US3270400A - Process of making niobium stannide bodies - Google Patents

Process of making niobium stannide bodies Download PDF

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US3270400A
US3270400A US301167A US30116763A US3270400A US 3270400 A US3270400 A US 3270400A US 301167 A US301167 A US 301167A US 30116763 A US30116763 A US 30116763A US 3270400 A US3270400 A US 3270400A
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critical current
heating
superconductor
solenoid
tin
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Eugen J Saur
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F6/00—Superconducting magnets; Superconducting coils
    • H01F6/06—Coils, e.g. winding, insulating, terminating or casing arrangements therefor
    • 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
    • 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
    • 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
    • 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
    • Y10S505/924—Making superconductive magnet or coil
    • 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
    • Y10T29/49002—Electrical device making
    • Y10T29/4902—Electromagnet, transformer or inductor
    • Y10T29/49071—Electromagnet, transformer or inductor by winding or coiling
    • 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
    • Y10T29/49764—Method of mechanical manufacture with testing or indicating
    • Y10T29/49771—Quantitative measuring or gauging
    • 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
    • Y10T29/4998—Combined manufacture including applying or shaping of fluent material
    • Y10T29/49982—Coating

Definitions

  • the present invention relates to superconducting electromagnets e.g. solenoids, particularly of the type wherein a thin coating of Nb Sn is formed on a refractory metal wire which is then wound into a solenoid.
  • superconducting electromagnets e.g. solenoids, particularly of the type wherein a thin coating of Nb Sn is formed on a refractory metal wire which is then wound into a solenoid.
  • Ductile forms of such wires have been made as described in the copending application of Allen and Stauffer, S.N. 102,593, filed April 12, 1961 and my own copending applications S.N. 208,925, filed July 10, 1962 and SN. 233,961, filed October 29, 1962. While these wires usually retain their critical current capacities after being wound into a solenoid, they can experience a lowering of critical current due to excessive stresses induced by mishandling. It appears that the reason for this lowering of critical current is that superconducting filaments within the Nb Sn coating are broken. These filaments can be restored or replaced through annealing of the wire. It would be expected that the annealing would have to take place at about 9001200 C.
  • low temperature insulations refers to plastics which can withstand less than about 100 C.
  • intermediate temperature insulations refers to Teflon, silicone rubber, magnesium fluoride which can withstand temperatures between 100 and in some cases up to about 800 C.
  • high temperature insulations refers to ceramic insulation which can withstand 1000 C.
  • Nb Sn wires may be wrapped into tight solenoids. Where the stresses of such winding cause the critical current to decrease, the original high critical current values may be restored by annealing at ZOO-600 C. I have discovered that heating at these temperatures is sufficient to restore high critical currents.
  • superconductive wire is prepared by treating a niobium surface to render it wettable by tin, applying a coating of tin and heating the coated wire at 1100 C. to form a diffusion coating of Nb Sn.
  • the details of the above process are set forth more fully in my above copending application of which the present application is a continuationin-part.
  • the wires made according to my method are characterized in the presence of substantial amounts of unreacted tin over the Nb Sn coating.
  • the superconductive wire is then coated with copper and with an outer layer of a temperature-resistant dielectric such as Teflon or magnesium fluoride.
  • a temperature-resistant dielectric such as Teflon or magnesium fluoride.
  • the resultant product is then wound into a solenoid and tested. When the testing reveals that the critical current readings are lower than those to be expected, the solenoid can be placed in an argon furnace and heated to the upper tin in the Nb Sn coatings.
  • Example 1 A niobium wire was cleaned by heating at 1100 C. in vacuum for one hour over a molten tin bath. The wire was then dipped into the tin bath for 4 minutes and postheated for 15 minutes.
  • the apparatus is the same as that shown in my copending application, S.N. 233,961, filed October 29, 1962.
  • the resultant coated wire, shown in FIG. 1 was ductile and had a critical current of 20 amps in a transverse magnetic field of 30 kilogauss, at 4.2 K. This indicates that substantial Nb Sn paths were present in the outer coating of the wire.
  • the wire was then strained by bending it about a spool having a 60 millimeter radius. After this distortion the wire was tested for critical current and had 15% less, only 17 amps at 30 kilogauss and 4.2 K.
  • the critical current was then 20 amps at 30 kilogauss and 4.2 K.
  • Example 2 The process of Example 1 was repeated save that in this case the substrate was a niobium ribbon, rather than a round wire.
  • the cross-sectional dimensions of the ribbon were .05 millimeter thick and 2 millimeters wide.
  • the Nb Sn coated ribbon had a critical current of 40 amps at 30 kilogauss and 4.2 K. Then the ribbon/was bent about a spool having a 10 millimeter radius. After this distortion, it had a critical current of 20 amps at 30 kilogauss and 4.2 K.
  • the ribbon was heat treated at 250 C. for 12 hours. After this treatment, it had a critical current of 28 amps at 30 kilogauss and 4.2 K.
  • Example 3 The process of Example 2 was repeated for a niobium ribbon which was .2 millimeter thick by 2.4 millimeters wide. Before distortion, the critical current was 50 amps. After bending about a 10 "millimeter radius, the critical current was 25 amps. Heating the ribbon at 250 C. for 12 hours restored its critical current to 35 amps. All critical current tests were at 30 kilogauss and 4.2 K.
  • Example 4 The tests of Examples 2 and 3 were repeated with heat treatments after distortion at C. for 12 hours. No improvement was obtained.
  • the critical current of the .05 by 2 ribbon remained at 20 amps and the critical current of the .2 by 2.4 ribbon remained at 25 amps.
  • Substantial healing can be obtained by heating the damaged wire or ribbon above 250 C. for times in excess of 10 hours. At higher temperatures, the times can be reduced. In any event, care should be taken to avoid completely reacting all the tin in the wire or ribbon when higher temperatures are used.
  • a method of making electromagnets comprising the steps of preparing an elongated superconductor with a thin layer of Nb Sn and excess tin on a refractory metal base, electrically insulating the superconductor with an insulation capable of withstanding temperatures in the range of from at least 200 C. to about 800 C., winding the superconductor into a solenoid, testing the solenoid to detect :any loss of critical current in the wire, then heating the solenoid between 200 C. and the upper temperature limit of the insulation whenever a lowering of critical current capacity is indicated by the test for a time sufficient to restore at least a portion of the lost critical current capacity but less than the period required to consume all of the excess tin.
  • a method of making superconductive elements comprising the steps of preparing adjacent layers of niobium 4 and tin, heating the layers at 9001200 C. to form a diffusion layer of Nb Sn and excess tin, testing the resultant product for critical current, working the resultant product into a desired shape and retesting for critical current, and heating the superconductor between 200 C. and 600 C. whenever lowering of the critical current capacity is indicated, the heating being continued for a sufi'lcient time and sufficiently low temperature to restore a substantial portion of the critical current without reacting all the excess tin.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)

