CN108597675B - MgB is used in a kind of extruding2The preparation method of single compound bar - Google Patents

MgB is used in a kind of extruding2The preparation method of single compound bar Download PDF

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CN108597675B
CN108597675B CN201810405718.7A CN201810405718A CN108597675B CN 108597675 B CN108597675 B CN 108597675B CN 201810405718 A CN201810405718 A CN 201810405718A CN 108597675 B CN108597675 B CN 108597675B
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oxygen
powder
free copper
mgb
metal tube
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CN108597675A (en
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王庆阳
闫果
冯建情
熊晓梅
杨芳
李成山
冯勇
张平祥
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Northwest Institute for Non Ferrous Metal Research
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Northwest Institute for Non Ferrous Metal Research
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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
    • H01B12/04—Single wire
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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

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  • Manufacturing & Machinery (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of extruding to use MgB2The preparation method of single compound bar, this method are as follows: one, successively aligned, cut, pickling, cleaning and drying and processing, obtain oxygen-free copper stub；Two, annealing heat-treatment is carried out to oxygen-free copper stub；Three, the port A of metal tube is blocked with oxygen-free copper stub, then Precursor Powder is filled in metal tube, the port B of metal tube is finally blocked with oxygen-free copper stub, an oxygen-free copper stub is placed into metal tube at interval of a distance during driving powder before filling the container, for Precursor Powder to be isolated；Four, the metal tube that will be filled with Precursor Powder is assembled into oxygen-free copper canning tube, and compound long stick is processed into drawing, and then the middle position of oxygen-free copper stub is cut along compound long stick, is obtained squeezing after pickling and is used MgB2Single compound bar.MgB is used in extruding prepared by the present invention2The both ends of single compound bar are blocked using oxygen-free copper stub, and acid liquid corrosion superconductive powder, can be realized mass production when avoiding pickling.

Description

MgB is used in a kind of extruding2The preparation method of single compound bar
Technical field
The invention belongs to superconduction bar preparation technical fields, and in particular to MgB is used in a kind of extruding2The preparation of single compound bar Method.
Background technique
Magnesium diboride (MgB2) material superconducting critical transition temperature (Tc) it is 39K, superconductivity is in 2001 by Japan Scientist has found that it is a kind of metallic compound with simple binary structure for the first time.With oxide high-temperature superconductor (OHTS) similar, which is similar to the frangible compounds phase of ceramic property, itself does not have working plasticity, can not directly process At wire strip, it usually needs using carrying out plastic processing after metallic cover.The current most common multicore MgB2The system of superconducting wire Preparation Method is so-called powder-in-tube method (PIT), is exactly by Mg, B mixed-powder or MgB2Superconductive powder is filled into metal guarantor In protecting pipe, then it is worked into after certain size by multi-pass plastic working technique and carries out secondary or multiple assembling and using rotation The methods of forging, drawing, rolling are worked into final size.But prepared multicore MgB in this way2Superconducting wire core filaments it Between binding force it is poor, be easy to disconnected core phenomenon occur in process, the mechanical performance of prepared Multi-core wire is also poor.
