EP0290820A2 - Process for preparing dispersion-hardened metal alloys - Google Patents

Process for preparing dispersion-hardened metal alloys Download PDF

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Publication number
EP0290820A2
EP0290820A2 EP88106164A EP88106164A EP0290820A2 EP 0290820 A2 EP0290820 A2 EP 0290820A2 EP 88106164 A EP88106164 A EP 88106164A EP 88106164 A EP88106164 A EP 88106164A EP 0290820 A2 EP0290820 A2 EP 0290820A2
Authority
EP
European Patent Office
Prior art keywords
solution
metal
salts
particles
metals
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.)
Granted
Application number
EP88106164A
Other languages
German (de)
French (fr)
Other versions
EP0290820B1 (en
EP0290820A3 (en
Inventor
Werner Dr. Ing. Hüther
Wolfgang Dr. Ing. Betz
Gerhard Andrees
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MTU Aero Engines GmbH
Original Assignee
MTU Motoren und Turbinen Union Muenchen GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE19873715979 external-priority patent/DE3715979A1/en
Application filed by MTU Motoren und Turbinen Union Muenchen GmbH filed Critical MTU Motoren und Turbinen Union Muenchen GmbH
Publication of EP0290820A2 publication Critical patent/EP0290820A2/en
Publication of EP0290820A3 publication Critical patent/EP0290820A3/en
Application granted granted Critical
Publication of EP0290820B1 publication Critical patent/EP0290820B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • Y10S75/00—Specialized metallurgical processes, compositions for use therein, consolidated metal powder compositions, and loose metal particulate mixtures
    • Y10S75/956—Producing particles containing a dispersed phase

Definitions

  • the invention relates to a method for producing dispersion-hardened metal alloys, in particular for components of complex shape that are resistant to high temperatures, particles of a second phase being incorporated into a metallic matrix with the aid of a colloidal suspension, wherein the metallic components are initially in the form of a salt solution, the solution is mixed with the particles of the second phase that do not react with the metallic components and their salt solution, optionally a deglomaration agent is added, the solution is atomized and after removal of the solvent, there is a reduction to metal, according to patent (patent application P3540255.5).
  • Metal alloys especially superalloys for high-temperature-resistant components in a complicated form, such as turbine blades or similarly complicated shaped bodies, often contain highly reactive elements, such as titanium, chromium, aluminum and the like.
  • highly reactive elements such as titanium, chromium, aluminum and the like.
  • mixed oxides can be formed already during removal of the solvent or the water of crystallization due to the reactive elements, which can not or only very difficultly be reduced to metal.
  • the object of the invention is to improve the method according to the main patent (patent application P35 40 255.5) so that the target alloys can be produced as metal powder almost as desired, although they contain highly reactive elements.
  • the invention is concerned with a method for producing dispersion-hardened metal alloys for high-temperature-resistant components of complicated shape, particles of a second phase being incorporated into a metallic matrix with the aid of a colloidal suspension.
  • the invention improves the method according to the main patent and extends its field of application significantly.
  • non-reactive, in particular oxidic, dispersions can be introduced into the suspension as a second phase in the form of particles.
  • a heat treatment in the temperature time program before or after compacting the powder allows the metal of the particles to be evenly diffused into the matrix, even if they are oxidized on the surface.
  • the examples given in the main patent also apply here.
  • Alloys can thus be processed to metal powder, which also contain the reactive elements mentioned.
  • Metal salts or mixtures of salts of reducible metals are used as starting materials for the solution.
  • a suspension of fine powder particles of the highly reactive elements or suitable master alloys from these elements is thus produced by slurrying, optionally with deglomerating agent. When atomizing, drying and reducing this mixture, at most a thin surface layer of this metal powder is oxidized. The remaining metallic residue can be distributed evenly in the metallic matrix to the desired extent by diffusion treatment before or after compacting the powder.
  • powders and sintered moldings can be produced therefrom, which additionally contain a uniform distribution of the finest oxidic particles. The particle size and distribution then depend on the sintering conditions of the shaped body. This results in optimally composed superalloys with different disperse populations to reinforce the matrix.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

