US3378916A - Manufacture of superconducting wire - Google Patents

Manufacture of superconducting wire Download PDF

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Publication number
US3378916A
US3378916A US500218A US50021865A US3378916A US 3378916 A US3378916 A US 3378916A US 500218 A US500218 A US 500218A US 50021865 A US50021865 A US 50021865A US 3378916 A US3378916 A US 3378916A
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sheath
niobium
zirconium
solution
temperature
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US500218A
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Robinson Peter
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Rolls Royce Power Engineering PLC
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International Research and Development Co Ltd
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Assigned to JOHN THOMPSON (PIPEWORK AND ORDNANCE DIVISION) LIMITED reassignment JOHN THOMPSON (PIPEWORK AND ORDNANCE DIVISION) LIMITED CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). 14, EFFECTIVE 1-15-74; 4-8-80 AND 12-8-80 Assignors: INTERNATIONAL RESEARCH & DEVELOPMENT COMPANY LIMITED
Assigned to NORTHERN ENGINEERING INDUSTRIES LIMITED, A BRITISH COMPANY reassignment NORTHERN ENGINEERING INDUSTRIES LIMITED, A BRITISH COMPANY ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: JOHN THOMPSON (PIPEWORK & ORDNANCE DIVISION) LIMITED
Assigned to NORTHERN ENGINEERING INDUSTRIES PLC. reassignment NORTHERN ENGINEERING INDUSTRIES PLC. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). EFFECTIVE FEB. 18, 1982 Assignors: NORTHERN ENGINEERING INDUSTRIES LIMITED
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00—Electrolytic stripping of metallic layers or coatings
    • 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
    • H10N60/0156—Manufacture or treatment of devices comprising Nb or an alloy of Nb with one or more of the elements of group 4, e.g. Ti, Zr, Hf
    • 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
    • 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
    • Y10S505/928—Metal deforming
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49014—Superconductor
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49801—Shaping fiber or fibered material
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/4981—Utilizing transitory attached element or associated separate material
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49826—Assembling or joining
    • Y10T29/49888—Subsequently coating

Definitions

  • a material having a refined crystal structure that is to say, a material in which dendritic crystal structure and high concentrations of impurities are substantially absent.
  • the as-cast structure should be broken down by mechanical working, prelfierably ho-t working.
  • the amount of working necessary to produce a refined crystal structure may be considerably less.
  • the -T he material of the sheath may be Inconel alloy.
  • the copper-plating step preferably includes hydriding the material and depositing a film of nickel before the copper is deposited.

