US3682719A - Process for producing nb-ti super conducting material - Google Patents

Process for producing nb-ti super conducting material Download PDF

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US3682719A
US3682719A US17374A US3682719DA US3682719A US 3682719 A US3682719 A US 3682719A US 17374 A US17374 A US 17374A US 3682719D A US3682719D A US 3682719DA US 3682719 A US3682719 A US 3682719A
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alloy
super conducting
temperature
treatment
ageing treatment
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US17374A
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Takuya Suzuki
Masaru Ikeda
Yoshio Furuto
Yukihiro Nagata
Takeshi Miura
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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
    • H10N60/01—Manufacture or treatment
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S505/00—Superconductor technology: apparatus, material, process
    • Y10S505/80—Material per se process of making same
    • Y10S505/815—Process of making per se
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S505/00—Superconductor technology: apparatus, material, process
    • Y10S505/825—Apparatus per se, device per se, or process of making or operating same
    • Y10S505/917—Mechanically manufacturing superconductor
    • Y10S505/918—Mechanically manufacturing superconductor with metallurgical heat treating
    • Y10S505/919—Reactive formation of superconducting intermetallic compound
    • Y10S505/921—Metal working prior to treating

Definitions

  • a process for producing a Nb-Ti super conducting material which comprises subjecting a super conducting Nb-Ti alloy having ,9 phase at room temperatures to a two-step ageing treatment comprising a first ageing treatment at a lower temperature for a longer period and a second ageing treatment at a higher temperature for a shorter period.
  • the present invention relates to a process for producing a super conducting Nb-Ti alloy, more particularly relates to an improvement for enhancing the super conducting characteristics, of such alloys as compared with those obtained by a conventional process.
  • the ageing treatment is conducted in two steps: the first step at a lower temperature for a longer period, and the second step at a higher temperature for a shorter period.
  • Nb-Ti alloys have been used as a most popular super conducting material, and it is well known that the super conducting characteristics of these alloys remarkably change depending upon heat treatments.
  • a Nb-Ti alloy was subjected to ageing treatments at various temperatures (T C.) for an optimum period (y, hr.) and the critical current density (Jc) was measured. The results are shown by the curve A in the drawing.
  • the conventional ageing treatment produces the curve A: T C. y hr. while the twostep ageing treatment according to the present invention produces the curve B: T C. x hr.+T C. y2hr.
  • the present invention is based on the above discovery that remarkably improved super conducting characteristics and mechanical properties of Nb-Ti alloys can be obtained as compared with those obtained by the conventional process by ageing the alloys at a relatively low temperature for a longer period as the first treatment and then ageing the alloys at a higher temperature for a shorter period as the second treatment as described above.
  • the present invention is a process for producing Nb-Ti super conducting materials which comprises subjecting a super conducting Nb-Ti alloy containing 30- 70% by weight of Nb to a solid solution treatment to transform the alloy from 0c phase to B phase, cooling the alloy to maintain the ,8 phase at normal temperatures, cold working the alloy, and then subjecting the alloy to a two-step ageing treatment which comprises heat treating the alloy at a temperature between ISO-400 C. for a period between 5-250 hours and heat treating the alloy at a temperature between 350-550 C. but higher than the temperature of the precedent heat treatment for a period between 03-10 hours.
  • the super conducting Nb-Ti alloys used in the present invention include an alloy contaimng 30-70% by weight of Nb, with the balance being Ti, and an alloy containing 30-70% by weight of Nb, with the balance being Ti and up to 4% by weight of one or more of Mo, V, Zr, Ta, Hf, C, 0 and N
  • the reason for limiting the Nb content to 30-70% by weight in the present invention is that a niobium content outside the above range does not give practically useful super conducting characteristics.
  • the present invention more remarkable improvement in the super conducting characteristics can be obtained as the niobium content increases or the a stabilizing element increases in an alloy containing 30- 70% weight of Ti.
  • the niobium content falls within the above range, even an alloy composition having so high a content of niobium as to render the alloy sluggish to the precipitates can produce better qualities through an appropriate selection of ageing treatment conditions than those obtained by the conventional process.
  • the present invention comprises steps of heat treating a Nb-Ti alloy at a temperature between 800-1000 C. to transform the alloy substantially into ,8 phase, then rapidly cooling the alloy in water, for example, cold working the alloy into a desirable form such as a sheet or wire, subjecting the alloy first to a first-step ageing treatment in which the alloy is treated at an appropriate temperature between ISO-400 C., depending on the alloy composition and the working history, for a long period, normally between 5-250 hours, and then subjecting the alloy to a second-step ageing treatment in which the alloy is treated at a temperature between 350- 550 C. but higher than the temperature of the first-step ageing treatment for a short period normally between 03-10 hours, preferably 0.5-6 hours.
  • the reason for limiting the temperature in the first-step ageing treatment to 150-400", C. is that no remarkable ageing effect can be expected with a treatment below 150 C. even with a longer treatment time; thus no practical usefulness is obtained, while no remarkable improvement in the super conducting characteristics can be obtained with a treatment above 400 C. as compared with those obtained by the conventional process.