Description

United States Patent 3,270,400 PROCESS OF MAKING NIOBIUM STANNIDE BODIES, Eugen J. Saur, 20 Jahnstn, Giessen, Germany N0 Drawing. Filed Aug. 9, 1963, Ser. No. 301,167 3 Claims. (Cl. 29155.5)
This application is a continuation-in-part of my copending application, Serial No. 208,925, file-d July 10, 1962 and Serial No. 233,961, filed October 29, 1962.
The present invention relates to superconducting electromagnets e.g. solenoids, particularly of the type wherein a thin coating of Nb Sn is formed on a refractory metal wire which is then wound into a solenoid.
Ductile forms of such wires have been made as described in the copending application of Allen and Stauffer, S.N. 102,593, filed April 12, 1961 and my own copending applications S.N. 208,925, filed July 10, 1962 and SN. 233,961, filed October 29, 1962. While these wires usually retain their critical current capacities after being wound into a solenoid, they can experience a lowering of critical current due to excessive stresses induced by mishandling. It appears that the reason for this lowering of critical current is that superconducting filaments within the Nb Sn coating are broken. These filaments can be restored or replaced through annealing of the wire. It would be expected that the annealing would have to take place at about 9001200 C. since these are the temperatures at which Nb Sn is formed in the course of making the superconductive wire. This would be prohibitive since many intermediate temperature insulations, which may be applied to the wire, cannot withstand such temperatures. As used herein, low temperature insulations refers to plastics which can withstand less than about 100 C.; intermediate temperature insulations refers to Teflon, silicone rubber, magnesium fluoride which can withstand temperatures between 100 and in some cases up to about 800 C.; and high temperature insulations refers to ceramic insulation which can withstand 1000 C.
It is therefore the object of the invention to provide a method of compensating for the effects of excessive stresses and to restore the critical currents of damaged superconductive wires and a further object that such a method will be compatible with conventional, intermediate temperature dielectric insulations which are applied to the wire.
In accord with the present invention, Nb Sn wires may be wrapped into tight solenoids. Where the stresses of such winding cause the critical current to decrease, the original high critical current values may be restored by annealing at ZOO-600 C. I have discovered that heating at these temperatures is sufficient to restore high critical currents.
In a preferred embodiment of the invention, superconductive wire is prepared by treating a niobium surface to render it wettable by tin, applying a coating of tin and heating the coated wire at 1100 C. to form a diffusion coating of Nb Sn. The details of the above process are set forth more fully in my above copending application of which the present application is a continuationin-part. The wires made according to my method are characterized in the presence of substantial amounts of unreacted tin over the Nb Sn coating.
The superconductive wire is then coated with copper and with an outer layer of a temperature-resistant dielectric such as Teflon or magnesium fluoride. The resultant product is then wound into a solenoid and tested. When the testing reveals that the critical current readings are lower than those to be expected, the solenoid can be placed in an argon furnace and heated to the upper tin in the Nb Sn coatings.
"ice
temperature limit of the dielectric. This heating will restore superconducting paths which may have been breached by stresses encountered in winding the solenoid. All the materials used in the solenoid are capable of withstanding this temperature range. It will be appreciated that, in the absence of the present method, it would be necessary to scrap faulty solenoids.
Some non-limiting examples showing the ability of the present method to restore the critical current of Nb Sn wires are now set forth.
Example 1 A niobium wire was cleaned by heating at 1100 C. in vacuum for one hour over a molten tin bath. The wire was then dipped into the tin bath for 4 minutes and postheated for 15 minutes. The apparatus is the same as that shown in my copending application, S.N. 233,961, filed October 29, 1962. The resultant coated wire, shown in FIG. 1, was ductile and had a critical current of 20 amps in a transverse magnetic field of 30 kilogauss, at 4.2 K. This indicates that substantial Nb Sn paths were present in the outer coating of the wire.
