WO2007071163A1 - Bande ou cable supraconducteur a base de mgb2 et de carbone et son procede de fabrication - Google Patents

Bande ou cable supraconducteur a base de mgb2 et de carbone et son procede de fabrication Download PDF

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Publication number
WO2007071163A1
WO2007071163A1 PCT/CN2006/003418 CN2006003418W WO2007071163A1 WO 2007071163 A1 WO2007071163 A1 WO 2007071163A1 CN 2006003418 W CN2006003418 W CN 2006003418W WO 2007071163 A1 WO2007071163 A1 WO 2007071163A1
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Prior art keywords
strip
mgb
powder
wire
nano
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PCT/CN2006/003418
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English (en)
Chinese (zh)
Inventor
Yanwei Ma
Xianping Zhang
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Institute Of Electrical Engineering, Chinese Academy Of Science
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Publication of WO2007071163A1 publication Critical patent/WO2007071163A1/fr

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/80—Constructional details
    • H10N60/85—Superconducting active materials
    • H10N60/855—Ceramic superconductors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/20—Permanent superconducting devices
    • H10N60/202—Permanent superconducting devices comprising metal borides, e.g. MgB2

Definitions

  • the new superconducting material of magnesium diboride (MgB 2 ) discovered in 2001 has attracted wide attention of researchers due to its high transformation temperature, low raw material cost, and processing technology of the single tube. It is well known that the critical current density J. It is to determine whether a superconducting material, a key characteristic of large-scale applications, however, the current magnetic field M g B 2 prepared material critical current density Jc is relatively low as compared with the low-temperature superconductors. Moreover, large-scale practical applications require MgB 2 materials to work in high magnetic field (> 4 T ), liquid helium or chiller cooling system environments (20-30 K), thus improving the flux pinning capability of MgB 2 superconducting materials. And superconducting performance under high field is a problem that must be solved in the practical application of MgB 2 superconducting materials.
  • the invention provides a high performance MgB 2 superconducting wire or strip and a preparation method thereof.
  • a wire or strip of a C-containing MgB 2 superconducting material wherein the superconducting material consists essentially of Mg, B and C, the chemical formula of which is MgB x C Y , wherein X The value is between 1 and 2, the value of Y is between 0 and 1, and the sum of X and Y is greater than 1.5. The value of the value is between 0.5 and 0.
  • a method of preparing a C-containing MgB 2 superconducting wire or tape comprising: a molar ratio of Mg powder, B powder, and nano C powder 1 : (1 - 2) : (Q - 1) Prepare and mix evenly; Put the mixture into iron pipe, iron-copper composite pipe, or other metal pipe and seal it (can be applied to metal pipes of different diameters); Machining the MgB 2 wire or strip containing C; under normal pressure argon atmosphere or under vacuum, the MgB 2 wire or strip is kept at 600-1200 ° C for 0.2- 3 hours, the preferred heat treatment temperature is 600 ° C - 900 ° C, the preferred heat treatment time is 0. 2 ⁇ 1 hour, and finally get the MgB 2 superconducting wire or strip containing C.
  • Figure 1 shows the different ratios of nano-C doping measured by a superconducting quantum interferometer. Transition temperature profile of the M g B 2 strip.
  • the molar percentage of nano-C is 0%, 2.5%, 5%, 10%, and 15%, respectively.
  • Figure 2 is an XRD pattern of different proportions of nano-C doped MgB 2 tapes obtained by X-ray diffractometry.
  • the molar percentage of nano-C is G%, 2.5%, 5%, 10%, and 15%, respectively.
  • Figure 3 is a graph showing the lattice constants "a" and 'V" of MgB 2 in various ratios of nano-C doped MgB 2 strips calculated by X-ray diffraction data.
  • the mole percentage of nano C is 0%, 2.5%, 5%, 10%, and 15%, respectively.
  • Figure 4 is a graph of critical current density and applied magnetic field for different ratios of nano-C doped MgB 2 strips tested using the standard four-lead method (1 ⁇ /cm).
  • the molar percentage of nano-C is 0%, 2.5%, 5%, 10%, 15%, 20%.
  • Figure 5 is a TEM image of a sample treated with different sintering temperatures, (a) 650 °C; (b) 750 °C; (c) nanoparticles embedded in the grains; (d) analyzed by energy dispersive spectroscopy The obtained energy diffraction spectrum was detected.
  • Figure 6 is a graph showing the relationship between the critical current density and the magnetic field of a strip sample and an undoped sample with a nano C doping amount of 5% by mole prepared by different heat treatment processes.
  • Figure 7 shows the high-field critical current performance data obtained by the standard four-lead method for a strip sample doped with 5% nanometer C.
  • the composition and preparation process of the superconducting material provided by the invention improves the density of the MgB 2 wire or strip superconducting core and improves the grain connectivity; refining the MgB 2 grains by doping the nano C, in the M
