CN105869781A - Preparation method of FeSe-based superconduction wire - Google Patents
Preparation method of FeSe-based superconduction wire Download PDFInfo
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
- H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Abstract
The invention discloses a preparation method of a FeSe-based superconduction wire. The preparation method includes the steps of firstly, evenly grinding and mixing iron powder and selenium powder to obtain mixed powder, and performing cold pressing to obtain a block; secondly, sintering, and grinding to obtain precursor powder; thirdly, loading the precursor powder into an iron sheath to obtain a power-in-tube complex, performing rotary swaging and drawing to obtain a single-core wire, and sequentially performing sizing, cutting and acid pickling; fourthly, performing secondary assembling to obtain a second complex; fifthly, soldering and sealing, and performing hot extrusion to obtain a multicore wire; sixthly, performing rotary swaging and drawing to obtain the FeSe-based superconduction wire. The preparation method has the advantages that the preparation process is simple, easy to control, high in repeatability and suitable for large-scale industrial production; the FeSe-based superconduction wire prepared by the method is high in superconduction phase content as compared with the wire prepared by traditional process, the core wire density of the FeSe-based superconduction wire is increased greatly, and good intercrystalline connectivity is achieved.
Description
Technical field
The invention belongs to superconducting wire processing technique field, be specifically related to one and there is higher superconducting phase contain
The preparation method of the FeSe base superconducting wire of amount.
Background technology
2008, Hosono seminar of Japan first reported and there is 26K critical temperature
LaO1-xFxFeAs, Fe base high temperature super conductive material (FHS) quickly grows subsequently.At present, developed
Be four Main Systems, be respectively " 1111 " system (such as LaFeAsOF), " 122 " system (as
BaFe2As2), " 111 " system (such as LiFeAs) and " 11 " system (such as FeSe).With high temperature Cu oxide
Superconductor (HTS) is similar to, and the crystal structure of FHS is all layer structure, by-FeAs-layer (or-FeSe-
Layer) as superconducting layer.
Developing rapidly of FHS mainly has three reasons, first, it is considered that the magnetic of Fe is to routine
Electron pairing in superconductor has destruction, so in FHS, magnetic and superconductivity coexist for
Explore superconducting mechanism and provide new way；On the other hand, FHS has higher superconductivity,
And anisotropy is weak, be suitable to the needs of actual application.Upper critical field (the Hc of FHS2) the highest
In Metal Substrate low temperature superconducting material, such as Nb3Sn, NbTi and MgB2Deng, general FHS is at 4.2K
Left and right, Hc2All can reach more than 50T, be Nb3Sn(Hc2For 30T) twice about, and
Sr0.6K0.4Fe2As2Hc2Reach about 140T especially.Meanwhile, iron-based superconducting material is critical
Electric current density (Jc) is higher, if SmFeAsOF monocrystalline is 2 × 10 at the Jc of 5K6A·cm-2,
Ba0.6K0.4Fe2A2Monocrystalline Jc when 4.2K is 4 × 105A·cm-2, FeTe0.61Se0.39Jc low
1 × 10 is can reach when its critical temperature 14K5A·cm-2, meanwhile, the current-carrying performance of FHS is at magnetic
Decay after the match is relatively slow, even under the magnetic field condition of 20T, the Jc of many FHS also can reach
105A·cm-2Above, these performance guarantees probability of the actual application of FHS.In numerous FHS,
Although the critical transition temperature of FeSe base superconductor is relatively low, but under liquid helium temperature, it is critical
Electric current density can reach the requirement of application, and, its raw material non precious metal, avirulence, lay in rich
Rich so that it is there is in commercial process bigger advantage.Therefore, prepare have actual should
It is the research emphasis of this system iron-based superconducting material at present with the FeSe baseline material of potentiality.
