CN103236322A - Preparation method of rectangular 7-core MgB2 superconducting strip - Google Patents
Preparation method of rectangular 7-core MgB2 superconducting strip Download PDFInfo
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- CN103236322A CN103236322A CN2013101326329A CN201310132632A CN103236322A CN 103236322 A CN103236322 A CN 103236322A CN 2013101326329 A CN2013101326329 A CN 2013101326329A CN 201310132632 A CN201310132632 A CN 201310132632A CN 103236322 A CN103236322 A CN 103236322A
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Abstract
The invention discloses a preparation method of a rectangular 7-core MgB2 superconducting strip. The method includes the steps of firstly, preparing tubing precursor powder, and loading the powder into a Fe-Nb composite tube to obtain a tubing composite; secondly, hole pattern rolling or rotary forging drawing the tubing composite to obtain a single-core wire; thirdly, sizing and cutting, and scouring to remove surface scale of the single-core wire; fourthly assembling a Cu-Nb composite bar with the single-core wire in an anaerobic copper tube to obtain a 7-core composite bar; fifthly drawing the 7-core composite bar, hole pattern rolling the drawn 7-core composite bar, vacuum annealing the rolled 7-core composite bar, drawing the annealed 7-core composite bar into a circular wire, and subjecting the circular wire to 3-5 rectangular dies to obtain the rectangular 7-core MgB2 strip; and sixthly, performing phase thermal treatment, and cooling to obtain the rectangular 7-core MgB2 superconducting strip. The critical current density Jc of the prepared 7-core MgB2 superconducting strip can reach more than 2.6*104A/cm<2> at 20K, 1T.
Description
Technical field
The invention belongs to superconductor processing engineering technology field, be specifically related to a kind of rectangle 7 core MgB
2The preparation method of superconducting tape.
Background technology
MgB
2Greatly, there are not advantages such as the weak connection of crystal boundary in superconductor owing to its critical temperature height (Tc=39K), coherence length, the preparation of its wire strip is the research emphasis of domestic and international each scientific research group always, and the selection of sheath material is the problem that must solve for the high performance wire strip of preparation, sheath material must be able to bear certain intensity and bendable curvature, and have superior thermal stability and a cheap cost, simultaneously, need avoid and starting powder generation chemical reaction, to guarantee to obtain high critical current densities, result of study finds to adopt the Fe pipe can make MgB
2Superconducting core has very high density, and the Fe pipe is more smooth with the interface of superconducting core, but the Fe pipe can generate the iron boron compound with the B reaction, and Ta and Nb then can not react with forerunner's powder, but the density for preparing wire rod is lower, and price is higher simultaneously.
At present, at multicore MgB
2Wire strip prepares the aspect, the main flow technology of preparing comprises with U.S. Hyper Tech. company being the continuous filling molding technology of representative in the world, it is CTFF (Continuous Tube Forming Filling) technology, be the powder tiretube process technology of representative, i.e. PIT(Powder In Tube with Italian Columbus Superconductor company and NW China non-ferrous metal research institute) technology.The PIT technology is divided into earlier two kinds of position methods (ex-situ) and in-situ method (in-situ).Ex-situ PIT technology adopts the MgB after being reacted into mutually
2Directly pack in the metal tube as pioneer's powder, be prepared into the wire strip of certain size by swage drawing or rolling mill practice.The characteristics of this technology are that technology is simple, are fit to very much mass production.But because MgB
2Material has the fragility of similar pottery, can cause the MgB in the wire rod in the cold working process
2The core silk forms gross imperfections such as crackle, causes the wire strip performance sharply to reduce.In-situ PIT technology adopts Mg powder and B powder to press MgB
2The atomicity ratio pack in the metal tube, be prepared into the wire rod of certain size by drawing, rolling mill practice, heat-treat again, finally in wire rod, generate MgB
2Phase.The advantage of In-situ PIT technology is that Mg fusing back is reacted into phase with B in heat treatment process, thereby can make formed micro-crack in the course of processing up, the MgB in the final wire rod
2Superconducting phase crystal grain connects better, simultaneously, and in order to improve the critical current density of wire strip under magnetic field, need to introduce effective doped chemical, and the TiC doping is one of effective alloy of generally acknowledging at present, studies show that, TiC will generate the TiB of nanometer with the B reaction under lower temperature
2Particle, C then substitute the B into MgB that mixes
2Lattice in.The C atom substitutes the B atom, has increased lattice distortion and the internal stress of B layer atom, thereby has strengthened MgB
2The intracell electron scattering has improved upper critical field (Hc
2) and irreversible (Hirr), cause MgB
2The critical current density of superconducting line strips (Jc) significantly improves under the highfield, simultaneously the TiB of Sheng Chenging
2Disperse is distributed in the crystal boundary place, can be used as the Jc of pinning center's raising wire strip under magnetic field effectively.