In view of the deficiency of the prior art, inventor is it is proposed that a kind of extrusion process prepares multicore MgB2Superconducting wire Method (ZL201410363120.8).This method proposes to process using biggish single pass on traditional PIT Process ba- sis Deflection, that is, hot extrusion processing technology prepares multicore MgB2Superconducting wire can significantly improve multicore MgB2The densification of superconducting wire Degree and yield strength, for practical km magnitude MgB2The mass production of superconducting wire provides a new way.And it squeezes Billet usually has certain draw ratio limitation, i.e. the height of extruding billet and diameter generally should be smaller than a certain ratio, for more Core Compound Extrusion jacket such as multicore MgB2Billet is squeezed, which is generally less than 3 times, and secondary single stick number when assembled Measure more, be required to carry out acid cleaning process before the assembling of all single sticks with scale removal, should during single stick end very It is easy to be corroded, touches acid solution so as to cause the higher Precursor Powder of activity in single stick and corrosion reaction occurs, and shadow It rings the activity of Precursor Powder and subsequent prepares multicore MgB2The technique of superconducting wire.Therefore, it is necessary to develop a kind of new extruding Use MgB2Single compound bar can prevent the active superconduction MgB in single stick2Material is not corroded.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of extruding use MgB2The preparation method of single compound bar.The MgB of this method preparation2There are oxygen-free copper plug, pickling in the both ends of single compound bar MgB2It can be avoided acid solution when single compound bar to contact with the higher precursor powder of activity in compound bar, influence precursor powder Superconduction activity, avoid by the MgB2The MgB of single compound bar preparation2The superconductivity of wire rod reduces, while also solving and keeping away Exempted from traditional single powder filling, drawing process chinese raw materials wastes larger disadvantage, can be realized mass preparation.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: MgB is used in a kind of extruding2Single compound bar Preparation method, which is characterized in that method includes the following steps:
Step 1: being cut into oxygen-free copper stub after the aligning long stick of oxygen-free copper, then acid successively is carried out to the oxygen-free copper stub It washes, clean and dries；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub after drying in step 1 is placed in vacuum heat treatment furnace；
Step 3: blocking the port A of metal tube with the oxygen-free copper stub after annealing heat-treatment in step 2 first, then will Precursor Powder is filled in the metal tube, and smashes pressure Precursor Powder with metal bar, finally with after annealing heat-treatment in step 2 Oxygen-free copper stub block the port B of the metal tube, wherein during driving powder before filling the container at interval of a distance to The oxygen-free copper stub in a step 2 after annealing heat-treatment is placed in the metal tube for Precursor Powder to be isolated；The metal Pipe is niobium pipe or nickel tube；The Precursor Powder is MgB2Superconductive powder or mixing by magnesium powder, boron powder and doping powder constituent Close powder；
Step 4: the metal tube after two-port in step 3 is blocked is assembled into oxygen-free copper canning tube, pulled up in broaching machine It pulls out and is processed into compound long stick, then the middle position of oxygen-free copper stub is cut along the compound long stick, is squeezed after pickling Use MgB2Single compound bar；The outer diameter of the metal tube is identical as the internal diameter of oxygen-free copper canning tube.
It is used as plug using oxygen-free copper stub in the present invention Precursor Powder is encapsulated in metal tube, and simultaneously using multiple The filling Precursor Powder in oxygen-free copper stub interval, the process can a disposably filling long metal tube, the metal tube Both ends all use oxygen-free copper stub to be blocked, and are assembled into oxygen-free copper canning tube and are drawn into compound long stick, along compound long stick The middle position of interior oxygen-free copper stub is cut, and the MgB of extruding is obtained after cutting2Single compound bar, the MgB2Single is compound The both ends of stick have oxygen-free copper to be blocked, and use the MgB subsequent2Single compound bar prepares multicore MgB2Pickling when wire rod MgB will not be eroded to2Superconduction activity Precursor Powder in single compound bar, and oxygen-free copper stub is also by the interval of Precursor Powder It is distributed in metal tube, therefore Jingxing assembles the MgB with the available more extruding of drawing after expendable powder2Single is multiple Stick is closed, MgB is substantially increased2The production efficiency of single compound bar is conducive to promote MgB2The large-scale production of single compound bar.
A kind of above-mentioned extruding MgB2The preparation method of single compound bar, which is characterized in that anaerobic described in step 1 The diameter of the long stick of copper is 15mm~20mm, and the diameter of the oxygen-free copper stub is 6mm~12mm, the length of the oxygen-free copper stub Degree is 1cm~10cm.
A kind of above-mentioned extruding MgB2The preparation method of single compound bar, which is characterized in that anneal described in step 2 Heat treatment is that vacuum annealing is heat-treated, and the temperature of vacuum annealing heat treatment is 500 DEG C~600 DEG C, and soaking time is 1h~2h, very Reciprocal of duty cycle is less than 10-3Pa, for the vacuum annealing process for activating oxygen-free copper stub, the effect that can block metal tube is more preferable, Be conducive to copper atom and penetrate into metal tube in subsequent drawing, binding force is stronger between two.