To produce dispersion-hardened metal alloys with incorporation of not easily reducible particles into a metallic matrix in a second phase, the metallic constituents are initially present as a salt solution, and metal salts or mixtures of such salts are used as starting materials.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung dipersionsgehär­teter Metallegierungen, insbesondere für hochtemperaturfeste Bauteile komplizierter Form, wobei Partikel einer zweiten Phase in eine metal­lische Matrix mit Hilfe einer kolloidalen Suspension eingebaut werden, wobei
die metallischen Bestandteile zunächst als Salzlösung vorliegen,
der Lösung die Partikel der zweiten Phase zugemischt werden, die mit den metallischen Bestandteilen und deren Salzlösung nicht reagieren,
gegebenenfalls ein Deglomarationsmittel zugegeben wird,
die Lösung verdüst wird und
nach Entfernen des Lösungsmittels eine Reduktion zu Metall erfolgt,
nach Patent (Patentanmeldung P3540255.5).The invention relates to a method for producing dispersion-hardened metal alloys, in particular for components of complex shape that are resistant to high temperatures, particles of a second phase being incorporated into a metallic matrix with the aid of a colloidal suspension, wherein
the metallic components are initially in the form of a salt solution,
the solution is mixed with the particles of the second phase that do not react with the metallic components and their salt solution,
optionally a deglomaration agent is added,
the solution is atomized and
after removal of the solvent, there is a reduction to metal,
according to patent (patent application P3540255.5).

Metallegierungen, insbesondere Superlegierungen für hochtemperaturfeste Bauteile in komplizierter Form, wie Turbinenschaufeln oder ähnlich komplizierte Förmkorper, enthalten häufig stark reaktive Elemente, wie Titan, Chrom, Aluminium und ähnliche. Bei der Umwandlung solcher Metallegierungen in Metallpulver, gemäß Anspruch 1 des Hauptpatentes können bereits beim Entfernen des Lösungsmittels bzw. des Kristallwas­sers wegen der reaktiven Elemente Mischoxide entstehen, die nicht oder nur sehr schwer zu Metall reduziert werden können.Metal alloys, especially superalloys for high-temperature-resistant components in a complicated form, such as turbine blades or similarly complicated shaped bodies, often contain highly reactive elements, such as titanium, chromium, aluminum and the like. In the conversion of such metal alloys into metal powder, mixed oxides can be formed already during removal of the solvent or the water of crystallization due to the reactive elements, which can not or only very difficultly be reduced to metal.

Aufgabe der Erfindung ist es, das Verfahren nach dem Hauptpatent (Patentanmeldung P35 40 255.5) so zu verbessern, daß die Ziellegierun­gen nahezu beliebig als Metallpulver hergestellt werden können, obwohl sie stark reaktive Elemente enthalten.The object of the invention is to improve the method according to the main patent (patent application P35 40 255.5) so that the target alloys can be produced as metal powder almost as desired, although they contain highly reactive elements.

Die Lösung der Erfindung ist in Anspruch 1 enthalten. Insbesondere befaßt sich die Erfindung mit einem Verfahren zur Herstellung disper­sionsgehärteter Metallegierungen für hochtemperaturfeste Bauteile komplizierter Form, wobei Partikel einer 2. Phase in eine metallische Matrix mit Hilfe einer kolloidalen Suspension eingebaut werden.The solution of the invention is contained in claim 1. In particular, the invention is concerned with a method for producing dispersion-hardened metal alloys for high-temperature-resistant components of complicated shape, particles of a second phase being incorporated into a metallic matrix with the aid of a colloidal suspension.

Die Erfindung verbessert das Verfahren nach dem Hauptpatent und erwei­tert seinen Anwendungsbereich ganz wesentlich.The invention improves the method according to the main patent and extends its field of application significantly.

