EP0045985B1 - Method of manufacturing a copper-based memory alloy - Google Patents

Method of manufacturing a copper-based memory alloy Download PDF

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Publication number
EP0045985B1
EP0045985B1 EP81200691A EP81200691A EP0045985B1 EP 0045985 B1 EP0045985 B1 EP 0045985B1 EP 81200691 A EP81200691 A EP 81200691A EP 81200691 A EP81200691 A EP 81200691A EP 0045985 B1 EP0045985 B1 EP 0045985B1
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Prior art keywords
process according
powder
copper
subjected
hot
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German (de)
French (fr)
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EP0045985A1 (en
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Gernot Dr. Gessinger
Olivier Dr. Mercier
Helmut Dr. Riegger
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BBC Brown Boveri AG Switzerland
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0425—Copper-based alloys
    • 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 a copper-based memory alloy according to the preamble of claim 1.
  • Memory alloys of the ⁇ special brass type have so far mainly been produced by melt metallurgy.
  • Methods for the powder metallurgical production of such alloys have also become known (e.g. M. Follon, E. Aernoudt, Powder-metallurgizally processed shape-memory alloys, 5th European Symposium on Powder Metallurgy, Swiss 1978, pp. 275-281). These methods, which mostly work with fine to very fine powders, are generally known from powder metallurgy.
  • manufacturing processes are also known which use relatively coarse-grained powders as starting materials. This applies in particular to the powder metallurgy of titanium alloys and nickel superalloys (e.g.
  • the invention is based on the object of specifying a production method for copper-based memory alloys which combines high reproducibility with the greatest possible simplicity and economy, and is suitable for mass production and enables homogeneous, dense products in the form of semi-finished or finished products.
  • the coarse powders (grain size> 0.05 mm) can be produced by plasma spheroidization, rotating electrode method, dropletization of a melt by means of ultrasonic excitation, atomization of a melt at high speed or by any other known method.
  • the steel cylinder was provided with a lid and sealed and welded under vacuum.
  • the capsule filled with powder in this way was subjected to a hot isostatic pressing process with the following characteristics:
  • the blank After pressing, the blank was subjected to hot working by open die forging at a temperature of approx. 800 ° C. The diameter of the workpiece was essentially reduced so that a rod of 18 mm in diameter was finally available.
  • the method is in no way limited to this embodiment variant.
  • the starting powder can also consist of powders of different compositions, which together form the final alloy.
  • the grain diameter (particle size) of the powder is between 0.05 and 0.8 mm.
  • the pressure used in isostatic pressing is 50 to 300 MPa depending on the proportions and size of the workpiece to be produced, the associated pressing temperature is 750 to 950 ° C depending on the alloy and the time period is 1/2 h to 5 h.
  • the hot forming operation by forging, pressing, round hammers and rolling is carried out in the temperature range between 750 and 850 ° C.
  • a hollow cylinder made of copper or a ductile copper alloy can also be used to encapsulate the powder.
  • the powder encapsulated in the rubber tube was subjected to a cold isostatic pressing process:
  • the cold-pressed blank was encapsulated in a copper cylinder of the following dimensions after removal from the rubber hose:
  • the copper cylinder was covered with a lid and sealed and welded under vacuum.
  • the capsule sealed in this way was then subjected to a hot isostatic pressing process with the following characteristics:
  • the blank was subjected to a heat treatment, which corresponded to a homogenization anneal under the following conditions:
  • Example 1 After homogenization, the workpiece was subjected to a forging operation similar to Example 1.
  • the method is not exhausted in this embodiment variant. Any mixture of master alloys and / or elementary powder in any number (two or more types of powder) can be used as the starting powder. The only requirement is that the desired final composition is achieved by mixing the powder.
  • a suitable plastic hose for cold isostatic pressing which is carried out at pressures of 300 to 800 mPa for 1 to 10 minutes, can also be used.
  • the homogenization annealing is carried out in the temperature range from 900 to 950 ° C for 1 to 20 h.
  • Alloys of the following composition are particularly suitable as alloys for this process:
  • the powder metallurgical process according to the invention and the semi-finished and finished products produced thereafter enable the production of workpieces from a memory alloy of the Cu / Al or Cu / Al / Ni type, which have better homogeneity compared to bodies produced by melt metallurgy or by conventional powder metallurgical methods and allow economical production.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Description

Die Erfindung geht aus von einem Verfahren zur Herstellung einer Kupferbasis-Gedächtnislegierung nach der Gattung des Anspruchs 1.The invention relates to a method for producing a copper-based memory alloy according to the preamble of claim 1.

