CN101872661A - Method for preparing naphthalene-doped MgB2 superconductive single-core wire - Google Patents
Method for preparing naphthalene-doped MgB2 superconductive single-core wire Download PDFInfo
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- CN101872661A CN101872661A CN201010180583A CN201010180583A CN101872661A CN 101872661 A CN101872661 A CN 101872661A CN 201010180583 A CN201010180583 A CN 201010180583A CN 201010180583 A CN201010180583 A CN 201010180583A CN 101872661 A CN101872661 A CN 101872661A
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Abstract
The invention discloses a method for preparing a naphthalene-doped MgB2 superconductive single-core wire, which comprises the following: 1, a step of making a holding pipe, in which dried magnesium powder and high-purity crystalline boron powder are fully and uniformly mixed in an atomic ratio of 1:2, 2 to 15 mass percent of crystalline naphthalene is added, the mixture is fully mixed and uniformly ground, and the obtained composite material is filled into a Nb/Cu composite metal pipe to make a holding pipe composite body; 2, a step of holding pipe composite body rotary swaging and drawing for making a primary product of the MgB2 superconductive single-core wire; and 3, a step of high temperature sintering, in which the primary product of the MgB2 superconductive single-core wire is subjected to high-temperature sintering in a protective atmosphere in a vacuum annealing furnace. The method of the invention adopts simple steps, requires low preparation cost and short preparation flow, and makes operation and control convenient. The prepared naphthalene-doped MgB2 superconductive single-core wire has excellent properties such as small hole size, high crystal connectivity, high compactness and high critical current density.
Description
Technical field
The present invention relates to a kind of MgB
2The preparation method of superconducting wire especially relates to a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire.
Background technology
New superconduction material MgB
2Have than high transition temperature (39K), big coherence length, be easy to introduce advantages such as flux pinning, simultaneously MgB
2Superconductor can be operated in GM refrigeration machine warm area, so MgB
2Superconductor has wide potential application at aspects such as superconducting power, electronic device, national defence.High J
c, high stable long wire strip be MgB
2The basis of superconductor applications, so MgB
2The superconducting line strips Study on Preparation Technology is significant.Original position powder tiretube process technology (in-situ PIT) is preparation MgB
2One of major technique of wire rod, its preparation process are at first according to MgB
2Atomicity pack into after mixing in the metal tube than batching, adopt swage drawing or rolling mill practice to be prepared into the wire rod of certain size then, generate MgB through Overheating Treatment at last
2Phase.The advantage of In-situ PIT technology is that thereby back being reacted into B of Mg fusing made formed micro-crack in the course of processing mutually up in heat treatment process, the MgB in the therefore final wire rod
2Superconducting phase crystal grain connects better.Simultaneously, adopting in-situ method to prepare MgB
2In the process of wire rod,, can effectively improve MgB by adjusting heat treatment parameter and introducing useful flux pinning center
2The J of wire rod under High-Field
cValue.
At present, the C element substitution of B position is to improve MgB
2One of effective way of superconducting wire performance, doped source are generally selected nanometer or micron C powder for use, and micron C powder particles causes reactivity very low more greatly, has only very a spot of carbon atom to enter MgB
2Lattice, and remaining carbon all is piled up in the crystal boundary place and reduced intercrystalline connectivity, so the critical current density of wire rod and irreversible improve limited; And nanometer C powder is easy to reunite, and causes the doped source skewness, thereby has also influenced the performance of wire rod to a certain extent.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of naphthalene-doped MgB at above-mentioned deficiency of the prior art
2The preparation method of superconductive single-core wire, its method step is simple, and preparation cost is low and flow process short, easy and simple to handle, control convenience, prepared naphthalene-doped MgB
2Superconductive single-core wire has that bore hole size is little, the crystal grain connectivity is good, good characteristics such as high-compactness, high critical current densities.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire is characterized in that this method may further comprise the steps:
Step 1, tubulature: at first, be that 1: 2 ratio fully mixes according to the atomicity ratio, just obtain compound with the magnesium powder of drying and high-purity crystalline state boron powder; In described compound, add the crystalline state naphtho-then and evenly obtain to make up and expect in the back through abundant mixed grinding, and to add the mass percent that the crystalline state naphthalene accounts for described compound be 2%～15%; Subsequently, described combination material is packed in the Nb/Cu composite metal pipe, just make the tubulature complex; Interior pipe that described Nb/Cu composite metal pipe is made by the Nb material and coaxial package are managed the outside and are made up of the outer tube that the Cu material is made in described;
Step 2, swage and drawing is handled: adopt swager and drawbench successively the tubulature complex in the step 1 to be swaged and drawing is handled, obtaining diameter is the MgB of Φ 1.0～3.0mm
2The superconductive single-core wire preliminary product; And when swaging with the drawing processing, pass reduction is 10%～20%;
Step 3, high temperature sintering are handled: adopt vacuum annealing furnace and under protective atmosphere to the MgB in the step 2
2The superconductive single-core wire preliminary product is carried out 700～850 ℃ of high temperature sinterings and is handled acquisition MgB
2The superconductive single-core wire finished product; When high temperature sintering was handled, heating rate was 20～30 ℃/min, and temperature retention time is 1.5～3h, and vacuum degree is 10
-3More than the Pa, being cooled to room temperature and cooldown rate after high temperature sintering is finished dealing with is 10～30 ℃/min.