Weitere Vorteile der Erfindung sind in Unteransprüchen und der Be­schreibung von Ausführungsbeispielen zu entnehmen.Further advantages of the invention can be found in the subclaims and the description of exemplary embodiments.

Weiterhin können erfindungsgemäß zusätzlich zu den metallischen Parti­keln nicht reaktive, insbesondere oxidische Dispersate als zweite Phase in Form von Partikeln in die Suspension eingebracht werden.Furthermore, according to the invention, in addition to the metallic particles, non-reactive, in particular oxidic, dispersions can be introduced into the suspension as a second phase in the form of particles.

Der Effekt einer gegebenenfalls vorgesehenen Dispersionshärtung nach dem Stand der Technik kann hierdurch wesentlich gesteigert werden. Dies ist besonders vorteilhaft, wenn man Kornwachstum, insbesondere beim Sintern, verhindern will und die Ausbildung enger Subkorngrenzen in den Formkörpern bei hoher Belastung, insbesondere bei Wärmedehnung (Krie­chen) einhalten will.The effect of a possibly provided dispersion hardening according to the prior art can hereby be increased considerably. This is particularly advantageous if you want to prevent grain growth, especially during sintering, and if you want to maintain the formation of narrow sub-grain boundaries in the moldings under high loads, in particular with thermal expansion (creep).

Durch eine Wärmebehandlung im Temperaturzeitprogramm vor oder nach dem Kompaktieren des Pulvers kann das Metall der Partikel, auch wenn sie oberflächlich oxidiert sind, in die Matrix gleichmässig eindiffundiert werden. Die im Hauptpatent angegebenen Beispiele gelten auch hier.A heat treatment in the temperature time program before or after compacting the powder allows the metal of the particles to be evenly diffused into the matrix, even if they are oxidized on the surface. The examples given in the main patent also apply here.

Somit können Legierungen zu Metallpulver verarbeitet werden, die auch die genannten reaktiven Elemente enthalten. Als Ausgangsstoffe der Lö­sung verwendet man Metallsalze oder Gemische von Salzen von reduzierba­ren Metallen. Damit wird eine Suspension feiner Pulverteilchen der stark reaktiven Elemente oder geeigneter Vorlegierungen aus diesen Ele­menten durch Aufschlämmen, gegebenenfalls mit Deglomerationsmittel er­zeugt. Beim Verdüsen, Trocknen und Reduzieren dieser Mischung wird dann hochstens eine dünne Oberflächenschicht dieser Metallpulver oxidiert. Der verbleibende metallische Rest kann durch Diffussionsbehandlung vor oder nach dem Kompaktieren des Pulvers in gewünschtem Maße gleichmäßig in der metallischen Matrix verteilt werden. Verwendet man eine Mischung von Salzlösungen aus reaktiven und nichtreaktiven Metallen, können Pul­ver und Sinter-Formkörper hieraus erzeugt werden, welche zusätzlich eine gleichmäßige Verteilung feinster oxidischer Partikel enthalten. Die Partikelgröße und -verteilung hängt dann von den Sinterbedingungen des Formkörpers ab. Damit erhält man optimal zusammengesetzte Superle­gierungen, mit unterschiedlichen Dispersat-Populationen zur Verstärkung der Matrix.Alloys can thus be processed to metal powder, which also contain the reactive elements mentioned. Metal salts or mixtures of salts of reducible metals are used as starting materials for the solution. A suspension of fine powder particles of the highly reactive elements or suitable master alloys from these elements is thus produced by slurrying, optionally with deglomerating agent. When atomizing, drying and reducing this mixture, at most a thin surface layer of this metal powder is oxidized. The remaining metallic residue can be distributed evenly in the metallic matrix to the desired extent by diffusion treatment before or after compacting the powder. If a mixture of salt solutions of reactive and non-reactive metals is used, powders and sintered moldings can be produced therefrom, which additionally contain a uniform distribution of the finest oxidic particles. The particle size and distribution then depend on the sintering conditions of the shaped body. This results in optimally composed superalloys with different disperse populations to reinforce the matrix.

