CN102522153A - Preparation method of multi-core MgB2 superconducting wire - Google Patents

Preparation method of multi-core MgB2 superconducting wire Download PDF

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CN102522153A
CN102522153A CN201110327753XA CN201110327753A CN102522153A CN 102522153 A CN102522153 A CN 102522153A CN 201110327753X A CN201110327753X A CN 201110327753XA CN 201110327753 A CN201110327753 A CN 201110327753A CN 102522153 A CN102522153 A CN 102522153A
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oxygen
wire
core wire
free copper
powder
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CN102522153B (en
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闫果
刘国庆
孙昱艳
焦高峰
冯建情
王庆阳
杨芳
李成山
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Northwest Institute for Non Ferrous Metal Research
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Abstract

The invention discloses a preparation method of a multi-core MgB2 superconducting wire. The method comprises: first, precursor power is prepared; second, the precursor power is placed in a Ta tube to prepare a tubulation complex; third, groove rolling is carried out on a single core wire; fourth, a NbTi/Cu composite rod and a plurality of single core wires are placed in an oxygen-free copper tube for assembling so as to obtain a secondary composite rod; fifth, rotary swaging and drawing are carried out on the secondary composite rod, groove rolling is carried out and rotary swaging and drawing are carried out again, so that a multi-core wire is obtained; and sixth, heat treatment is carried out on the multi-core wire to obtain a multi-core MgB2 superconducting wire. According to the invention, processes of rotary swaging, drawing and groove rolling are combined and employed; therefore, not only is density of the multi-core wire improved, but also connectivity between crystal grains can be improved; it is beneficial to prepare a multi-core MgB2 superconducting wire with high performances; and the prepared wire has high mechanical strength and can bear great stress and strain without obvious reduction of the superconductive current carrying performance, so that a superconducting wire practical requirement can be well met.

Description

A kind of multicore MgB 2The preparation method of superconducting wire
Technical field
The invention belongs to superconductor processing engineering technology field, be specifically related to a kind of multicore MgB 2The preparation method of superconducting wire.
Background technology
MgB 2Superconductor is since calendar year 2001 is found; Because its critical temperature is 39K, has coherence length and greatly, do not have advantages such as the weak connection of crystal boundary, scientist's concern extremely both at home and abroad; On a large amount of, the systematic research of having passed through 10 years is basic, find that element doping is to improve MgB 2The effective means of wire rod High-Field current capacity, and the TiC doping is the most effectively one of the alloy of generally acknowledging at present.MgB 2It is the emphasis of research that the wire rod preparation that practicability requires is especially satisfied in wire rod preparation always, and at present, a plurality of in the world producers (like U.S. Hype Tech company, Italian Columbus company etc.) have possessed mass provides the km level MgB near practicability 2The multicore wire rod.What U.S. Hype Tech company was adopted is continuous pipeline forming (CTFF:Continuous Tube Forming Filling) technology, and the complicated and expensive equipment of this arts demand has only scientific research institution of several family to adopt this technology both at home and abroad as the basis.What Italy Columbus company adopted is traditional powder tiretube process (PIT) technology, and this technology is simple, and is easy to operate, is to prepare the MgB2 wire rod at present to adopt maximum technology.