  • the introduction of defects in the g B 2 lattice enhances the flux pinning ability and the critical current density of the magnetic field of the MgB 2 material.
  • the examples described below can show the superconductivity provided by the present invention.
  • the material composition and preparation process can obtain MgB 2 superconducting wire or strip with high magnetic flux pinning ability and good critical current performance under high field.
  • Mg powder purity 99%
  • amorphous B powder purity 99.99%
  • Figure 1 is a graph of critical transition temperature and transition width for undoped samples and different ratios of nano-C doped samples.
  • the initial transition temperature of the undoped sample was 36.5 K, which is similar to the values in most literatures.
  • the critical transition temperature of the C-doped sample is reduced by about 3. 5K, even in the sample with a C-doping amount of 15%. This indicates that the effect of nano-C doping on the critical transition temperature of the 1 ⁇ 8 2 material is relatively small.
  • Figure 2 is an X-ray diffraction pattern of doped and undoped samples. It can be seen from the diffraction pattern that the Mg 2 C 3 formed by the reaction of nano-C and Mg increases with the increase of C doping amount, and the full width at half maximum of the diffraction peak also increases with the increase of the doping amount, indicating that the sample The content of impurities increases as the amount of doping increases.
  • the (110) diffraction peak near 60 ° also gradually shifted to the right with increasing doping amount, which indicates that the substitution of C to B in the sample increases with the increase of doping amount.
  • the change of the lattice constants a and c in 3 is more clear, such as the lattice constant ', does not change with the C doping amount, and the lattice constant "a" decreases with the increase of the nano C doping amount. .
  • Figure 4 is a graph of critical current density versus applied magnetic field for nano-C doped and undoped samples. It can be seen that the critical current density of the strip after nano-C doping is obvious. The improvement, and the dependence on the magnetic field is greatly reduced. This shows that the sample goes through the nano
  • the magnetic flux pinning ability is remarkably enhanced. More significantly, the high doping amount of the sample has a lower current density in the low field, and is higher in the high field than in the low doping sample, which means that the nano C doping is for M g B 2 .
  • the magnetic field properties of the wire or strip have a further increased space. Without wishing to be bound by any theory, it is presumed that the increase in flux pinning ability is related to lattice distortion caused by nano-C doping and the substitution of C to B. It can be seen from Figure 5 (a, b, c) that MgB 2 Lattice defects present in the crystal, Figure 5 (d) shows that these defects are related to the presence of C.
  • Fig. 6 is a graph showing the current-magnetic relationship between a sample having a nano C doping amount of 5% total moles and an undoped sample prepared at different heat treatment temperatures. It can be seen that different heat treatment temperatures have an effect on the critical current density of the sample and the dependence of the current on the magnetic field. This shows that the performance of the 3 ⁇ 4 ⁇ 8 2 wire or strip can be further improved by optimizing the preparation process when preparing the sample.
  • Figure 7 is a graph of critical current density versus magnetic field for nano 5 % C doped and undoped samples. It can be seen from the figure that the high field critical current performance of the strip after doping with nano-C is J. It is significantly improved compared to the undoped sample, which is J. Increase by more than an order of magnitude in the high field, at 4 ⁇ 2 ⁇ , 10 ⁇ , J. It reached 2.11 X 10 4 A/cm 2 ; and the irreversible field of the C-doped strip was also increased from 16 T (pure sample) to 23 T.
  • nano-C doping has a good effect on improving the current performance under high field of 1 ⁇ 8 2 wire or strip, and is not expected to be bound by any theory.
  • the reason for the improvement is presumed to be:
  • the nano-C doping has the effect of refining crystal grains.
  • the presence of a large number of grain boundaries in the crystal plays an important role in improving the magnetic flux pinning ability of the material.
  • the lattice distortion caused by nano-C doping, the introduction of nano-scale impurity particles, and the substitution of C for yttrium can achieve the effect of improving the magnetic flux-clamping ability.
  • nano-C doping does not bring a lot of impurities in the superconducting material like other dopants.
  • Good grain connectivity requirements are very beneficial because the presence of large amounts of impurities will reduce the proportion of superconducting portions in the superconducting material and reduce the passage of superconducting current.
  • Mg powder, B powder and nano-C powder can be used to obtain a high critical current density, irreversible field and the like, which are significantly improved by the above molar ratio, preparation process and heat treatment process.