  • the reason for limiting the temperature in the second-step ageing treatment to 350550 C. is that no remarkable improvement in the super conducting characteristics can be obtained with a treatment below 350 C. as compared with those obtained by the conventional process, while the precipitation of particles of on phase or to phase becomes ditficult with a treatment above 550 C.
  • EXAMPLE 1 A Nb-65T i alloy was heated at 950 C. for one hour, rapidly cooled, wire drawn with 99.9% reduction of area, heated at 300 C. for 127 hours in vacuum and then heated at 375 C. for one hour.
  • the critical current density at 42 K. of the alloy was 2.5 10 a./cm. when it was placed in an external magnetic field of 30 kilogauss so that the current passed in a perpendicular direction to the line of magnetic force, and the tensile strength at room temperature was 175 kg./mm.
  • an alloy having the same composition and working history showed a Jc value of 1.8 10 a./cm. at best under the optimum treating conditions (heating at 400 C. for one hour) according to the conventional process, and showed a tensile strength of 160 kg./mm.
  • EXAMPLE 2 A Nb-35Ti alloy was heated at 950 C. for one hour, cooled rapidly, then clad with copper and cold worked into copper clad wire having a Nb-Ti core of 0.25 m. diameter and an out diameter of 0.33 m. with 99.9% reduction of area. The wire was heated at 250 C. for 250 hours in vacuum, and heated at 400 C. for one hour. The 10 value of the material measured under the same conditions as in Example 1 was 2.15 l a./cm. and the tensile strength was 120 kg./mm.
  • a material having the same composition and working history showed a value of 1.65X l0 a./crn. when treated under optimum conditions (heating at 425 C. for one hour) according to the conventional process, and showed a tensile strength of 110 kg./mm.
  • EXAMPLE 3 A Nb-50Ti alloy with addition of 1% by weight of Ta, 0.28% by weight of oxygen, 0.12% by weight of nitrogen was heated at 1000 C. for one hour, cooled rapidly and cold worked into wire with 99.5% reduction of area. The wire was heated at 250 C. for 120 hours in vacuum and then heated at 400 C. for one hour. The J e value of the above wire as measured under the same conditions as in Example 1 was 2.3 X 10 a./cm.
  • an alloy having the same composition and working history showed a la value of 1.75 X 10 a./cm. when treated under optimum conditions (heating at 425 C. for one hour) according to a conventional process.
  • EXAMPLE 4 A Nb-Ti-Zr-Ta alloy containing 30% by weight of titanium, 1.5% by weight of zirconium, 2.5% by weight of tantalum, with the balance being niobium and less than 350 p.p.m. of oxygen was heat treated at 950 C. for one hour, cooled rapidly, and cold worked into wire with 99.8% reduction of area. The alloy wire heat treated at 375 for 200 hours in vacuum and then heat treated at 480 C. for 1.5 hours. The Jc value of this material as measured under same conditions as in Example 1 was 1.2x 10 a./cm. at 75 kilogauss.
  • EXAMPLE 5 A Nb-Ti-O-C alloy containing 30% by weight of titanium, 0.2% by weight of carbon, 1.1% by weight of oxygen, with the balance being niobium was heat treated at 950 C. for one hour, quenched in water, cold worked into wire with 99.5% reduction of area. The wire was then heat treated at 300 C. for hours and further heat treated at 430 C. for 5 hours.
  • the Jc value of this material as measured under same conditions as in Example 1 was 1.5 10 a./cm. at 75 kilogauss. This Jc value is the highest one ever obtained in a high magnetic field with super conducting alloys known up to now.
  • the super conducting characteristics and the mechanical properties of super conducting Nb-Ti alloys can be remarkably improved by an appropriate heat treatment according to the present invention.
  • Another remarkable advantage of the present invention is that a certain desirable Jc value can be obtained with a less working ratio. For example, a working ratio more than 99.95% is required in order to obtain a Jc value of 2.2)(10 a./cm. in a conventional ageing treatment, while according to the present invention only 99.5 working ratio is enough for the same purpose.
  • the present invention is also advantageous for stabilized properties as magnet colings.
  • a process for producing super conducting Nb-Ti material comprising subjecting a super conducting Nb-Ti alloy containing 3070% by weight of Nb to a solid solution treatment to transform the alloy from a phase to 5 phase, cooling the alloy so that the alloy is maintained in substantial ⁇ 3 phase at normal temperatures, cold working the alloy, then heat treating the alloy between ISO-400 C. for 5-250 hours, and further heat treating the alloy at a temperature between 350550 C. but higher than the temperature of the preceding heat treatment for 0.3-10 hours.
  • a process for producing a Nb-Ti super conducting material which comprises the steps of heat treating a Nb-Ti alloy at a temperature between 800-1000 C. to transform the alloy into substantially [3 phase, then rapidly cooling the alloy (cold working the alloy into a desirable form such as a sheet or wire, subjecting the alloy first to a first-step ageing treatment in which the alloy is treated at an appropriate temperature between ISO-400 C., depending on the alloy composition and the working history,
  • the alloy for a long period, and then subjecting the alloy to a second-step ageing treatment in which the alloy is treated at a temperature between 350-550 C. but higher than the temperature of the first-step ageing treatment for a short period.
  • Nb-Ti super conducting material in which the super conducting Nb-Ti alloy contains 3070% by weight of Nb with the balance being Ti and up to 4% by weight of one or more of Mo, V, Zr, Ta, Hf, C, and N 7.
  • a process for producing super conducting Nb-Ti material comprising subjecting a super conducting Nb-Ti alloy containing 70% by weight of Nb to a solid solution treatment to transform the alloy from 0: phase to 6 phase, cooling the alloy so that the alloy is maintained in substantial 5 phase at normal temperatures, cold working the alloy, then heat treating the alloy between 400 C. for at least 5 hours, and further heat treating the alloy at a temperature of between 350550 C. but higher than the temperature of the preceding heat treatment for 03-10 hours.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Conductive Materials (AREA)
  • Superconductor Devices And Manufacturing Methods Thereof (AREA)
US17374A 1969-03-11 1970-03-09 Process for producing nb-ti super conducting material Expired - Lifetime US3682719A (en)

