CN110853830A - Preparation method of Bi-2212 multi-core superconducting wire - Google Patents

Preparation method of Bi-2212 multi-core superconducting wire Download PDF

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Publication number
CN110853830A
CN110853830A CN201911145654.2A CN201911145654A CN110853830A CN 110853830 A CN110853830 A CN 110853830A CN 201911145654 A CN201911145654 A CN 201911145654A CN 110853830 A CN110853830 A CN 110853830A
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tube
metal salt
salt solution
core
filling
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Inventor
刘国庆
金利华
郝淸滨
崔利军
罗添文
徐晓燕
焦高峰
郑会玲
闫果
李成山
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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
    • 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

Abstract

The invention discloses a preparation method of a Bi-2212 multi-core superconducting wire, which comprises the following steps: first, Bi2O3、CuO、CaCO3And SrCO3Preparing a metal salt solution; atomizing the metal salt solution to obtain metal salt solution fog drops, heating for decomposition, and collecting spray decomposition raw material powder; thirdly, carrying out heat treatment on the spray decomposed raw material powder in a phase manner to obtain tube-filling precursor powder; fourthly, after the pipe-filling precursor powder is filled into a pipe, performing rotary swaging and drawing, secondary compounding, tertiary compounding and rotary swaging and drawing to obtain the multi-core wire; and fifthly, performing heat treatment on the multi-core wire to obtain the Bi-2212 multi-core superconducting wire. According to the invention, the raw materials are prepared into the metal salt solution to prepare the spray decomposition raw material powder, and the pipe-filling precursor powder is obtained through the phase-forming heat treatment, so that the component uniformity and the particle size distribution of the spray decomposition raw material powder are improved, the quality of the pipe-filling precursor powder is improved, and the current-carrying performance and the stability of the Bi-2212 multi-core superconducting wire are further improved.

