EP2990141B1 - Method for producing TiAl components - Google Patents

Method for producing TiAl components Download PDF

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Publication number
EP2990141B1
EP2990141B1 EP14182981.2A EP14182981A EP2990141B1 EP 2990141 B1 EP2990141 B1 EP 2990141B1 EP 14182981 A EP14182981 A EP 14182981A EP 2990141 B1 EP2990141 B1 EP 2990141B1
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EP
European Patent Office
Prior art keywords
capsule
powder
component
alloy
temperature
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.)
Not-in-force
Application number
EP14182981.2A
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German (de)
French (fr)
Other versions
EP2990141A1 (en
Inventor
Martin Schloffer
Wilfried Smarsly
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 AG
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MTU Aero Engines AG
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Filing date
Publication date
Application filed by MTU Aero Engines AG filed Critical MTU Aero Engines AG
Priority to EP14182981.2A priority Critical patent/EP2990141B1/en
Priority to ES14182981T priority patent/ES2728527T3/en
Priority to US14/838,802 priority patent/US10029309B2/en
Publication of EP2990141A1 publication Critical patent/EP2990141A1/en
Application granted granted Critical
Publication of EP2990141B1 publication Critical patent/EP2990141B1/en
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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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/009—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine components other than turbine blades
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D29/00—Removing castings from moulds, not restricted to casting processes covered by a single main group; Removing cores; Handling ingots
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • 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
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/04—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine blades
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • 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
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • 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
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00—Electrolytic stripping of metallic layers or coatings
    • 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
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/13—Use of plasma
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • 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