Description

United States Patent Olfice 3,378,916 MANUFACTURE OF SUPERCONDUCTING WIRE Peter Robinson, Fossway, Newcastle-upon-Tyne, England, assignor to International Research & Development Company Limited, Fossway, Newcastle-upon-Tyne, England No Drawing. Filed Oct. 21, 1965, Ser. No. 500,218 Claims priority, application Great Britain, Oct. 30, 1964, 44,416/64 2 Claims. (Cl. 29-599) The present invention relates to processes for the production of superconducting niobium-zirconium alloy wire.
Niobium-zirconium alloys, in the form in which they are normally obtained, are relatively brittle and dilficult to fabricate into wire. This is particularly true of alloys with high oxygen, carbon, hydrogen and nitrogen contents.
The present invention provides a process in which the material is subjected to a series of treatments to overcome these difiiculties and to produce niobium-zirconium alloy wire of improved superconducting properties.
It is necessary to start with a material having a refined crystal structure, that is to say, a material in which dendritic crystal structure and high concentrations of impurities are substantially absent. When the material has been formed by casting, the as-cast structure should be broken down by mechanical working, prelfierably ho-t working. When the material has been formed by powder metallurgy techniques, the amount of working necessary to produce a refined crystal structure may be considerably less.
The process in accordance with the invention for the production of superconducting niobium-zirconium alloy wire comprises the following steps:
('1) Heat-treating a niobium-zirconium material having a refined crystal structure as herein defined, in a temperature range l000-l250 C. under inert conditions for 3 -120 minutes.
(2) Quenching the material as quickly as possible to retain the second phase constituents in solution.
(3) Working the material at a temperature below 500 C. to reduce its cross-section and removing any surface defects which may be present.
(4) Further heat-treating the material at a temperature in the range 750 C.825 C. under inert conditions for 15430 minutes.
(5) Enclosing the material in a sheath of different material having substantially similar working properties to the material regarding ductility, rate of work-hardening and hardness.
(6) Deforming the material and sheath together to the required final cross-section of the material.
(7) Dissolving the sheath.
(8) Copper-plating the material.
-T he material of the sheath may be Inconel alloy. The copper-plating step preferably includes hydriding the material and depositing a film of nickel before the copper is deposited.
The process will now be described in more detail with the aid of an example. A cast ingot of niobium-zirconium was used having the analysis by weight: Zirconium V 27.8%, balance niobium, oxygen 74 parts per million, ni-
trogen 50 parts per million, carbon 125 parts per million and hydrogen 2 par-ts per million. The ingot was hotextruded to a diameter of to break down the as-cast structure and then heat-treated at 1200 C. for one hour in an atmosphere of static inert gas, for example, argon, or in vacuum. The heat treatment was carried out in a metal canister, for example, of mild steel protected against oxidation by a refractory frit and the whole subsequently quenched in water at room temperature (about C).
3,378,916 Patented Apr. 23, 1968 The heat-treated ingot was then cold swaged at room temperature to 0.110 inch diameter rod and dressed, for example, "by grinding and filing, to remove any surface defects. It was then given further heat treatment at 800 C. for fifteen minutes in a static argon atmosphere. This treatment was carried out in an argon-filled copper tube which was a loose fit on the rod. The ends of the tube were sealed by high-temperature brazing. The canned rod was passed continuously through a furnace to give the desired heat treatment.
After removal from the copper can the rod was placed in a cold drawn Inconel tube 0.160 outer diameter and 0.130 inner diameter. One end of the tube was swaged on to the rod and the tube then drawn tightly on to the rod. The composite member was then cold drawn until the diameter of the wire forming the core of the composite member was 0.010 inch.
The In conel sheath was then dissolved off the rod by an electrolytic process by a batch technique using a solution of 5% sulphuric acid at 2.3 volts potential difference.
Finally, the wire was plated using a continuous process apparatus such as is described in our oopending application No. 27,614/64. The wire was first degreased then etched in 10% hydrofluoric acid solution at 38 C. and then hydrided electrolytically in 2% hydrofluoric acid (cold) at a current density of 40 amps. per square foot.
A nickel flash plating 0.0001 inch thick was then given to the wire at a current density of 40 amps. per square foot and finally copper was deposited from an acid sulphate bath at a current density of amps. per square foot to give a final overall plating thickness on the wire of 0.001 inch.
In the casting of the niobium-zirconium alloy the second phase constituents, that is to say, oxygen, carbon, hydrogen and nitrogen, are preferentially precipitated at the grain boundaries, resulting in enrbrittlement of the material. After extrusion of the ingot to break down the as cast structure, the first heat treatment produces solution of the second phase constituents and the quenching retains most of the second phase constituents in solution. Any second phase constituents which are precipitated during the quenching are dispersed throughout the material and are thus less harmful. The resulting reduction in embrittlement means that alloys with high oxygen, carbon, hydrogen and nitrogen contents can be fabricated. The case of fabrication can be estimated by measuring the hardness of the material before and after the initial heat treatment. It is found that the all-0y can be more easily fabricated if its hardness before the heat treatment is below 26-5 VPN (Vickers Pyramid Number) and is not increased by the treatment.
The initial heat treatment followed by cold working and subsequent thermal precipitation treatment (Step 4) has a beneficial effect on the superconducting properties of the material.
The process can be used to advantage from the points of view of fabrication and improvement of superconducting properties with most niobium-zirconium alloys.
In the example described above the working of the material after the first heat treatment took place at room temperature, but this working can be carried out at temperatures up to about 500 C.
Materials other than Inconel can be used for the enclosing sheath providing they have properties similar to those of the niobium-zirconium alloy regarding ductibility, rate of work-hardening and hardness. The purpose of the sheath is to reduce the effect of ga-lling between the wire and the die through which the wire is drawn.
I claim:
1. A method or process for the production of super- 3 conducting niobium-zirconium alloy wire comprising the following steps:
(a) heat-treating a niobium-zirconium material containing a second phase constituent and having a substantially non-dendritic refined crystal structure sub- 'stantially free of high concentrations of impurities, in a temperature range 10001250 C. under inert conditions for 30-120 minutes, whereby said second phase is placed in solution with said material;
(b) quenching the material as quickly as possible to retain the second-phase constituents in solution;
(c) Working the material at a temperature below 500 C. to reduce its cross section and removing any sur- =fa'ce defects which may be present;
(-d) further heat-treating the material at a temperature in the range 750 C.8"25 C. under inert conditions for 15-130 minutes;
(e) enclosing the material in a sheath of different material having substantially similar working properties to the material regarding ductility, rate of workharden-ing and hardness;
(f) deforming the material and sheath together to the required final cross-section of the material; (g) dissolving the sheath; '(h) copper-plating the material. 2. A process as claimed in claim 1 in which the copperplating step includes hydriding the material and depositing a film of nickel before the copper is deposited.
References Cited UNITED STATES PATENTS 3,109,963 1 1/1963 Geballe 29599 3,131,469 5/ 1964 Glaze. 3,204,326 9/1965 Granitas. 3,218,693 111/1965 Allen et al. 29-599 3,239,919 '3/ 19661 Levi. 3,277,564 IO/1966 Webber et a1. 29419 JOHN F. CAMPBELL, Primary Examiner.
20 PAUL M. COHEN, Assistant Examiner.