All there is problem more or less in single barrier material, and just reacting together with B in lower temperature such as Fe generates FeB
xCompound, the superconductivity of reduction material, yet the mechanical strength height of Fe, the core silk density height of preparation band; If adopt single Ta or Nb, then cost is higher, and such barrier material mechanical strength is lower, causes final core silk density lower, is unfavorable for improving the superconductivity of band.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, and a kind of rectangle 7 core MgB are provided
2The preparation method of superconducting tape.Single-core wire of the present invention adopts Nb as interior barrier layer, can avoid B with the chemical reaction between the interior barrier layer, and outsourcing material adopts pure Fe, can improve the core silk density of preparation band, thereby improve the current capacity of band, the structure that adopts central copper niobium compound bar to strengthen during the single-core wire assembling, generation of defects and development have been suppressed to a great extent, simultaneously because the center intensity height, and outer jacket adopts pure Fe, intensity is also higher, is conducive to improve the densification degree of core silk, efficient hardening MgB
2Crystal grain connectivity, thereby the critical current density of raising multicore band.Suitable excessive magnesium powder can make the processing crackle up in the tubulature forerunner powder of the present invention, improves the connectivity of intergranule, can reduce the porosity in the band simultaneously to a certain extent, improves the current-carrying area of superconductor, increases its critical current capacity.Adopt the rectangle 7 core MgB of method preparation of the present invention
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.6 * 10
4A/cm
2More than.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of rectangle 7 core MgB
2The preparation method of superconducting tape is characterized in that, this method may further comprise the steps:
Step 4, the single-core wire after pickling in a Cu-Nb compound bar and the six roots of sensation step 3 packed into assemble in the oxygen-free copper pipe, obtain 7 core compound bar, wherein the Cu-Nb compound bar is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire is along the circumferential direction around the Cu-Nb compound bar; Size and the single-core wire of described Cu-Nb compound bar are measure-alike;
Step 5, pass reduction with 15%～20% carries out the drawing processing of 3～5 passages to 7 core compound bar described in the step 4, with 10%～15% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 8～10 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.6mm～2.0mm through 7 core compound bar of annealing in process with 10%～15% pass reduction again, it is 0.8mm～1.2mm that last pass reduction with 8%～10% is drawn into thickness with described circular wire rod through 3～5 rectangular mould, and width is the rectangle 7 core MgB of 1.8mm～3.5mm
2Band;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 2h～4h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 10 ℃/min～20 ℃/min, and becoming mutually heat treated temperature is 650 ℃～800 ℃, and temperature retention time is 15min～120min.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the quality purity of the powder of magnesium described in the step 1 is 99.8%, and the granularity of magnesium powder is-500 orders, and the quality purity of described amorphous boron powder is not less than 99%, and the quality purity of described micron order TiC powder is 99%.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the Fe pipe is the outer tube of Fe-Nb multiple tube in the multiple tube of Fe-Nb described in the step 1, and the wall thickness of Fe pipe is 1.0mm～1.5mm, and the mass content of Fe is not less than 99.9% in the Fe pipe; The Nb pipe is the inner layer pipe of Fe-Nb multiple tube in the Fe-Nb multiple tube, and the wall thickness of Nb pipe is 0.8mm～1.0mm, and the mass content of Nb is not less than 99.9% in the Nb pipe.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the diameter that has the single-core wire of circular cross-section described in the step 2 is 4mm～6mm, the described cross section length of side with single-core wire of regular hexagonal section is 2mm～3mm.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the residual resistivity of oxygen-free copper pipe described in the step 4 is not less than 80, and the internal diameter of oxygen-free copper pipe is 15mm～24mm, and wall thickness is 1.5mm～3mm.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the compound bar of Cu-Nb described in the step 4 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.6～0.8.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the pressure that vacuum annealing described in the step 5 is handled is not more than 0.2Pa, and annealing temperature is 450 ℃～500 ℃, and annealing time is 1h～2h.