A kind of above-mentioned extruding MgB2The preparation method of single bar, which is characterized in that for blocking gold in step 3 The length for belonging to the oxygen-free copper stub of pipe port A is 1cm, and the length of the oxygen-free copper stub of intermediate isolating powder is 1cm~3cm, is used In block metal pipe end opening B oxygen-free copper stub length be 8cm~10cm；Drawing described in step 4 is processed as unidirectionally drawing It pulls out, the direction of the drawing processing is to be assembled from metal pipe end opening B to metal pipe end opening A by metal tube and oxygen-free copper canning tube Afterwards, obtain drawing pipe, the port side B of drawing pipe is fixed on broaching machine collet, pulls out to port A layback, due to block whether there is or not It is more firm to clamp drawing pipe of the force ratio of drawing pipe in the prior art without metal closure for oxygen copper stub.It realizes more A MgB2The Continuous maching of single stick avoids traditional single MgB2Chuck position caused by single stick drawing process Waste of raw materials phenomenon.
A kind of above-mentioned extruding MgB2The preparation method of single bar, which is characterized in that mixed powder described in step 3 The ratio between the mole of integral molar quantity and magnesium powder of boron powder and doping powder is 1:2 in end, and the mole of the doping powder is institute The 0.03%~0.08% of the mole of boron powder is stated, the doping powder is amorphous carbon powder, SiC powder or TiC powder, is used The mixed-powder of the formula can effectively improve MgB as superconductive powder2The flux pinning ability of superconductor.
A kind of above-mentioned extruding MgB2The preparation method of single bar, which is characterized in that compound length described in step 4 Stick is six square rods, and the opposite side distance of six square rod is 5mm~12mm.
Compared with the prior art, the present invention has the following advantages:
1, MgB prepared by the present invention2Single compound bar both ends have been all made of oxygen-free copper stub and have been blocked, and avoid subsequent In process when bar pickling, the internal higher superconduction powder of activity is contacted with acid solution to react, and makes forerunner's superconduction powder Inactivation, solves multicore MgB2MgB before squeezing the secondary assembling of jacket2Single compound bar can not pickling the problem of, can be realized batch Quantifying is standby.
2, jacket can generate heat during being wrapped in vacuum electron beam soldering and sealing due to the extruding of existing multicore, with the increasing of temperature Add, existing MgB2The vapour pressure of magnesium powder increases in single bar, influences vacuum seal process, and therefore, the present invention uses anaerobic Copper stub blocks the problems such as single stick both ends port can avoid the volatilization of magnesium powder as plug.
3, the draw ratio of multicore Compound Extrusion billet is usually within 3 times in the prior art, MgB2Single bar length It is shorter, previous MgB2It squeezes and uses every MgB in the preparation process of billet2Single stick is individually blocked after superconductive powder tubulature, is drawn It pulls out, every MgB2Single stick requires reserved drawing collet, and waste of raw materials is serious.Using continuous dress powder of the invention and plug Partition method, hence it is evident that reduce the waste of raw material, improve sample preparation efficiency.
Technical solution of the present invention is described in further detail below by drawings and examples.
Detailed description of the invention
Fig. 1 is that the metal tube after two-port of the present invention blocks is assembled into the vertical section structure signal after oxygen-free copper canning tube Figure.
Description of symbols:
1-oxygen-free copper stub；2-Precursor Powders；3-metal tubes；
4-oxygen-free copper canning tubes.
