EP0693564A1 - Process for preparing articles composed of intermetallic phases from pulverulent ductile components - Google Patents
Process for preparing articles composed of intermetallic phases from pulverulent ductile components Download PDFInfo
- Publication number
- EP0693564A1 EP0693564A1 EP95110967A EP95110967A EP0693564A1 EP 0693564 A1 EP0693564 A1 EP 0693564A1 EP 95110967 A EP95110967 A EP 95110967A EP 95110967 A EP95110967 A EP 95110967A EP 0693564 A1 EP0693564 A1 EP 0693564A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- pressing
- intermetallic phases
- ratio
- extrusion
- pulverulent
- 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
Links
Classifications
-
- 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
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
-
- 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
- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
Definitions
- the invention relates to a method for producing bodies from intermetallic phases from powdery, ductile components, which are mixed in a predetermined mixing ratio, subsequently compacted, then extruded to form the body and finally heat-treated.
- a method of this type is known (DE-PS 38 22 686).
- the material produced using the known method has a homogeneous structure and is significantly tougher than known materials of the same type. Any known reproducibility of alloys is also possible with the known method, ie they can be produced in any quantity with the same predetermined properties.
- the heat treatment step following the extrusion step is required to react the unreacted ductile components to form the desired intermetallic phases.
- the object is achieved according to the invention in that the heat required for the heat treatment is the heat generated in the course of the extrusion.
- the advantage of the method according to the invention consists essentially in that the manufacturing time and thus the manufacturing costs can be reduced by eliminating a previously necessary heat treatment step, at the same time advantageously achieving that the porosity and / or the homogeneity of the body produced in this way is reduced or improved can be.
- the pressing parameters during the extrusion process are selected such that the body temperature during the pressing reaches the phase formation temperature or only slightly exceeds it. If the compacting were to take place above the temperature at which the components react with one another during the pressing to form the intermetallic phases, the extrusion could be used as a compacting method if necessary, the advantage of the ductility of the element powders can be canceled. If brittle intermetallic phases are formed during extrusion, the forming process is unsteady due to their poor plasticity, which could result in large porosity and surface defects in the body.
- the powdery, ductile components that are elemental or pre-alloyed may be present, mixed in a predetermined mixing ratio.
- a typical alloy can consist of Ti48Al2Cr (in at%), for example.
- the 2 at.% Cr was mixed in to ensure their homogeneous distribution in the Ti48Al2Cr as pre-alloy powder Al-15 wt.% Cr according to the stoichiometric alloy composition.
- the subsequent precompacting of this powder mixture into a body for example into a transportable press bolt, is carried out by cold isostatic pressing (CIP). With a pressure of 450 Nmm ⁇ 2 93.8% of the theoretically calculated material density could be achieved.
- the precompacted bodies are encapsulated in AlMgSiO, 5 pipes before extrusion.
- the extrusion is then carried out, the heat required for the heat treatment being the heat generated in the course of the extrusion.
- the pressing conditions such as pin / pick-up temperature T B / A , the pressing ratio R and the punch speed v St are selected such that the temperature increase in the press strand produced by the deformation is sufficient to trigger an in-situ reaction after the pressing process, and that, on the other hand, the strand temperature during the forming process must not exceed the phase formation temperature to such an extent that the phase reaction proceeds faster than the pressing process.
- extrusion ratio must therefore be further increased and the body structure refined more by extruding extruded strands again (double extrusion).
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von Körpern aus intermetallischen Phasen aus pulverförmigen, duktilen Komponenten, die in einem vorbestimmten Mischungsverhältnis gemischt, nachfolgend kompaktiert, anschließend zur Bildung des Körpers stranggepreßt werden und schließlich wärmebehandelt werden.The invention relates to a method for producing bodies from intermetallic phases from powdery, ductile components, which are mixed in a predetermined mixing ratio, subsequently compacted, then extruded to form the body and finally heat-treated.