Claims (1)

1. A METHOD OR PROCESS FOR THE PRODUCTION OF SUPERCONDUCTING NIOBIUM-ZIRCONIUM ALLOY WIRE COMPRISING THE FOLLOWING STEPS: (A) HEAT-TREATING A NIOBIUM-ZIRCONIUM MATERIAL CONTAINING A SECOND PAHSE CONSTITUENT AND HAVING A SUBSTANTIALLY NON-DENDRITIC REFINED CRYSTAL STRUCTURE SUBSTANTIALLY FREE OF HIGH CONCETRATIONS OF IMPURITIES, IN A TEMPERATURE RANGE 1000*-1250*C. UNDER INERT CONDITIONS FOR 30-120 MINUTERS, WHEREBY SAID SECOND PHASE IS PLACED IN SOLUTION WITH SAID MATERIAL; (B) QUENCHING THE MATERIAL AS QUICKLY AS POSSIBLE TO RETAIN THE SECOND-PHASE CONSTITUENTS IN SOLUTION; (C) WORKING THE MATERIAL AT A TEMPERATURE BELOW 500* C. TO REDUCE ITS CROSS SECTION AND REMOVING ANY SURFACE DEFECTS WHICH MAY BE PRESENT; (D) FURTHER HEAT-TRETING THE MATERIAL AT A TEMPERATURE IN THE RANGE 750*C.-825-C. UNDER INERT CONDITIONS FOR 15-130 MINUTES; (E) ENCLOSING THE MATERIAL IN A SHEATH OF DIFFERENT MATERIAL HAVING SUBSTANTIALLY SIMILAR WORKING PROPERTIES TO THE MATERIAL REGARDING DUCTILITY, RATE OF WORKHARDENING AND HARDNESS: (F) DEFORMING THE MATERIAL AND SHEATH TOGETHER TO THE REQUIRED FINAL CROSS-SECTION OF THE MATERIAL; (G) DISSOLVING THE SHEATH; (H) COPPER-PLATING THE MATERIAL.
US500218A 1964-10-30 1965-10-21 Manufacture of superconducting wire Expired - Lifetime US3378916A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB44416/64A GB1092467A (en) 1964-10-30 1964-10-30 Improvements in and relating to the manufacture of superconducting wire