CTFF technology preparation MgB 2Superconducting wire is directly with MgB 2Powder places on the metal tape, and the method through continuous coating welded tube is prepared into wire rod, under argon shield, heat-treats then.This techniqueflow once was used for the Bi based high-temperature superconductive strip, and technology is also ripe relatively, but has comparatively shortcomings such as complicacy, cost height of process equipment, only had few studies unit to adopt this prepared MgB2 wire strip at present.Powder tiretube process (PIT) is preparation MgB 2One of major technique of wire rod, PIT technology processing MgB 2Wire rod mainly contains two kinds of technology paths, i.e. elder generation's position method (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, through the wire rod of swaging, drawing and rolling mill practice are prepared into certain size.These technological characteristics are that technology is simple, are fit to very much mass production.But because MgB 2Material has the fragility of similar pottery, and ex-situ PIT prepares the high-intensity Fe base of needs use sheath material in the process, to MgB 2The core silk applies enough stress constraints and connects to strengthen crystal grain.Simultaneously, 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 rod 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 through 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 mutually 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.But because a lot of sheath material comprises Nb commonly used, Fe etc.; When heat treatment temperature is higher (greater than 750 degree); Chemical reaction will take place with Mg or B in sheath material; Generate certain thickness diffusion layer, the existence of this diffusion layer will be played inhibitory action to the wire rod critical current density, and because the carbon atom in the low TiC alloy of heat treatment temperature is difficult to replace boron position atom; And the TiC alloy can only be present in the crystal boundary place as the two-phase particle, is difficult to obviously improve the critical current density of wire rod under High-Field.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art, provides a kind of employing drawing of swaging to combine with groove rolling and prepare multicore MgB 2The method of superconducting wire.Adopt the wire rod of method of the present invention preparation to have higher mechanical strength, can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of multicore MgB 2The preparation method of superconducting wire is characterized in that, this method may further comprise the steps:
Step 1, magnesium powder, amorphous boron powder and the sodium rice TiC powder atomic ratio according to Mg: B: TiC=1: (2-x): x is mixed, then that mixture ground and mixed under argon shield is even, obtain forerunner's powder; The value of said x is 0.02～0.10;
Step 2, the powder of forerunner described in the step 1 is packed in the Ta pipe after the pickling processes, the Ta pipe that forerunner's powder will be housed is then packed in the oxygen-free copper pipe after the pickling processes, makes the tubulature complex;
Step 3, the complex of tubulature described in the step 2 is carried out groove rolling, obtain having the single-core wire of circular cross-section, single-core wire is carried out scale successively, blocks and pickling; The pass reduction of said groove rolling is 10%～20%;
Step 4, place oxygen-free copper pipe after the pickling processes to carry out the secondary assembling single-core wire after the pickling in NbTi/Cu compound bar and 6 or 12 step 3 to obtain the secondary compound bar; Said NbTi/Cu compound bar is by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material; The mass ratio of said oxygen-free copper and niobium titanium alloy is 1: 0.8～1.2; The residual resistivity of said oxygen-free copper is not less than 80; The quality percentage composition of niobium is 45%～55% in the said niobium titanium alloy, and surplus is a titanium; NbTi/Cu compound bar in the said secondary assembling process after the pickling places the oxygen-free copper pipe center after the pickling processes, and the single-core wire after the pickling along the circumferential direction NbTi/Cu compound bar after the pickling is arranged in circular ring and packs in the oxygen-free copper pipe after the pickling processes; When the quantity of said single-core wire is 6, the size of said NbTi/Cu compound bar and single-core wire measure-alike; When the quantity of said single-core wire was 12, the diameter of said NbTi/Cu compound bar was 3 times of single-core wire diameter;
Step 5, the pass reduction with 10%～20% carry out swaging of 3～5 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 10%～15% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 10～15 passages; With 10%～15% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is the multicore wire rod of 0.8mm～1.5mm;
Step 6, the wire rod of multicore described in step 5 sealed at both ends is placed in the tube furnace heat-treats, obtain multicore MgB 2Superconducting wire; Said heat treated process is: the speed with 300mL/min～500mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1h～2h; Be incubated 0.5h～3h after with the heating rate of 10 ℃/min～20 ℃/min temperature in the stove being risen to 650 ℃～850 ℃, the rate of temperature fall with 10 ℃/min～20 ℃/min is cooled to room temperature with temperature in the stove then.
The quality purity of magnesium powder described in the above-mentioned steps one is 99.8%, and the granularity of magnesium powder is-200 orders, and the quality purity of said amorphous boron powder is 99.999%, and the quality purity of said nano TiC powder is 99%.
The external diameter of the pipe of Ta described in the above-mentioned steps two is 10mm～12mm, and wall thickness is 1.0mm～1.5mm, and the mass content of Ta is not less than 99.9% in the Ta pipe.
The external diameter of oxygen-free copper pipe described in the above-mentioned steps two is 12.5mm～15.5mm, and wall thickness is 1.0mm～1.5mm, and the residual resistivity of said oxygen-free copper pipe is not less than 80.