Description

Preparation method of Bi-2212 multi-core superconducting wire
Technical Field
The invention belongs to the technical field of preparation of high-temperature superconducting wires, and particularly relates to a preparation method of a Bi-2212 multi-core superconducting wire.
Background
Bi2Sr2CaCu2OxThe high-temperature superconductor (Bi 2212 for short) is one of the most important branches in the high-temperature superconducting material, is the only high-temperature superconductor which can be processed into isotropic round wires and has higher current-carrying performance, and can replace a low-temperature superconductor to be used for preparing a large-current cable or winding an inserted magnet to prepare an ultrahigh-magnetic-field magnet. Because the Bi-2212 superconducting material has irreplaceable advantages in a high-field magnet system, the research on the material is very difficult to pay attention to in developed countries such as the United states and the Japan.
The preparation of the high-performance Bi-2212 multi-core wire is the premise of practicality, and the high-quality precursor powder is the basis for preparing the high-performance Bi-2212 multi-core wire. Powder characteristic parameters such as proper stoichiometric ratio, uniform fine powder particle size, and satisfactory phase composition are conditions that high quality precursor powder must satisfy.
While the european Nexans company, as the sole seller of Bi-2212 powder, has been using the melt process to make Bi-2212 precursor powder by 2015, the Nexans company has stopped making and selling Bi-2212 precursor powder for various reasons in the last two years. Currently, the companies trying to prepare the Bi-2212 precursor powder mainly include the company nbimat and Metamaterial in the united states, and nbimat adopts a nano atomization calcination technology to prepare the Bi-2212 precursor powder; meta materials company selects coprecipitation to prepare Bi-2212 precursor powder. The powder preparation technology adopted by the company nGimat is low in preparation efficiency and complex in process control, while the coprecipitation method adopted by the company Metamaterial is easy to cause the deviation of the atomic ratio in the powder, and impurities are easy to introduce by multiple phase-forming heat treatments.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the Bi-2212 multi-core superconducting wire aiming at the defects of the prior art. The method comprises the steps of preparing the raw materials into a metal salt solution, then obtaining spray decomposition raw material powder by adopting a spray thermal decomposition method, and then obtaining tube-filling precursor powder by phase-forming thermal treatment, so that the component uniformity and the particle size distribution of the spray decomposition raw material powder are obviously improved, the activity of the spray decomposition raw material powder is improved, the quality of the tube-filling precursor powder is improved, and the current-carrying performance and the stability of the Bi-2212 multi-core superconducting wire are further improved.
The spray pyrolysis raw material powder is prepared from the metal salt solution of the raw materials by adopting a spray thermal decomposition method, and because the uniformity of each raw material component in the metal salt solution is higher, the component uniformity and the particle size distribution of the spray pyrolysis raw material powder are obviously improved, the original activity is higher, the quality of the tubulation precursor powder is improved, and the current-carrying performance and the stability of the Bi-2212 multi-core superconducting wire are further improved.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a Bi-2212 multi-core superconducting wire is characterized by comprising the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into acid liquor according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal salt solution;
injecting the metal salt solution obtained in the step one into an atomizing chamber of an atomizer for atomization to obtain metal salt solution fog drops, wherein the metal salt solution fog drops enter a tubular furnace preheated to a constant temperature under the drive of carrier gas for heating decomposition, then enter a filter screen collector under the traction of an air blower, and are collected to obtain spray decomposition raw material powder;
step three, carrying out phase-forming heat treatment on the spray decomposition raw material powder obtained in the step two under a high-temperature condition to obtain tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a multi-core wire; the tube body adopted in the secondary compounding is a silver tube, and the tube body adopted in the tertiary compounding is a silver-manganese alloy tube;
and step five, placing the multi-core wire material obtained in the step four in a circulating atmosphere with the total pressure of 50-100 atm and the oxygen partial pressure of 1atm for heat treatment, and then cooling the multi-core wire material to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire material.
According to the invention, the raw materials are firstly prepared into the metal salt solution, and then the spray decomposition raw material powder is prepared by adopting a spray thermal decomposition method, because the uniformity of each raw material component in the metal salt solution is higher, the component uniformity and the particle size distribution of the spray decomposition raw material powder are obviously improved, the original activity is higher, the quality of the pipe-filling precursor powder is improved, the current-carrying performance and the stability of the Bi-2212 multi-core superconducting wire are further improved, meanwhile, the temperature, the time and the times of the phase-forming heat treatment are also shortened, the phase-forming heat treatment time is only 1/5-1/4 of a coprecipitation method, the power consumption of the phase-forming heat treatment is greatly reduced, and the preparation cost is reduced.
