCO-2212 is pressed into column and packs in the silver-colored sleeve pipe, obtain the round wire rod of single core through mechanical deformation, the round wire rod of gained is divided equally in the silver alloy sleeve pipe of packing into after being 61 sections, and to become diameter be 1.6 millimeters multicore garden wire rod to draw again.This multicore wire rod is heat-treated (HT1) at 820 ℃, and argon gas and oxygen or nitrogen and oxygen are done protective gas, and partial pressure of oxygen is 0.2atm, and heat treatment time is 25 hours.Then, wire rod rolling is become the band of 1.0mm (thick) * 1.5mm (wide).In 820 ℃ of heat treatments 25 hours (HT2), argon gas and oxygen or nitrogen and oxygen are done protective gas with this band, and partial pressure of oxygen is 0.2atm.Then wire rod rolling is become the band of size 0.23mm (thick) * 4.1mm (wide).
The superconducting tape intercepted length of above-mentioned preparation is that the short sample of 5 about 4.5cm is heat-treated (HT3) in atmosphere control stove; do protective gas at argon gas and oxygen or nitrogen and oxygen; 0.01atm the partial pressure of oxygen condition under be warming up to 800 ℃ respectively by room temperature, heating rate is 200 ℃/hour.After insulation 10 hours, reduce to room temperature with 80 ℃/hour speed.Then the sample after the above-mentioned heat treatment is suppressed under the pressure of 2.0GPa.Sample is carried out the 4th heat treatment, and the technological parameter of HT4 is identical with HT3.At last, all samples is done protective gas at argon gas and oxygen or nitrogen and oxygen, carry out after annealing at 720 ℃ under the partial pressure of oxygen of 0.05atm and handle, temperature retention time is 5 hours.With the critical current (77K, self-fields) of standard four leads method measuring samples, five sample critical current averages are 100A.The content of BSCCO-2223 phase is 97% in the band.
Embodiment 3
With principal phase is that forerunner's powder 10 gram of BSCCO-2212 is pressed into column and packs in the silver-colored sleeve pipe, obtain the round line of single core then through mechanical deformation, the round line of gained is divided equally in the silver alloy sleeve pipe of packing into after being 19 sections, and to become diameter be 1.75 millimeters multicore garden wire rod to draw again.This multicore wire rod is heat-treated (HT1) at 720 ℃, and argon gas and oxygen or nitrogen and oxygen are done protective gas, and partial pressure of oxygen is 0.1atm, and heat treatment time is 10 hours.Then, wire rod rolling is become the band of 0.5mm (thick) * 0.7mm (wide).In 720 ℃ of heat treatments 15 hours (HT2), wherein argon gas and oxygen or nitrogen and oxygen are done protective gas with this band, and partial pressure of oxygen is 0.1atm.Then wire rod rolling is become the band of size 0.21mm (thick) * 4.2mm (wide).
From the superconducting tape intercepted length of above-mentioned preparation is that 10 short samples about 4.5cm are heat-treated (HT3) in atmosphere control stove; argon gas and oxygen or nitrogen and oxygen are done protective gas; be warming up to 840 ℃ respectively by room temperature under the partial pressure of oxygen condition of 0.2atm, heating rate is 100 ℃/hour.After insulation 20 hours, reduce to room temperature with 60 ℃/hour speed.Then the sample after the above-mentioned heat treatment is suppressed under the pressure of 1.0GPa.Sample is carried out the 4th heat treatment, and the technological parameter of HT4 is identical with HT3.At last, all samples is done protective gas at argon gas and oxygen or nitrogen and oxygen, carry out after annealing at 820 ℃ under the partial pressure of oxygen of 0.2atm and handle, temperature retention time is 20 hours.With the critical current (77K, self-fields) of standard four leads method measuring samples, five sample critical current averages are 86A.With the content of phase in the X-ray diffraction analysis sample, the content of BSCCO-2223 phase is 90% in the band.
Principal phase of the present invention is BSCCO-2212, second be mutually CuO, (Ca, Sr)
2CuO
3, (Ca, Sr)
14Cu
24O
41, Bi
2Sr
2CuO
6, Ca
2PbO
4, SrCaCuO, CaCuO, Pb
3Sr
2.5Bi
0.5Ca
2CuO
yIn forerunner's powder of any two kinds or two or more combinations, the kind of its second phase and content thereof can be controlled by the roasting technique condition at superconducting precursor powder end, principal phase is that forerunner's powder of BSCCO-2212 can adopt the inventive method to make high-performance bismuth series high-temperature superconducting strip of the present invention, and the gained high-performance bismuth series high-temperature superconducting strip all has performance of the present invention.
Though the present invention discloses as above with preferred embodiment; right its is not in order to limit the present invention; any person of ordinary skill in the field; without departing from the spirit and scope of the invention; when can doing a little change and improvement, so the present invention's protection range is as the criterion when looking the claim person of defining.