Above-mentioned a kind of rectangle 7 core MgB
2The preparation method of superconducting tape, the feeding speed of argon gas described in the step 6 is 300mL/min～500mL/min.
The present invention compared with prior art has the following advantages: the present invention is based on In-situ PIT technology, select for use metal Nb as interior barrier layer, pure Fe prepares single-core wire as outer sheath material, it is outer liptinite that multicore complex outsourcing material is selected oxygen-free copper for use, the center adopts the Cu-Nb compound bar to strengthen structure, prepare the rectangular multi-core band in conjunction with drawing and two kinds of process technologies of groove rolling, major advantage of the present invention comprise following some:
1, the present invention adopts Nb as interior barrier layer, can avoid B with the chemical reaction between the interior barrier layer, and outsourcing material adopts pure Fe, can improve the core silk density of preparation band, thereby improves the current capacity of band.
2, the present invention adopts the technology path that drawing and groove rolling combine, and when improving superconducting core silk density, can improve intercrystalline connectivity, the MgB that makes preparation
2Multicore band current-carrying performance further improves.
3, the present invention adopts the structure that central copper niobium compound bar strengthens, and has suppressed generation of defects and development to a great extent, and simultaneously owing to the center intensity height, and outer jacket adopts pure Fe, and intensity is also higher, is conducive to improve the densification degree of core silk, efficient hardening MgB
2Crystal grain connectivity, thereby the critical current density of raising multicore band.
4, suitable excessive magnesium powder can make the processing crackle up in the tubulature forerunner powder of the present invention, improves the connectivity of intergranule, can reduce the porosity in the band simultaneously to a certain extent, improves the current-carrying area of superconductor, increases its critical current capacity.
5, the band that adopts this method to prepare has the contour structures of rectangle, and more circular wire rod more is conducive to the preparation of practicability magnet.
6, the rectangle 7 core MgB of the present invention's preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.6 * 10
4A/cm
2More than.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is that the embodiment of the invention 1, embodiment 2 and embodiment 3 assemble the structural representation of the 7 core compound bar that obtain.
Fig. 2 is that the embodiment of the invention 4, embodiment 5 and embodiment 6 assemble the structural representation of the 7 core compound bar that obtain.
Description of reference numerals:
1-single-core wire; 2-Cu-Nb compound bar; 3-oxygen-free copper pipe.