Specific embodiment
Embodiment 1
Step 1: the commodity non-oxygen copper bar drawing of original dimension Φ 15mm to be worked into the long stick of oxygen-free copper of Φ 8mm, align The oxygen-free copper stub 1 that several segment length are respectively 10mm, 15mm and 80mm, every oxygen-free copper are cut into linear cutting equipment afterwards The both ends port difference reconditioning of stub 1 is smooth, then carries out pickling and removes surface oxide layer, and residual acid is removed after cleaning up and is dried It is dry；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub 1 after drying in step 1 is placed in vacuum heat treatment furnace； The annealing heat-treatment is vacuum annealing heat treatment, and the temperature of vacuum annealing heat treatment is 500 DEG C, soaking time 2h, vacuum Degree is less than 10-3Pa；
Step 3: blocking gold with the oxygen-free copper stub 1 that the size after annealing heat-treatment in step 2 is 8 × 10mm of Φ first Belong to the port A of pipe 3, the size of the metal tube 3 is Φ 10 (outer diameter) × 1mm
Then Precursor Powder 2 is filled in the metal tube 3 by (wall thickness), and smash pressure Precursor Powder 2 with metal bar, most It is afterwards port B that Φ 8 × 80mm oxygen-free copper stub 1 blocks the metal tube 3 with the size after annealing heat-treatment in step 2, Wherein, during driving powder 2 before filling the container, every filling 2g Precursor Powder 2 places a step 2 into the metal tube 3 Size after middle annealing heat-treatment is 8 × 15mm of Φ oxygen-free copper stub 1, for Precursor Powder 2 to be isolated；The metal tube 3 is niobium Pipe or nickel tube；The Precursor Powder 2 is by magnesium powder, boron powder and doping powder constituent, the total moles of the boron powder and doping powder The ratio between amount and the mole of the magnesium powder are 1:2, and the mole of the doping powder is the 0.08% of the mole of the boron powder, The doping powder is amorphous carbon powder；
Step 4: the metal tube 3 after two-port in step 3 is blocked is assembled into as Φ 12.5 (outer diameter) × 1mm (wall It is thick) in oxygen-free copper canning tube 4, as shown in Figure 1, being worked into Φ through 9 passage drawings with 10% pass deformation rate on broaching machine 7.7mm, then six square rods of 6.5mm are drawn into the mold of six side 7.2mm, 6.85mm and 6.5mm, then along the compound length The middle position cutting of oxygen-free copper stub 1 in stick, obtains squeezing after pickling and uses MgB2Single compound bar；The compound long stick is six Square rod, the opposite side distance of six square rod are 6.5mm；The outer diameter of the metal tube 3 is identical as the internal diameter of oxygen-free copper canning tube 4, institute It states drawing and is processed as unidirectional drawing, the direction of the drawing processing is from metal tube 3 port B to port A.
MgB is used to extruding manufactured in the present embodiment2MgB is cut in single compound bar pickling2The end of single compound bar, to institute State MgB2The phase structure of mixed-powder in single compound bar is analyzed, the MgB in result and step 32Superconductive powder Phase structure is identical, shows that oxygen-free copper stub 1 is used as plug and has been effectively isolated acid solution and MgB2The contact of superconductive powder. MgB is used using prepared squeeze of the present invention simultaneously2Single compound bar avoids traditional single powder filling, drawing process Central Plains The larger disadvantage of waste of material can be realized mass preparation.
Embodiment 2
Step 1: the commodity non-oxygen copper bar drawing of original dimension Φ 16mm to be worked into the long stick of oxygen-free copper of Φ 9.5mm, rectify The oxygen-free copper stub 1 that several segment length are respectively 10mm, 20mm and 90mm, every anaerobic are cut into linear cutting equipment after straight The both ends port difference reconditioning of copper stub 1 is smooth, then carries out pickling and removes surface oxide layer, residual acid is removed after cleaning up simultaneously Drying；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub 1 after drying in step 1 is placed in vacuum heat treatment furnace； The annealing heat-treatment is vacuum annealing heat treatment, and the temperature of vacuum annealing heat treatment is 550 DEG C, soaking time 1.5h, very Reciprocal of duty cycle is less than 10-3Pa；
Step 3: being blocked first with the oxygen-free copper stub 1 that the size after annealing heat-treatment in step 2 is 9.5 × 10mm of Φ The size of the port A of metal tube 3, the metal tube 3 are Φ 11.5 (outer diameter) × 1.2mm (wall thickness), then by Precursor Powder 2 It is filled in the metal tube 3, and smashes pressure Precursor Powder 2 with metal bar, finally with the size after annealing heat-treatment in step 2 The port B of the metal tube 3 is blocked for Φ 9.5 × 90mm oxygen-free copper stub 1, wherein during driving powder 2 before filling the container, Every filling 3g Precursor Powder 2 placed into the metal tube 3 size in a step 2 after annealing heat-treatment be Φ 9.5 × 20mm oxygen-free copper stub 1, for Precursor Powder 2 to be isolated；The metal tube 3 is niobium pipe or nickel tube；The Precursor Powder 2 is by magnesium Powder, boron powder and doping powder constituent, the ratio between mole of integral molar quantity and the magnesium powder of the boron powder and doping powder is 1: 2, the mole of the doping powder is the 0.03% of the mole of the boron powder, and the doping powder is SiC powder；