The preparation method of the Bi-2212 multi-core superconducting wire is characterized in that in the step one, the acid solution is a nitric acid solution, the metal salt solution is a metal nitrate solution, and the total concentration of metal cations in the nitrate solution is 0.1-1.5 mol/L. The preparation cost is reduced by adopting the nitric acid solution which is relatively low in price and good in dissolving effect; the optimized total concentration of the metal cations is beneficial to preparing the spray decomposition raw material powder with uniform components and particle size distribution by a spray thermal decomposition method, and the adhesion of the spray decomposition raw material powder is avoided.
The preparation method of the Bi-2212 multi-core superconducting wire is characterized in that the atomization power in the step two is 30W-100W, the flow rate of the carrier gas is 30L/min-150L/min, and the furnace temperature of the tubular furnace preheated to a constant temperature is 750 ℃ to 1000 ℃.
The preparation method of the Bi-2212 multi-core superconducting wire is characterized in that the temperature of the phase forming heat treatment in the third step is 800-860 ℃, the time is 10-20 h, and the times are 1-3.
Compared with the prior art, the invention has the following advantages:
1. the spray pyrolysis raw material powder is prepared from the metal salt solution of the raw materials by adopting a spray thermal decomposition method, and because the uniformity of each raw material component in the metal salt solution is higher, the component uniformity and the particle size distribution of the spray pyrolysis raw material powder are obviously improved, the original activity is higher, the quality of the tubulation precursor powder is improved, and the current-carrying performance and the stability of the Bi-2212 multi-core superconducting wire are further improved.
2. According to the invention, the spray pyrolysis raw material powder with uniform components and uniform particle size distribution is obtained by adopting a spray pyrolysis method, so that the temperature, time and times of phase forming heat treatment are shortened, the phase forming heat treatment is only 1/5-1/4 of a coprecipitation method, the power consumption of the phase forming heat treatment is greatly reduced, and the preparation cost is reduced.
3. The preparation process of the tubulation precursor powder is simple and reliable, is suitable for batch production, and meets the practical requirement.
4. The vacuum vibration tubulation method greatly reduces the content of gas in the precursor powder of the tubulation, avoids the bubbling phenomenon in the subsequent heat treatment, and simultaneously adopts the high-pressure heat treatment to better improve the density of the core wire and improve the connectivity among crystal grains, thereby greatly improving the current-carrying performance of the Bi-2212 multi-core superconducting wire.
5. The Bi-2212 multi-core superconducting wire prepared by the invention has the engineering critical current density of 1250A/mm under the conditions of 4.2K and self-field2The current-carrying performance of the Bi2212 multi-core wire rod is higher than that of a Bi2212 multi-core wire rod prepared by a coprecipitation process in the prior art.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into a nitric acid solution according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal nitrate solution; the total concentration of metal cations in the nitrate solution is 0.1 mol/L;
injecting the metal nitrate solution obtained in the step one into an atomization chamber of an atomizer for atomization under the condition of power of 30W to obtain metal nitrate solution fog drops, enabling the metal nitrate solution fog drops to enter a tubular furnace preheated to 750 ℃ under the drive of carrier gas with the flow rate of 30L/min for heating decomposition, then enabling the metal nitrate solution fog drops to enter a filter screen collector under the traction of an air blower, and collecting to obtain spray decomposition raw material powder;
step three, carrying out phase forming heat treatment on the spray decomposition raw material powder obtained in the step two for 3 times at the temperature of 800 ℃, wherein the time of the phase forming heat treatment for each time is 20 hours, so as to obtain tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube with the inner diameter of 20mm and the wall thickness of 1.5mm by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a 666 core wire; the tube body adopted by the secondary compounding is a silver tube with the inner diameter of 20mm and the wall thickness of 1.0mm, and the tube body adopted by the tertiary compounding is a silver-manganese alloy tube with the inner diameter of 23mm and the wall thickness of 1.5 mm;
and step five, placing the 666 core wire rods obtained in the step four in a circulating atmosphere with the total pressure of 50atm and the oxygen partial pressure of 1atm, performing high-pressure semi-melting treatment at the temperature of 888 ℃, and then cooling to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire rod with the diameter of 1.0 mm.
Through detection, the Bi-2212 multi-core superconducting wire prepared by the embodiment has the engineering critical current density of 1250A/mm under the conditions of 4.2K and self-field2。
Example 2
The embodiment comprises the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into a nitric acid solution according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal nitrate solution; the total concentration of metal cations in the metal nitrate solution is 1.5 mol/L;