Gedächtnislegierungen des β-Sondermessingtyps wurden bisher vorwiegend schmelzmetallurgisch hergestellt. Ferner sind Verfahren zur pulvermetallurgischen Herstellung derartiger Legierungen bekannt geworden (z. B. M. Follon, E. Aernoudt, Powder-metallurgizally processed shape-memory alloys, 5th European Symposium on Powder Metallurgy, Stockholm 1978, S.275-281). Diese meist mit feinen bis sehr feinen Pulvern arbeitenden Methoden sind ganz allgemein aus der Pulvermetallurgie bekannt. Andererseits sind auch Herstellungsverfahren bekannt, welche verhältnismässig grobkörnige Pulver als Ausgangsmaterialien verwenden. Dies gilt vor allem für die Pulvermetallurgie von Titanlegierungen und von Nickelsuperlegierungen (z. B. G. H. Gessinger, Brown Boveri Research Center, « Titanium powder metallurgy and composites », Int. Titankonferenz, Kyoto, Mai 1980 ; G. H. Gessinger and M. J. Bomford, « Powder metallurgy of superalloys •, International Metallurgical Reviews 1974, Vol. 19, p. 51-76).Memory alloys of the β special brass type have so far mainly been produced by melt metallurgy. Methods for the powder metallurgical production of such alloys have also become known (e.g. M. Follon, E. Aernoudt, Powder-metallurgizally processed shape-memory alloys, 5th European Symposium on Powder Metallurgy, Stockholm 1978, pp. 275-281). These methods, which mostly work with fine to very fine powders, are generally known from powder metallurgy. On the other hand, manufacturing processes are also known which use relatively coarse-grained powders as starting materials. This applies in particular to the powder metallurgy of titanium alloys and nickel superalloys (e.g. BGH Gessinger, Brown Boveri Research Center, "Titanium powder metallurgy and composites", Int. Titan Conference, Kyoto, May 1980; GH Gessinger and MJ Bomford, "Powder metallurgy of superalloys •, International Metallurgical Reviews 1974, vol. 19, p. 51-76).

Versucht man, nach den üblichen pulvermetallurgischen Methoden, d. h. durch Mischen, Pressen, Sintern, ev. abwechslungsweises mehrmaliges Pressen und Sintern von groben Pulvern aus Kupferlegierungen Werkstücke herzustellen, so erhält man bestenfalls filterähnliche poröse Gebilde, die für Sonderzwecke bereits seit einiger Zeit im Handel sind. Es besteht daher ein Bedürfnis nach einem Verfahren, welches kompakte, dichte Erzeugnisse liefert.If one tries, according to the usual powder metallurgical methods, d. H. to produce workpieces by mixing, pressing, sintering, possibly alternately pressing and sintering coarse powders from copper alloys alternately, at best you get filter-like porous structures that have been on the market for special purposes for some time. There is therefore a need for a process that provides compact, dense products.

Der Erfindung liegt die Aufgabe zugrunde, ein Herstellungsverfahren für Kupferbasis-Gedächtnislegierungen anzugeben, welches hohe Reproduzierbarkeit mit grösstmöglicher Einfachheit und Wirtschaftlichkeit verbindet, sich für die Massenerzeugung eignet un homogene, dichte Produkte in Form von Halbzeug oder Fertigerzeugnissen ermöglicht.The invention is based on the object of specifying a production method for copper-based memory alloys which combines high reproducibility with the greatest possible simplicity and economy, and is suitable for mass production and enables homogeneous, dense products in the form of semi-finished or finished 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.

Die Erfindung wird anhand der nachfolgenden, durch Figuren erläuterten Ausführungsbeispiele beschrieben.The invention is described on the basis of the following exemplary embodiments explained by figures.

Dabei zeigt:

  • Figur 1 das Fliessbild (Blockdarstellung) der grundsätzlichen Verfahrensschritte,
  • Figur 2 das Fliessbild einer Ausführungsvariante des Verfahrens mit zusätzlichem kalt-isostatischem Pressen und Homogenisieren.
It shows:
  • FIG. 1 shows the flow diagram (block diagram) of the basic method steps,
  • FIG. 2 shows the flow diagram of an embodiment variant of the method with additional cold isostatic pressing and homogenization.