The diameter of single-core wire described in the above-mentioned steps three is 3mm～8mm, when the single-core wire diameter is 3mm～5mm, adopts 12 single-core wires to carry out the secondary assembling, when the single-core wire diameter is 5mm～8mm, adopts 6 single-core wires to carry out secondary and assembles.
The acid cleaning process of single-core wire is described in the above-mentioned steps three: it is to soak 5min～8min in 10%～15% the nitric acid that single-core wire sealed at both ends protection is placed on mass concentration; Water washes away single-core wire remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 50 ℃～60 ℃ conditions, dry at last again.
The residual resistivity of oxygen-free copper pipe is not less than 80 described in the above-mentioned steps four, and the external diameter of oxygen-free copper pipe is 19mm～31mm, and wall thickness is 1.5mm～3mm.
The present invention compared with prior art has the following advantages:
1, the present invention adopts the technology that swage drawing and groove rolling combine, and not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire.
2, superconducting wire in the course of processing because wire rod is outside stressed bigger; Cause defective to develop to the center, the higher NbTi/Cu compound bar of intensity is adopted at the superconducting wire center of the present invention preparation, to a certain degree limit the development of defective; Improved the density of multicore wire rod, efficient hardening MgB 2Crystal grain connectivity, simultaneously NbTi is a kind of cryogenic superconductor, under less than the temperature of 9.8K, certain current capacity can be provided, more help improving wire rod low temperature, in low critical current density after the match.
3, heat treatment of the present invention is carried out in 650 ℃～850 ℃ scopes, and the liquid phase in the Mg-B course of reaction can well be made the micro-crack that forms in the course of processing up, and metal Ta is to MgB simultaneously 2Material has the better chemical inertia, has avoided Ta/MgB 2Dispersal behavior between the interface, and oxygen-free copper has good heat conduction, conductivity, can play the static stabilization of shunting, heat radiation to superconducting wire.
4, adopt the wire rod of method preparation of the present invention to have higher mechanical strength; The normal temperature lower yield strength reaches more than the 129MPa; Tensile strength reaches more than the 258MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Below in conjunction with accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description.
Description of drawings
Fig. 1 is the structural representation that the embodiment of the invention 1, embodiment 2 and embodiment 3 secondaries are assembled the secondary compound bar that obtains.
Fig. 2 is the structural representation that the embodiment of the invention 4, embodiment 5 and embodiment 6 secondaries are assembled the secondary compound bar that obtains.
Description of reference numerals:
The 1-single-core wire; The 2-NbTi/Cu compound bar; The 3-oxygen-free copper pipe.
Embodiment
Embodiment 1
7 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.98: 0.02 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 10mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.0mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 12.5mm, and wall thickness is 1.0mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 10% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 5mm; Length according to 1.0m is carried out scale, is blocked single-core wire 1, and it is to soak 8min in 10% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 50 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 5mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 0.8; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 45% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 19mm, and wall thickness is 1.5mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 6 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 1);
Step 5, the pass reduction with 20% carry out swaging of 3 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 10% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 15 passages; With 10% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 7 core wires of 0.8mm;
Step 6,7 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 7 core MgB 2Superconducting wire; Said heat treated process is: the speed with 300mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 2h; Be incubated 3h after with the heating rate of 10 ℃/min temperature in the stove being risen to 650 ℃, the rate of temperature fall with 10 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 148MPa; Tensile strength reaches 282MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Embodiment 2
7 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.9: 0.1 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 12mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.5mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 15.5mm, and wall thickness is 1.5mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 20% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 8mm; Length according to 1.5m is carried out scale, is blocked single-core wire 1, and it is to soak 5min in 15% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 60 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 8mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 1.2; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 55% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 31mm, and wall thickness is 3mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 6 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 1);
Step 5, the pass reduction with 10% carry out swaging of 5 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 15% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 10 passages; With 15% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 7 core wires of 1.5mm;
Step 6,7 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 7 core MgB 2Superconducting wire; Said heat treated process is: the speed with 500mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1h; Be incubated 0.5h after with the heating rate of 20 ℃/min temperature in the stove being risen to 850 ℃, the rate of temperature fall with 15 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 129MPa; Tensile strength reaches 258MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Embodiment 3