Definitions

  • the present invention relates to a method for producing a component, in particular a component for a turbomachine, such as an aircraft engine, from a high temperature material, in particular a TiAl alloy.
  • turbomachinery For the operation of turbomachinery special materials for certain components are required due to the conditions of use of the components used in some high temperatures, aggressive environments and high forces acting, which are optimally adapted both by their chemical composition and by their microstructure to the intended use.
  • Alloys based on intermetallic titanium aluminide compounds are used in the construction of turbomachinery, such as stationary gas turbines or aircraft engines, for example as a material for rotor blades, since they have the mechanical properties required for the application and additionally have a low specific weight. so that the use of such alloys can increase the efficiency of stationary gas turbines and aircraft engines. Accordingly, there are already a large number of TiAl alloys and processes for producing corresponding components thereof.
  • Components made of TiAl alloys can be produced similarly to comparable components from other high - temperature alloys, for example based on Ni, Fe or Co, both by melt metallurgy and powder metallurgy.
  • the alloy used to make the component is provided in the form of a melt and is poured off in a mold.
  • the cast material must usually be subjected to suitable forming and / or heat treatments to destroy the cast structure and to set a desired microstructure of the material.
  • the corresponding component can then be brought into the desired shape by suitable post-processing, for example by machining, mechanical processing or electrochemical machining.
  • the manufacturing steps additionally or alternatively to the individual steps of the fusion metallurgical production include the use of powder materials in order to produce a desired composition of the material, for example by mechanical alloying.
  • An example of the production of a TiAl alloy article using powder materials is shown in U.S.P. US 5,424,027 described.
  • HIP hot isostatic pressing
  • the corresponding method should be simple and reliable feasible and can be set reproducibly suitable microstructures in high-temperature alloys and in particular TiAl alloys that provide the necessary properties, especially for components of turbomachinery.
  • a component in particular a component for a turbomachine, such as a stationary gas turbine or an aircraft engine, from a TiAl alloy by first producing a powder of the desired alloy, filling this powder into a capsule is whose shape largely corresponds to the shape of the component to be manufactured, and hot isostatically press these capsules with the filled powder and subjected to a heat treatment, so that after removal of the capsule and the post-processing of the component to produce the final contour by material removal the finished component ,
  • a near-net shape capsule which takes into account or approximates the shape of the component to be produced, elaborate rework can be avoided by removing a large volume of excess material by removing material, so that the use of materials and the associated effort can be reduced.
  • the close-to-net shape of the capsule therefore only has to take into account the subsequent processing steps in which, however, no extensive change in shape of the component takes place, as would be the case, for example, with a required hot forming. For example, only a slight oversize to the final shape or contour of the component to be produced can be provided, which variations due to production in hot isostatic pressing, heat treatment or removal the capsule takes into account so that the desired shape of the component can be obtained by the subsequent material removal.
  • the production method described above can be used in particular for TiAl alloys and in particular highly alloyed TiAl alloys and / or TiAl alloys with high Al contents, for example with Al contents of more than 30 at.% Al, in particular more than 45 at.% Al , preferably more than 50 at.% And up to 60 at.% Al or more are used, since in these alloys, the formation of finely divided precipitates and a fine-grained, homogeneous microstructure with the present method is to achieve low.
  • various starting materials may be used, such as powder of the individual elements to be alloyed or powder or powder of master alloys to be recycled, that is, alloys comprising parts of the later alloy composition.
  • the starting materials can be pressed into compacts, which can then be used for melting the alloy.
  • the melting of the alloy can be carried out by single or multiple plasma arc melting (PAM), vacuum arc melting (VAR) or vacuum induction melting (VIM).
  • PAM plasma arc melting
  • VAR vacuum arc melting
  • VIM vacuum induction melting
  • the powder can directly from the corresponding melt or after reflowing after an intermediate casting of the melt from a molten bath or from a meanwhile poured ingot can be produced by spraying.
  • the vacuum inert gas atomization (VIG), the plasma melting induction induction atomization (PIGA) or the electrode induction gas atomization (EIGA) can be used.
  • the powder may also be subjected to an additional purification process, for example, to reduce the oxygen occupancy of the powder surface and thus to reduce the oxygen contamination of the material used for component manufacturing and to reduce or eliminate organic and / or inorganic impurities.
  • the powder particles can be processed to set a spherical particle shape and / or to influence the size of the particles (grain size). For example, this can be done in a plasma cleaning process in which the powder particles are introduced into a plasma so that contaminants can be removed and the surface shape of the particles can approach a spherical shape.
  • the produced powder can be classified according to the particle size and one or more powder fractions can be selected for the further production of the component. Fractionation may be carried out before or after the purification process, with purification prior to fractionation being preferred, as the size of the particles may be altered by plasma purification.
  • the fractionation may be carried out by various known methods, and in particular, a two-stage fractionation is possible wherein e.g. First, a prefractionation takes place by means of a centrifuge, and then, in a second step, a main fraction is produced by sieving and / or sifting. For the production of a fine-grained TiAl material, in particular powder fractions with average or maximum particle sizes ⁇ 125 ⁇ m in diameter or corresponding to the maximum extent can be selected.
  • the capsule into which the powder is filled for the subsequent hot isostatic pressing can be made of a sheet of a material similar to the powder, in particular of the base material of the powder used, that is, for example, an alloy having the same main constituent.
  • the capsule may be formed with, for example, 1 to 3 mm, preferably 2 to 3 mm, wall thickness of titanium or a titanium alloy.
  • the capsule can be formed from at least two mold parts, which can be connected together to close the capsule, for example by welding under inert gas.
  • the molded parts of the capsule can be formed from deep-drawn sheets of the corresponding capsule material, so that a contour of the capsule which is similar to the shape of the component to be produced can be produced in a simple manner.
  • the contour or shape of the capsule can be formed with a certain allowance, which takes into account the shape changes in the subsequent hot isostatic pressing and the heat treatments or allows a subsequent post-processing by material removal, which gives the possibility of the exact desired shape of the To produce component.
  • the filling of the powder in the capsule can be done under inert gas, so as to further reduce the burden of contamination.
  • the filling of the powder into the capsule can take place directly after the cleaning under vacuum or inert gas, so that the powder is no longer exposed to the ambient atmosphere.
  • the filled but not yet sealed capsule - or alternatively the powder prior to filling into the capsule - can be subjected to a heat treatment under vacuum (cleaning heat treatment) to effect further purification of the powder material by evaporation or outgassing.
  • a heat treatment under vacuum cleaning heat treatment
  • the heat treatment at a temperature in the range of 200 ° C to 500 ° C, preferably between 440 ° C and 460 ° C under vacuum with a pressure ⁇ 10 -3 mbar, in particular ⁇ 10 -5 mbar above the powder can be performed.