Grundsätzlich können die groben Pulver (Korngrösse > 0,05 mm) durch Plasma-Sphäroidisierung, Verfahren der rotierenden Elektrode, Zertropfen einer Schmelze mittels Ultraschallanregung, Verdüsen einer Schmelze unter hoher Geschwindigkeit oder durch jedes beliebige andere bekannte Verfahren hergestellt werden.Basically, the coarse powders (grain size> 0.05 mm) can be produced by plasma spheroidization, rotating electrode method, dropletization of a melt by means of ultrasonic excitation, atomization of a melt at high speed or by any other known method.

Ausführungsbeispiel 1Embodiment 1 Siehe Fliessbild Fig. 1See flow diagram Fig. 1

Nach dem Verfahren der rotierenden Elektrode wurde ein der endgültigen Legierung entsprechendes Grobkornpulver folgender Zusammensetzung und Partikelgrösse hergestellt :

Figure imgb0001
A coarse-grain powder of the following composition and particle size, corresponding to the final alloy, was produced using the rotating electrode method:
Figure imgb0001

1 500 g des Grobkornpulvers wurde gemischt und unter Vakuum in ein metallenes Gefäss abgefüllt. Im vorliegenden Fall bestand letzteres aus einem dünnwandigen Hohlzylinder aus rostfreiem Stahl mit den folgenden Abmessungen :

Figure imgb0002
1,500 g of the coarse-grain powder was mixed and filled into a metal vessel under vacuum. In the present case, the latter consisted of a thin-walled hollow cylinder made of stainless steel with the following dimensions:
Figure imgb0002

Der Stahlzylinder wurde mit einem Deckel versehen und unter Vakuum verschlossen und verschweisst. Die auf diese Weise mit Pulver gefüllte Kapsel wurde einem heiss-isostatischen Pressvorgang mit folgenden Kenndaten unterworfen :

Figure imgb0003
The steel cylinder was provided with a lid and sealed and welded under vacuum. The capsule filled with powder in this way was subjected to a hot isostatic pressing process with the following characteristics:
Figure imgb0003

Nach erfolgtem Pressen wurde der Rohling einer Warmverformung durch Freiformschmieden bei einer Temperatur von ca. 800 °C unterworfen. Dabei wurde im wesentlichen der Durchmesser des Werkstücks reduziert, so dass schliesslich ein Stab von 18 mm Durchmesser vorlag.After pressing, the blank was subjected to hot working by open die forging at a temperature of approx. 800 ° C. The diameter of the workpiece was essentially reduced so that a rod of 18 mm in diameter was finally available.

Das Verfahren ist keineswegs auf diese Ausführungsvariante begrenzt. Das Ausgangspulver kann auch aus Pulvern verschiedener Zusammensetzung bestehen, welche gesamthaft die Endlegierung ergeben. Der Korndurchmesser (Partikelgrösse) des Pulvers liegt zwischen 0,05 und 0,8 mm. Der beim isostatischen Pressen angewandte Druck beträgt je nach Verhältnissen und Grösse des zu erzeugenden Werkstücks 50 bis 300 MPa, die dazugehörige Presstemperatur je nach Legierung 750 bis 950 °C und die Zeitdauer 1/2 h bis 5 h. Die Warmverformungsoperation durch Schmieden, Pressen, Rundhämmern und Walzen wird im Temperaturbereich zwischen 750 und 850 °C durchgeführt. Statt eines Gefässes aus rostfreiem Stahl kann auch ein Hohlzylinder aus Kupfer oder einer duktilen Kupferlegierung zur Einkapselung des Pulvers verwendet werden.The method is in no way limited to this embodiment variant. The starting powder can also consist of powders of different compositions, which together form the final alloy. The grain diameter (particle size) of the powder is between 0.05 and 0.8 mm. The pressure used in isostatic pressing is 50 to 300 MPa depending on the proportions and size of the workpiece to be produced, the associated pressing temperature is 750 to 950 ° C depending on the alloy and the time period is 1/2 h to 5 h. The hot forming operation by forging, pressing, round hammers and rolling is carried out in the temperature range between 750 and 850 ° C. Instead of a stainless steel vessel, a hollow cylinder made of copper or a ductile copper alloy can also be used to encapsulate the powder.

