US3277557A - Production of nb3sn diffusion layers - Google Patents
Production of nb3sn diffusion layers Download PDFInfo
- Publication number
- US3277557A US3277557A US239254A US23925462A US3277557A US 3277557 A US3277557 A US 3277557A US 239254 A US239254 A US 239254A US 23925462 A US23925462 A US 23925462A US 3277557 A US3277557 A US 3277557A
- Authority
- US
- United States
- Prior art keywords
- wire
- tin
- bath
- coating
- nb3sn
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000009792 diffusion process Methods 0.000 title description 8
- 238000004519 manufacturing process Methods 0.000 title description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 17
- 238000000576 coating method Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 230000004907 flux Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- 239000010955 niobium Substances 0.000 description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002344 surface layer Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000001464 adherent effect Effects 0.000 description 3
- 229910002056 binary alloy Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002887 superconductor Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/08—Tin or alloys based thereon
-
- 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
- H10N60/0184—Manufacture or treatment of devices comprising intermetallic compounds of type A-15, e.g. Nb3Sn
-
- 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
- FIG. 3 there is shown a third embodiment of the process wherein a niobium wire 214 is drawn through inert atmosphere chambers 220, 222 and 224. Inlet and outlet valves 226 are provided.
- the chamber 222 contains a tin bath 210.
- the Wire 214 is dipped in this bath and removed via a die 216 which may be made of diamond.
- a broach 22-8 is employed -to strip a surface layer from the Wire thus exposing a cleaner surface of the wire which is immediately dipped and drawn through the die.
- the improvement comprising the process of cleaning a niobium wire to remove surface contaminants therefrom by removing a surface layer of the niobium wire in a broaching operation, passing the wire to a tin bath wherein a surface layer of tin is accreted thereon, removing the wire from the bath via a die adapted to reduce the diameter of the wire to obtain a uniform adherent coating of tin and subsequently heating the reduced composite wire to produce a surface diffusion layer of Nb Sn.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Coating With Molten Metal (AREA)
Description
Oct. 11, 1966 J. L. HAM
PRODUCTION OF NB SN DIFFUSION LAYERS Filed Nov. 21, 1962 WElifi/EAWOKPER? g L.+ FURNACE Fig. I
l l i l l I24 I I22 I 120 no i '-:-IIO
=3: m/m m/ :2: 2. II! //V1., 7 E:
1% EMESFHEEF WET? I Fig. 2
INVENTOR.
JOHN L. HAM
United States Patent Oflice 3,277,557 Patented Oct. 11, 1966 3,277,557 PRODUCTEON F Nb Sn DIFFUSION LAYERS John L. Ham, Wellesley Hills, Mass., assignor, by mesne assignments, to National Research Corporation, a corporation of Massachusetts Filed Nov. 21, 1962, Ser. No. 239,254 1 Claim. (Cl. 29-155.5)
The present invention relates to the preparation of coatings of hard superconductor binary alloys. Such coating processes comprise the selection of the higher melting constituent as the substrate to be coated and depositing the other constituent as a thin coating. The coated substrate is then heat treated in a furnace to react the substrate and coating to form a resultant diffusion surface layer of the alloy. The process and resultant product are set forth in the copending application of Allen and Stauffer, S.N. 133,653, filed Aug. 24, 1961.
In such processes, it is important to render the substrate surface wettable so that the coating material wets it completely to form an adherent coating which will react with the substrate before it can be vaporized and driven off by heat treatment.
It is therefore the principal object of this invention to provide a process of coating a metallic substrate with another metal to make the coated article suitable for subsequent heat treatment to form a diffusion surface layer of a binary alloy of the two metals.
The method is particularly applicable to niobium substrates to be coated with tin. The binary alloy layer formed by subsequent heat treatment comprises the hard superconductor Nb Sn.
Other objects of the invention will in part be obvious and will in part appear hereinafter. The invention comprises the coating process involving the several steps and the relation and the order of one or more of such steps with respect to each of the others which are exemplified in the following detailed disclosure and the scope of the application of which will be indicated in the claim.
In the following detailed description, reference is made to the drawings wherein:
FIG. 1 is a schematic representation of a process for coating a niobium wire with tin;
FIG. 2 is a schematic representation of a second embodiment of the process; and
FIG. 3 is a schematic representation of a third embodiment of the process.
Referring now to FIG. 1, there is shown a bath of molten flux and a molten tin bat-h 12. Both are maintained in an inert gas atmosphere, such as argon. One example of a suitable flux would be sodium hydroxide. A niobium wire 14 is passed through the flux bath to remove surface oxides and then is passed through the tin bath. The wire is removed from the bath via a die 16. The die may be made of aluminum oxide or if not exposed to atmosphere, of diamond. Suitable heaters (not shown) are provided to maintain the baths in their molten state. Tin melts at 230 C. and most useful fluxes melt in the range 500-800 C.
The die 16 produces a very slight reduction, on the order of 5%, in the diameter of the wire. Yet the die produces a uniform, and adherent, tin coating on the Wire. This Wire may then be placed in an inert gas furnace and heated up to about 1000 C. to produce a surface diffusion layer comprising Nb Sn. The high superconductivity characteristics of such wire have been demonstrated by Allen and Stauffer in the said copending appli cation.
Referring now to FIG. 2, there is shown a second embodiment of the coating process wherein a tank holds tin bath and a flux bath 114 floating on the bath. A die 116 is provided at the tin bath, as in the first embodiment.