  • the oxygen content in the production of a component made of a TiAl alloy can be reduced to a range of ⁇ 600 ppm.
  • the cooling of the surface of the capsule with the filled powder after the cleaning heat treatment can at a cooling rate of 25 ° C / min to 35 ° C / min, preferably at 30 ° C / min up to a temperature of 120 ° C or below, in particular 100 ° C, are carried out under vacuum, wherein subsequently the closure of the capsule can be done for example by welding under inert gas. Rapid cooling can improve the prevailing vacuum, allowing lower pressures to be generated and cleaning of the powder can be further improved. For example, the vacuum can improve from 10 -3 mbar to 10 -4 mbar.
  • the powder in the capsule may be densified by mechanical stimulation such as vibration, vibration, tapping or the like.
  • the capsule can still be open or closed, wherein in an open capsule, the mechanical compression can be carried out under vacuum.
  • the thus prepared capsule can be hot isostatically pressed at temperatures in the range of 1100 ° C to 1400 ° C, especially 1150 ° C to 1300 ° C at a pressure of 100 to 250 MPa for a period of two to six hours, so that a compacted Material block in a near-net shape of the component results.
  • the shape close to the final contour can be chosen such that the manufactured component meets the requirements of the production of net - shape components or near - net - shape components.
  • the hot isostatically pressed capsule may have an oversize of the finished component of 0.5 mm to 5 mm, in particular 0.5 mm or 1 mm to 2 mm (net shape) or 2 mm to 5 mm (near net shape) plus the respective have corresponding capsule thickness.
  • the capsule After the hot isostatic pressing, the capsule is subjected to a multi-stage heat treatment in which solution annealing, high-temperature annealing and aging annealing are performed in this order according to the powder material used.
  • solution annealing is carried out at a temperature up to 1400 ° C for 15 to 45 minutes.
  • the high-temperature annealing is carried out at a temperature of 1100 ° C to 1300 ° C and an aging annealing is carried out at a temperature of 850 ° C to 1100 ° C for six to one hundred hours.
  • the heating and / or cooling rates for the heat treatment can be selected as a function of the size and / or the shape of the component, whereby, for example, relatively lower heating and / or cooling rates are selected for larger components, while for small components greater heating and / or or cooling rates can be realized. In addition, you can the heating and / or cooling rates are determined so that as far as possible no distortion of the component takes place.
  • the capsule is removed, for example by chemical pickling, electrochemical machining, blasting with particles, in particular with plastic granules and / or machining, such as milling or grinding. Thereafter, the post-processing of the outer shape (contour) of the component by mechanical, spannabariade processing, in particular by milling, grinding, polishing, etc. and / or electrochemical machining done.
  • Various functional layers can be applied to the component produced in this way, for example wear protection layers, corrosion protection layers, oxidation protection layers and the like.
  • the component and / or the material or the material of which the component is made can be characterized, in particular by non-destructive methods, such as, for example, by X-ray diffractometry.
  • a material having as main constituents of titanium and aluminum is understood according to the present invention, a material having as main constituents of titanium and aluminum.
  • Main constituents are understood to mean those elements whose proportion in at.% Or wt.% Is the largest, ie in the case of a TiAl alloy titanium and aluminum as elements having the largest proportions in at.% Or wt.% In the alloy.
  • a TiAl alloy which is processed into a component according to the present method it can be, in particular, a high-alloy TiAl alloy, which is particularly suitable for high temperatures, for example.
  • B. can be used as a blade material for turbomachinery.
  • chemical elements such as niobium, molybdenum, tungsten, cobalt, chromium, vanadium, zirconium, silicon, carbon, erbium, gadolinium, hafnium, yttrium and boron may be included.
  • the method according to the invention forms a rotor blade of an aircraft engine made of a highly alloyed TiAl alloy, wherein first in a first step, a compact of powders of the individual elements to be alloyed and / or of so-called master alloys is pressed.
  • the compact may contain titanium sponge (step I).
  • the compact is subsequently melted (method step II) by a single plasma arc melting process, so that an alloy melt results.
  • This is first poured off and then melted a second time in a third process step (process step III) for powder production in order to make a gas atomization from the molten bath can.
  • the gas atomization from the molten bath can be carried out by VIGA or PIGA process, whereby as spherical as possible powder particles are to be produced by the gas atomization.
  • the particle size fractions desired for further processing are selected from the powder produced, for example particle size fractions with maximum or average diameters of the particles in the range from 15 to 150 ⁇ m or preferably 45 to 125 ⁇ m. In the chosen embodiment, the particle size ⁇ 125 ⁇ m is maintained in order to achieve a fine-grained structure.
  • a fifth method step (method step V) the selected powder fraction is introduced into a plasma, so that the plasma cleans the powder particles and forms a spherical formation of the powder particles.
  • the plasma reduces the oxygen occupancy of the powder surface and approximates the surface shape to a spherical shape.
  • the thus purified powder is filled under protective gas, for example helium or argon in capsules made of titanium (step VI), for example, have a wall thickness of 1 to 2 mm, and are formed according to the shape of the component to be produced, for example, two deep-drawn titanium sheets.
  • protective gas for example helium or argon in capsules made of titanium (step VI)
  • step VI have a wall thickness of 1 to 2 mm, and are formed according to the shape of the component to be produced, for example, two deep-drawn titanium sheets.
  • the titanium material used for the capsules may be so-called titanium grade I material.
  • a further purification of the material is carried out in a seventh process step (step VII) by the powder-filled, but not yet sealed capsule under vacuum conditions at a pressure of ⁇ 10 -3 mbar , in particular ⁇ 10 -5 mbar is heated at temperatures up to 450 ° C, so that further impurities volatilize by evaporation. In this way, for example, the oxygen content ⁇ 600 ppm can be set.
  • the capsule which is furthermore kept under vacuum, can be cooled to 120 ° C. or 100 ° C., wherein a cooling rate of 30 ° C./min can be selected (method step VIII).
  • the capsule is closed by welding, so that in the tenth process step (process step X) the capsule can be hot isostatically pressed with the powder enclosed therein at a pressure in the range of 100 to 240 MPa and a temperature in the range from 1150 ° C to 1400 ° C for a period of two to six hours.
  • process step XI After hot isostatic pressing (process step X), the eleventh process step (process step XI) is followed by a multi-stage heat treatment, with the aid of which the microstructure of the component can be adjusted.
  • a solution heat treatment at 1400 ° C or just below for a period of 15 to 45 minutes.
  • a high-temperature annealing is carried out at 1100 ° C to 1300 ° C
  • an aging annealing is carried out at 850 ° C to 1100 ° C for a period of six to one hundred hours.
  • the component is finished with respect to the material structure and it only need to be done final work on the shape of the component.
  • the capsule is removed in a twelfth method step (method step XII), namely by pickling the outer layer and / or electrochemical machining, blasting with particles, in particular plastic particles, and / or by mechanical processing, such as milling, grinding or the like.
  • a thirteenth method step (method step XIII), the excess material is now removed from the component by mechanical, in particular machining, for example by milling, grinding, polishing and the like.
  • the material removal can also be done by electrochemical machining, so that the final dimension is set.
  • the set microstructure of the component can be checked by X-ray diffractometry and other nondestructive testing methods. Furthermore, required on the component layers such as corrosion protection layers, oxidation protection layers, wear protection layers and the like can be deposited.