The abundant mixed grinding time described in the above-mentioned steps one is 0.5～1.0h.
The quality purity of high-purity crystalline state boron powder is 99.999% described in the above-mentioned steps one, and the quality purity of described magnesium powder and crystalline state naphthalene is 99%, and the particle diameter of described magnesium powder is not more than 325 orders.
Protective atmosphere described in the above-mentioned steps three is that bulk purity is not less than 99.999% high-purity argon gas atmosphere.
MgB described in the above-mentioned steps two
2The cross section of superconductive single-core wire preliminary product is regular hexagon or circle.
Also need before the tubulature in the above-mentioned steps one described Nb/Cu composite metal pipe is carried out pickling processes, and when carrying out pickling processes, the mixed acid that employing is made up of nitric acid and hydrofluoric acid carries out pickling, and pickling is dewatered with alcohol afterwards and dried, and the volume ratio of described nitric acid and hydrofluoric acid is 3: 1.
The present invention compared with prior art has the following advantages:
1, method step is simple, and preparation cost is low and flow process short.
2, reasonable in design, easy and simple to handle and control makes things convenient for, raw material is selected crystalline state high purity boron powder ,-325 order magnesium powder and crystalline state naphthalene for use, with above-mentioned magnesium powder and boron powder according to Mg: B=1: 2 atomicity than batching after, after adding quality again and be the doping crystalline state naphthalene of mixed-powder quality x% and fully mixing, the Cu/Nb multiple tube of packing into by hand is drawn to certain size with the 10-20% pass reduction, and heat-treats, and finally obtains naphthalene-doped MgB
2Superconductive single-core wire.
3, prepared naphthalene-doped MgB
2The superconductive single-core wire function admirable, the present invention when heat treatment effectively refinement MgB
2Crystal grain has reduced bore hole size, has strengthened MgB
2Crystal grain connects, and has improved flux pinning force.Because the crystalline state naphthalene is solid-state at normal temperatures and pressures, can be easy to grind into powder and Mg powder, the B powder evenly mixes, at MgB
2Under the heat treated hot conditions of superconducting wire, can decompose the generation activated carbon by trace, fraction can enter MgB
2Lattice plays a part to substitute and pinning center.Simultaneously, naphthalene is at MgB
2Under the heat treated temperature conditions of superconductor with the gaseous form even dispersion in the Mg-B system, Mg-B system and liquid Mg dripped the secondary mixing is arranged, broken effect, effectively therefore the bore hole size of wire rod after the minimizing heat treatment can prepare the superconducting wire that hole is little, the crystal grain connectivity is good.
4, adopt the Nb/Cu composite material as sheath material, not only can avoid the dispersal behavior between the metal level and superconducting layer when heat treatment, and Cu has good electrical conductivity, can play the effect of stabilisation.
5, adopt the Nb/Cu multiple tube that processing characteristics is good, intensity is higher to help in the course of processing, carrying out the processing of aximal deformation value, be suitable for the preparation of the long wire rod of multicore, the pickling of single-core wire simultaneously can be dispeled surface scale, more help single-core line compound with secondary copper pipe and center non-oxygen copper bar, improved metal flow in the course of processing, reduced the generation of phenomenon of rupture, simultaneously can efficient hardening MgB
2Crystal grain connectivity.
6, heat treatment process not only can be made the micro-crack that the course of processing forms up, and metal Nb is to MgB
2Material has good chemical inertness, has reduced Nb/MgB to a great extent
2Dispersal behavior between the interface.