Abwandlungen der gegebenen Ausführungsbeispiele können selbstverständ­lich vorgenommen werden, ohne hierdurch den Rahmen der Erfindung zu ver­lassen. Beispielsweise kann anstelle der kolloidalen Suspension auch eine nichtkolloidale Partikelverteilung in der Lösung als Suspension eingesetzt werden.Modifications of the given exemplary embodiments can of course be carried out without thereby leaving the scope of the invention. For example, instead of the colloidal suspension, a non-colloidal particle distribution in the solution can also be used as a suspension.

Claims (5)

1. Verfahren zur Herstellung dispersionsgehärteter Metallegierungen, insbesondere für hochtemperaturfeste Bauteile komplizierter Form, wobei Partikel einer zweiten Phase in eine metallische Matrix mit Hilfe einer kolloidalen Suspension eingebaut werden, wobei die metallischen Bestandteile zunächst als Salzlösung vorliegen,
der Lösung die Partikel der zweiten Phase zugemischt werden, die mit den metallischen Bestandteilen und deren Salzlösung nicht re­agiert,
ein Deglomerationsmittel zugegeben wird,
die Lösung verdüst wird und
nach Entfernen des Lösungsmittels eine Reduktion zu Metall erfolgt,
nach Patent (Patentanmeldung P 35 40 255.5).
dadurch gekennzeichnet, daß als Ausgangsstoffe Metallsalze oder Gemische von Salzen reduzierbarer Metalle eingesetzt werden und der Lösung Metallpulverteilchen als zweite Phase zugemischt werden, aus Metallen oder ihren Legierungen, die nicht ohne weiteres einem Reduktionsverfahren unterzogen werden können.1. A process for the preparation of dispersion-hardened metal alloys, in particular for components of complex shape which are resistant to high temperatures, particles of a second phase being incorporated into a metallic matrix with the aid of a colloidal suspension, the metallic constituents first being present as a salt solution,
particles of the second phase are added to the solution, which do not react with the metallic components and their salt solution,
a deglomering agent is added,
the solution is atomized and
after removal of the solvent, there is a reduction to metal,
according to patent (patent application P 35 40 255.5).
characterized in that metal salts or mixtures of salts of reducible metals are used as starting materials and Metal powder particles are mixed into the solution as a second phase, made of metals or their alloys, which cannot easily be subjected to a reduction process. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß zusätzlich zu den Pulverteilchen, nicht reaktive, insbesondere oxidische Dispersate in die Lösung eingebracht werden.2. The method according to claim 1, characterized in that in addition to the powder particles, non-reactive, in particular oxidic dispersions are introduced into the solution. 3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Lösung auch Salze von reaktiven Metallen beigefügt werden, die bei der Trocknung und Reduktionsbehandlung Metalloxide bilden.3. The method according to claim 1 or 2, characterized in that the solution also salts of reactive metals are added, which form metal oxides during the drying and reduction treatment. 4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß der Lösung Salze von Metallen, wie Titan, Chrom, Aluminium und ähnlich reak­tive Elemente zugesetzt werden.4. The method according to claim 3, characterized in that salts of metals such as titanium, chromium, aluminum and similar reactive elements are added to the solution. 5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekenn­zeichnet, daß das Metallpulver einschließlich etwa oberflächlich oxidierten Metallpulverteilchen durch eine Diffusionswärmebehand­lung vor oder nach dem Kompaktieren des Pulvers gleichmäßig in der metallischen Matrix verteilt wird.5. The method according to any one of the preceding claims, characterized in that the metal powder including approximately superficially oxidized metal powder particles by a diffusion heat treatment before or after compacting the powder is evenly distributed in the metallic matrix.
EP88106164A 1987-05-13 1988-04-19 Process for preparing dispersion-hardened metal alloys Expired - Lifetime EP0290820B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19873715979 DE3715979A1 (en) 1985-11-13 1987-05-13 Process for producing dispersion-hardened metal alloys
DE3715979 1987-05-13