Ausführungsbeispiel IIEmbodiment II Siehe Fliessbild Fig. 2See flow diagram Fig. 2

Nach dem Verfahren der rotierenden Elektrode wurden 2 grobkörnige Vorlegierungspulver der nachfolgenden Zusammensetzung und Partikelgrösse hergestellt :

Figure imgb0004
Figure imgb0005
 Two coarse-grained pre-alloy powders with the following composition and particle size were produced using the rotating electrode method:
Figure imgb0004
Figure imgb0005

Je 500 g der beiden Pulver wurden gemischt und von der Mischung 800 g unter Vakuum in einen Gummischlauch von 88 mm Innendurchmesser und 110 mm Länge abgefüllt. Die Pulvermischung entsprach somit einer Legierung folgender Endzusammensetzung :

Figure imgb0006
500 g each of the two powders were mixed and 800 g of the mixture were filled under vacuum into a rubber tube with an inside diameter of 88 mm and a length of 110 mm. The powder mixture thus corresponded to an alloy with the following final composition:
Figure imgb0006

Das im Gummischlauch eingekapselte Pulver wurde einem kaltisostatischen Pressvorgang unterworfen :

Figure imgb0007
The powder encapsulated in the rubber tube was subjected to a cold isostatic pressing process:
Figure imgb0007

Der kalt vorgepresste Rohling wurde nach Entnahme aus dem Gummischlauch in einen Kupferzylinder folgender Abmessungen eingekapselt :

Figure imgb0008
The cold-pressed blank was encapsulated in a copper cylinder of the following dimensions after removal from the rubber hose:
Figure imgb0008

Der Kupferzylinder wurde mit einem Deckel versehen und unter Vakuum verschlossen und verschweisst. Hierauf wurde die auf diese Weise abgeschlossene Kapsel einem heissisostatischen Pressvorgang mit folgenden Kenndaten unterworfen :

Figure imgb0009
The copper cylinder was covered with a lid and sealed and welded under vacuum. The capsule sealed in this way was then subjected to a hot isostatic pressing process with the following characteristics:
Figure imgb0009

Nach dem Pressen wurde der Rohling einer Warmbehandlung unterworfen, welche in einer Homogenisierungsglühung unter folgenden Bedingungen entsprach :

Figure imgb0010
After pressing, the blank was subjected to a heat treatment, which corresponded to a homogenization anneal under the following conditions:
Figure imgb0010

Nach erfolgter Homogenisierung wurde das Werkstück einer Schmiedeoperation ähnlich Beispiel 1 unterworfen.After homogenization, the workpiece was subjected to a forging operation similar to Example 1.

Das Verfahren erschöpft sich nicht in dieser Ausführungsvariante. Als Ausgangspulver können beliebige Mischungen von Vorlegierungen und/oder Elementarpulver in beliebiger Anzahl (zwei oder mehr Pulverarten) Verwendung finden. Bedingung ist lediglich, dass durch das Mischen des Pulvers die gewünschte Endzusammensetzung erzielt wird.The method is not exhausted in this embodiment variant. Any mixture of master alloys and / or elementary powder in any number (two or more types of powder) can be used as the starting powder. The only requirement is that the desired final composition is achieved by mixing the powder.

Statt eines Gummischlauches kann auch ein geeigneter Kunststoffschlauch zum kalt-isostatischen Pressen, welches bei Drücken von 300 bis 800 mPa während 1 bis 10 min durchgeführt wird, verwendet werden. Die Homogenisierungsglühung wird im Temperaturbereich von 900 bis 950 °C während 1 bis 20 h durchgefürt.Instead of a rubber hose, a suitable plastic hose for cold isostatic pressing, which is carried out at pressures of 300 to 800 mPa for 1 to 10 minutes, can also be used. The homogenization annealing is carried out in the temperature range from 900 to 950 ° C for 1 to 20 h.

Als Legierungen für dieses Verfahren eignen sich insbesondere solche der nachfolgenden Zusammensetzung :

Figure imgb0011
Alloys of the following composition are particularly suitable as alloys for this process:
Figure imgb0011

Durch das erfindungsgemässe pulvermetallurgische Verfahren sowie die danach erzeugten Halbfabrikate und Fertigerzeugnisse wird die Herstellung von Werkstücken aus einer Gedächtnislegierung des Cu/AI- oder Cu/AI/Ni-Typs ermöglicht, welche gegenüber schmelzmetallurgisch oder nach herkömmlichen pulvermetallurgischen Methoden hergestellten Körpern eine bessere Homogenität aufweisen und eine wirtschaftliche Fertigung erlauben.The powder metallurgical process according to the invention and the semi-finished and finished products produced thereafter enable the production of workpieces from a memory alloy of the Cu / Al or Cu / Al / Ni type, which have better homogeneity compared to bodies produced by melt metallurgy or by conventional powder metallurgical methods and allow economical production.

