CN105869774B - It is a kind of to add the method that Nanometer Copper prepares Bi 2223/Ag multi-core superconducting bands - Google Patents
It is a kind of to add the method that Nanometer Copper prepares Bi 2223/Ag multi-core superconducting bands Download PDFInfo
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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Abstract
The method that Nanometer Copper prepares Bi 2223/Ag multi-core superconducting bands is added the invention discloses a kind of, this method includes：First, prepare and copper nanoparticle ball milling mixing is added after the front axle shells of Bi 2223 that copper owes amount, sintering uniformly, obtain tubulature front axle shell；2nd, tubulature prepares tubulature complex；3rd, single-core wire is processed into tubulature complex drawing；4th, carry out scale successively to single-core wire, block, align and clean, Multi-core wire is then made using bundle drawing method method；5th, multi-filamentary tape is rolled into, is heat-treated, obtains Bi 2223/Ag multi-core superconducting bands.The present invention replaces the part copper in the front axle shells of Bi 2223 using appropriate copper nanoparticle, in final heat treatment, the oxygen of powder adsorption absorbs generation cupric oxide by copper nanoparticle, avoid the influence of impurity opposing webs performance, and can be on the premise of band current-carrying performance be ensured, the generation of bubbling is avoided as far as possible, improves the uniformity of band performance.
Description
Technical field
The invention belongs to superconducting line strips preparing technical field, and in particular to one kind addition Nanometer Copper prepares Bi-2223/Ag
The method of multi-core superconducting band.
Background technology
Bi-2223(Bi2Sr2Ca2Cu3Ox) high-temperature superconductor is most important branch in high temperature superconducting materia, due to its appearance
Easy processing and with higher current-carrying performance, becomes most one of high temperature superconducting materia of future.Current powder-in-tube technique
And the technology of preparing that is combined of fusion method is the mainstream technology for preparing high-performance Bi system high-temperature superconducting wire strips (PIT).The technology
It is that superconducting precursor powder end is loaded into silver pipe, multicore complex, wire strip chi of the reprocessing to design is prepared into by drawing, assembling
It is very little, then it is heat-treated the wire strip that can obtain superconduction.
All the time, the bubbling problem of Bi-2223 bands limits the raising of material property always, the reason for for bubbling
Most of scholar thinks that the main cause of band bubbling is that carbon in powder discharges CO at high temperature2.Hellstrom groups are to Bi anchor line (string)s
Band macroscopic view bubbling problem carried out systematic research, it is believed that the formation of bubbling is H2O、CO2Or O2The expansion of gas, is added
The low coefficient result of intensity of silver-colored jacket under high temperature.Even if selecting rational heat treating regime largely to reduce
C content in powder, but during the tubulature in later stage, if control is improper because powder has higher activity, easily
Adsorb the H in air2O and CO2Gas, causes the generation of final bubbling.It can largely suppress bulging using high voltage driving IC
The generation of bubble, while core filaments consistency is improved, it is hereby achieved that high current-carrying performance, but suitable high-tension apparatus is held high very much
Expensive, only SUMITOMO CHEMICAL company possesses the kind equipment at present, and the reason in technical know-how, equipment embargo.And it is domestic
For various reasons, the high voltage driving IC equipment of manufacture is not significantly improved the current-carrying performance of band, therefore, by rational
Technology and control avoids the generation of bubbling, and the uniformity for improving band performance just seems very necessary.
The content of the invention
The technical problems to be solved by the invention are to add Nanometer Copper there is provided one kind for above-mentioned the deficiencies in the prior art
The method for preparing Bi-2223/Ag multi-core superconducting bands.This method is replaced in Bi-2223 front axle shells using appropriate copper nanoparticle
Part copper, tubulature front axle shell is placed and the tubulature under oxygen atmosphere under oxygen atmosphere before tubulature so that band is most
The oxygen of powder adsorption absorbs generation cupric oxide by copper nanoparticle during heat treatment eventually, and the cupric oxide generated can participate in Bi-
2223 into during phase, it is to avoid the influence of impurity opposing webs performance, and can ensure the premise of band current-carrying performance
Under, the generation of bubbling is avoided as far as possible, improves the uniformity of band performance.