Step 4: the metal tube 3 after two-port in step 3 is blocked is assembled into as Φ 15 (outer diameter) × 1.4mm (wall It is thick) in oxygen-free copper canning tube 4, as shown in Figure 1, being worked into Φ through 7 passage drawings with 10% pass deformation rate on broaching machine 10.4mm, then six square rods of 8.65mm are drawn into the mold of six side 9.6mm, 9.1mm and 8.65mm, then along described compound The middle position cutting of oxygen-free copper stub 1 in long stick, obtains squeezing after pickling and uses MgB2Single compound bar；The compound long stick is Six square rods, the opposite side distance of six square rod are 8.65mm；The outer diameter of the metal tube 3 is identical as the internal diameter of oxygen-free copper canning tube 4, The drawing is processed as unidirectional drawing, and the direction of the drawing processing is from metal tube 3 port B to port A.
MgB is used to extruding manufactured in the present embodiment2MgB is cut in single compound bar pickling2The end of single compound bar, to institute State MgB2The phase structure of mixed-powder in single compound bar is analyzed, the MgB in result and step 32Superconductive powder Phase structure is identical, shows that oxygen-free copper stub 1 is used as plug and has been effectively isolated acid solution and MgB2The contact of superconductive powder. MgB is used using prepared squeeze of the present invention simultaneously2Single compound bar avoids traditional single powder filling, drawing process Central Plains The larger disadvantage of waste of material can be realized mass preparation.
Embodiment 3
Step 1: the commodity non-oxygen copper bar drawing of original dimension Φ 18mm to be worked into the long stick of oxygen-free copper of Φ 10mm, rectify The oxygen-free copper stub 1 that several segment length are respectively 10mm, 30mm and 100mm, every anaerobic are cut into linear cutting equipment after straight The both ends port difference reconditioning of copper stub 1 is smooth, then carries out pickling and removes surface oxide layer, residual acid is removed after cleaning up simultaneously Drying；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub 1 after drying in step 1 is placed in vacuum heat treatment furnace； The annealing heat-treatment is vacuum annealing heat treatment, and the temperature of vacuum annealing heat treatment is 600 DEG C, soaking time 1h, vacuum Degree is less than 10-3Pa；
Step 3: being blocked first with the oxygen-free copper stub 1 that the size after annealing heat-treatment in step 2 is 10 × 10mm of Φ The size of the port A of metal tube 3, the metal tube 3 are Φ 13 (outer diameter) × 1.5mm (wall thickness), then fill Precursor Powder 2 It is attached in the metal tube 3, and smashes pressure Precursor Powder 2 with metal bar, be finally with the size after annealing heat-treatment in step 2 Φ 9.5 × 100mm oxygen-free copper stub 1 blocks the port B of the metal tube 3, wherein during driving powder 2 before filling the container, often It is 9.5 × 30mm of Φ that filling 5g Precursor Powder 2, which places the size in a step 2 after annealing heat-treatment into the metal tube 3, Oxygen-free copper stub 1, for Precursor Powder 2 to be isolated；The metal tube 3 is niobium pipe or nickel tube；The Precursor Powder 2 is MgB2It is super Lead powder；The MgB2Superconductive powder is by magnesium powder, boron powder and doping powder constituent, the integral molar quantity of the boron powder and doping powder It is 1:2 with the ratio between the mole of the magnesium powder, the mole of the doping powder is the 0.06% of the mole of the boron powder, The doping powder is TiC powder；
Step 4: the metal tube 3 after two-port in step 3 is blocked is assembled into as Φ 16 (outer diameter) × 1.5mm (wall It is thick) oxygen-free copper canning tube 4 in, as shown in Figure 1, being worked into Φ through 6 passage drawings with 10% pass deformation rate on broaching machine 11.7mm, then six square rods of 10mm are drawn into the mold of six side 11.2mm, 10.6mm and 10mm, then along the compound length The middle position cutting of oxygen-free copper stub 1 in stick, obtains squeezing after pickling and uses MgB2Single compound bar；The compound long stick is Six square rods, the opposite side distance of six square rod are 10mm；The outer diameter of the metal tube 3 is identical as the internal diameter of oxygen-free copper canning tube 4, institute It states drawing and is processed as unidirectional drawing, the direction of the drawing processing is from metal tube 3 port B to port A.