And main problem is present in the FeSe base superconductor preparation process: owing to FeSe has
Having two kinds of crystal structures, one is hexagonal phase, and wherein, Fe:Se mol ratio is slightly below 1:1, due to knot
Restriction hexagonal phase FeSe of structure does not possess superconductivity；Another kind is Tetragonal, in this structure,
-FeSe-is distributed in sheet, for the superconducting layer structure similar to-FeAs-and-CuO-, therefore,
Suiperconducting transition is there is at about 10K.In the sintering process of material, have between both structures
The relation mutually converted.At present, use in FeSe base superconducting wire prepared by conventional sintering method,
Not only existing substantial amounts of hexagonal phase and hole therein is more, these holes and the second phase form intergranular
Weak link, is unfavorable for the transport process of electric current, is therefore difficult to obtain the breakthrough of wire rod current-carrying performance.Cause
This proposes a kind of novel FeSe base superconducting wire preparation method, to follow-up high performance Fe Se base superconduction
The exploration of wire rod and Fe base superconductor Superconducting Mechanism all has great importance.
Summary of the invention
The technical problem to be solved is for above-mentioned deficiency of the prior art, it is provided that one
Planting the preparation method of FeSe base superconducting wire, the method preparation technology is simple and easy to control, repeatable strong,
Be suitable to industrialization large-scale production.Use the FeSe base superconducting wire prepared of the method and traditional handicraft
Comparing and have higher superconducting phase content, and its core filaments density obtains bigger raising, intergranular is even
Connecing property is good.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of FeSe base superconducting line
The preparation method of material, it is characterised in that the method comprises the following steps:
Step one, by uniform for iron powder and selenium powder ground and mixed in the glove box of full noble gas,
To mixed powder, then described mixed powder is placed in cold stamping die and carries out cold moudling, obtain block
Body；The pressure of described cold moudling is 10MPa～18MPa, and the dwell time is 2min～50min；Institute
The mol ratio stating iron powder and selenium powder is (0.9～1.5): 1；
Step 2, block described in step one is sintered under argon gas atmosphere or vacuum condition place
Reason, is then down to 25 DEG C of room temperatures by the block after sintering processes with the rate of temperature fall of not higher than 30 DEG C/h,
Then the block after cooling is ground, obtains precursor powder；Described precursor powder average
Particle diameter is not more than 100 μm, and the temperature of described sintering processes is 600 DEG C～900 DEG C, and temperature retention time is 10h
～30h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and obtaining cross section is orthohexagonal single
Wire rod, carries out scale afterwards successively, blocks and pickling processes described single-core wire；Described positive six limits
The opposite side distance of shape is 5mm～10mm；
Step 4, the single-core wire after pickling processes in 1 iron staff and 18 step 3 is placed in nothing
Carrying out secondary assembling in oxygen copper pipe, obtain secondary complex, the detailed process that described secondary assembles is:
1 iron staff is placed in the center of oxygen-free copper pipe, 18 single-core wires are arranged in around 1 iron staff
Circular ring loads in oxygen-free copper pipe；Or, after pickling in 7 iron staffs and 12 step 3
Single-core wire be placed in oxygen-free copper pipe and carry out secondary assembling, obtain secondary complex, described secondary group
The detailed process of dress is: 1 iron staff is placed in the center of oxygen-free copper pipe, by remaining 6 iron staff around institute
State 1 iron staff to be arranged in circular ring loading oxygen-free copper pipe, then 12 single-core wires are enclosed
It is arranged in circular ring around described 6 iron staffs to load in oxygen-free copper pipe；Or, by 13 iron staffs
It is placed in oxygen-free copper pipe with the single-core wire after pickling in 6 step 3 and carries out secondary assembling, obtain two
Secondary complex, the detailed process that described secondary assembles is: 1 iron staff is placed in the center of oxygen-free copper pipe,
6 single-core wires are arranged in circular ring around described 1 iron staff and load in oxygen-free copper pipe, so
After 12 iron staffs be arranged in circular ring around described 6 single-core wires load in oxygen-free copper pipe；
Iron staff employed in described secondary assembling process is homogeneous with the shape of cross section of single-core wire and size
With, the residual resistivity of the oxygen-free copper pipe employed in described secondary assembling process is not less than 80, described
The external diameter of oxygen-free copper pipe is 65mm～200mm, and wall thickness is not less than 10mm；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 450 DEG C～750 DEG C, and temperature retention time is 1h～6h, and extruding force is 150t～500t,
Extruding rate is 10m/min～50m/min；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, obtain FeSe base