Ein Verfahren dieser Art ist bekannt (DE-PS 38 22 686). Der mit dem bekannten Verfahren hergestellte Werkstoff weist eine homogene Struktur auf und ist gegenüber bekannten Werkstoffen gleicher Art deutlich zäher. Auch ist mit dem bekannten Verfahren eine beliebige Reproduzierbarkeit von Legierungen möglich, d.h. diese sind in beliebigen Mengen mit fortwährend gleichen vorbestimmten Eigenschaften herstellbar.A method of this type is known (DE-PS 38 22 686). The material produced using the known method has a homogeneous structure and is significantly tougher than known materials of the same type. Any known reproducibility of alloys is also possible with the known method, ie they can be produced in any quantity with the same predetermined properties.
Der Wärmebehandlungsschritt, der dem Strangpreßschritt folgt, ist erforderlich, um die unreagierten duktilen Komponenten zur Bildung der gewünschten intermetallischen Phasen reagieren zu lassen.The heat treatment step following the extrusion step is required to react the unreacted ductile components to form the desired intermetallic phases.
Es ist Aufgabe der vorliegenden Erfindung, ein Verfahren zu schaffen, mit dem die Herstellung von Körpern aus intermetallischen Phasen der eingangs genannten Art erleichtert sowie schneller und kostengünstiger durchgeführt werden kann, wobei auch die Eigenschaften der derart hergestellten Körper in bezug auf Porosität und Homogenität des Werkstoffs verbessert werden sollen.It is an object of the present invention to provide a method with which the production of bodies from intermetallic phases of the type mentioned in the introduction can be carried out more easily and more quickly and cost-effectively, the properties of the bodies produced in this way also with respect to porosity and homogeneity of the material should be improved.
Gelöst wird die Aufgabe gemäß der Erfindung dadurch, daß die für die Wärmebehandlung nötige Wärme die im Zuge der Strangpressung erzeugte Wärme ist.The object is achieved according to the invention in that the heat required for the heat treatment is the heat generated in the course of the extrusion.
Der Vorteil des erfindungsgemäßen Verfahrens besteht im wesentlichen darin, daß die Herstellungszeit und damit die Herstellungskosten durch Wegfall eines bisher gesondert nötigen Wärmebehandlungsschrittes gesenkt werden können, wobei gleichzeitig vorteilhafterweise erreicht wird, daß die Porosität und/oder die Homogenität des derart hergestellten Körpers verringert bzw. verbessert werden kann.The advantage of the method according to the invention consists essentially in that the manufacturing time and thus the manufacturing costs can be reduced by eliminating a previously necessary heat treatment step, at the same time advantageously achieving that the porosity and / or the homogeneity of the body produced in this way is reduced or improved can be.
Bei einer vorteilhaften Ausführungsform der Erfindung sind die Preßparameter beim Strangpreßvorgang derart gewählt, daß die Körpertemperatur während der Pressung die Phasenbildungstemperatur erreicht oder lediglich geringfügig überschreitet. Würde das Kompaktieren oberhalb der Temperatur, bei der die Komponenten während des Pressens zur Bildung der intermetallischen Phasen miteinander reagieren, erfolgen, könnte bei der Anwendung des Strangpressens als Kompaktierungsverfahren gegebenenfalls der Vorteil der Duktilität der Elementpulver aufgehoben werden. Kommt es nämlich während des Strangpressens zur Bildung spröder intermetallischer Phasen, dann verläuft der Umformprozeß, bedingt durch deren schlechte Bildsamkeit, instationär, was gegebenenfalls eine große Porosität und Oberflächenfehler des Körpers zur Folge haben könnte. Durch die Wahl geeigneter Preßparameter wie Bolzen-/Aufnehmertemperatur TB/A, Preßverhältnis R, Stempelgeschwindigkeit vSt wird es ermöglicht, daß die vor allem durch innere Werkstoffverschiebungen hervorgerufene Temperaturerhöhung im Preßstrang die Bildungstemperatur intermetallischer Phasen gerade erreicht bzw. nur geringfügig überschreitet, so daß dann die Duktilität der Pulverkomponenten beim Kompaktieren voll ausgenutzt werden kann, weil dadurch sichergestellt ist, daß die Phasenumwandlung erst unmittelbar nach dem Umformvorgang einsetzt.In an advantageous embodiment of the invention, the pressing parameters during the extrusion process are selected such that the body temperature during the pressing reaches the phase formation temperature or only slightly exceeds it. If the compacting were to take place above the temperature at which the components react with one another during the pressing to form the intermetallic phases, the extrusion could be used as a compacting method if necessary, the advantage of the ductility of the element powders can be canceled. If brittle intermetallic phases are formed during extrusion, the forming process is unsteady due to their poor plasticity, which could result in large porosity and surface defects in the body. The choice of suitable pressing parameters such as pin / receiver temperature T B / A , pressing ratio R, punch speed v St makes it possible for the temperature increase in the press strand, which is primarily caused by internal material displacements, to just reach or only slightly exceed the formation temperature of intermetallic phases, so that then the ductility of the powder components can be fully utilized when compacting, because this ensures that the phase change only begins immediately after the forming process.
