EP0060575A1 - Process for manufacturing semi-finished products from a copper-containing memory alloy - Google Patents
Process for manufacturing semi-finished products from a copper-containing memory alloy Download PDFInfo
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- EP0060575A1 EP0060575A1 EP82200172A EP82200172A EP0060575A1 EP 0060575 A1 EP0060575 A1 EP 0060575A1 EP 82200172 A EP82200172 A EP 82200172A EP 82200172 A EP82200172 A EP 82200172A EP 0060575 A1 EP0060575 A1 EP 0060575A1
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- European Patent Office
- Prior art keywords
- die
- memory alloy
- press
- conical part
- conical
- 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.)
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- 239000010949 copper Substances 0.000 title claims abstract description 9
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 8
- 239000011265 semifinished product Substances 0.000 title claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 9
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 239000000314 lubricant Substances 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 4
- 230000004323 axial length Effects 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 229910001069 Ti alloy Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 4
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- 229910001000 nickel titanium Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910002058 ternary alloy Inorganic materials 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- C22F1/006—Resulting in heat recoverable alloys with a memory effect
Definitions
- the invention relates to a method for producing semi-finished products from a memory alloy according to the preamble of claim 1.
- the invention has for its object to provide a manufacturing process for semi-finished products made of ternary Ni / Ti / Cu alloys, which provides flawless, dense products.
- a round bar was first cast from a ternary memory alloy of the following composition using customary methods.
- the components were first cleaned in elementary form, dried and melted in a graphite crucible under vacuum together with an alloy premelted on the crucible bottom.
- the melt was poured into a graphite mold, producing a cast ingot 20 mm in diameter and 140 mm in length.
- the cast ingot was subjected to a homogenization annealing just below the solidus line, in the present case at a temperature of 900 ° C. for 24 hours under an argon atmosphere. From the cast and homogenized rod was cut off a piece and turned to a diameter of 18 mm and a length of 35 mm. This diameter was slightly below the inside diameter of the recipient of the extrusion press.
- the workpiece was kept at a temperature of 700 ° C. for 10 minutes, a thin oxide layer being formed on the surface.
- Boron nitride was used as the lubricant.
- the extrusion was carried out isothermally at a temperature of 750 C under a punch force of 150 kN and a punch speed of 0.1 mm / s.
- the strand obtained in this way had a diameter of 9 mm, which corresponds to a reduction ratio of 4: 1.
- a press die was used as the tool, which had a conical surface with a 45 ° half opening angle and 4.5 mm axial length on the inlet side and a cylindrical part of 9 mm diameter and 5 mm axial length on the outlet side. There was a radius of 5 mm at the inlet of the conical part and a radius of 2 mm at the outlet.
- the strand with a diameter of 9 mm (semi-finished product) was encapsulated in a steel tube with a wall thickness of 1 mm and hammered to a diameter of 3 mm at 750 ° C.
- the steel jacket was then removed and the wire was drawn down cold in several steps to a diameter of 1 mm.
- the cross-sectional decrease per step was 10% in each case.
- the wire was annealed at 800 ° C for 15 minutes.
- the finished wire was finally subjected to a soft annealing process at 900 ° C for 1 h in order to meet the structural requirements for optimal subsequent martensite formation.
- composition of the memory alloy to which the present method for producing semifinished products is directed can basically be as follows:
- the homogenization annealing of the cast ingot can be carried out for 1 to 200 h at temperatures which are 10 to 200 ° C. below the solidus line of the alloy.
- Hot processing by extrusion can be carried out isothermally in the temperature range from 700 to 850 ° C with stamp speeds of 0.01 mm / s upwards.
- the reduction ratio can be 4: 1 to 20: 1.
- the stamper used should have a conical portion having preferably 45 0 half-opening angle, wherein the transition radius from the recipient in this part preferably 1 to 10 mm or 1 to 25% of the recipient diameter.
- the corresponding transition radius at the outlet of the conical into the cylindrical part of the die should preferably also be 1 to 10 mm or 1 to 25% of the recipient diameter.
- the cylindrical part of the die (outlet) should be longer in the axial direction than the conical part (inlet).