Embodiment
Step 4, as shown in Figure 1, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 that diameter is the 4mm circular cross-section single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 15mm, and wall thickness is 1.5mm; Described Cu-Nb compound bar 2 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.6;
Step 5, the pass reduction with 15% carry out the drawing processing of 5 passages to 7 core compound bar described in the step 4, with 10% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 10 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.6mm through 7 core compound bar of annealing in process with 10% pass reduction again, at last with 8% pass reduction with described circular wire rod through 5 rectangular mould, obtaining thickness is 0.8mm, and width is the rectangle 7 core MgB of 1.8mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 450 ℃, and annealing time is 2h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 4h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 10 ℃/min, and becoming mutually heat treated temperature is 650 ℃, and temperature retention time is 120min; The feeding speed of described argon gas is 300mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.6 * 10
4A/cm
2
Step 4, as shown in Figure 1, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 that diameter is the 6mm circular cross-section single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 24mm, and wall thickness is 3mm; Described Cu-Nb compound bar 2 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.8;
Step 5, the pass reduction with 20% carry out the drawing processing of 3 passages to 7 core compound bar described in the step 4, with 15% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 8 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 2.0mm through 7 core compound bar of annealing in process with 15% pass reduction again, at last with 10% pass reduction with described circular wire rod through 3 rectangular mould, obtaining thickness is 1.2mm, and width is the rectangle 7 core MgB of 1.9mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 500 ℃, and annealing time is 1h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 2h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 20 ℃/min, and becoming mutually heat treated temperature is 800 ℃, and temperature retention time is 15min; The feeding speed of described argon gas is 500mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 3.2 * 10
4A/cm
2
Step 4, as shown in Figure 1, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 that diameter is the 5mm circular cross-section single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 20mm, and wall thickness is 2mm; Described Cu-Nb compound bar 2 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.7;
Step 5, the pass reduction with 18% carry out the drawing processing of 4 passages to 7 core compound bar described in the step 4, with 12% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 9 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.8mm through 7 core compound bar of annealing in process with 13% pass reduction again, at last with 9% pass reduction with described circular wire rod through 4 rectangular mould, obtaining thickness is 1.0mm, and width is the rectangle 7 core MgB of 3.5mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 480 ℃, and annealing time is 1.5h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 3h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 15 ℃/min, and becoming mutually heat treated temperature is 700 ℃, and temperature retention time is 60min; The feeding speed of described argon gas is 400mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.7 * 10
4A/cm
2
Embodiment 4
Step 4, as shown in Figure 2, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 of regular hexagonal section that the length of side is 2mm the single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 17mm, and wall thickness is 2.5mm; Described Cu-Nb compound bar is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.7;
Step 5, the pass reduction with 18% carry out the drawing processing of 4 passages to 7 core compound bar described in the step 4, with 12% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 10 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.8mm through 7 core compound bar of annealing in process with 12% pass reduction again, at last with 9% pass reduction with described circular wire rod through 4 rectangular mould, obtaining thickness is 0.9mm, and width is the rectangle 7 core MgB of 2.0mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 480 ℃, and annealing time is 1.5h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 3h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 20 ℃/min, and becoming mutually heat treated temperature is 750 ℃, and temperature retention time is 45min; The feeding speed of described argon gas is 400mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.9 * 10
4A/cm
2
Embodiment 5
Step 4, as shown in Figure 2, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 of regular hexagonal section that the length of side is 3mm the single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 24mm, and wall thickness is 3mm; Described Cu-Nb compound bar 2 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.8;
Step 5, the pass reduction with 20% carry out the drawing processing of 3 passages to 7 core compound bar described in the step 4, with 15% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 8 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 2.0mm through 7 core compound bar of annealing in process with 15% pass reduction again, at last with 8% pass reduction with described circular wire rod through 5 rectangular mould, obtaining thickness is 0.8mm, and width is the rectangle 7 core MgB of 3.5mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 500 ℃, and annealing time is 1h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 4h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 15 ℃/min, and becoming mutually heat treated temperature is 650 ℃, and temperature retention time is 15min; The feeding speed of described argon gas is 300mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.8 * 10
4A/cm
2
Embodiment 6
Step 4, as shown in Figure 2, having in Cu-Nb compound bar 2 and the six roots of sensation step 3 of regular hexagonal section that the length of side is 2.5mm the single-core wire 1 after pickling with one packs into and assembles in the oxygen-free copper pipe 3, obtain 7 core compound bar, wherein Cu-Nb compound bar 2 is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire 1 is along the circumferential direction around Cu-Nb compound bar 2; The residual resistivity of described oxygen-free copper pipe 3 is not less than 80, and the internal diameter of oxygen-free copper pipe 3 is 15mm, and wall thickness is 1.5mm; Described Cu-Nb compound bar 2 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.6;
Step 5, the pass reduction with 15% carry out the drawing processing of 5 passages to 7 core compound bar described in the step 4, with 10% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 9 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.6mm through 7 core compound bar of annealing in process with 10% pass reduction again, at last with 10% pass reduction with described circular wire rod through 3 rectangular mould, obtaining thickness is 1.2mm, and width is the rectangle 7 core MgB of 1.8mm
2Band; The pressure that described vacuum annealing is handled is not more than 0.2Pa, and annealing temperature is 450 ℃, and annealing time is 2h;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 2h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 10 ℃/min, and becoming mutually heat treated temperature is 800 ℃, and temperature retention time is 15min; The feeding speed of described argon gas is 500mL/min.