  • M g B 2 superconducting wire or strip containing nano C powder As for the selection of specific process parameters for implementing the present invention, those skilled in the art can determine the performance according to the content of the present disclosure based on the content of the present disclosure, and are not limited to the specific embodiments and examples of the present invention. For example, in the present invention, in addition to the use of iron pipes, other metal pipes or composite casing bushings may be used, and the specific dimensions of the pipes may be determined as needed.
  • Preparation (MgB 2 ). 975 C. D25 superconducting tape. Mg powder, B powder, and nano-C powder were accurately weighed and mixed according to a molar ratio of 0. 975: 1. 95: 0. 025, and placed in a steel tube having a diameter of 8 mm and sealed at a deformation rate of 10%. 5 ⁇ Forging, drawing, rolling and other mechanical processing, to obtain a strip of 3. 2 ⁇ meters, thick 0. 5 ⁇ meters. The strip in an argon gas atmosphere flowing in a vacuum oven 650 ° C for 1 hour, then cooled to room temperature in a vacuum oven to afford containing C M g B 2 superconducting tape. The measurement of the critical current density of the strip obtained by the standard four-lead method is 4. 5 10 4 A/cra 2 at a condition of 4. 2 K, 14 T. 6 10 3 A/cm 2 .
  • MgB 2 Preparation (MgB 2 ). , 85 C. , 15 super wire.
  • the Mg powder, the B powder, and the nano-C powder are accurately weighed and uniformly mixed according to a molar ratio of 0. 8: 1. 6: 0.2, and are placed in an iron pipe having a diameter of 8 mm to be sealed at a deformation rate of 5%. 8 ⁇
  • the wire was kept at 900 ° C in a flowing atmosphere in an argon vacuum oven at 0.5 ° C for 0.5 hour, and then cooled to room temperature in a vacuum oven to obtain a C-containing MgB 2 superconducting wire.
  • Example 3 Example 3
  • MgB 2 Preparation (MgB 2 ). 95 C. ,. 5 superconducting tape. Mg powder, B powder, and nano-C powder were accurately weighed and mixed according to a molar ratio of 0.95: 1.9: 0.05. The steel tube was sealed in a steel tube with a diameter of 8 mm, and then swaged and drawn at a deformation rate of 15%. Machining by rolling, etc., to obtain a strip having a width of 4 mm and a thickness of 0.5 mm. The strip was held at 800 ° C for 0.5 hour in a flowing atmosphere argon vacuum furnace, and then cooled to room temperature in a vacuum oven to obtain a C-containing MgB 2 superconducting tape.
  • MgB 2 Preparation (MgB 2 ). 95 C. ,. 5 superconducting tape. Mg powder, B powder, and nano-C powder were accurately weighed and uniformly mixed according to a molar ratio of 0.95: 1.9: 0.05, and filled into a steel pipe having a diameter of 8 mils, and then subjected to rotary forging (or hole) at a deformation rate of 20%. Type rolling, drawing, etc., to obtain a wire with a diameter of 1.0 mm. The strip was kept at 600 ° C for 1 hour in a flowing atmosphere argon vacuum furnace, and then cooled to room temperature in a vacuum furnace to obtain a C-containing MgB 2 superconducting wire.
  • MgB 2 Preparation (MgB 2 ). 85 C. , 15 superconducting tape. Mg powder, B powder, and nano-C powder were accurately weighed and mixed uniformly according to a molar ratio of 0.8:1.6:0.2. After being sealed in an iron tube with a diameter of 8 mm, the mixture was swaged and drawn at a deformation rate of 10%. Machining by rolling, etc., a strip having a width of 5 mm and a thickness of 0.5 mm is obtained. The strip was held at 700 ° C for 1.5 hours in a flowing atmosphere argon vacuum furnace, and then cooled to room temperature in a vacuum oven to obtain a C-containing MgB 2 superconducting tape.
  • MgB 2 975 C Q . 25 superconducting tape.
  • Mg powder, B powder, and nano-C powder were accurately weighed and mixed according to a molar ratio of 0. 975: 1. 95: 0. 025, and filled into a steel pipe having a diameter of 8 mils and sealed at a deformation rate of 15%. 5 ⁇
  • the machine is subjected to rotary forging, drawing, rolling, etc., to obtain a strip having a width of 3 mm and a thickness of 0.5 mm.
  • the strip was incubated in a flowing atmosphere argon vacuum oven at 600 ° C for 1.5 hours, and then cooled to room temperature in a vacuum oven to obtain a C g- containing Mg 2 superconducting tape.
  • the process for preparing a MgB 2 superconducting wire or strip using the present invention is generally as follows:
  • the prepared wire or strip is heat treated at a temperature ranging from 600 ° C to 1000 ° C for 10 minutes to 3 hours.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne une bande ou un câble supraconducteur à base de MgB2 et de carbone et son procédé de fabrication. Ce matériau supraconducteur est essentiellement composé de Mg, de B et de C. Sa formule chimique est la suivante : MgB2-xCx. Dans cette formule, x désigne une valeur comprise entre 1 et 2 et y désigne une valeur comprise entre 0 et 1, la somme de x et de y étant supérieure à 1,5. La bande ou le câble supraconducteur à base de MgB2 de la présente application se caractérise par les propriétés suivantes : un champ irréversible élevé, une excellente densité de courant critique, et une bonne reproductibilité.
PCT/CN2006/003418 2005-12-23 2006-12-14 Bande ou cable supraconducteur a base de mgb2 et de carbone et son procede de fabrication WO2007071163A1 (fr)