In order to solve the above technical problems, the technical solution adopted by the present invention is：One kind addition Nanometer Copper prepares Bi-2223/
The method of Ag multi-core superconducting bands, it is characterised in that comprise the following steps：
Step 1: preparing the Bi-2223 front axle shells that copper owes amount, it will add after forerunner's powder sintering into the front axle shell of sintering
Entering copper nanoparticle makes the mass content of copper in front axle shell reach Theoretical Mass content, then will add copper nanoparticle under argon gas protection
Front axle shell ball milling mixing it is uniform, obtain tubulature front axle shell；The Bi-2223 front axle shells that the copper owes amount refer to copper in front axle shell
Quality is 92%~95% of copper Theoretical Mass in Bi-2223；
Step 2: tubulature front axle shell described in step one is placed into 2h~3h in the glove box that oxygen atmosphere is protected, so
The tubulature front axle shell after placement is fitted into silver-colored pipe in glove box afterwards, tubulature complex is made；
Step 3: the drawing of tubulature complex described in step 2 is processed into single-core wire；
Step 4: carrying out scale successively to single-core wire described in step 3, blocking, align and clean, then using collection
Multi-core wire is made in many single-core wires by beam Hubbing method；
Step 5: Multi-core wire described in step 4 is rolled into multi-filamentary tape using flat rolling system, then to described many
Core ribbon material is heat-treated and intermediate rolling, obtains Bi-2223/Ag multi-core superconducting bands.
The method that a kind of above-mentioned addition Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that step
The quality purity of copper nanoparticle described in one is not less than 99.9%, and granularity is not more than 50nm.
The method that a kind of above-mentioned addition Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that step
The ratio of grinding media to material that the bulk purity of argon gas described in one is not less than in 99.99%, mechanical milling process is (2~5):1, the time of ball milling is
1h~2h, wherein ratio of grinding media to material refer to mass ratio.
The method that a kind of above-mentioned addition Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that step
Oxygen described in two is high purity oxygen gas, and stagnation pressure superatmospheric 400Pa~600Pa of glove box, the temperature in glove box is 20
DEG C~25 DEG C.
The method that a kind of above-mentioned addition Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that step
Two vibrate tubulature in glove box using shake table.
The method that a kind of above-mentioned addition Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that described
The vibration frequency of shake table is 40Hz~60Hz.
The present invention has advantages below compared with prior art：
1st, this invention simplifies preparation technology, degassing process is reduced, it is to avoid existing degassing process needs to expend more
Manpower and electric power energy defect, simultaneously, it is to avoid influence of the human factor to degassing effect.
2nd, the present invention replaces the part copper in Bi-2223 front axle shells using appropriate copper nanoparticle, by tubulature before tubulature
Front axle shell is placed and the tubulature under oxygen atmosphere under oxygen atmosphere so that the oxygen of band powder adsorption in final heat treatment
Generation cupric oxide is absorbed by copper nanoparticle, and the cupric oxide generated can participate in Bi-2223 into during phase, it is to avoid impurity
The influence of opposing webs performance, and can avoid the generation of bubbling as far as possible on the premise of band current-carrying performance is ensured, carry
The uniformity of high band performance.
3rd, the tubulature of the invention under oxygen atmosphere, can avoid other gases such as powder adsorption water, carbon dioxide, it is to avoid
Influence of other side reactions to band during high temperature.
4th, method of the invention can largely improve the current-carrying uniformity of band.Avoid because bubbling rupture is made
Into pollution of the effusion to band so that causing band to quench the generation of phenomenon.Simultaneously as absorption oxygen by powder from
Body is absorbed, so avoiding influence of the high pressure produced under gas high temperature to core filaments consistency, core can be improved to a certain extent
Silk consistency.
With reference to the accompanying drawings and examples, technical scheme is described in further detail.
Figure of description
Fig. 1 is the apparent form photo of Bi-2223/Ag multi-core superconducting bands prepared by the embodiment of the present invention 1.
Fig. 2 is the apparent form photo of Bi-2223/Ag multi-core superconducting bands prepared by comparative example 1.