MgB is used to extruding manufactured in the present embodiment2MgB is cut in single compound bar pickling2The end of single compound bar, to institute State MgB2The phase structure of mixed-powder in single compound bar is analyzed, the MgB in result and step 32Superconductive powder Phase structure is identical, shows that oxygen-free copper stub 1 is used as plug and has been effectively isolated acid solution and MgB2The contact of superconductive powder. MgB is used using prepared squeeze of the present invention simultaneously2Single compound bar avoids traditional single powder filling, drawing process Central Plains The larger disadvantage of waste of material can be realized mass preparation.
Embodiment 4
Step 1: the commodity non-oxygen copper bar drawing of original dimension Φ 20mm to be worked into the long stick of oxygen-free copper of Φ 12mm, rectify The oxygen-free copper stub 1 that several segment length are respectively 15mm, 30mm and 100mm, every anaerobic are cut into linear cutting equipment after straight The both ends port difference reconditioning of copper stub 1 is smooth, then carries out pickling and removes surface oxide layer, residual acid is removed after cleaning up simultaneously Drying；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub 1 after drying in step 1 is placed in vacuum heat treatment furnace； The annealing heat-treatment is vacuum annealing heat treatment, and the temperature of vacuum annealing heat treatment is 550 DEG C, soaking time 1.5h, very Reciprocal of duty cycle is less than 10-3Pa；
Step 3: being blocked first with the oxygen-free copper stub 1 that the size after annealing heat-treatment in step 2 is 12 × 15mm of Φ The port A of metal tube 3, the size of the metal tube 3 is Φ 16 (outer diameter) × 2mm (wall thickness), then that Precursor Powder 2 is filling Pressure Precursor Powder 2 is smash into the metal tube 3, and with metal bar, is finally Φ with the size after annealing heat-treatment in step 2 12 × 100mm oxygen-free copper stub 1 blocks the port B of the metal tube 3, wherein during driving powder 2 before filling the container, often fills out Fill 8g Precursor Powder 2 placed into the metal tube 3 size in a step 2 after annealing heat-treatment be 12 × 30mm of Φ without Oxygen copper stub 1, for Precursor Powder 2 to be isolated；The metal tube 3 is niobium pipe or nickel tube；The Precursor Powder 2 is MgB2Superconduction Powder；
Step 4: the metal tube 3 after two-port in step 3 is blocked is assembled into as Φ 20 (outer diameter) × 2.0mm (wall It is thick) oxygen-free copper canning tube 4 in, as shown in Figure 1, being worked into Φ through 6 passage drawings with 10% pass deformation rate on broaching machine 14.5mm, then six square rods of 12mm are drawn into the mold of six side 13.2mm, 12.6mm and 12mm, then along the compound length The middle position cutting of oxygen-free copper stub 1 in stick, obtains squeezing after pickling and uses MgB2Single compound bar；The compound long stick is Six square rods, the opposite side distance of six square rod are 12mm；The outer diameter of the metal tube 3 is identical as the internal diameter of oxygen-free copper canning tube 4, institute It states drawing and is processed as unidirectional drawing, the direction of the drawing processing is from metal tube 3 port B to port A.