7 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.95: 0.05 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 11mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.2mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 14mm, and wall thickness is 1.2mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 15% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 6mm; Length according to 1.0m is carried out scale, is blocked single-core wire 1, and it is to soak 6min in 12% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 55 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 6mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 1; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 50% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 22mm, and wall thickness is 1.5mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 6 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 1);
Step 5, the pass reduction with 15% carry out swaging of 4 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 12% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 12 passages; With 13% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 7 core wires of 1mm;
Step 6,7 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 7 core MgB 2Superconducting wire; Said heat treated process is: the speed with 400mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1.5h; Be incubated 2h after with the heating rate of 15 ℃/min temperature in the stove being risen to 750 ℃, the rate of temperature fall with 20 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 143MPa; Tensile strength reaches 274MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Embodiment 4
13 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.9: 0.1 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 12mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.5mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 15.5mm, and wall thickness is 1.5mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 20% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 3mm; Length according to 1.5m is carried out scale, is blocked single-core wire 1, and it is to soak 5min in 15% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 60 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 9mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 1.2; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 55% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 19mm, and wall thickness is 1.5mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 12 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 2);
Step 5, the pass reduction with 15% carry out swaging of 5 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 15% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 10 passages; With 15% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 13 core wires of 0.8mm;
Step 6,13 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 13 core MgB 2Superconducting wire; Said heat treated process is: the speed with 500mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1h; Be incubated 0.5h after with the heating rate of 20 ℃/min temperature in the stove being risen to 850 ℃, the rate of temperature fall with 20 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 132MPa; Tensile strength reaches 258MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Embodiment 5
13 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.95: 0.05 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 11mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.2mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 14mm, and wall thickness is 1.2mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 10% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 4mm; Length according to 1.2m is carried out scale, is blocked single-core wire 1, and it is to soak 6min in 12% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 55 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 12mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 1; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 47% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 25mm, and wall thickness is 2mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 12 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 2);
Step 5, the pass reduction with 20% carry out swaging of 4 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 10% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 15 passages; With 10% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 13 core wires of 1.2mm;
Step 6,13 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 13 core MgB 2Superconducting wire; Said heat treated process is: the speed with 400mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1.5h; Be incubated 1.5h after with the heating rate of 15 ℃/min temperature in the stove being risen to 750 ℃, the rate of temperature fall with 15 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 142MPa; Tensile strength reaches 271MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
Embodiment 6
13 core MgB 2The preparation of superconducting wire:
Step 1, (granularity is-200 orders with the magnesium powder; Quality purity is 99.8%), amorphous boron powder (quality purity is 99.999%) and sodium rice TiC powder (quality purity is 99%) be according to Mg: B: TiC=1: 1.98: 0.02 atomic ratio mixes; Then that mixture ground and mixed under argon shield is even, obtain forerunner's powder;
Step 2, the powder of forerunner described in the step 1 packed into (external diameter is 10mm for Ta pipe after the conventional method pickling processes; Wall thickness is 1.0mm; The mass content of Ta is not less than 99.9%) in, the Ta pipe that forerunner's powder will be housed is then packed into, and (external diameter is 12.5mm, and wall thickness is 1mm for oxygen-free copper pipe after the conventional method pickling processes; Residual resistivity is not less than 80) in, make the tubulature complex;