Superconducting wire.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that institute in step one
Stating cold stamping die is stainless steel mould, and the die cavity of described stainless steel mould is a diameter of 6mm～10mm
Cylindrical mold cavities, the thickness of described block be less than 4mm.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that institute in step one
The mol ratio stating iron powder and selenium powder is (1.10～1.25): 1, and the pressure of described cold moudling is
15MPa～18MPa, the dwell time is 10min～20min, and described iron powder is that quality purity is not less than
The reduced iron powder of 98%, the quality purity of described selenium powder is not less than 99.9%.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that institute in step one
The mol ratio stating iron powder and selenium powder is 1.15: 1, and the pressure of described cold moudling is 18MPa, pressurize
Time is 15min.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that institute in step 2
The temperature stating sintering processes is 600 DEG C～800 DEG C, and temperature retention time is 10h～24h.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that described in step 2
The temperature of sintering processes is 800 DEG C, and temperature retention time is 12h.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that described in step 3
The external diameter of ferrum jacket is 8mm～12mm, and wall thickness is 0.8mm～2mm, and the quality of described ferrum jacket is pure
Degree is not less than 99%.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that described in step 5
The heating-up temperature of hot extrusion processing is 600 DEG C～700 DEG C, and temperature retention time is 1h～2h, and extruding force is 200t
～400t, extruding rate is 15m/min～30m/min.
The preparation method of above-mentioned a kind of FeSe base superconducting wire, it is characterised in that described in step 5
The heating-up temperature of hot extrusion processing is 650 DEG C, and temperature retention time is 1.5h, and extruding force is 250t, extruding
Speed is 20m/min.
The present invention compared with prior art has the advantage that
1, the present invention uses the method for hot extrusion to prepare multicore FeSe base superconducting wire, first by Fe
The mixed-powder of powder and Se powder carries out tubulature, then carries out hot extrusion, it is thus achieved that having can processing dimension
Wire rod, and by further cold deformation, it is thus achieved that the Multi-core wire of final size.The present invention
Preparation technology is simple and easy to control, repeatable strong, is suitable to industrialization large-scale production.
2, the FeSe base superconducting wire using the present invention to prepare has higher surpassing compared with traditional handicraft
Leading phase content, and its core filaments density obtains bigger raising, intergranular connectivity is good.
3, compared with conventional powder tubulature technique, hot extrusion technique can preferably ensure that high core filaments is close
The acquisition of degree FeSe base superconductor.For FeSe base superconductor, processing
During often cannot obtain optimum chemical metering ratio superconducting phase, cause the decline of its superconductivity,
It addition, wire rod exists more hole, and superconducting phase nonstoichiometry ratio and hole produce one
Individual common cause is fusing and the volatilization of Se.And in hot extrusion process, ingot casting closed at both ends, because of
This sample in hot extrusion process, present in core filaments Se simple substance fusing, and in closed environment with
The fully reaction such as Fe and FeSe compound, generates the FeSe superconducting phase of design composition, institute after this
The follow-up heat treatment process carried out there will be no Se simple substance fusing residual hole and cause superconduction to be coordinated
The problem of the raw deviation of distribution.
4, hot extrusion process is more beneficial for the combination of core filaments and jacket.FeSe base superconducting wire typically uses
Fe jacket, although Fe jacket will not generate other impurity the second phases with core filaments, and can have enough
Mechanical strength ensure that wire rod has enough core filaments density.But due to powder in cold deformation
And the difference of deformation nature between metal capsule, often in generation gap, interface, affect agglutinating property
Energy and follow-up transmission performance.And in hot extrusion process, ingot casting is to become at a higher temperature
Shape is processed, and now, the deformation performance of metal capsule is more preferable, it is easier to realization is combined closely with core filaments.
5, hot extrusion can be used for the preparation of the FeSe long line of base superconduction.Owing to hot extrusion process can be used for adding
The large-sized ingot casting of work, therefore, makes to can ensure that in this way the acquisition of at least hundred long lines of meter level.
Below by drawings and Examples, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 and the structural representation of 4 two complexs of embodiment.
Fig. 2 is the embodiment of the present invention 2 and the structural representation of 5 two complexs of embodiment.
Fig. 3 is the embodiment of the present invention 3 and the structural representation of 6 two complexs of embodiment.