injecting the metal nitrate solution obtained in the step one into an atomization chamber of an atomizer for atomization under the condition of power of 100W to obtain metal nitrate solution fog drops, enabling the metal nitrate solution fog drops to enter a tubular furnace preheated to 1000 ℃ under the drive of carrier gas with flow rate of 150L/min for heating decomposition, then enabling the metal nitrate solution fog drops to enter a filter screen collector under the traction of an air blower, and collecting to obtain spray decomposition raw material powder;
step three, carrying out phase forming heat treatment on the spray decomposition raw material powder obtained in the step two for 1 time at the temperature of 860 ℃, wherein the phase forming heat treatment time is 20 hours, and obtaining tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube with the inner diameter of 20mm and the wall thickness of 1.7mm by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a 666 core wire; the tube body adopted by the secondary compounding is a silver tube with the inner diameter of 20mm and the wall thickness of 1.5mm, and the tube body adopted by the tertiary compounding is a silver-manganese alloy tube with the inner diameter of 23mm and the wall thickness of 1.7 mm;
and step five, placing the 666 core wire rod obtained in the step four in a circulating atmosphere with the total pressure of 100atm and the oxygen partial pressure of 1atm, performing high-pressure semi-melting treatment at the temperature of 890 ℃, and then cooling to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire rod with the diameter of 1.0 mm.
Through detection, the Bi-2212 multi-core superconducting wire prepared by the embodiment has the engineering critical current density of 1330A/mm under the conditions of 4.2K and self-field2。
Example 3
The embodiment comprises the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into a nitric acid solution according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal nitrate solution; the total concentration of metal cations in the metal nitrate solution is 0.5 mol/L;
injecting the metal nitrate solution obtained in the step one into an atomization chamber of an atomizer, atomizing under the condition of power of 65W to obtain metal nitrate solution fog drops, feeding the metal nitrate solution fog drops into a tubular furnace preheated to 875 ℃ under the drive of carrier gas with flow rate of 90L/min for heating decomposition, feeding the metal nitrate solution fog drops into a filter screen collector under the traction of an air blower, and collecting to obtain spray decomposition raw material powder;
step three, carrying out phase forming heat treatment on the spray decomposition raw material powder obtained in the step two for 2 times at the temperature of 830 ℃, wherein the time of the phase forming heat treatment for each time is 15 hours, so as to obtain tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube with the inner diameter of 21mm and the wall thickness of 1.5mm by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a 666 core wire; the tube body adopted by the secondary compounding is a silver tube with the inner diameter of 21mm and the wall thickness of 1.5mm, and the tube body adopted by the tertiary compounding is a silver-manganese alloy tube with the inner diameter of 23mm and the wall thickness of 1.5 mm;
and step five, placing the multi-core wire material obtained in the step four in a circulating atmosphere with the total pressure of 75atm and the oxygen partial pressure of 1atm, performing high-pressure semi-melting treatment at the temperature of 892 ℃, and then cooling to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire material with the diameter of 1.0 mm.
Through detection, the Bi-2212 multi-core superconducting wire prepared by the embodiment has the engineering critical current density of 1550A/mm under the conditions of 4.2K and self-field2。
Example 4
The embodiment comprises the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into a nitric acid solution according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal nitrate solution; the total concentration of metal cations in the metal nitrate solution is 1.0 mol/L;
injecting the metal nitrate solution obtained in the step one into an atomization chamber of an atomizer, atomizing under the condition of power of 70W to obtain metal nitrate solution fog drops, feeding the metal nitrate solution fog drops into a tubular furnace preheated to 800 ℃ under the drive of carrier gas with the flow speed of 100L/min for heating decomposition, then feeding the metal nitrate solution fog drops into a filter screen collector under the traction of an air blower, and collecting to obtain spray decomposition raw material powder;
step three, carrying out phase forming heat treatment on the spray decomposition raw material powder obtained in the step two for 2 times at the temperature of 850 ℃, wherein the time of the phase forming heat treatment for each time is 10 hours, so as to obtain tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube with the inner diameter of 22mm and the wall thickness of 1.5mm by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a 666 core wire; the tube body adopted by the secondary compounding is a silver tube with the inner diameter of 22mm and the wall thickness of 1.5mm, and the tube body adopted by the tertiary compounding is a silver-manganese alloy tube with the inner diameter of 23mm and the wall thickness of 1.5 mm;
and step five, placing the 666 core wire rod obtained in the step four in a circulating atmosphere with the total pressure of 50atm and the oxygen partial pressure of 1atm, performing high-pressure semi-melting treatment at the temperature of 890 ℃, and then cooling to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire rod with the diameter of 1.0 mm.
Through detection, the Bi-2212 multi-core superconducting wire prepared by the embodiment has the engineering critical current density of 1630A/mm under the conditions of 4.2K and self-field2。
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (4)