- the tools used for isothermal extrusion can also have dimensions other than those mentioned above in practice, depending on the requirements. This applies above all to the design of the press die, the shape of which also depends to a certain extent on the profile to be created (whether round, triangular, square, rectangular, hollow, ribbon-shaped, etc.).
- the surface oxidation process given in the example to facilitate the application of the lubricant can also be omitted and is not essential to the invention.
- the method according to the invention enables the production of semi-finished products from the brittle Ni / Ti / Cu alloy, which is difficult to deform per se, even in the case of higher copper contents.
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Forging (AREA)
- Extrusion Of Metal (AREA)
Abstract
Spröde, kupferhaltige Ni/Ti-Gedächtnislegierungen können vom Gusszustand dadurch in für die Weiterverarbeitung geeignetes Halbzeug übergeführt werden, indem ein Gussbarren knapp unterhalb der Soliduslinie homogenisiert und anschliessend im Temperaturbereich von 700 bis 850°C isotherm stranggepresst wird.Brittle, copper-containing Ni / Ti memory alloys can be converted from the as-cast state into semi-finished products suitable for further processing by homogenizing a cast ingot just below the solidus line and then extruding it isothermally in the temperature range from 700 to 850 ° C.
Description
Die Erfindung geht aus von einem Verfahren zur Herstellung von Halbzeug aus einer Gedächtnislegierung nach der Gattung des Anspruchs 1.The invention relates to a method for producing semi-finished products from a memory alloy according to the preamble of claim 1.
Die Warmverarbeitung von Gedächtnislegierungen auf der Basis von Nickel/Titan ist ein bereits allgemein bekannter Prozess. Ueber das Schmieden, Rundhämmern, Walzen und Ziehen dieser Legierungen existiert bereits eine ansehnliche Literatur (z.B. C.M. Jackson, H.J. Wagner and R.J. Wasilewski, 55 - Nitinol - The alloy with a memory: its physical metallurgy, properties and applications, NASA SP5110, p. 19-21; US-PS 3,508,914. US-PS 3,700,434). Ueber das Strangpressen von Nickel/Titan-Legierungen wurde ebenfalls berichtet (J.H. Hanlon, S.R. Butler, R.J. Wasilewski, Effect of martensitic transformation on the electrical and magnetic properties of NiTi,Trans. Met. Soc. of AIME, 239, p. 1323, 1967). Dabei gelangten verschiedene Strangpressmethoden bei 900°C und Reduktionsverhältnissen von 4:1 bis 16:1 zur Anwendung.The hot processing of memory alloys based on nickel / titanium is a process that is already well known. There is already considerable literature on the forging, round hammering, rolling and drawing of these alloys (e.g. CM Jackson, HJ Wagner and RJ Wasilewski, 55 - Nitinol - The alloy with a memory: its physical metallurgy, properties and applications, NASA SP5110, p. 19-21; U.S. Patent 3,508,914. U.S. Patent 3,700,434). Extrusion of nickel / titanium alloys has also been reported (JH Hanlon, SR Butler, RJ Wasilewski, Effect of martensitic transformation on the electrical and magnetic properties of NiTi, Trans. Met. Soc. Of AIME, 239, p. 1323, 1967). Various extrusion methods at 900 ° C and reduction ratios from 4: 1 to 16: 1 were used.
Diese Verfahren sind praktisch ausschliesslich für binäre Nickel/Titan-Legierungen entwickelt worden und sind für kupferhaltige ternäre Legierungen ungeeignet, insbesondere bei höheren Kupfergehalten. Die ternären Legierungen des Ni/Ti/Cu-Typs sind bedeutend spröder und enthalten höhere Anteile der sekundären Phase sowie Poren als binäre Ni/Ti-Legierungen. Sie stellen daher an die Verarbeitungsmethoden weit höhere Ansprüche. Da derartige Legierungen grosse technische Bedeutung haben, besteht ein lebhaftes Bedürfnis nach geeigneten Fabrikationsprozessen.These methods have been developed practically exclusively for binary nickel / titanium alloys and are unsuitable for copper-containing ternary alloys, especially with higher copper contents. The ternary alloys of the Ni / Ti / Cu type are significantly more brittle and contain higher proportions of the secondary phase and pores than binary Ni / Ti alloys. They therefore place far higher demands on the processing methods. Since such alloys are of great technical importance, there is a lively need for suitable manufacturing processes.