Detailed description of the invention
Embodiment 1
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 1.15: 1 and selenium
Powder grinds 30min and makes mix homogeneously, obtains mixed powder, is then placed in by described mixed powder and colds pressing
Carrying out cold moudling in mould, described cold stamping die is stainless steel mould, the mould of described stainless steel mould
Chamber is the cylindrical mold cavities of a diameter of 10mm, obtains the block that thickness is 2mm；Described it is cold-pressed into
The pressure of type is 18MPa, and the dwell time is 15min, and described iron powder is that quality purity is not less than 98%
Reduced iron powder, the quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 25 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 800 DEG C, and temperature retention time is 12h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 10%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 6.65mm；The external diameter of described ferrum jacket is 8mm,
Wall thickness is 1mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling processes in 1 iron staff and 18 step 3 is placed in nothing
Carrying out secondary assembling in oxygen copper pipe, obtain secondary complex, the detailed process that described secondary assembles is:
1 iron staff is placed in the center of oxygen-free copper pipe, 18 single-core wires are arranged in around 1 iron staff
Circular ring loads in oxygen-free copper pipe；Described iron staff is equal with the shape of cross section of single-core wire and size
Identical, the residual resistivity of described oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is
65mm, wall thickness is 13.5mm；
The structure of the present embodiment secondary complex as it is shown in figure 1, as shown in Figure 1, the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 650 DEG C, and temperature retention time is 1.5h, and extruding force is 250t (i.e. 250 tons),
Extruding rate is 20m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than
10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
10%, obtain the FeSe base superconducting wire of a diameter of 1.0mm.
By the wire rod structure before and after observation the present embodiment hot extrusion it can be seen that the core of wire rod after Ji Ya
Silk structure is the finest and close, and, the knot between core filaments Yu Fe jacket, and Fe jacket and Cu jacket
Close closely.Meanwhile, after the wire rod through cold working acquisition final size, by measuring FeSe
Superconductor transmission method measures made wire rod critical current density jc under the conditions of 4.2K null field, its
Under null field, Jc is about 1620A cm-2, the Jc 1027A cm for preparing with conventional method-2Compare, reach
To the raising of more than 60%, illustrate that the present embodiment is adopted in the preparation process of FeSe base superconducting wire
By the method for hot extrusion, it is possible to the effective current-carrying performance improving FeSe base superconducting wire.
Embodiment 2
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 0.9: 1 and selenium powder
Ground and mixed is uniform, obtains mixed powder, is then placed in cold stamping die by described mixed powder and carries out
Cold moudling, described cold stamping die is stainless steel mould, and the die cavity of described stainless steel mould is a diameter of
The cylindrical mold cavities of 6mm, obtains the block that thickness is 4mm；The pressure of described cold moudling is
10MPa, the dwell time is 30min, and described iron powder is the reduced iron powder that quality purity is not less than 98%,
The quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 20 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 900 DEG C, and temperature retention time is 10h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 10%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 7.5mm；The external diameter of described ferrum jacket is 12mm,
Wall thickness is 2mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling in 7 iron staffs and 12 step 3 is placed in oxygen-free copper
Carrying out secondary assembling in pipe, obtain secondary complex, the detailed process that described secondary assembles is: by 1
Root iron staff is placed in the center of oxygen-free copper pipe, and around 1 iron staff, remaining 6 iron staff is arranged in circular knot
Structure loads in oxygen-free copper pipe, then around described 6 iron staffs, 12 single-core wires is arranged in annulus
Shape structure loads in oxygen-free copper pipe；Described iron staff is homogeneous with the shape of cross section of single-core wire and size
With, the residual resistivity of described oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is 120mm,
Wall thickness is 37mm；
The structure of the present embodiment secondary complex as in figure 2 it is shown, as shown in Figure 2, the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 750 DEG C, and temperature retention time is 6h, and extruding force is 500t, and extruding rate is
10m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than 10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
10%, obtain the FeSe base superconducting wire of a diameter of 2.0mm.