1. A preparation method of a Bi-2212 multi-core superconducting wire is characterized by comprising the following steps:
step one, adding Bi2O3、CuO、CaCO3And SrCO3Adding the mixture into acid liquor according to the atomic ratio of Bi, Sr, Ca and Cu being 2:2:1:2, and uniformly mixing to obtain a metal salt solution;
injecting the metal salt solution obtained in the step one into an atomizing chamber of an atomizer for atomization to obtain metal salt solution fog drops, wherein the metal salt solution fog drops enter a tubular furnace preheated to a constant temperature under the drive of carrier gas for heating decomposition, then enter a filter screen collector under the traction of an air blower, and are collected to obtain spray decomposition raw material powder;
step three, carrying out phase-forming heat treatment on the spray decomposition raw material powder obtained in the step two under a high-temperature condition to obtain tube-filling precursor powder;
step four, filling the tube filling precursor powder obtained in the step three into a silver tube by adopting a vacuum vibration tube filling method to obtain a tube filling composite body, then carrying out rotary swaging and drawing on the tube filling composite body to obtain a single-core wire, sequentially carrying out secondary compounding and tertiary compounding on the single-core wire, and carrying out rotary swaging and drawing to obtain a multi-core wire; the tube body adopted in the secondary compounding is a silver tube, and the tube body adopted in the tertiary compounding is a silver-manganese alloy tube;
and step five, placing the multi-core wire material obtained in the step four in a circulating atmosphere with the total pressure of 50-100 atm and the oxygen partial pressure of 1atm for heat treatment, and then cooling the multi-core wire material to the room temperature along with a furnace to obtain the Bi-2212 multi-core superconducting wire material.
2. The method according to claim 1, wherein the acid solution in the first step is a nitric acid solution, the metal salt solution is a metal nitrate solution, and the total concentration of metal cations in the nitrate solution is 0.1mol/L to 1.5 mol/L.
3. The method according to claim 1, wherein the atomizing power in the second step is 30W-100W, the flow rate of the carrier gas is 30L/min-150L/min, and the furnace temperature of the tube furnace preheated to a constant temperature is 750 ℃ to 1000 ℃.
4. The method for preparing the Bi-2212 multi-core superconducting wire rod as claimed in claim 1, wherein the temperature of the phase forming heat treatment in the third step is 800-860 ℃, the time is 10-20 h, and the times are 1-3.
CN201911145654.2A 2019-11-21 2019-11-21 Preparation method of Bi-2212 multi-core superconducting wire Pending CN110853830A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113603138A (en) * 2021-09-08 2021-11-05 西北有色金属研究院 Method for preparing Bi2212 micro-nano powder by chemical combustion
CN113735166A (en) * 2021-09-08 2021-12-03 西北有色金属研究院 Preparation method of Bi-2212 superconducting film

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CN108597681A (en) * 2018-04-20 2018-09-28 西北有色金属研究院 A kind of preparation method of Bi-2212 multi-core superconductings wire rod
CN109727720A (en) * 2019-02-28 2019-05-07 西北有色金属研究院 A kind of preparation method of Bi2212 high-temperature superconductor powder

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CN101547862A (en) * 2007-07-18 2009-09-30 住友电气工业株式会社 Process for producing raw material powder for oxide superconductor
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Publication number Priority date Publication date Assignee Title
CN113603138A (en) * 2021-09-08 2021-11-05 西北有色金属研究院 Method for preparing Bi2212 micro-nano powder by chemical combustion
CN113735166A (en) * 2021-09-08 2021-12-03 西北有色金属研究院 Preparation method of Bi-2212 superconducting film
CN113735166B (en) * 2021-09-08 2022-04-26 西北有色金属研究院 Preparation method of Bi-2212 superconducting film
CN113603138B (en) * 2021-09-08 2022-08-02 西北有色金属研究院 Method for preparing Bi2212 micro-nano powder by chemical combustion

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Application publication date: 20200228