Claims (7)

1. Process for manufacturing a copper-based memory alloy by a powder-metallurgical route, characterised in that a coarse-grained alloy powder is used as the starting material, this powder having a particle size, expressed in terms of particle diameter, of 0.05 to 0.8 mm, in that the alloy powder, after being mixed, is introduced into a vessel, is vacuum-sealed, and is subjected to hot isostatic pressing for a period ranging from half an hour to 5 hours, at a pressure of 50 to 300 Mpa, and at a temperature of 750 to 950 °C, and in that the resulting compact is then subjected to a hot-working operation, at a temperature of 750 to 850 °C, carried out by forging, extrusion, swaging, or rolling.
2. Process according to Claim 1, characterised in that an alloy powder having a composition corresponding to the final composition of the memory alloy is used as the starting material.
3. Process according to Claim 1, characterised in that two or more prealloyed powders are used as the starting material.
4. Process according to Claim 1, characterised in that stainless steel or copper is used as the material for the casing which forms the vessel, this casing being sealed by welding, vacuum-thightness being ensured.
5. Process according to Claim 1, characterised in that the alloy powder is initially introduced, under vacuum, into a flexible tube, made of rubber or plastic,- and is then isostatically pressed for 1 to 10 minutes, at a pressure of 300 to 800 Mpa, at ambient temperature, and the compact, thus obtained, is encased in a copper cylinder prior to being subjected to hot-isostatic pressing.
6. Process according to Claim 1, characterised in that, following hot isostatic pressing, and prior to the hot-working operation, the compact is subjected to a homogenising annealing treatment for a period ranging from 1 to 20 hours, this annealing treatment being carried out under a protective gas atmosphere at a temperature of 900 to 950 °C.
7. Process according to Claim 1, characterised in that the alloy powder which is used as the starting material is such as to correspond to a memory alloy having the following final composition : 10.5 to 15 % by weight of aluminium and 0 to 6 % by weight of nickel, the balance being copper.
EP81200691A 1980-08-07 1981-06-19 Method of manufacturing a copper-based memory alloy Expired EP0045985B1 (en)

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CH5986/80 1980-08-07

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Cited By (1)

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CN103028729A (en) * 2011-09-29 2013-04-10 河南省大地合金股份有限公司 Method of producing rigid alloy super thin rod with diameter less than 0.6mm

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CH664515A5 (en) * 1984-12-20 1988-03-15 Bbc Brown Boveri & Cie Powder metallurgical prodn. of shape memory article - of beta brass type copper alloy contg. metal oxide dispersoid
US4602952A (en) * 1985-04-23 1986-07-29 Cameron Iron Works, Inc. Process for making a composite powder metallurgical billet
DE3530741C1 (en) * 1985-08-28 1993-01-14 Avesta Nyby Powder AB, Torshälla Process for the manufacture of powder metallurgical objects
US6089781A (en) * 1998-08-12 2000-07-18 Hughes Electronics Corporation Structure utilizing a shape-memory alloy fastener
US6526648B1 (en) 2001-07-27 2003-03-04 Raytheon Company Positioning of an optical device using a non-force-applying external agent
DE102007047523B3 (en) 2007-10-04 2009-01-22 Forschungszentrum Jülich GmbH Process for the production of semi-finished products from NiTi shape memory alloys
US20130280120A1 (en) * 2010-04-23 2013-10-24 United States Department Of Energy Hard and Super-hard Metal Alloys and Methods for Making the Same
CN114807652B (en) * 2021-12-24 2022-10-04 昆明冶金研究院有限公司北京分公司 Preparation method of powder metallurgy composite material for art

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US3775101A (en) * 1970-04-20 1973-11-27 Nasa Method of forming articles of manufacture from superalloy powders
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Publication number Priority date Publication date Assignee Title
CN103028729A (en) * 2011-09-29 2013-04-10 河南省大地合金股份有限公司 Method of producing rigid alloy super thin rod with diameter less than 0.6mm
CN103028729B (en) * 2011-09-29 2015-05-13 河南省大地合金股份有限公司 Method of producing rigid alloy super thin rod with diameter less than 0.6mm

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