Step 3, the pass reduction with 15% carry out groove rolling to the complex of tubulature described in the step 2; The diameter that obtains having circular cross-section is the single-core wire 1 of 5mm; Length according to 1.2m is carried out scale, is blocked single-core wire 1, and it is to soak 8min in 10% the nitric acid that the protection of single-core wire 1 sealed at both ends after will blocking then is placed on mass concentration, and water washes away single-core wire 1 remained on surface acid solution then; With the absolute ethyl alcohol dehydration, under 50 ℃ of conditions, dry at last again;
Step 4, be that NbTi/Cu compound bar 2 after the conventional method pickling of 15mm is (by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material with diameter; Wherein the mass ratio of oxygen-free copper and niobium titanium alloy is 1: 0.8; The residual resistivity of oxygen-free copper is not less than 80; The quality percentage composition of niobium is 45% in the niobium titanium alloy; Surplus is a titanium) place in the oxygen-free copper pipe 3 (residual resistivity is not less than 80, and external diameter is 31mm, and wall thickness is 3mm) after the conventional method pickling processes; Single-core wire 1 after the pickling in 12 step 3 along the circumferential direction is arranged in circular ring around NbTi/Cu compound bar 2 packs in the oxygen-free copper pipe 3, obtain secondary compound bar (as shown in Figure 2);
Step 5, the pass reduction with 10% carry out swaging of 3 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 14% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 14 passages; With 14% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is 13 core wires of 1.5mm;
Step 6,13 core wire sealed at both ends described in the step 5 are placed in the tube furnace heat-treat, obtain 13 core MgB 2Superconducting wire; Said heat treated process is: the speed with 300mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 2h; Be incubated 3h after with the heating rate of 10 ℃/min temperature in the stove being risen to 650 ℃, the rate of temperature fall with 10 ℃/min is cooled to room temperature with temperature in the stove then.
The technology that present embodiment adopts swage drawing and groove rolling to combine not only can improve copper/niobium and niobium/MgB 2Between compound degree, increase the uniformity of core deformation of filament, and can improve the density of multicore wire rod, improve the connectivity of intergranule, more help preparing high performance multicore MgB 2Superconducting wire, the wire rod of preparation has higher mechanical strength, and the normal temperature lower yield strength reaches 139MPa; Tensile strength reaches 268MPa; Can carry bigger ess-strain and superconduction current-carrying performance does not have obvious reduction, more meet the requirement of superconducting wire practicability, satisfy the requirement of magnet preparation.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every according to inventing technical spirit to any simple modification, change and equivalent structure variation that above embodiment did, all still belong in the protection range of technical scheme of the present invention.

Claims (7)

1. multicore MgB 2The preparation method of superconducting wire is characterized in that, this method may further comprise the steps:
Step 1, magnesium powder, amorphous boron powder and the sodium rice TiC powder atomic ratio according to Mg: B: TiC=1: (2-x): x is mixed, then that mixture ground and mixed under argon shield is even, obtain forerunner's powder; The value of said x is 0.02～0.10;
Step 2, the powder of forerunner described in the step 1 is packed in the Ta pipe after the pickling processes, the Ta pipe that forerunner's powder will be housed is then packed in the oxygen-free copper pipe after the pickling processes, makes the tubulature complex;
Step 3, the complex of tubulature described in the step 2 is carried out groove rolling, obtain having the single-core wire (1) of circular cross-section, single-core wire (1) is carried out scale successively, blocks and pickling; The pass reduction of said groove rolling is 10%～20%;
Step 4, place oxygen-free copper pipe (3) after the pickling processes to carry out the secondary assembling single-core wire (1) after the pickling in NbTi/Cu compound bar (2) and 6 or 12 step 3 to obtain the secondary compound bar; Said NbTi/Cu compound bar (2) is by forming as the oxygen-free copper of cladding material with as the niobium titanium alloy of inner layer material; The mass ratio of said oxygen-free copper and niobium titanium alloy is 1: 0.8～1.2; The residual resistivity of said oxygen-free copper is not less than 80; The quality percentage composition of niobium is 45%～55% in the said niobium titanium alloy, and surplus is a titanium; NbTi/Cu compound bar (2) in the said secondary assembling process after the pickling places oxygen-free copper pipe (3) center after the pickling processes, and the single-core wire after the pickling (1) the along the circumferential direction NbTi/Cu compound bar (2) after the pickling is arranged in circular ring and packs in the oxygen-free copper pipe (3) after the pickling processes; When the quantity of said single-core wire (1) is 6, the size of said NbTi/Cu compound bar (2) and single-core wire (1) measure-alike; When the quantity of said single-core wire (1) was 12, the diameter of said NbTi/Cu compound bar (2) was 3 times of single-core wire (1) diameter;
Step 5, the pass reduction with 10%～20% carry out swaging of 3～5 passages and drawing processing to the compound bar of secondary described in the step 4; Then with 10%～15% pass reduction to through swage with drawing processing after the secondary compound bar carry out the groove rolling of 10～15 passages; With 10%～15% pass reduction the secondary compound bar after groove rolling is swaged and drawing processing at last, obtaining diameter is the multicore wire rod of 0.8mm～1.5mm;
Step 6, the wire rod of multicore described in step 5 sealed at both ends is placed in the tube furnace heat-treats, obtain multicore MgB 2Superconducting wire; Said heat treated process is: the speed with 300mL/min～500mL/min feeds argon gas in tube furnace; After treating that argon gas feeds 1h～2h; Be incubated 0.5h～3h after with the heating rate of 10 ℃/min～20 ℃/min temperature in the stove being risen to 650 ℃～850 ℃, the rate of temperature fall with 10 ℃/min～20 ℃/min is cooled to room temperature with temperature in the stove then.
2. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire 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-200 orders, and the quality purity of said amorphous boron powder is 99.999%, and the quality purity of said nano TiC powder is 99%.
3. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire is characterized in that, the external diameter of the pipe of Ta described in the step 2 is 10mm～12mm, and wall thickness is 1.0mm～1.5mm, and the mass content of Ta is not less than 99.9% in the Ta pipe.
4. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire is characterized in that, the external diameter of oxygen-free copper pipe described in the step 2 is 12.5mm～15.5mm, and wall thickness is 1.0mm～1.5mm, and the residual resistivity of said oxygen-free copper pipe is not less than 80.
5. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire is characterized in that, the diameter of single-core wire described in the step 3 (1) is 3mm～8mm.
6. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire; It is characterized in that; The acid cleaning process of single-core wire described in the step 3 (1) is: it is to soak 5min～8min in 10%～15% the nitric acid that single-core wire (1) sealed at both ends protection is placed on mass concentration; Water washes away single-core wire (1) remained on surface acid solution then, with the absolute ethyl alcohol dehydration, under 50 ℃～60 ℃ conditions, dries at last again.
7. a kind of multicore MgB according to claim 1 2The preparation method of superconducting wire is characterized in that, the residual resistivity of oxygen-free copper pipe described in the step 4 (3) is not less than 80, and the external diameter of oxygen-free copper pipe (3) is 19mm～31mm, and wall thickness is 1.5mm～3mm.
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CN103440931A (en) * 2013-09-13 2013-12-11 西北有色金属研究院 Preparation method of rectangular multicore composite superconductive strip
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CN113192686A (en) * 2021-04-26 2021-07-30 福建师范大学 Improved Nb3Al precursor wire and preparation method thereof
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CN116779240A (en) * 2023-08-16 2023-09-19 西安聚能超导线材科技有限公司 Preparation method of magnesium diboride superconducting wire and magnesium diboride superconducting wire

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CN103151114B (en) * 2013-02-25 2016-01-20 宝胜科技创新股份有限公司 Single core MgB 2the preparation method of superconducting wire
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CN105845278A (en) * 2016-04-12 2016-08-10 东南大学 Manufacturing method for practical multi-core MgB2 composite superconductive wire rods
CN113192685A (en) * 2021-04-26 2021-07-30 福建师范大学 Nb with high current-carrying density and low loss3Al precursor wire and preparation method thereof
CN113192686A (en) * 2021-04-26 2021-07-30 福建师范大学 Improved Nb3Al precursor wire and preparation method thereof
CN114783680A (en) * 2022-06-17 2022-07-22 西部超导材料科技股份有限公司 Preparation method of superconducting wire for quantum computer
CN116779240A (en) * 2023-08-16 2023-09-19 西安聚能超导线材科技有限公司 Preparation method of magnesium diboride superconducting wire and magnesium diboride superconducting wire
CN116779240B (en) * 2023-08-16 2023-10-20 西安聚能超导线材科技有限公司 Preparation method of magnesium diboride superconducting wire and magnesium diboride superconducting wire

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