Embodiment
Embodiment 1
The preparation method of the Bi-2223/Ag multi-core superconducting bands of the present embodiment comprises the following steps：
Step 1: the Bi-2223 front axle shells that copper owes amount are prepared using conventional coprecipitation, forerunner's powder sintering is backward
Copper nanoparticle is added in the front axle shell of sintering makes the mass content of copper in front axle shell reach Theoretical Mass content, then in argon gas protection
It is lower that the front axle shell ball milling mixing for adding copper nanoparticle is uniform, obtain tubulature front axle shell；The copper owes the Bi-2223 front axle shells of amount
The quality for referring to copper in front axle shell is 95% of copper Theoretical Mass in Bi-2223；The quality purity of the copper nanoparticle is not less than
99.9%, granularity is not more than 50nm；The ratio of grinding media to material that the bulk purity of the argon gas is not less than in 99.99%, mechanical milling process is 2:
1, the time of ball milling is 2h, and wherein ratio of grinding media to material refers to mass ratio；
Step 2: tubulature front axle shell described in step one is placed into 2h, Ran Hou in the glove box that oxygen atmosphere is protected
The tubulature front axle shell after placement is fitted into silver-colored pipe using shake table in glove box, tubulature complex is made；The oxygen is height
Temperature in purity oxygen, the stagnation pressure superatmospheric 400Pa of glove box, glove box is 25 DEG C, and the vibration frequency of shake table is
40Hz；
Step 3: using 10% pass reduction, the drawing of tubulature complex described in step 2 is processed into cross section
For diameter 2.8mm circular single-core wire, single-core wire of the cross section for regular hexagon then is processed into through three passages,
The circumscribed circle diameter of regular hexagon is 2.5mm；
Step 4: to section described in step 3 for regular hexagon single-core wire according to being blocked after 0.4m scales, then
Aligned and cleaned, many single-core wires are made by Multi-core wire using bundle drawing method method；Preparing for Multi-core wire is specific
For：(can be using silver-colored manganese alloy, silver-colored manganese tin alloy by 37 single-core wires loading silver alloy jackets from the conductor structure of 37 cores
Deng) in obtain secondary complex, using 10% pass reduction, secondary complex drawing is machined into cross-sectional diameter is
During 4mm, intermediate annealing is carried out at 350 DEG C, the time of intermediate annealing is 60min, and continuation drawing is machined to cross-sectional diameter and is
1.71mm；
Step 5: using flat rolling system, using each reduction in pass as 0.1mm, Multi-core wire described in step 4 is rolled
The thick multi-filamentary tapes of 0.31mm are made, then the multi-filamentary tape is heat-treated 60 hours in 835 DEG C of constant temperature, used after cooling
10% working modulus carries out intermediate rolling, is heat-treated 80 hours then at 835 DEG C of constant temperature, and Bi-2223/Ag multicores are obtained after cooling and are surpassed
Conduction band material, whole heat treatment process is protected using the gaseous mixture of oxygen and argon gas, the volume of oxygen and argon gas in gaseous mixture
Than for 8:92.
The apparent form photo of Bi-2223/Ag multi-core superconductings band manufactured in the present embodiment is as shown in figure 1, without obvious
Bubble, bubbling phenomenon is greatly improved, under the conditions of 77K, self-fields, and critical current density has reached 2.0 × 104A/cm2。
Comparative example 1
Bi-2223 front axle shells are prepared using conventional coprecipitation, will directly be carried out after Bi-2223 forerunner's powder sintering of preparation
Tubulature, then prepares Bi-2223/Ag multi-core superconducting bands according to the method for embodiment 1.The band apparent form photo of preparation is such as
Shown in Fig. 2.
Comparison diagram 1 and Fig. 2 are, it is apparent that the Bi-2223/Ag multi-core superconducting bands prepared using the method for the present invention
Bubbling phenomenon is greatly improved.