The wire was then strained by bending it about a spool having a 60 millimeter radius. After this distortion the wire was tested for critical current and had 15% less, only 17 amps at 30 kilogauss and 4.2 K.
Then the wire was heated in vacuum at 250 C. for 12 hours and retested. The critical current was then 20 amps at 30 kilogauss and 4.2 K.
Example 2 The process of Example 1 was repeated save that in this case the substrate was a niobium ribbon, rather than a round wire. The cross-sectional dimensions of the ribbon were .05 millimeter thick and 2 millimeters wide. The Nb Sn coated ribbon had a critical current of 40 amps at 30 kilogauss and 4.2 K. Then the ribbon/was bent about a spool having a 10 millimeter radius. After this distortion, it had a critical current of 20 amps at 30 kilogauss and 4.2 K.
The ribbon was heat treated at 250 C. for 12 hours. After this treatment, it had a critical current of 28 amps at 30 kilogauss and 4.2 K.
Example 3 The process of Example 2 was repeated for a niobium ribbon which was .2 millimeter thick by 2.4 millimeters wide. Before distortion, the critical current was 50 amps. After bending about a 10 "millimeter radius, the critical current was 25 amps. Heating the ribbon at 250 C. for 12 hours restored its critical current to 35 amps. All critical current tests were at 30 kilogauss and 4.2 K.
Example 4 The tests of Examples 2 and 3 were repeated with heat treatments after distortion at C. for 12 hours. No improvement was obtained. The critical current of the .05 by 2 ribbon remained at 20 amps and the critical current of the .2 by 2.4 ribbon remained at 25 amps.
It is necessary to make the wires or ribbons with excess It is believed that this facilitates low temperature healing by permitting broken sections of superconductive filaments to move easily towards each other and to be rejoined. It is preferred that the healing heat treatment be carried out in a manner to avoid reacting all the excess tin.
Substantial healing can be obtained by heating the damaged wire or ribbon above 250 C. for times in excess of 10 hours. At higher temperatures, the times can be reduced. In any event, care should be taken to avoid completely reacting all the tin in the wire or ribbon when higher temperatures are used.
What is claimed is:
1. A method of making electromagnets, such as solenoids and the like, comprising the steps of preparing an elongated superconductor with a thin layer of Nb Sn and excess tin on a refractory metal base, electrically insulating the superconductor with an insulation capable of withstanding temperatures in the range of from at least 200 C. to about 800 C., winding the superconductor into a solenoid, testing the solenoid to detect :any loss of critical current in the wire, then heating the solenoid between 200 C. and the upper temperature limit of the insulation whenever a lowering of critical current capacity is indicated by the test for a time sufficient to restore at least a portion of the lost critical current capacity but less than the period required to consume all of the excess tin.
2. The method of claim 1 wherein the superconductor is coated with an inner sheath of copper and an outer sheath of the insulation prior to winding into a solenoid.
3. A method of making superconductive elements comprising the steps of preparing adjacent layers of niobium 4 and tin, heating the layers at 9001200 C. to form a diffusion layer of Nb Sn and excess tin, testing the resultant product for critical current, working the resultant product into a desired shape and retesting for critical current, and heating the superconductor between 200 C. and 600 C. whenever lowering of the critical current capacity is indicated, the heating being continued for a sufi'lcient time and sufficiently low temperature to restore a substantial portion of the critical current without reacting all the excess tin.
References Cited by the Examiner UNITED STATES PATENTS 3,163,832 12/1964 Nahrnan et al. 29-155.5 3,181,936 5/1965 Perry et al. 29155.5 3,218,693 11/1965 Allen et al. 29155.5
JOHN F. CAMPBELL, Primary Examiner.
P. M. COHEN, Assistant Examiner.