The present embodiment measures made wire rod at 4.2K null field bar by measuring FeSe superconductor transmission method
Critical current density jc under part, under its null field, Jc is about 1440A cm-2, with conventional method system
Standby Jc 1027A cm-2Compare, reached the raising of more than 40%, illustrate that the present embodiment is at FeSe
The method using hot extrusion in the preparation process of base superconducting wire, it is possible to the effective FeSe base that improves surpasses
The current-carrying performance of wire material.
Embodiment 3
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 1.3: 1 and selenium powder
Ground and mixed is uniform, obtains mixed powder, is then placed in cold stamping die by described mixed powder and carries out
Cold moudling, described cold stamping die is stainless steel mould, and the die cavity of described stainless steel mould is a diameter of
The cylindrical mold cavities of 8mm, obtains the block that thickness is 1mm；The pressure of described cold moudling is
18MPa, the dwell time is 2min, and described iron powder is the reduced iron powder that quality purity is not less than 98%,
The quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 10 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 700 DEG C, and temperature retention time is 30h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 10%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 6.9mm；The external diameter of described ferrum jacket is 10mm,
Wall thickness is 1mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling in 13 iron staffs and 6 step 3 is placed in oxygen-free copper
Carrying out secondary assembling in pipe and obtain secondary complex, the detailed process that described secondary assembles is: by 1
Iron staff is placed in the center of oxygen-free copper pipe, and around 1 iron staff, 6 single-core wires are arranged in circular knot
Structure loads in oxygen-free copper pipe, then around 6 single-core wires, 12 iron staffs is arranged in circular knot
Structure loads in oxygen-free copper pipe；Described iron staff is the most identical with the shape of cross section of single-core wire and size, institute
The residual resistivity stating oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is 65mm, wall thickness
For 11.5mm；
The structure of the present embodiment secondary complex is as it is shown on figure 3, from the figure 3, it may be seen that the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 450 DEG C, and temperature retention time is 2h, and extruding force is 150t, and extruding rate is 50
m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than 10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
10%, obtain the FeSe base superconducting wire of a diameter of 1.5mm.
The present embodiment measures made wire rod at 4.2K null field bar by measuring FeSe superconductor transmission method
Critical current density jc under part, under its null field, Jc is about 1140A cm-2, with conventional method system
Standby Jc 1027A cm-2Compare, reached the raising of more than 11%, illustrate that the present embodiment is at FeSe
The method using hot extrusion in the preparation process of base superconducting wire, it is possible to the effective FeSe base that improves surpasses
The current-carrying performance of wire material.
Embodiment 4
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 1.10: 1 and selenium
Powder grinds 30min and makes mix homogeneously, obtains mixed powder, is then placed in by described mixed powder and colds pressing
Carrying out cold moudling in mould, described cold stamping die is stainless steel mould, the mould of described stainless steel mould
Chamber is the cylindrical mold cavities of a diameter of 10mm, obtains the block that thickness is 4mm；Described it is cold-pressed into
The pressure of type is 15MPa, and the dwell time is 10min, and described iron powder is that quality purity is not less than 98%
Reduced iron powder, the quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 15 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 600 DEG C, and temperature retention time is 24h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 10%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 6.65mm；The external diameter of described ferrum jacket is 8mm,
Wall thickness is 1mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling processes in 1 iron staff and 18 step 3 is placed in nothing
Carrying out secondary assembling in oxygen copper pipe, obtain secondary complex, the detailed process that described secondary assembles is:
1 iron staff is placed in the center of oxygen-free copper pipe, 18 single-core wires are arranged in around 1 iron staff
Circular ring loads in oxygen-free copper pipe；Described iron staff is equal with the shape of cross section of single-core wire and size
Identical, the residual resistivity of described oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is
65mm, wall thickness is 13.5mm；
The structure of the present embodiment secondary complex as it is shown in figure 1, as shown in Figure 1, the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 600 DEG C, and temperature retention time is 1h, and extruding force is 200t, and extruding rate is
20m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than 10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
10%, obtain the FeSe base superconducting wire of a diameter of 1.0mm.