Schließlich kann es vorteilhaft sein, daß vor dem Preßschritt, bei dem es zur Phasenbildung kommt, mindestens ein Preßschritt ohne Phasenbildung vorgeschaltet wird. Hierdurch ist es möglich, die Porosität des hergestellten Körpers gezielt zu verringern.Finally, it can be advantageous that before the pressing step, in which phase formation occurs, at least one pressing step without phase formation is connected upstream. This makes it possible to specifically reduce the porosity of the body produced.
Auch kann es schließlich vorteilhaft sein, das Preßverhältnis bei der weiteren Pressung gegenüber dem Preßverhältnis der ersten Pressung zu erhöhen, wobei durch die Erhöhung des Preßverhältnisses die Partikelgröße der Komponenten im Körper verringert und damit auch aus diesem Grunde Einfluß auf eine geringe Porosität im Körper genommen werden kann.Finally, it may also be advantageous to increase the pressing ratio in the further pressing compared to the pressing ratio of the first pressing, the particle size of the components in the body being reduced by the increasing pressing ratio and thus also influencing a low porosity in the body for this reason can.
Das Verfahren wird nun anhand der einzelnen Verfahrensschritte gemäß einer typischen Ausgestaltung der Erfindung beschrieben. Zuerst werden die pulverförmigen, duktilen Komponenten, die elementar oder vorlegiert vorliegen können, in einem vorbestimmten Mischungsverhältnis gemischt. Eine typische Legierung kann beispielsweise aus Ti48Al2Cr (in At.-%) bestehen. Ausgehend von reinen Ti-Al-Elementpulvern wurden die 2 At.-% Cr zur Gewährleistung ihrer homogenen Verteilung im Ti48Al2Cr als Vorlegierungspulver Al-15 Gew.-% Cr gemäß der stöchiometrischen Legierungszusammensetzung zugemischt. Das anschließende Vorkompaktieren dieser Pulvermischung zu einem Körper, beispielsweise zu einem transportfähigen Preßbolzen, erfolgt durch kaltisostatisches Pressen (CIP). Mit einem Preßdruck von 450 Nmm⁻² konnten 93,8 % der theoretisch berechneten Werkstoffdichte erreicht werden.The method is now described using the individual method steps according to a typical embodiment of the invention. First, the powdery, ductile components that are elemental or pre-alloyed may be present, mixed in a predetermined mixing ratio. A typical alloy can consist of Ti48Al2Cr (in at%), for example. Starting from pure Ti-Al element powders, the 2 at.% Cr was mixed in to ensure their homogeneous distribution in the Ti48Al2Cr as pre-alloy powder Al-15 wt.% Cr according to the stoichiometric alloy composition. The subsequent precompacting of this powder mixture into a body, for example into a transportable press bolt, is carried out by cold isostatic pressing (CIP). With a pressure of 450 Nmm⁻² 93.8% of the theoretically calculated material density could be achieved.
Zur Erzielung einer rißfreien Strangoberfläche werden die vorkompaktierten Körper vor dem Strangpressen in AlMgSiO,5-Rohre gekapselt.In order to achieve a crack-free strand surface, the precompacted bodies are encapsulated in AlMgSiO, 5 pipes before extrusion.