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DE (1) DE1483361A1 (en)
GB (1) GB1092467A (en)
NL (1) NL6513891A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3471925A (en) * 1965-11-17 1969-10-14 Avco Corp Composite superconductive conductor and method of manufacture
US3793700A (en) * 1972-09-01 1974-02-26 Gen Dynamics Corp Method of reshaping metal matrix composite material
US3800061A (en) * 1969-03-05 1974-03-26 Norton Co Composite conductor containing superconductive wires
US6112395A (en) * 1997-11-12 2000-09-05 Usf Filtration And Separations Group, Inc. Process of making fine and ultra fine metallic fibers
US20030135971A1 (en) * 1997-11-12 2003-07-24 Michael Liberman Bundle draw based processing of nanofibers and method of making
WO2018015009A1 (en) * 2016-07-18 2018-01-25 Ceramtec Gmh Galvanic copper deposition on refractory metallic coatings

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4629515A (en) * 1981-04-30 1986-12-16 Mitsubishi Denki Kabushiki Kaisha Superconductive materials and process for the production thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3109963A (en) * 1960-08-29 1963-11-05 Bell Telephone Labor Inc Insulated superconducting wire
US3131469A (en) * 1960-03-21 1964-05-05 Tyler Wayne Res Corp Process of producing a unitary multiple wire strand
US3204326A (en) * 1960-12-19 1965-09-07 American Optical Corp Multi-element energy-conducting structures and method of making the same
US3218693A (en) * 1962-07-03 1965-11-23 Nat Res Corp Process of making niobium stannide superconductors
US3239919A (en) * 1961-08-15 1966-03-15 Rola Company Australia Proprie Method of producing high energy permanent magnets
US3277564A (en) * 1965-06-14 1966-10-11 Roehr Prod Co Inc Method of simultaneously forming a plurality of filaments

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3131469A (en) * 1960-03-21 1964-05-05 Tyler Wayne Res Corp Process of producing a unitary multiple wire strand
US3109963A (en) * 1960-08-29 1963-11-05 Bell Telephone Labor Inc Insulated superconducting wire
US3204326A (en) * 1960-12-19 1965-09-07 American Optical Corp Multi-element energy-conducting structures and method of making the same
US3239919A (en) * 1961-08-15 1966-03-15 Rola Company Australia Proprie Method of producing high energy permanent magnets
US3218693A (en) * 1962-07-03 1965-11-23 Nat Res Corp Process of making niobium stannide superconductors
US3277564A (en) * 1965-06-14 1966-10-11 Roehr Prod Co Inc Method of simultaneously forming a plurality of filaments

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3471925A (en) * 1965-11-17 1969-10-14 Avco Corp Composite superconductive conductor and method of manufacture
US3800061A (en) * 1969-03-05 1974-03-26 Norton Co Composite conductor containing superconductive wires
US3793700A (en) * 1972-09-01 1974-02-26 Gen Dynamics Corp Method of reshaping metal matrix composite material
US6112395A (en) * 1997-11-12 2000-09-05 Usf Filtration And Separations Group, Inc. Process of making fine and ultra fine metallic fibers
US6497029B1 (en) 1997-11-12 2002-12-24 Pall Filtration And Separations Group Inc. Process for making fine and ultra fine metallic fibers
US20030135971A1 (en) * 1997-11-12 2003-07-24 Michael Liberman Bundle draw based processing of nanofibers and method of making
WO2018015009A1 (en) * 2016-07-18 2018-01-25 Ceramtec Gmh Galvanic copper deposition on refractory metallic coatings

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Publication number Publication date
CH478248A (en) 1969-09-15
GB1092467A (en) 1967-11-22
NL6513891A (en) 1966-05-02
DE1483361A1 (en) 1969-09-18

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