In sum, the inventive method step is simple, and preparation cost is low and flow process short, easy and simple to handle, control convenience, prepared naphthalene-doped MgB
2Superconductive single-core wire has that bore hole size is little, the crystal grain connectivity is good, good characteristic such as high-compactness, high critical current densities, it adopts the alternative dopings source of crystalline state naphthalene as B position C, can improve intercrystalline connectivity to a certain extent, very easily distil owing to naphthalene simultaneously, the naphthalene that exists with gaseous form when heat treatment drips with liquid Mg the Mg-B system the secondary mixing, the effect of fragmentation, effectively therefore the bore hole size of wire rod after the minimizing heat treatment can prepare the MgB that bore hole size is little, the crystal grain connectivity is good
2Superconductive single-core wire.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is a process chart of the present invention.
Embodiment
A kind of naphthalene-doped MgB as shown in Figure 1
2The preparation method of superconductive single-core wire may further comprise the steps:
Step 1, tubulature: at first, be that 1: 2 ratio fully mixes according to the atomicity ratio, just obtain compound with the magnesium powder of drying and high-purity crystalline state boron powder; In described compound, add the crystalline state naphtho-then and evenly obtain to make up and expect in the back through abundant mixed grinding, and to add the mass percent that the crystalline state naphthalene accounts for described compound be 2%～15%; Subsequently, described combination material is packed in the Nb/Cu composite metal pipe, just make the tubulature complex; Interior pipe that described Nb/Cu composite metal pipe is made by the Nb material and coaxial package are managed the outside and are made up of the outer tube that the Cu material is made in described.
During actual being prepared, fully the mixed grinding time is 0.5～1.0h.The purity of described high-purity crystalline state boron powder is 99.999%, and the purity of described magnesium powder and crystalline state naphthalene is 99%, and the particle diameter of described magnesium powder is not more than 325 orders.
Step 2, swage and drawing is handled: adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, and to obtain diameter be the MgB of Φ 1.0～3.0mm
2The superconductive single-core wire preliminary product; And when swaging with the drawing processing, pass reduction is 10%～20%.
Step 3, high temperature sintering are handled: adopt vacuum annealing furnace and under protective atmosphere to the MgB described in the step 2
2The superconductive single-core wire preliminary product is carried out 700～850 ℃ of high temperature sinterings processing, and obtains MgB
2The superconductive single-core wire finished product; And when carrying out the high temperature sintering processing, heating rate is 20～30 ℃/min, and temperature retention time is 1.5～3h, and vacuum degree is 10
-3More than the Pa, being cooled to room temperature and cooldown rate after high temperature sintering is finished dealing with is 10～30 ℃/min.
Embodiment 1
In the present embodiment, to naphthalene-doped MgB
2When superconductive single-core wire was prepared, its preparation process was as follows:
Step 1, tubulature: at first, be that 1: 2 ratio fully mixes according to the atomicity ratio, just obtain compound with the magnesium powder of drying and high-purity crystalline state boron powder; Afterwards, in described compound, add the crystalline state naphtho-again and evenly obtain to make up and expect in the back through abundant mixed grinding, and to add the mass percent that the crystalline state naphthalene accounts for described compound be 2%; Subsequently, described combination material is packed in the Nb/Cu composite metal pipe, just make the tubulature complex; Interior pipe that described Nb/Cu composite metal pipe is made by the Nb material and coaxial package are managed the outside and are made up of the outer tube that the Cu material is made in described.
During actual being prepared, fully the mixed grinding time is 0.5h.The quality purity of described high-purity crystalline state boron powder is 99.999%, and the quality purity of described magnesium powder and crystalline state naphthalene is 99%, and the particle diameter of described magnesium powder is not more than 325 orders.Before the tubulature, also need to carry out pickling processes, and when carrying out pickling processes, adopt the mixed acid of forming by nitric acid and hydrofluoric acid to carry out pickling described Nb/Cu composite metal pipe, pickling is dewatered with alcohol afterwards and is dried, and the volume ratio of described nitric acid and hydrofluoric acid is 3: 1.And during tubulature, adopt manual mode to carry out tubulature.
Step 2, swage and drawing is handled: adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, and to obtain diameter be the MgB of Φ 1.0mm
2The superconductive single-core wire preliminary product; And when swaging with the drawing processing, pass reduction is 10%.