Nachfolgend erfolgt das Strangpressen, wobei die für die Wärmebehandlung nötige Wärme die im Zuge der Strangpressung erzeugte Wärme ist. Dabei sind die Preßbedingungen wie Bolzen-/Aufnehmertemperatur TB/A, das Preßverhältnis R und die Stempelgeschwindigkeit vSt derart gewählt, daß einerseits die durch die Umformung erzeugte Temperaturerhöhung im Preßstrang ausreicht, um eine in-situ-Reaktion nach dem Preßvorgang auszulösen, und daß andererseits die Strangtemperatur während des Umformprozesses die Phasenbildungstemperatur aber nicht soweit überschreiten darf, daß die Phasenreaktion schneller abläuft als der Preßvorgang.The extrusion is then carried out, the heat required for the heat treatment being the heat generated in the course of the extrusion. The pressing conditions such as pin / pick-up temperature T B / A , the pressing ratio R and the punch speed v St are selected such that the temperature increase in the press strand produced by the deformation is sufficient to trigger an in-situ reaction after the pressing process, and that, on the other hand, the strand temperature during the forming process must not exceed the phase formation temperature to such an extent that the phase reaction proceeds faster than the pressing process.
Zahlreiche Versuche haben belegt, daß durch Erhöhung des Preßverhältnisses R die Al-Partikelgröße im Preßstrang verringert und damit Einfluß auf eine geringe Porosität im Titanaluminid-Körper genommen werden kann. Die Größe des Preßverhältnisses wird jedoch durch die damit verbundenen höheren Umformtemperaturen begrenzt, die zu einer vorzeitigen Phasenbildung während des Strangpressens, siehe oben, führen können. Das ist für Ti48Al2Cr bei TB/A = 350° C bis zu R < 32:1 bzw. bei TB/A = 450° C nur bis R < 18:1 möglich.Numerous tests have shown that increasing the compression ratio R reduces the Al particle size in the press strand and can thus influence a low porosity in the titanium aluminide body. The size However, the pressing ratio is limited by the associated higher forming temperatures, which can lead to premature phase formation during extrusion, see above. This is possible for Ti48Al2Cr at T B / A = 350 ° C up to R <32: 1 or at T B / A = 450 ° C only up to R <18: 1.
Durch nochmaliges Strangpressen bereits gepreßter Stränge (Doppelstrangpressen) muß deshalb das Preßverhältnis weiter gesteigert und das Körpergefüge stärker verfeinert werden.The extrusion ratio must therefore be further increased and the body structure refined more by extruding extruded strands again (double extrusion).
Bei Versuchen standen dafür als Ausgangsmaterial von 85 mm Durchmesser an 20 mm Durchmesser gepreßte Rundstangen (TB/A = 350° C, R = 18:1, vSt = 3 mms⁻¹) zur Verfügung. Nach Abdrehen des Kapselmaterials von der Strangoberfläche wurden 19 Stäbe mit je 16 mm Durchmesser in ein 85 x 1,5 mm Durchmesser AlMgSiO,5-Rohr gesteckt und erneut stranggepreßt. Zur Vermeidung vorzeitiger Phasenreaktionen erfolgte dabei eine Herabsetzung der Bolzen-/Aufnehmertemperatur auf 250 °C und der Stempelgeschwindigkeit auf 0,8 mms⁻¹. Dadurch war es möglich, daß die durch die Umformwärme ausgelöste Phasenreaktion tatsächlich nicht während, sondern unmittelbar nach dem Preßvorgang quasi zeitverzögert im Körper ablief.In experiments, round bars (T B / A = 350 ° C, R = 18: 1, v St = 3 mms⁻¹) were available as starting material of 85 mm diameter to 20 mm diameter. After unscrewing the capsule material from the surface of the strand, 19 rods, each 16 mm in diameter, were inserted into an 85 x 1.5 mm diameter AlMgSiO, 5 pipe and extruded again. To avoid premature phase reactions, the stud / receiver temperature was reduced to 250 ° C and the punch speed to 0.8 mms⁻¹. This made it possible that the phase reaction triggered by the heat of deformation actually did not take place in the body with a time delay, but rather immediately after the pressing process.