Der Erfindung liegt die Aufgabe zugrunde, ein Herstellungsverfahren für Halbzeug aus ternären Ni/Ti/Cu-Legierungen anzugeben, welches einwandfreie, dichte Erzeugnisse liefert.The invention has for its object to provide a manufacturing process for semi-finished products made of ternary Ni / Ti / Cu alloys, which provides flawless, dense products.
Diese Aufgabe wird erfindungsgemäss durch die Merkmale des Anspruchs 1 gelöst.According to the invention, this object is achieved by the features of claim 1.
Aus einer ternären Gedächtnislegierung der nachfolgenden Zusammensetzung wurde zunächst nach üblichen Verfahren ein Rundbarren gegossen.
Die Komponenten wurden zunächst in elementarer Form gereinigt, getrocknet und in einem Graphittiegel unter Vakuum zusammen mit einer auf dem Tiegelboden vorgeschmolzenen Legierung eingeschmolzen. Die Schmelze wurde in eine Graphitform abgegossen, wobei ein Gussbarren von 20 mm Durchmesser und 140 mm Länge erzeugt wurde. Der Gussbarren wurde einer Homogenisierungsglühung knapp unterhalb der Soliduslinie, im vorliegenden Fall bei einer Temperatur von 9000C während 24 h unter Argonatmosphäre unterzogen. Von der gegossenen und homogenisierten Stange wurde ein Stück abgetrennt und auf einen Durchmesser von 18 mm und eine Länge von 35 mm abgedreht. Dieser Durchmesser lag geringfügig unter dem Innendurchmesser des Rezipienten der Strangpresse. Um einen geeigneten Träger für den nachträglich aufzubringenden Schmiermittelfilm zu erhalten, wurde das Werkstück während 10 min auf einer Temperatur von 700°C gehalten, wobei an der Oberfläche eine dünne Oxydschicht gebildet wurde. Als Schmiermittel wurde Bornitrid verwendet. Das Strangpressen wurde isotherm bei einer Temperatur von 750 C unter einer Stempelkraft von 150 kN bei einer Stempelgeschwindigkeit von 0,1 mm/s durchgeführt. Der auf diese Weise erhaltene Strang wies einen Durchmesser von 9 mm auf, was einem Reduktionsverhältnis von 4:1 entspricht. Als Werkzeug wurde eine Pressmatrize verwendet, welche auf der Einlaufseite eine konische Fläche mit 45°halbem Oeffnungswinkel und 4,5 mm axialer Länge und auf der Auslaufseite einen zylindrischen Teil von 9 mm Durchmesser und 5 mm axialer Länge aufwies. Am Einlauf des konischen Teils war ein Radius von 5 mm, am Auslauf ein solcher von 2 mm vorhanden.The components were first cleaned in elementary form, dried and melted in a graphite crucible under vacuum together with an alloy premelted on the crucible bottom. The melt was poured into a graphite mold, producing a cast ingot 20 mm in diameter and 140 mm in length. The cast ingot was subjected to a homogenization annealing just below the solidus line, in the present case at a temperature of 900 ° C. for 24 hours under an argon atmosphere. From the cast and homogenized rod was cut off a piece and turned to a diameter of 18 mm and a length of 35 mm. This diameter was slightly below the inside diameter of the recipient of the extrusion press. In order to obtain a suitable carrier for the subsequently applied lubricant film, the workpiece was kept at a temperature of 700 ° C. for 10 minutes, a thin oxide layer being formed on the surface. Boron nitride was used as the lubricant. The extrusion was carried out isothermally at a temperature of 750 C under a punch force of 150 kN and a punch speed of 0.1 mm / s. The strand obtained in this way had a diameter of 9 mm, which corresponds to a reduction ratio of 4: 1. A press die was used as the tool, which had a conical surface with a 45 ° half opening angle and 4.5 mm axial length on the inlet side and a cylindrical part of 9 mm diameter and 5 mm axial length on the outlet side. There was a radius of 5 mm at the inlet of the conical part and a radius of 2 mm at the outlet.