In the present embodiment, described MgB
2The cross section of superconductive single-core wire preliminary product is regular hexagon or circle, and actual swaging and drawing when handling also can be according to the concrete needs of reality, with described MgB
2The cross section of superconductive single-core wire preliminary product is processed into the Else Rule shape.
Step 3, high temperature sintering are handled: adopt vacuum annealing furnace and under protective atmosphere to the MgB described in the step 2
2The superconductive single-core wire preliminary product is carried out the high temperature sintering processing, and obtains MgB
2The superconductive single-core wire finished product; And when carrying out the high temperature sintering processing, sintering temperature is 750 ℃, and heating rate is 25 ℃/min, and temperature retention time is 3h, and vacuum degree is 10
-3More than the Pa, being cooled to room temperature and cooldown rate after high temperature sintering is finished dealing with is 20 ℃/min.Described protective atmosphere is that bulk purity is not less than 99.999% high-purity argon gas atmosphere, and during actual fabrication, also can adopt other protective atmosphere.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 35.3K down, and 15K does not have external magnetic field condition lower critical current density and reaches 1.1 * 10
5A/cm
2
Embodiment 2
In the present embodiment, as different from Example 1: in the step 1 during tubulature, adding the mass percent that the crystalline state naphthalene accounts for described compound in described compound is 5%, and fully the mixed grinding time is 0.8h; Swage in the step 2 and drawing when handling, adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, pass reduction is 15%, and to obtain diameter be the MgB of Φ 1.0mm
2The superconductive single-core wire preliminary product; When carrying out the high temperature sintering processing in the step 3, sintering temperature is 800 ℃, and heating rate is 20 ℃/min, and temperature retention time is 1.5h.In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 34.7K down, and 15K does not have external magnetic field condition lower critical current density and reaches 1.4 * 10
5A/cm
2
Embodiment 3
In the present embodiment, as different from Example 1: in the step 1 during tubulature, adding the mass percent that the crystalline state naphthalene accounts for described compound in described compound is 8%, and fully the mixed grinding time is 0.6h; Swage in the step 2 and drawing when handling, adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, pass reduction is 15%, and to obtain diameter be the MgB of Φ 1.5mm
2The superconductive single-core wire preliminary product; When carrying out the high temperature sintering processing in the step 3, sintering temperature is 750 ℃, and heating rate is 20 ℃/min, and temperature retention time is 2.5h, and cooldown rate is 15 ℃/min.In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 34.8K down, and 15K does not have external magnetic field condition lower critical current density and reaches 1.6 * 10
5A/cm
2
Embodiment 4
In the present embodiment, as different from Example 1: in the step 1 during tubulature, adding the mass percent that the crystalline state naphthalene accounts for described compound in described compound is 10%, and fully the mixed grinding time is 0.6h; Swage in the step 2 and drawing when handling, adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, pass reduction is 20%, and to obtain diameter be the MgB of Φ 2.0mm
2The superconductive single-core wire preliminary product; When carrying out the high temperature sintering processing in the step 3, sintering temperature is 700 ℃, and heating rate is 25 ℃/min, and temperature retention time is 2.0h, and cooldown rate is 10 ℃/min.In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 34.2K down, and 15K does not have external magnetic field condition lower critical current density and reaches 1.0 * 10
5A/cm
2
Embodiment 5
In the present embodiment, as different from Example 1: in the step 1 during tubulature, adding the mass percent that the crystalline state naphthalene accounts for described compound in described compound is 12%, and fully the mixed grinding time is 0.6h; Swage in the step 2 and drawing when handling, adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, pass reduction is 20%, and to obtain diameter be the MgB of Φ 2.5mm
2The superconductive single-core wire preliminary product; When carrying out the high temperature sintering processing in the step 3, sintering temperature is 850 ℃, and heating rate is 30 ℃/min, and temperature retention time is 1.5h, and cooldown rate is 30 ℃/min.In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 34.0K down, and 15K does not have external magnetic field condition lower critical current density and reaches 9.8 * 10
4A/cm
2
Embodiment 6
In the present embodiment, as different from Example 1: in the step 1 during tubulature, adding the mass percent that the crystalline state naphthalene accounts for described compound in described compound is 15%, and fully the mixed grinding time is 1.0h; Swage in the step 2 and drawing when handling, adopt swager and drawbench successively the tubulature complex described in the step 1 to be swaged and drawing is handled, pass reduction is 15%, and to obtain diameter be the MgB of Φ 3.0mm
2The superconductive single-core wire preliminary product; When carrying out the high temperature sintering processing in the step 3, sintering temperature is 800 ℃, and heating rate is 28 ℃/min, and temperature retention time is 1.8h, and cooldown rate is 25 ℃/min.In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The MgB that finally makes
2The superconductive single-core wire finished product has that bore hole size is little, the crystal grain connectivity is good, characteristics such as high-compactness and high critical current densities, superconducting transition temperature T
cOutside magnetic field 0T is 33.6K down, and 15K does not have external magnetic field condition lower critical current density and reaches 9.6 * 10
4A/cm
2
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection range of technical solution of the present invention according to the technology of the present invention essence.