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4426205 | 1994-07-23 | ||
| DE4426205A DE4426205A1 (en) | 1994-07-23 | 1994-07-23 | Process for the production of bodies from intermetallic phases from powdery, ductile components |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0693564A1 true EP0693564A1 (en) | 1996-01-24 |
| EP0693564B1 EP0693564B1 (en) | 1999-01-20 |
Family
ID=6524016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP95110967A Expired - Lifetime EP0693564B1 (en) | 1994-07-23 | 1995-07-13 | Process for preparing articles composed of intermetallic phases from pulverulent ductile components |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0693564B1 (en) |
| AT (1) | ATE176005T1 (en) |
| DE (2) | DE4426205A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996028578A1 (en) * | 1995-03-14 | 1996-09-19 | Imperial College Of Science, Technology & Medicine | Formation and use of intermetallics |
| EP0738782A2 (en) * | 1995-04-20 | 1996-10-23 | Philip Morris Products Inc. | Iron aluminide useful as electrical resistance heating elements |
| US6280682B1 (en) | 1996-01-03 | 2001-08-28 | Chrysalis Technologies Incorporated | Iron aluminide useful as electrical resistance heating elements |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3809550A1 (en) * | 1988-03-22 | 1989-10-19 | Vaw Ver Aluminium Werke Ag | Process for the powder-metallurgical production of a light and heat-resistant component |
| DE3822686A1 (en) | 1988-07-05 | 1990-01-11 | Geesthacht Gkss Forschung | METHOD FOR PRODUCING INTERMETALLIC PHASES FROM POWDER-SHAPED DUCTILE COMPONENTS |
| EP0360468A1 (en) * | 1988-09-22 | 1990-03-28 | Texas Instruments Incorporated | Member of a refractory metal material of selected shape and method of making |
-
1994
- 1994-07-23 DE DE4426205A patent/DE4426205A1/en not_active Withdrawn
-
1995
- 1995-07-13 AT AT95110967T patent/ATE176005T1/en not_active IP Right Cessation
- 1995-07-13 DE DE59504872T patent/DE59504872D1/en not_active Expired - Fee Related
- 1995-07-13 EP EP95110967A patent/EP0693564B1/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3809550A1 (en) * | 1988-03-22 | 1989-10-19 | Vaw Ver Aluminium Werke Ag | Process for the powder-metallurgical production of a light and heat-resistant component |
| DE3822686A1 (en) | 1988-07-05 | 1990-01-11 | Geesthacht Gkss Forschung | METHOD FOR PRODUCING INTERMETALLIC PHASES FROM POWDER-SHAPED DUCTILE COMPONENTS |
| FR2633853A1 (en) * | 1988-07-05 | 1990-01-12 | Geesthacht Gkss Forschung | PROCESS FOR THE PREPARATION OF INTERMETALLIC PHASES FROM PULVERULENT DUCTILE COMPONENTS |
| EP0360468A1 (en) * | 1988-09-22 | 1990-03-28 | Texas Instruments Incorporated | Member of a refractory metal material of selected shape and method of making |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6607576B1 (en) | 1994-12-29 | 2003-08-19 | Chrysalis Technologies Incorporated | Oxidation, carburization and/or sulfidation resistant iron aluminide alloy |
| WO1996028578A1 (en) * | 1995-03-14 | 1996-09-19 | Imperial College Of Science, Technology & Medicine | Formation and use of intermetallics |
| EP0738782A2 (en) * | 1995-04-20 | 1996-10-23 | Philip Morris Products Inc. | Iron aluminide useful as electrical resistance heating elements |
| EP0738782A3 (en) * | 1995-04-20 | 1998-08-05 | Philip Morris Products Inc. | Iron aluminide useful as electrical resistance heating elements |
| US5976458A (en) * | 1995-04-20 | 1999-11-02 | Philip Morris Incorporated | Iron aluminide useful as electrical resistance heating elements |
| US6280682B1 (en) | 1996-01-03 | 2001-08-28 | Chrysalis Technologies Incorporated | Iron aluminide useful as electrical resistance heating elements |
Also Published As
| Publication number | Publication date |
|---|---|
| DE59504872D1 (en) | 1999-03-04 |
| DE4426205A1 (en) | 1996-01-25 |
| EP0693564B1 (en) | 1999-01-20 |
| ATE176005T1 (en) | 1999-02-15 |
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