The flotation of the flux on the tin insures against any possibility of contaminating the niobium surface prior to dipping in the tin bath. Heaters 118 are provided to heat the flux and tin to their melting points. The tank 100 is provided with an intermediate neck 120 and cooling fins 122 to maintain the temperature gradient. Part of the flux tends to freeze into a solid layer 124. However, the wire 114 is easily pulled through this layer and the separation of liquid flux from liquid tin avoids an undesired reaction.
Referring now to FIG. 3, there is shown a third embodiment of the process wherein a niobium wire 214 is drawn through inert atmosphere chambers 220, 222 and 224. Inlet and outlet valves 226 are provided. The chamber 222 contains a tin bath 210. The Wire 214 is dipped in this bath and removed via a die 216 which may be made of diamond. A broach 22-8 is employed -to strip a surface layer from the Wire thus exposing a cleaner surface of the wire which is immediately dipped and drawn through the die.
While the invention has been discussed principally in its utility for coating wire, it is also applicable to rod and sheet with appropriate changes in die construction or using rollers to simulate the action of a die.
Since certain changes may be made in the above process without departing from the scope of the invention herein involved, it is intended that all matter contained in the above description, or shown in the accompanying drawing, shall be interpreted as illustrative and not in a limiting sense.
What is claimed is:
In the art of heating tin coated wires to produce a surface diffusion layer of Nb Sn, the improvement comprising the process of cleaning a niobium wire to remove surface contaminants therefrom by removing a surface layer of the niobium wire in a broaching operation, passing the wire to a tin bath wherein a surface layer of tin is accreted thereon, removing the wire from the bath via a die adapted to reduce the diameter of the wire to obtain a uniform adherent coating of tin and subsequently heating the reduced composite wire to produce a surface diffusion layer of Nb Sn.
References Cited by the Examiner UNITED STATES PATENTS 2,906,018 9/1959 Baker 29-528 2,950,526 8/1960 Buehler et al. 29528 X 3955, 102 9/1962 Shaw et al. 72--275 X 3,157,093 11/1964 Shaw et al. 72--275 X 3,181,936 5/1965 Denny et al.
JOHN F. CAMPBELL, Primary Examiner.
P. W. COHEN, Assistant Examiner.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US239254A US3277557A (en) | 1962-11-21 | 1962-11-21 | Production of nb3sn diffusion layers |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US239254A US3277557A (en) | 1962-11-21 | 1962-11-21 | Production of nb3sn diffusion layers |
Publications (1)
Publication Number | Publication Date |
---|---|
US3277557A true US3277557A (en) | 1966-10-11 |
Family
ID=22901329
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US239254A Expired - Lifetime US3277557A (en) | 1962-11-21 | 1962-11-21 | Production of nb3sn diffusion layers |
Country Status (1)
Country | Link |
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US (1) | US3277557A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4411712A (en) * | 1980-12-15 | 1983-10-25 | Airco, Inc. | Method of manufacture of multifilamentary intermetallic superconductors |
EP0690143A1 (en) * | 1994-06-27 | 1996-01-03 | General Electric Company | Method of coating niobium foil |
EP0691691A1 (en) * | 1994-07-05 | 1996-01-10 | General Electric Company | Method for making triniobium tin superconductor |
US20230121858A1 (en) * | 2016-03-03 | 2023-04-20 | Michael T. Stawovy | Fabrication of metallic parts by additive manufacturing |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2906018A (en) * | 1953-03-12 | 1959-09-29 | Armco Steel Corp | Finishing machine and method for use in the hot dip metallic coating of steel strip, and coated strip |
US2950526A (en) * | 1957-04-22 | 1960-08-30 | William J Buehler | Elevated temperature working of metals and alloys |
US3055102A (en) * | 1956-10-11 | 1962-09-25 | Lasalle Steel Co | Metal finishing means and method for use of same |
US3157093A (en) * | 1957-10-22 | 1964-11-17 | Lasalle Steel Co | Method of removing metal by shaving |
US3181936A (en) * | 1960-12-30 | 1965-05-04 | Gen Electric | Superconductors and method for the preparation thereof |
-
1962
- 1962-11-21 US US239254A patent/US3277557A/en not_active Expired - Lifetime
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2906018A (en) * | 1953-03-12 | 1959-09-29 | Armco Steel Corp | Finishing machine and method for use in the hot dip metallic coating of steel strip, and coated strip |
US3055102A (en) * | 1956-10-11 | 1962-09-25 | Lasalle Steel Co | Metal finishing means and method for use of same |
US2950526A (en) * | 1957-04-22 | 1960-08-30 | William J Buehler | Elevated temperature working of metals and alloys |
US3157093A (en) * | 1957-10-22 | 1964-11-17 | Lasalle Steel Co | Method of removing metal by shaving |
US3181936A (en) * | 1960-12-30 | 1965-05-04 | Gen Electric | Superconductors and method for the preparation thereof |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4411712A (en) * | 1980-12-15 | 1983-10-25 | Airco, Inc. | Method of manufacture of multifilamentary intermetallic superconductors |
EP0690143A1 (en) * | 1994-06-27 | 1996-01-03 | General Electric Company | Method of coating niobium foil |
EP0691691A1 (en) * | 1994-07-05 | 1996-01-10 | General Electric Company | Method for making triniobium tin superconductor |
US20230121858A1 (en) * | 2016-03-03 | 2023-04-20 | Michael T. Stawovy | Fabrication of metallic parts by additive manufacturing |
US11919070B2 (en) * | 2016-03-03 | 2024-03-05 | H.C. Starck Solutions Coldwater, LLC | Fabrication of metallic parts by additive manufacturing |
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