MgB is used to extruding manufactured in the present embodiment2MgB is cut in single compound bar pickling2The end of single compound bar, to institute State MgB2The phase structure of mixed-powder in single compound bar is analyzed, the MgB in result and step 32Superconductive powder Phase structure is identical, shows that oxygen-free copper stub 1 is used as plug and can be effectively isolated acid solution and MgB2Superconductive powder connects Touching.MgB is used using extruding prepared by the present invention simultaneously2Single compound bar avoids traditional single powder filling, drawing process Chinese raw materials wastes larger disadvantage, can be realized mass preparation.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention Protection scope in.

Claims (7)

1. MgB is used in a kind of extruding2The preparation method of single compound bar, which is characterized in that method includes the following steps:
Step 1: be cut into oxygen-free copper stub after the aligning long stick of oxygen-free copper, then pickling, clear successively is carried out to the oxygen-free copper stub It washes and dries；
Annealing heat-treatment is carried out Step 2: the oxygen-free copper stub after drying in step 1 is placed in vacuum heat treatment furnace；
Step 3: the port A of metal tube is blocked with the oxygen-free copper stub after annealing heat-treatment in step 2 first, then by forerunner In powder filling to the metal tube, and pressure Precursor Powder is smash with metal bar, finally with the nothing after annealing heat-treatment in step 2 Oxygen copper stub blocks the port B of the metal tube, wherein at interval of a distance to described during driving powder before filling the container The oxygen-free copper stub in a step 2 after annealing heat-treatment is placed in metal tube for Precursor Powder to be isolated；The metal tube is Niobium pipe or nickel tube；The Precursor Powder is MgB2Superconductive powder or by magnesium powder, boron powder and adulterate powder constituent mixed powder End；
Step 4: the metal tube after two-port in step 3 is blocked is assembled into oxygen-free copper canning tube, then drawing is processed into Compound long stick, then the middle position of oxygen-free copper stub is cut along the compound long stick, is obtained squeezing after pickling and is used MgB2It is single Core compound bar；The outer diameter of the metal tube is identical as the internal diameter of oxygen-free copper canning tube.
2. MgB is used in a kind of extruding according to claim 12The preparation method of single compound bar, which is characterized in that step 1 Described in the diameter of the long stick of oxygen-free copper be 15mm ~ 20mm, the diameter of the oxygen-free copper stub is 6mm ~ 12mm, and the oxygen-free copper is short The length of stick is 1cm ~ 10cm.
3. MgB is used in a kind of extruding according to claim 12The preparation method of single compound bar, which is characterized in that step 2 Described in annealing heat-treatment be vacuum annealing heat treatment, the temperature of vacuum annealing heat treatment is 500 DEG C ~ 600 DEG C, and soaking time is 1h ~ 2h, vacuum degree is less than 10-3Pa。
4. MgB is used in a kind of extruding according to claim 22The preparation method of single bar, which is characterized in that in step 3 Length for blocking the oxygen-free copper stub of metal pipe end opening A is 1cm, and the length of the oxygen-free copper stub of intermediate isolating powder is 1cm ~ 3cm, the length of the oxygen-free copper stub for blocking metal pipe end opening B are 8cm ~ 10cm.
5. MgB is used in a kind of extruding according to claim 42The preparation method of single bar, which is characterized in that in step 4 The drawing is processed as unidirectional drawing, and the direction of the drawing processing is from metal pipe end opening B to metal pipe end opening A.
6. MgB is used in a kind of extruding according to claim 12The preparation method of single bar, which is characterized in that in step 3 The ratio between the mole of integral molar quantity and magnesium powder of boron powder and doping powder is 1:2 in the mixed-powder, the doping powder Mole is the 0.03% ~ 0.08% of the mole of the boron powder, and the doping powder is amorphous carbon powder, SiC powder or TiC powder End.
7. MgB is used in a kind of extruding according to claim 12The preparation method of single bar, which is characterized in that in step 4 The compound long stick is six square rods, and the opposite side distance of six square rod is the mm of 5mm ~ 12.
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