Embodiment 2
The preparation method of the Bi-2223/Ag multi-core superconducting bands of the present embodiment comprises the following steps：
Step 1: the Bi-2223 front axle shells that copper owes amount are prepared using conventional coprecipitation, forerunner's powder sintering is backward
Copper nanoparticle is added in the front axle shell of sintering makes the mass content of copper in front axle shell reach Theoretical Mass content, then in argon gas protection
It is lower that the front axle shell ball milling mixing for adding copper nanoparticle is uniform, obtain tubulature front axle shell；The copper owes the Bi-2223 front axle shells of amount
The quality for referring to copper in front axle shell is 92% of copper Theoretical Mass in Bi-2223；The quality purity of the copper nanoparticle is not less than
99.9%, granularity is not more than 50nm；The ratio of grinding media to material that the bulk purity of the argon gas is not less than in 99.99%, mechanical milling process is 5:
1, the time of ball milling is 1h, and wherein ratio of grinding media to material refers to mass ratio；
Step 2: tubulature front axle shell described in step one is placed into 3h, Ran Hou in the glove box that oxygen atmosphere is protected
The tubulature front axle shell after placement is fitted into silver-colored pipe using shake table in glove box, tubulature complex is made；The oxygen is height
Temperature in purity oxygen, the stagnation pressure superatmospheric 600Pa of glove box, glove box is 20 DEG C, and the vibration frequency of shake table is
60Hz；
Step 3: using 10% pass reduction, the drawing of tubulature complex described in step 2 is processed into cross section
For diameter 1.6mm circular single-core wire, single-core wire of the cross section for regular hexagon then is processed into through two passages,
The circumscribed circle diameter of regular hexagon is 1.4mm；
Step 4: to section described in step 3 for regular hexagon single-core wire according to being blocked after 0.5m scales, then
Aligned and cleaned, many single-core wires are made by Multi-core wire using bundle drawing method method；Preparing for Multi-core wire is specific
For：(can be using silver-colored manganese alloy, silver-colored manganese tin alloy by 61 single-core wires loading silver alloy jackets from the conductor structure of 61 cores
Deng) in obtain secondary complex, using 10% pass reduction, secondary complex drawing is machined into cross-sectional diameter is
During 4.3mm, intermediate annealing is carried out at 350 DEG C, the time of intermediate annealing is 30min, continues drawing and is machined to cross-sectional diameter
For 1.63mm；
Step 5: using flat rolling system, using each reduction in pass as 0.1mm, Multi-core wire described in step 4 is rolled
The thick multi-filamentary tapes of 0.33mm are made, then the multi-filamentary tape is heat-treated 50 hours in 840 DEG C of constant temperature, used after cooling
10% working modulus carries out intermediate rolling, is heat-treated 70 hours then at 840 DEG C of constant temperature, and Bi-2223/Ag multicores are obtained after cooling and are surpassed
Conduction band material, whole heat treatment process is protected using the gaseous mixture of oxygen and argon gas, the volume of oxygen and argon gas in gaseous mixture
Than for 7:93.
Bi-2223/Ag multi-core superconductings band manufactured in the present embodiment does not have obvious bubble, and bubbling phenomenon is changed significantly
Kind, under the conditions of 77K, self-fields, critical current density has reached 1.8 × 104A/cm2。
Embodiment 3
The preparation method of the Bi-2223/Ag multi-core superconducting bands of the present embodiment comprises the following steps：
Step 1: the Bi-2223 front axle shells that copper owes amount are prepared using conventional spray heating decomposition, by forerunner's powder sintering
Copper nanoparticle is added in the front axle shell sintered backward makes the mass content of copper in front axle shell reach Theoretical Mass content, then in argon gas
It is under protection that the front axle shell ball milling mixing for adding copper nanoparticle is uniform, obtain tubulature front axle shell；The copper is owed before the Bi-2223 of amount
Drive powder and refer to that the quality of copper in front axle shell is 94% of copper Theoretical Mass in Bi-2223；The quality purity of the copper nanoparticle is not
Less than 99.9%, granularity is not more than 50nm；The bulk purity of the argon gas is not less than the ratio of grinding media to material in 99.99%, mechanical milling process
For 3:1, the time of ball milling is 1.5h, and wherein ratio of grinding media to material refers to mass ratio；
Step 2: tubulature front axle shell described in step one is placed into 2.5h in the glove box that oxygen atmosphere is protected, then
The tubulature front axle shell after placement is fitted into silver-colored pipe using shake table in glove box, tubulature complex is made；The oxygen is
Temperature in high purity oxygen gas, the stagnation pressure superatmospheric 500Pa of glove box, glove box is 22 DEG C, and the vibration frequency of shake table is
50Hz；
Step 3: using 10% pass reduction, the drawing of tubulature complex described in step 2 is processed into cross section
For diameter 3.8mm circular single-core wire, single-core wire of the cross section for regular hexagon then is processed into through two passages,
The circumscribed circle diameter of regular hexagon is 3.53mm；
Step 4: to section described in step 3 for regular hexagon single-core wire according to being blocked after 0.5m scales, then
Aligned and cleaned, many single-core wires are made by Multi-core wire using bundle drawing method method；Preparing for Multi-core wire is specific
For：(can be using silver-colored manganese alloy, silver-colored manganese tin alloy by 19 single-core wires loading silver alloy jackets from the conductor structure of 19 cores
Deng) in obtain secondary complex, using 10% pass reduction, secondary complex drawing is machined into cross-sectional diameter is
During 3.8mm, intermediate annealing is carried out at 350 DEG C, the time of intermediate annealing is 30min, continues drawing and is machined to cross-sectional diameter
For 1.5mm；
Step 5: using flat rolling system, using each reduction in pass as 0.1mm, Multi-core wire described in step 4 is rolled
The thick multi-filamentary tapes of 0.30mm are made, then the multi-filamentary tape is heat-treated 60 hours in 838 DEG C of constant temperature, used after cooling
10% working modulus carries out intermediate rolling, is heat-treated 70 hours then at 838 DEG C of constant temperature, and Bi-2223/Ag multicores are obtained after cooling and are surpassed
Conduction band material, whole heat treatment process is protected using the gaseous mixture of oxygen and argon gas, the volume of oxygen and argon gas in gaseous mixture
Than for 8:92.