Wire rod structure figure before and after the present embodiment hot extrusion is as shown in Figure 2, it can be seen that wire rod after extruding
Core filaments structure the finest and close, and, between core filaments Yu Fe jacket, and Fe jacket and Cu jacket
Combination closely.Meanwhile, after the wire rod through cold working acquisition final size, by measuring
FeSe superconductor transmission method measures made wire rod critical current density under the conditions of 4.2K null field
Jc, under its null field, Jc is about 1620A cm-2, the Jc 1027A cm for preparing with conventional method-2
Compare, reached the raising of more than 60%, the present embodiment preparation at FeSe base superconducting wire is described
During use the method for hot extrusion, it is possible to the effective current-carrying performance improving FeSe base superconducting wire.
Embodiment 5
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 1.5: 1 and selenium powder
Ground and mixed is uniform, obtains mixed powder, is then placed in cold stamping die by described mixed powder and carries out
Cold moudling, described cold stamping die is stainless steel mould, and the die cavity of described stainless steel mould is a diameter of
The cylindrical mold cavities of 10mm, obtains the block that thickness is 3mm；The pressure of described cold moudling is
10MPa, the dwell time is 50min, and described iron powder is the reduced iron powder that quality purity is not less than 98%,
The quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 30 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 700 DEG C, and temperature retention time is 30h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 5%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 8.3mm；The external diameter of described ferrum jacket is 10mm,
Wall thickness is 1mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling in 7 iron staffs and 12 step 3 is placed in oxygen-free copper
Carrying out secondary assembling in pipe, obtain secondary complex, the detailed process that described secondary assembles is: by 1
Root iron staff is placed in the center of oxygen-free copper pipe, and around 1 iron staff, remaining 6 iron staff is arranged in circular knot
Structure loads in oxygen-free copper pipe, then around described 6 iron staffs, 12 single-core wires is arranged in annulus
Shape structure loads in oxygen-free copper pipe；Described iron staff is homogeneous with the shape of cross section of single-core wire and size
With, the residual resistivity of described oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is 200mm,
Wall thickness is 77.5mm；
The structure of the present embodiment secondary complex as in figure 2 it is shown, as shown in Figure 2, the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 500 DEG C, and temperature retention time is 4h, and extruding force is 200t, and extruding rate is 40
m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than 10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
5%, obtain FeSe base superconducting wire.
The present embodiment measures made wire rod at 4.2K null field bar by measuring FeSe superconductor transmission method
Critical current density jc under part, under its null field, Jc is about 1340A cm-2, with conventional method system
Standby Jc 1027A cm-2Compare, reached the raising of more than 30%, illustrate that the present embodiment is at FeSe
The method using hot extrusion in the preparation process of base superconducting wire, it is possible to the effective FeSe base that improves surpasses
The current-carrying performance of wire material.
Embodiment 6
The preparation method of the present embodiment FeSe base superconducting wire comprises the following steps:
Step one, in the glove box of full noble gas by iron powder that mol ratio is 1.25: 1 and selenium
Powder ground and mixed is uniform, obtains mixed powder, then is placed in cold stamping die by described mixed powder
Row cold moudling, described cold stamping die is stainless steel mould, and the die cavity of described stainless steel mould is diameter
For the cylindrical mold cavities of 8mm, obtain the block that thickness is 1mm；The pressure of described cold moudling is
18MPa, the dwell time is 15min, and described iron powder is the reduced iron powder that quality purity is not less than 98%,
The quality purity of described selenium powder is not less than 99.9%；
Step 2, block described in step one under vacuum or is sintered in argon gas atmosphere place
Reason, is then down to 25 DEG C of room temperatures with the rate of temperature fall of 10 DEG C/h, then grinds the block after cooling,
Obtain precursor powder；The mean diameter of described precursor powder is not more than 100 μm, at described sintering
The temperature of reason is 700 DEG C, and temperature retention time is 30h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and pass reduction is 5%, obtains transversal
Face is orthohexagonal single-core wire, described single-core wire carries out scale afterwards successively, blocks and acid