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CN200510130713.0 2005-12-23
CNA2005101307130A CN1986407A (zh) 2005-12-23 2005-12-23 含碳的MgB2超导材料及其制备方法

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CN113571995A (zh) * 2021-07-09 2021-10-29 北京大学 一种MgB2超导接头的制备方法

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CN101168441B (zh) * 2007-09-25 2010-06-23 中国科学院电工研究所 一种MgB2超导材料的制备方法
CN101168442B (zh) * 2007-09-25 2010-08-11 中国科学院电工研究所 一种高性能MgB2超导材料及其制备方法
CN101271747B (zh) * 2008-05-07 2013-05-01 中国科学院电工研究所 一种铁基化合物超导线材、带材及其制备方法
CN101386529B (zh) * 2008-10-24 2014-03-19 中国科学院电工研究所 一种铁基化合物超导体的制备方法
CN106205861B (zh) * 2016-06-29 2017-05-10 西北有色金属研究院 一种石墨烯负载多元掺杂二硼化镁超导块材的制备方法
CN105931750B (zh) * 2016-06-29 2017-05-24 西北有色金属研究院 石墨烯包覆硼粉制备二硼化镁超导线材的方法
CN106206925A (zh) * 2016-08-30 2016-12-07 河南省豫星华晶微钻有限公司 一种超导线材芯材、由该芯材制成多芯复合超导线及其制备方法
JP6723179B2 (ja) * 2017-03-03 2020-07-15 株式会社日立製作所 超伝導体の製造方法

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US20050245400A1 (en) * 2002-06-18 2005-11-03 Dou Shi X Superconducting material and method of synthesis
CN1411004A (zh) * 2002-12-03 2003-04-16 西北有色金属研究院 一种硼化镁超导线材及其制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113571995A (zh) * 2021-07-09 2021-10-29 北京大学 一种MgB2超导接头的制备方法
CN113571995B (zh) * 2021-07-09 2022-03-25 北京大学 一种MgB2超导接头的制备方法

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