Bi-2223/Ag multi-core superconductings band manufactured in the present embodiment does not have obvious bubble, and bubbling phenomenon is changed significantly
Kind, under the conditions of 77K, self-fields, critical current density has reached 2.1 × 104A/cm2。
It is described above, only it is presently preferred embodiments of the present invention, any limitation is not done to the present invention, it is every according to invention skill
Any simple modification, change and equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (5)
1. a kind of add the method that Nanometer Copper prepares Bi-2223/Ag multi-core superconducting bands, it is characterised in that comprises the following steps：
Step 1: preparing the Bi-2223 front axle shells that copper owes amount, received being added after forerunner's powder sintering into the front axle shell of sintering
Rice copper powder makes the mass content of copper in front axle shell reach Theoretical Mass content, then before it will add copper nanoparticle under argon gas is protected
Drive sphere of powder mill well mixed, obtain tubulature front axle shell；The Bi-2223 front axle shells of the deficient amount of the copper refer to the quality of copper in front axle shell
For 92%~95% of copper Theoretical Mass in Bi-2223；The quality purity of the copper nanoparticle is not less than 99.9%, and granularity is little
In 50nm；
Step 2: tubulature front axle shell described in step one is placed into 2h~3h, Ran Hou in the glove box that oxygen atmosphere is protected
The tubulature front axle shell after placement is fitted into silver-colored pipe in glove box, tubulature complex is made；
Step 3: the drawing of tubulature complex described in step 2 is processed into single-core wire；
Step 4: carrying out scale successively to single-core wire described in step 3, blocking, align and clean, then drawn using boundling
Multi-core wire is made in many single-core wires by draw out method；
Step 5: Multi-core wire described in step 4 is rolled into multi-filamentary tape using flat rolling system, then to many core ribbon
Material is heat-treated and intermediate rolling, obtains Bi-2223/Ag multi-core superconducting bands.
2. the method that a kind of addition Nanometer Copper according to claim 1 prepares Bi-2223/Ag multi-core superconducting bands, it is special
Levy and be, the ratio of grinding media to material that the bulk purity of argon gas described in step one is not less than in 99.99%, mechanical milling process is (2~5):1,
The time of ball milling is 1h~2h, and wherein ratio of grinding media to material refers to mass ratio.
3. the method that a kind of addition Nanometer Copper according to claim 1 prepares Bi-2223/Ag multi-core superconducting bands, it is special
Levy and be, oxygen described in step 2 is high purity oxygen gas, stagnation pressure superatmospheric 400Pa~600Pa of glove box, in glove box
Temperature be 20 DEG C~25 DEG C.
4. the method that a kind of addition Nanometer Copper according to claim 1 prepares Bi-2223/Ag multi-core superconducting bands, it is special
Levy and be, step 2 vibrates tubulature in glove box using shake table.
5. the method that a kind of addition Nanometer Copper according to claim 4 prepares Bi-2223/Ag multi-core superconducting bands, it is special
Levy and be, the vibration frequency of the shake table is 40Hz~60Hz.
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| US5958842A (en) * | 1996-02-28 | 1999-09-28 | The Regents Of The Uniersity Of California | Melt processing of Bi--2212 superconductors using alumina |
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