Claims (2)

1. A METHOD OF MAKING ELECTROMAGNETS, SUCH AS SOLENOIDS AND THE LIKE, COMPRISING THE STEPS OF PREPARING AN ELONGATED SUPERCONDUCTOR WITH A THIN LAYER OF NB3SN AND EXCESS TIN ON A REFRACTORY METAL BASE, ELECTRICALLY INSULATING THE SUPERCONDUCTOR WITH AN INSULATION CAPABLE OF WITHSTANDING TEMPERATURES IN THE RANGE OF FROM AT LEAST 200*C. TO ABOUT 800*C., WINDING THE SUPERCONDUCTOR INTO A SOLENOID, TESTING THE SOLENOID TO DETECT ANY LOSS OF CRITICAL CURRENT IN THE WIRE, THEN HEATING THE SOLENOID BETWEEN 200*C. AND THE UPPER TEMPERATURE LIMIT OF THE INSULATION WHENEVER A LOWERING OF CRITICAL CURRENT CAPACITY IS INDICATED BY THE TEST FOR A TIME SUFFICIENT TO RESTORE AT LEAST A PORTION OF THE LOST CRITICAL CURRENT CAPACITY BUT LESS THAN THE PERIOD REQUIRED TO CONSUME ALL OF THE EXCESS TIN.
3. A METHOD OF MAKING SUPERCONDUCTIVE ELEMENTS COMPRISING THE STEPS OF PREPARING ADJACENT LAYERS OF NIOBIUM AND TIN, HEATING THE LAYERS AT 900-1200*C. TO FORM A DIFFUSION LAYER OF NB3SN AND EXCESS TIN, TESTING THE RESULTANT PRODUCT FOR CRITICAL CURRENT, WORKING THE RESULTANT PRODUCT INTO A DESIRED SHAPE AND RETESTING FOR CRITICAL CURRENT, AND HEATING THE SUPERCONDUCTOR BETWEEN 200* C. AND 600*C. WHENEVER LOWERING OF THE CRITICAL CURRENT CAPACITY IS INDICATED, THE HEATING BEING CONTINUED FOR A SUFFICIENT TIME AND SUFFICIENTLY LOW TEMPERATURE TO RESTORE A SUBSTANTIAL PORTION OF THE CRITICAL CURRENT WITHOUT REACTING ALL THE EXCESS TIN.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3429032A (en) * 1963-10-15 1969-02-25 Gen Electric Method of making superconductors containing flux traps
US3466237A (en) * 1965-09-17 1969-09-09 Imp Metal Ind Kynoch Ltd Method of obtaining an intermetallic compound of niobium and tin in fabricated form
US3907550A (en) * 1973-03-19 1975-09-23 Airco Inc Method of making same composite billets

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3163832A (en) * 1961-09-15 1964-12-29 Univ Kansas State Superconductive coaxial line useful for delaying signals
US3181936A (en) * 1960-12-30 1965-05-04 Gen Electric Superconductors and method for the preparation thereof
US3218693A (en) * 1962-07-03 1965-11-23 Nat Res Corp Process of making niobium stannide superconductors

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3181936A (en) * 1960-12-30 1965-05-04 Gen Electric Superconductors and method for the preparation thereof
US3163832A (en) * 1961-09-15 1964-12-29 Univ Kansas State Superconductive coaxial line useful for delaying signals
US3218693A (en) * 1962-07-03 1965-11-23 Nat Res Corp Process of making niobium stannide superconductors

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3429032A (en) * 1963-10-15 1969-02-25 Gen Electric Method of making superconductors containing flux traps
US3466237A (en) * 1965-09-17 1969-09-09 Imp Metal Ind Kynoch Ltd Method of obtaining an intermetallic compound of niobium and tin in fabricated form
US3907550A (en) * 1973-03-19 1975-09-23 Airco Inc Method of making same composite billets

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