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JP44018483A JPS4814397B1 (enExample) 1969-03-11 1969-03-11

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JP (1) JPS4814397B1 (enExample)
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GB (1) GB1283293A (enExample)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011575A (zh) * 2016-07-26 2016-10-12 西北有色金属研究院 一种Nb-Ti-Ta-C合金棒材及其制备方法
RU2627304C1 (ru) * 2016-10-19 2017-08-07 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Интерметаллидный сплав на основе титана и изделие из него
EP3502288B1 (fr) 2017-12-21 2020-10-14 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie
CN112322937A (zh) * 2020-11-19 2021-02-05 郑州大学 一种具有超导性能的（Ti，Zr）-Nb-O合金及其制备方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3502289B1 (fr) * 2017-12-21 2022-11-09 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie
CN108677060B (zh) * 2018-04-25 2020-12-11 东南大学 一种高强度高弹性耐热钛合金及制备方法
CN109554650A (zh) * 2018-12-14 2019-04-02 中国兵器科学研究院宁波分院 一种高强β钛合金的热处理工艺

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011575A (zh) * 2016-07-26 2016-10-12 西北有色金属研究院 一种Nb-Ti-Ta-C合金棒材及其制备方法
RU2627304C1 (ru) * 2016-10-19 2017-08-07 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Интерметаллидный сплав на основе титана и изделие из него
EP3502288B1 (fr) 2017-12-21 2020-10-14 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie
CN112322937A (zh) * 2020-11-19 2021-02-05 郑州大学 一种具有超导性能的（Ti，Zr）-Nb-O合金及其制备方法
CN112322937B (zh) * 2020-11-19 2022-03-04 郑州大学 一种具有超导性能的（Ti，Zr）-Nb-O合金及其制备方法

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DE2011581B2 (de) 1972-01-20
JPS4814397B1 (enExample) 1973-05-07
DE2011581A1 (enExample) 1970-09-24
GB1283293A (en) 1972-07-26

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