Der Strang von 9 mm Durchmesser (Halbzeug) wurde in ein Stahlrohr von 1 mm Wandstärke eingekapselt und bei 750°C auf einen Durchmesser von 3 mm rundgehämmert. Der Stahlmantel wurde hierauf entfernt und der Draht kalt in mehreren Schritten auf einen Durchmesser von 1 mm heruntergezogen. Die Querschnittabnahme pro Schritt betrug jeweils 10%. Zwischen zwei Schritten wurde der Draht bei 800°C während 15 min zwischengeglüht. Der fertige Draht wurde schliesslich einem Weichglühprozess bei 900°C während 1 h unterworfen, um die gefügemässigen Voraussetzungen für eine optimale nachherige Martensitbildung zu erhalten.The strand with a diameter of 9 mm (semi-finished product) was encapsulated in a steel tube with a wall thickness of 1 mm and hammered to a diameter of 3 mm at 750 ° C. The steel jacket was then removed and the wire was drawn down cold in several steps to a diameter of 1 mm. The cross-sectional decrease per step was 10% in each case. Between two steps, the wire was annealed at 800 ° C for 15 minutes. The finished wire was finally subjected to a soft annealing process at 900 ° C for 1 h in order to meet the structural requirements for optimal subsequent martensite formation.
Die Zusammensetzung der Gedächtnislegierung, auf die das vorliegende Verfahren zur Herstellung von Halbzeug gerichtet ist, kann grundsätzlich wie folgt lauten:
Die Homogenisierungsglühung des Gussbarrens kann während l bis 200 h bei Temperaturen, die 10 bis 200°C unterhalb der Soliduslinie der Legierung liegen, durchgeführt werden. Die Warmverarbeitung durch Strangpressen kann isotherm im Temperaturbereich von 700 bis 850°C mit Stempelgeschwindigkeiten von 0,01 mm/s an aufwärts durchgeführt werden. Das Reduktionsverhältnis kann 4:1 bis 20:1 betragen. Die verwendete Pressmatrize soll einen konischen Teil mit vorzugsweise 450 halbem Oeffnungswinkel besitzen, wobei der Uebergangsradius vom Rezipient in diesen Teil vorzugsweise 1 bis 10 mm oder 1 bis 25% des Rezipientendurchmessers beträgt. Der entsprechende Uebergangsradius am Auslauf des konischen in den zylindrischen Teil der Matrize soll vorzugsweise ebenfalls 1 bis 10 mm oder 1 bis 25% des Rezipientendurchmessers betragen. Der zylindrische Teil der Matrize (Auslauf) soll in axialer Richtung länger als der konische Teil (Einlauf) sein.The homogenization annealing of the cast ingot can be carried out for 1 to 200 h at temperatures which are 10 to 200 ° C. below the solidus line of the alloy. Hot processing by extrusion can be carried out isothermally in the temperature range from 700 to 850 ° C with stamp speeds of 0.01 mm / s upwards. The reduction ratio can be 4: 1 to 20: 1. The stamper used should have a conical portion having preferably 45 0 half-opening angle, wherein the transition radius from the recipient in this part preferably 1 to 10 mm or 1 to 25% of the recipient diameter. The corresponding transition radius at the outlet of the conical into the cylindrical part of the die should preferably also be 1 to 10 mm or 1 to 25% of the recipient diameter. The cylindrical part of the die (outlet) should be longer in the axial direction than the conical part (inlet).
Es versteht sich von selbst, dass die verwendeten Werkzeuge zum isothermen Strangpressen entsprechend den Anforderungen in der Praxis auch andere als die obengenannten Dimensionen aufweisen können. Dies gilt vor allem auch für die Ausbildung der Pressmatrize, deren Form ausserdem in gewissem Grade vom zu erzeugenden Profil (ob rund, dreieckig, quadratisch, rechteckig, hohl, bandförmig etc.) abhängt.It goes without saying that the tools used for isothermal extrusion can also have dimensions other than those mentioned above in practice, depending on the requirements. This applies above all to the design of the press die, the shape of which also depends to a certain extent on the profile to be created (whether round, triangular, square, rectangular, hollow, ribbon-shaped, etc.).