Wash process；Described orthohexagonal opposite side distance is 6.9mm；The external diameter of described ferrum jacket is 10mm,
Wall thickness is 1mm, and the quality purity of described ferrum jacket is not less than 99%；
Step 4, the single-core wire after pickling in 13 iron staffs and 6 step 3 is placed in oxygen-free copper
Carrying out secondary assembling in pipe and obtain secondary complex, the detailed process that described secondary assembles is: by 1
Iron staff is placed in the center of oxygen-free copper pipe, and around 1 iron staff, 6 single-core wires are arranged in circular knot
Structure loads in oxygen-free copper pipe, then around 6 single-core wires, 12 iron staffs is arranged in circular knot
Structure loads in oxygen-free copper pipe；Described iron staff is the most identical with the shape of cross section of single-core wire and size, institute
The residual resistivity stating oxygen-free copper pipe is not less than 80, and the external diameter of described oxygen-free copper pipe is 65mm, wall thickness
For 11.5mm；
The structure of the present embodiment secondary complex is as it is shown on figure 3, from the figure 3, it may be seen that the present embodiment secondary
Complex is by being positioned at the regular hexagon structure of core and being coated on the annulus of regular hexagon structural outer
Shape structure forms, and wherein, externally-located and without fill color cirque structure represents oxygen-free copper pipe, position
In the regular hexagon structure of core, represent iron staff, with oblique line with the regular hexagon structure of filled black
The regular hexagon structure filled represents the single-core wire after pickling processes；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 700 DEG C, and temperature retention time is 1h, and extruding force is 400t, and extruding rate is
13m/min；The weld penetration of described soldering and sealing is not less than 3mm, and vacuum is not more than 10-1Pa；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, pass reduction is
5%, obtain the FeSe base superconducting wire of a diameter of 1.5mm.
The present embodiment measures made wire rod at 4.2K null field bar by measuring FeSe superconductor transmission method
Critical current density jc under part, under its null field, Jc is about 1140A cm-2, with conventional method system
Standby Jc 1027A cm-2Compare, reached the raising of more than 11%, illustrate that the present embodiment is at FeSe
The method using hot extrusion in the preparation process of base superconducting wire, it is possible to the effective FeSe base that improves surpasses
The current-carrying performance of wire material.
Equipment of the present invention is the commercially available conventional equipment being easy to get, the specific embodiment of the invention
The sintering furnace of middle selection is that the KSL-1400-A1 type that Hefei Ke Jing Materials Technology Ltd. produces is high
Temperature batch-type furnace, the glove box of selection is Germany's Braun UNILAB type glove box.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every
Any simple modification, change and equivalent structure above example made according to the technology of the present invention essence
Change, all still falls within the protection domain of technical solution of the present invention.
Claims (9)
1. the preparation method of a FeSe base superconducting wire, it is characterised in that the method includes following
Step:
Step one, by uniform for iron powder and selenium powder ground and mixed in the glove box of full noble gas,
To mixed powder, then described mixed powder is placed in cold stamping die and carries out cold moudling, obtain block
Body；The pressure of described cold moudling is 10MPa～18MPa, and the dwell time is 2min～50min；Institute
The mol ratio stating iron powder and selenium powder is (0.9～1.5): 1；
Step 2, block described in step one is sintered under argon gas atmosphere or vacuum condition place
Reason, is then down to 25 DEG C of room temperatures by the block after sintering processes with the rate of temperature fall of not higher than 30 DEG C/h,
Then the block after cooling is ground, obtains precursor powder；Described precursor powder average
Particle diameter is not more than 100 μm, and the temperature of described sintering processes is 600 DEG C～900 DEG C, and temperature retention time is 10h
～30h；
Step 3, precursor powder described in step 2 is loaded in ferrum jacket, obtains tubulature complex,
Then drawing of swaging described tubulature complex is processed, and obtaining cross section is orthohexagonal single
Wire rod, carries out scale afterwards successively, blocks and pickling processes described single-core wire；Described positive six limits
The opposite side distance of shape is 5mm～10mm；
Step 4, the single-core wire after pickling processes in 1 iron staff and 18 step 3 is placed in nothing
Carrying out secondary assembling in oxygen copper pipe, obtain secondary complex, the detailed process that described secondary assembles is:
1 iron staff is placed in the center of oxygen-free copper pipe, 18 single-core wires are arranged in around 1 iron staff
Circular ring loads in oxygen-free copper pipe；Or, after pickling in 7 iron staffs and 12 step 3
Single-core wire be placed in oxygen-free copper pipe and carry out secondary assembling, obtain secondary complex, described secondary group
The detailed process of dress is: 1 iron staff is placed in the center of oxygen-free copper pipe, by remaining 6 iron staff around institute
State 1 iron staff to be arranged in circular ring loading oxygen-free copper pipe, then 12 single-core wires are enclosed
It is arranged in circular ring around described 6 iron staffs to load in oxygen-free copper pipe；Or, by 13 iron staffs
It is placed in oxygen-free copper pipe with the single-core wire after pickling in 6 step 3 and carries out secondary assembling, obtain two
Secondary complex, the detailed process that described secondary assembles is: 1 iron staff is placed in the center of oxygen-free copper pipe,
6 single-core wires are arranged in circular ring around described 1 iron staff and load in oxygen-free copper pipe, so
After 12 iron staffs be arranged in circular ring around described 6 single-core wires load in oxygen-free copper pipe；
Iron staff employed in described secondary assembling process is homogeneous with the shape of cross section of single-core wire and size
With, the residual resistivity of the oxygen-free copper pipe employed in described secondary assembling process is not less than 80, described
The external diameter of oxygen-free copper pipe is 65mm～200mm, and wall thickness is not less than 10mm；
Step 5, under vacuum the two ends of secondary complex described in step 4 are carried out soldering and sealing,
Then the secondary complex after soldering and sealing is carried out hot extrusion processing, obtain Multi-core wire；Described hot extrusion
The heating-up temperature of processing is 450 DEG C～750 DEG C, and temperature retention time is 1h～6h, and extruding force is 150t～500t,
Extruding rate is 10m/min～50m/min；
Step 6, drawing of swaging Multi-core wire described in step 5 processing, obtain FeSe base
Superconducting wire.
2. according to the preparation method of a kind of FeSe base superconducting wire described in claim 1, its feature
Being, cold stamping die described in step one is stainless steel mould, and the die cavity of described stainless steel mould is straight
Footpath is the cylindrical mold cavities of 6mm～10mm, and the thickness of described block is less than 4mm.
3. according to the preparation method of a kind of FeSe base superconducting wire described in claim 1, its feature
Being, iron powder described in step one is (1.10～1.25) with the mol ratio of selenium powder: 1, described cold moudling
Pressure be 15MPa～18MPa, the dwell time is 10min～20min, and described iron powder is that quality is pure
Degree is not less than the reduced iron powder of 98%, and the quality purity of described selenium powder is not less than 99.9%.
4. according to the preparation method of a kind of FeSe base superconducting wire described in claim 3, its feature
Being, iron powder described in step one is 1.15: 1 with the mol ratio of selenium powder, the pressure of described cold moudling
Power is 18MPa, and the dwell time is 15min.
5. according to the preparation method of a kind of FeSe base superconducting wire described in claim 1, its feature
Being, the temperature of sintering processes described in step 2 is 600 DEG C～800 DEG C, and temperature retention time is 10h
～24h.
6. according to the preparation method of a kind of FeSe base superconducting wire described in claim 5, its feature
Being, the temperature of sintering processes described in step 2 is 800 DEG C, and temperature retention time is 12h.
7. according to the preparation method of a kind of FeSe base superconducting wire described in claim 1, its feature
Being, the external diameter of ferrum jacket described in step 3 is 8mm～12mm, and wall thickness is 0.8mm～2mm,
The quality purity of described ferrum jacket is not less than 99%.
8. according to the preparation method of a kind of FeSe base superconducting wire described in claim 1, its feature
Being, the heating-up temperature of the processing of hot extrusion described in step 5 is 600 DEG C～700 DEG C, and temperature retention time is
1h～2h, extruding force is 200t～400t, and extruding rate is 15m/min～30m/min.
9. according to the preparation method of a kind of FeSe base superconducting wire described in claim 8, its feature
Being, the heating-up temperature of the processing of hot extrusion described in step 5 is 650 DEG C, and temperature retention time is 1.5h,
Extruding force is 250t, and extruding rate is 20m/min.
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| CN110600191A (en) * | 2019-07-22 | 2019-12-20 | 中国科学院电工研究所 | Iron-based superconducting multi-core wire and preparation method thereof |
| CN110867283A (en) * | 2019-11-29 | 2020-03-06 | 西北有色金属研究院 | Preparation method of FeSe-based superconducting wire |
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