Claims (6)
1. naphthalene-doped MgB
2The preparation method of superconductive single-core wire is characterized in that this method may further comprise the steps:
Step 1, tubulature: at first, be that 1: 2 ratio fully mixes according to the atomicity ratio, just obtain compound with the magnesium powder of drying and high-purity crystalline state boron powder; In described compound, add the crystalline state naphtho-then and evenly obtain to make up and expect in the back through abundant mixed grinding, and to add the mass percent that the crystalline state naphthalene accounts for described compound be 2%～15%; Subsequently, described combination material is packed in the Nb/Cu composite metal pipe, just make the tubulature complex; Interior pipe that described Nb/Cu composite metal pipe is made by the Nb material and coaxial package are managed the outside and are made up of the outer tube that the Cu material is made in described;
Step 2, swage and drawing is handled: adopt swager and drawbench successively the tubulature complex in the step 1 to be swaged and drawing is handled, obtaining diameter is the MgB of Φ 1.0～3.0mm
2The superconductive single-core wire preliminary product; And when swaging with the drawing processing, pass reduction is 10%～20%;
Step 3, high temperature sintering are handled: adopt vacuum annealing furnace and under protective atmosphere to the MgB in the step 2
2The superconductive single-core wire preliminary product is carried out 700～850 ℃ of high temperature sinterings and is handled acquisition MgB
2The superconductive single-core wire finished product; When high temperature sintering was handled, heating rate was 20～30 ℃/min, and temperature retention time is 1.5～3h, and vacuum degree is 10
-3More than the Pa, being cooled to room temperature and cooldown rate after high temperature sintering is finished dealing with is 10～30 ℃/min.
2. according to the described a kind of naphthalene-doped MgB of claim 1
2The preparation method of superconductive single-core wire is characterized in that: the abundant mixed grinding time described in the step 1 is 0.5～1.0h.
3. according to claim 1 or 2 described a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire is characterized in that: the quality purity of high-purity crystalline state boron powder is 99.999% described in the step 1, and the quality purity of described magnesium powder and crystalline state naphthalene is 99%, and the particle diameter of described magnesium powder is not more than 325 orders.
4. according to claim 1 or 2 described a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire is characterized in that: the protective atmosphere described in the step 3 is that bulk purity is not less than 99.999% high-purity argon gas atmosphere.
5. according to claim 1 or 2 described a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire is characterized in that: MgB described in the step 2
2The cross section of superconductive single-core wire preliminary product is regular hexagon or circle.
6. according to claim 1 or 2 described a kind of naphthalene-doped MgB
2The preparation method of superconductive single-core wire, it is characterized in that: also need before the tubulature in the step 1 described Nb/Cu composite metal pipe is carried out pickling processes, and when carrying out pickling processes, the mixed acid that employing is made up of nitric acid and hydrofluoric acid carries out pickling, pickling is dewatered with alcohol afterwards and is dried, and the volume ratio of described nitric acid and hydrofluoric acid is 3: 1.
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| CN102280198A (en) * | 2011-08-17 | 2011-12-14 | 西北有色金属研究院 | Preparation method for multi-core MgB2 superconducting wire/band |
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| CN103151114A (en) * | 2013-02-25 | 2013-06-12 | 宝胜科技创新股份有限公司 | Single-conductor MgB2 superconducting wire preparation method |
| 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 |
| CN105048237A (en) * | 2015-08-20 | 2015-11-11 | 西北有色金属研究院 | Connection method for MgB2 superconductive wire rods |
| CN109694136A (en) * | 2018-12-29 | 2019-04-30 | 苏州凯虹高分子科技有限公司 | A kind of scale inhibition pipe and its production technology |
| CN109694136B (en) * | 2018-12-29 | 2022-05-10 | 苏州凯虹高分子科技有限公司 | Scale inhibition pipe and production process thereof |
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