Der Strangpressgeschwindigkeit ist theoretisch nach oben keine Grenze gesetzt, sofern nur die Bedingung des isothermen Verformungsprozesses eingehalten wird. Eine obere Grenze wird nur durch die Praxis festgesetzt und ist wiederum von den Dimensionen des Pressbolzens, vom herzustellenden Profil, der Grösse der Strangpresse, der Legierungszusammensetzung etc. abhängig.Theoretically, there is no upper limit on the extrusion speed, provided that only the condition of the isothermal deformation process is met. An upper limit is only set by practice and is in turn dependent on the dimensions of the press bolt, the profile to be manufactured, the size of the extrusion press, the alloy composition, etc.
Der zur Erleichterung des Aufbringens des Schmiermittels im Beispiel angeführte Oberflächenoxydationsprozess kann auch weggelassen werden und ist für die Erfindung nicht wesentlich.The surface oxidation process given in the example to facilitate the application of the lubricant can also be omitted and is not essential to the invention.
Durch das erfindungsgemässe Verfahren wird die Herstellung von Halbzeug aus der an sich schwer verformbaren spröden Ni/Ti/Cu-Legierung auch bei höheren Kupfergehalten in einfacher Weise ermöglicht.The method according to the invention enables the production of semi-finished products from the brittle Ni / Ti / Cu alloy, which is difficult to deform per se, even in the case of higher copper contents.
Claims (7)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH172881 | 1981-03-13 | ||
CH1728/81 | 1981-03-13 |
Publications (1)
Publication Number | Publication Date |
---|---|
EP0060575A1 true EP0060575A1 (en) | 1982-09-22 |
Family
ID=4217211
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82200172A Withdrawn EP0060575A1 (en) | 1981-03-13 | 1982-02-15 | Process for manufacturing semi-finished products from a copper-containing memory alloy |
Country Status (2)
Country | Link |
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US (1) | US4404025A (en) |
EP (1) | EP0060575A1 (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4479833A (en) * | 1981-06-26 | 1984-10-30 | Bbc Brown, Boveri & Company, Limited | Process for manufacturing a semi-finished product or a finished component from a metallic material by hot working |
US5169463A (en) * | 1987-10-19 | 1992-12-08 | Sps Technologies, Inc. | Alloys containing gamma prime phase and particles and process for forming same |
US4908069A (en) * | 1987-10-19 | 1990-03-13 | Sps Technologies, Inc. | Alloys containing gamma prime phase and process for forming same |
US5540718A (en) * | 1993-09-20 | 1996-07-30 | Bartlett; Edwin C. | Apparatus and method for anchoring sutures |
US5961538A (en) * | 1996-04-10 | 1999-10-05 | Mitek Surgical Products, Inc. | Wedge shaped suture anchor and method of implantation |
US6106642A (en) | 1998-02-19 | 2000-08-22 | Boston Scientific Limited | Process for the improved ductility of nitinol |
US6149742A (en) * | 1998-05-26 | 2000-11-21 | Lockheed Martin Corporation | Process for conditioning shape memory alloys |
US6548013B2 (en) | 2001-01-24 | 2003-04-15 | Scimed Life Systems, Inc. | Processing of particulate Ni-Ti alloy to achieve desired shape and properties |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3594239A (en) * | 1968-02-26 | 1971-07-20 | Us Navy | Method of treating unique martensitic alloys |
DE2644041A1 (en) * | 1976-08-26 | 1978-03-02 | Bbc Brown Boveri & Cie | MEMORY ALLOY |
-
1982
- 1982-02-15 EP EP82200172A patent/EP0060575A1/en not_active Withdrawn
- 1982-02-23 US US06/351,530 patent/US4404025A/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3594239A (en) * | 1968-02-26 | 1971-07-20 | Us Navy | Method of treating unique martensitic alloys |
DE2644041A1 (en) * | 1976-08-26 | 1978-03-02 | Bbc Brown Boveri & Cie | MEMORY ALLOY |
Non-Patent Citations (1)
Title |
---|
CHEMICAL ABSTRACTS, Band 91, Nr. 4, 1979, Seiten 304-305, Columbus, Ohio, USA * |
Also Published As
Publication number | Publication date |
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US4404025A (en) | 1983-09-13 |
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