Publications (3)

Publication Number Publication Date
EP0290820A2 true EP0290820A2 (en) 1988-11-17
EP0290820A3 EP0290820A3 (en) 1990-03-21
EP0290820B1 EP0290820B1 (en) 1994-03-16

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EP (1) EP0290820B1 (en)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2009062610A1 (en) 2007-11-12 2009-05-22 Ika-Werke Gmbh & Co. Kg Rotor-stator-device for dispersing or homogenising

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AT391435B (en) * 1988-04-14 1990-10-10 Plansee Metallwerk METHOD FOR PRODUCING AN ODSS ALLOY
US5380482A (en) * 1991-10-18 1995-01-10 Aspen Research, Inc. Method of manufacturing ingots for use in making objects having high heat, thermal shock, corrosion and wear resistance
US6338809B1 (en) * 1997-02-24 2002-01-15 Superior Micropowders Llc Aerosol method and apparatus, particulate products, and electronic devices made therefrom
US6428823B1 (en) * 2001-03-28 2002-08-06 Council Of Scientific & Industrial Research Biologically active aqueous fraction of an extract obtained from a mangrove plant Salvadora persica L
US7419528B2 (en) * 2003-02-19 2008-09-02 General Electric Company Method for fabricating a superalloy article without any melting
US7410610B2 (en) * 2002-06-14 2008-08-12 General Electric Company Method for producing a titanium metallic composition having titanium boride particles dispersed therein
US6737017B2 (en) * 2002-06-14 2004-05-18 General Electric Company Method for preparing metallic alloy articles without melting
US7416697B2 (en) * 2002-06-14 2008-08-26 General Electric Company Method for preparing a metallic article having an other additive constituent, without any melting
US7329381B2 (en) * 2002-06-14 2008-02-12 General Electric Company Method for fabricating a metallic article without any melting
US6926754B2 (en) * 2003-06-12 2005-08-09 General Electric Company Method for preparing metallic superalloy articles having thermophysically melt incompatible alloying elements, without melting
US7531021B2 (en) * 2004-11-12 2009-05-12 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US7833472B2 (en) 2005-06-01 2010-11-16 General Electric Company Article prepared by depositing an alloying element on powder particles, and making the article from the particles
US20070141374A1 (en) * 2005-12-19 2007-06-21 General Electric Company Environmentally resistant disk

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GB737398A (en) * 1952-10-24 1955-09-28 Gen Electric Co Ltd Improvements in or relating to the manufacture of alloys
GB917005A (en) * 1960-09-01 1963-01-30 Gen Electric Co Ltd Improvements in or relating to the manufacture of sintered metallic bodies
US3192042A (en) * 1961-08-01 1965-06-29 Gen Electric Method of forming a cermet
US3310400A (en) * 1962-01-31 1967-03-21 Du Pont Process of making metal powder compositions wherein some metal grains contain dispersed refractory metal oxide particles
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GB737398A (en) * 1952-10-24 1955-09-28 Gen Electric Co Ltd Improvements in or relating to the manufacture of alloys
GB917005A (en) * 1960-09-01 1963-01-30 Gen Electric Co Ltd Improvements in or relating to the manufacture of sintered metallic bodies
US3192042A (en) * 1961-08-01 1965-06-29 Gen Electric Method of forming a cermet
US3310400A (en) * 1962-01-31 1967-03-21 Du Pont Process of making metal powder compositions wherein some metal grains contain dispersed refractory metal oxide particles
US3415640A (en) * 1966-10-28 1968-12-10 Fansteel Metallurgical Corp Process for making dispersions of particulate oxides in metals

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009062610A1 (en) 2007-11-12 2009-05-22 Ika-Werke Gmbh & Co. Kg Rotor-stator-device for dispersing or homogenising

Also Published As

Publication number Publication date
US4894086A (en) 1990-01-16
EP0290820B1 (en) 1994-03-16
EP0290820A3 (en) 1990-03-21

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