Claims (3)
1. the preparation method of a high-performance bismuth series high-temperature superconducting strip, described band is made up of metallic sheath and the superconducting core that is positioned at metallic sheath, described superconducting core principal phase be (Bi, Pb)
2Sr
2Ca
2Cu
3O
y, its weight percent content be 75～98%, second of superconducting core be mutually CuO or (Ca, Sr)
2CuO
3Or (Ca, Sr)
14Cu
24O
41Or Bi
2Sr
2CuO
6Or Ca
2PbO
4Or Pb
3Sr
2.5Bi
0.5Ca
2CuO
yIn any two kinds or two or more combinations, its weight percent content is 2～25% of a superconducting core, described metallic sheath is silver or silver alloy, it is characterized in that the preparation method has the following steps:
1) the superconducting precursor powder end that will have a superconducting core composition is pressed into column, pack in silver or the silver alloy sleeve pipe,, divide round wire rod again equally for plurality of sections through obtaining single core circle line behind the draw of multi-pass, pack in another metal sleeve, obtain multicore circle wire rod behind the process draw of multi-pass;
2) the multicore circle wire rod of step 1) preparation is 600～840 ℃ in temperature, the partial pressure of oxygen is to carry out the heat treatment first time under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～30 hour, and the crystallite dimension that makes the superconducting phase in the wire rod is greater than 1 micron;
3) step 2) to become thickness be 15～80% band of gauge or diameter of wire in the multicore circle wire rod rolling of preparation, the band of gained carries out the heat treatment second time, heat treated holding temperature is 600～840 ℃, the partial pressure of oxygen is 0.01～0.21atm in the protective atmosphere, and the heat treatment temperature retention time is 1～30 hour;
4) rolling step 3) gained band obtains thickness and is 0.2～0.4 millimeter multi-core superconducting wire rod;
5) the multi-core superconducting wire rod of step 4) preparation is 800～850 ℃ in temperature, the partial pressure of oxygen is to carry out heat treatment for the third time under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～20 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the wire rod is 30～80%;
6) machine work prepares the multicore band;
7) the multicore band of step 6) preparation is 800～850 ℃ in temperature, the partial pressure of oxygen is to carry out the 4th heat treatment under the condition of 0.01～0.21atm in the protective atmosphere, heat treatment time is 1～80 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the band is 75～98%;
8) the multicore band of step 7) preparation carries out the after annealing processing, the temperature that after annealing is handled is 600～840 ℃, the partial pressure of oxygen is 0.01～0.21atm in the protective atmosphere, and heat treatment time is 1～20 hour, and the content of the superconducting core first phase superconducting phase after the heat treatment in the band is 75～98%;
The first phase superconducting phase is above-mentioned principal phase.
2. method according to claim 1 is characterized in that: described phase content is measured with X-ray diffraction method.
3. method according to claim 1 is characterized in that: the protective gas of described protective atmosphere is argon gas and oxygen or nitrogen and oxygen.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101976599A (en) * | 2010-11-19 | 2011-02-16 | 重庆大学 | Composite reinforced Bi-based high-temperature superconductive strip and preparation method thereof |
| CN103173705B (en) * | 2013-02-01 | 2016-04-27 | 北京英纳超导技术有限公司 | A kind of method optimizing oxygen level in superconducting tape Bi-2223 phase and the superconductivity wire thus obtained |
| CN103440932B (en) * | 2013-09-14 | 2016-01-20 | 西北有色金属研究院 | A kind of preparation method of Bi system high-temperature superconducting wire/band |
| CN103617840B (en) * | 2013-09-16 | 2018-01-19 | 清华大学 | A kind of preparation method of isotropism Bi-based high-temperature superconductive fine rule |
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| CN101002291A (en) * | 2004-07-29 | 2007-07-18 | 住友电气工业株式会社 | Method for producing superconducting wire |
| CN101061555A (en) * | 2005-04-06 | 2007-10-24 | 住友电气工业株式会社 | Process for producing bismuth-based oxide superconductor, and superconductive wire |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101002291A (en) * | 2004-07-29 | 2007-07-18 | 住友电气工业株式会社 | Method for producing superconducting wire |
| CN101061555A (en) * | 2005-04-06 | 2007-10-24 | 住友电气工业株式会社 | Process for producing bismuth-based oxide superconductor, and superconductive wire |
Non-Patent Citations (5)
| Title |
|---|
| JP特开2003-203532A 2003.07.18 |
| T.-M. Qu et al.The evolution of Bi-2223 phase and liquid phase during the first heat treatment in Bi-2223/Ag superconducting tapes.《Physica C》.2008,4681767-1770. * |
| 孙树军 等.Bi-2223/Ag多芯超导薄带的制备及其性能研究.《低温物理学报》.2003,第25卷增刊197-199. |
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| 易汉平,张劲松,刘庆,韩征和.实用Bi系高温超导带材.《中国有色金属学报》.2004,第14卷专辑1341-346. * |
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