The rectangle 7 core MgB of present embodiment preparation
2Superconducting tape is at 20K, and during 1T, critical current density jc reaches 2.8 * 10
4A/cm
2
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, every any simple modification, change and equivalent structure of above embodiment being done according to the invention technical spirit changes, and all still belongs in the protection range of technical solution of the present invention.
Claims (8)
1. the preparation method of rectangle 7 core MgB2 superconducting tapes is characterized in that this method may further comprise the steps:
Step 1, with amorphous boron powder, magnesium powder and micron order TiC powder according to Mg: B: TiC=(1+x): (2-y): the atomic ratio batching of y, ground and mixed is even in vacuum glove box, obtain tubulature forerunner powder, 0.03≤x≤0.08 wherein, 0.04≤y≤0.08, the atomicity of TiC is with the atomicity sum metering of Ti and C; Then described tubulature forerunner powder is packed in the Fe-Nb multiple tube, obtain the tubulature complex;
Step 2, the pass reduction with 10%～20% carry out groove rolling to the complex of tubulature described in the step 1, obtain having the single-core wire (1) of circular cross-section; Or with 10%～20% pass reduction to the drawing of swaging of the complex of tubulature described in the step 1, the single-core wire (1) that obtains having regular hexagonal section;
Step 3, single-core wire described in the step 2 (1) is carried out scale and blocking, surface scale is removed in pickling then;
Step 4, the single-core wire (1) after pickling in a Cu-Nb compound bar (2) and the six roots of sensation step 3 packed into assemble in the oxygen-free copper pipe (3), obtain 7 core compound bar, wherein Cu-Nb compound bar (2) is positioned at the center of 7 core compound bar, and six roots of sensation single-core wire is along the circumferential direction around Cu-Nb compound bar (2); The size of described Cu-Nb compound bar (2) and single-core wire (1) are measure-alike;
Step 5, pass reduction with 15%～20% carries out the drawing processing of 3～5 passages to 7 core compound bar described in the step 4, with 10%～15% pass reduction 7 core compound bar after drawing are carried out the groove rolling of 8～10 passages then, then handle carry out vacuum annealing through 7 core compound bar of groove rolling, to be drawn into the circular wire rod that diameter is 1.6mm～2.0mm through 7 core compound bar of annealing in process with 10%～15% pass reduction again, it is 0.8mm～1.2mm that last pass reduction with 8%～10% is drawn into thickness with described circular wire rod through 3～5 rectangular mould, and width is the rectangle 7 core MgB2 bands of 1.8mm～3.5mm;
Step 6, with the 7 core MgB of rectangle described in the step 5
2The sealed at both ends protection of band is placed in the tube furnace, feeds argon gas 2h～4h earlier in tube furnace, then keeping heating tube furnace under the constant condition of argon gas feeding speed, to the rectangle 7 core MgB of sealed at both ends protection
2Band becomes phase heat treatment, with obtaining rectangle 7 core MgB after the stove cooling
2Superconducting tape; The heating rate of described heating is 10 ℃/min～20 ℃/min, and becoming mutually heat treated temperature is 650 ℃～800 ℃, and temperature retention time is 15min～120min.
2. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the quality purity of the powder of magnesium described in the step 1 is 99.8%, and the granularity of magnesium powder is-500 orders, and the quality purity of described amorphous boron powder is not less than 99%, and the quality purity of described micron order TiC powder is 99%.
3. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the Fe pipe is the outer tube of Fe-Nb multiple tube in the multiple tube of Fe-Nb described in the step 1, and the wall thickness of Fe pipe is 1.0mm～1.5mm, and the mass content of Fe is not less than 99.9% in the Fe pipe; The Nb pipe is the inner layer pipe of Fe-Nb multiple tube in the Fe-Nb multiple tube, and the wall thickness of Nb pipe is 0.8mm～1.0mm, and the mass content of Nb is not less than 99.9% in the Nb pipe.
4. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the diameter that has the single-core wire of circular cross-section described in the step 2 is 4mm～6mm, and the described cross section length of side with single-core wire of regular hexagonal section is 2mm～3mm.
5. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the residual resistivity of oxygen-free copper pipe described in the step 4 is not less than 80, and the internal diameter of oxygen-free copper pipe is 15mm～24mm, and wall thickness is 1.5mm～3mm.
6. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape, it is characterized in that, the compound bar of Cu-Nb described in the step 4 is not less than 80 oxygen-free copper and is not less than 99.9% metal niobium as the quality purity of inner layer material by the residual resistivity as cladding material to be formed, and wherein the mass ratio of oxygen-free copper and metal niobium is 1: 0.6～0.8.
7. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the pressure that vacuum annealing described in the step 5 is handled is not more than 0.2Pa, and annealing temperature is 450 ℃～500 ℃, and annealing time is 1h～2h.
8. a kind of rectangle 7 core MgB according to claim 1
2The preparation method of superconducting tape is characterized in that, the feeding speed of argon gas described in the step 6 is 300mL/min～500mL/min.
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| CN108428509A (en) * | 2018-03-30 | 2018-08-21 | 西北有色金属研究院 | A kind of graphene doping multicore MgB2The magnesium scattering preparation of superconducting wire |
| CN111164713A (en) * | 2018-01-31 | 2020-05-15 | 株式会社日立制作所 | MgB2 superconducting wire and preparation method thereof |
| CN111547769A (en) * | 2020-05-26 | 2020-08-18 | 福建师范大学 | Preparation method of high-density PSMS superconducting strip |
| CN112007949A (en) * | 2020-08-27 | 2020-12-01 | 西北有色金属研究院 | Preparation method of reinforced Cu-Nb composite wire |
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| CN107887077A (en) * | 2017-10-30 | 2018-04-06 | 西北有色金属研究院 | A kind of first position method prepares multicore MgB2The method of superconducting tape |
| CN107887077B (en) * | 2017-10-30 | 2019-04-09 | 西北有色金属研究院 | A kind of elder generation's position method prepares multicore MgB2The method of superconducting tape |
| CN111164713A (en) * | 2018-01-31 | 2020-05-15 | 株式会社日立制作所 | MgB2 superconducting wire and preparation method thereof |
| CN111164713B (en) * | 2018-01-31 | 2023-02-21 | 株式会社日立制作所 | MgB 2 Superconducting wire and method for producing same |
| CN108428509A (en) * | 2018-03-30 | 2018-08-21 | 西北有色金属研究院 | A kind of graphene doping multicore MgB2The magnesium scattering preparation of superconducting wire |
| CN111547769B (en) * | 2020-05-26 | 2022-08-30 | 合肥夸夫超导科技有限公司 | Preparation method of high-density PSMS superconducting strip |
| CN111547769A (en) * | 2020-05-26 | 2020-08-18 | 福建师范大学 | Preparation method of high-density PSMS superconducting strip |
| CN112007949A (en) * | 2020-08-27 | 2020-12-01 | 西北有色金属研究院 | Preparation method of reinforced Cu-Nb composite wire |
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| CN113571254A (en) * | 2021-08-05 | 2021-10-29 | 西北有色金属研究院 | Superfine cored wire multicore MgB2Method for preparing superconducting wire strip |
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