Description

HINTERGRUND DER ERFINDUNGBACKGROUND OF THE INVENTION GEBIET DER ERFINDUNGFIELD OF THE INVENTION

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung eines Bauteils, insbesondere eines Bauteils für eine Strömungsmaschine, wie beispielsweise ein Flugtriebwerk, aus einem Hochtemperaturwerkstoff, insbesondere einer TiAl - Legierung.The present invention relates to a method for producing a component, in particular a component for a turbomachine, such as an aircraft engine, from a high temperature material, in particular a TiAl alloy.

STAND DER TECHNIKSTATE OF THE ART

Für den Betrieb von Strömungsmaschinen sind auf Grund der Einsatzbedingungen der verwendeten Bauteile mit zum Teil hohen Temperaturen, aggressiven Umgebungen und hohen einwirkenden Kräften spezielle Werkstoffe für bestimmte Bauteile erforderlich, die sowohl durch ihre chemische Zusammensetzung als auch durch ihre Mikrostruktur optimal an den Einsatzzweck angepasst sind.For the operation of turbomachinery special materials for certain components are required due to the conditions of use of the components used in some high temperatures, aggressive environments and high forces acting, which are optimally adapted both by their chemical composition and by their microstructure to the intended use.

Legierungen auf Basis von intermetallischen Titanaluminid - Verbindungen (TiAl - Legierungen) finden beim Bau von Strömungsmaschinen, wie stationären Gasturbinen oder Flugtriebwerken, beispielsweise als Werkstoff für Laufschaufeln Verwendung, da sie die für den Einsatz erforderlichen mechanischen Eigenschaften aufweisen und zusätzlich ein geringes spezifisches Gewicht besitzen, sodass der Einsatz derartiger Legierungen die Effizienz von stationären Gasturbinen und Flugtriebwerken steigern kann. Entsprechend gibt es bereits eine Vielzahl von TiAl - Legierungen sowie Verfahren zur Herstellung von entsprechenden Bauteilen daraus.Alloys based on intermetallic titanium aluminide compounds (TiAl alloys) are used in the construction of turbomachinery, such as stationary gas turbines or aircraft engines, for example as a material for rotor blades, since they have the mechanical properties required for the application and additionally have a low specific weight. so that the use of such alloys can increase the efficiency of stationary gas turbines and aircraft engines. Accordingly, there are already a large number of TiAl alloys and processes for producing corresponding components thereof.

Bauteile aus TiAl - Legierungen lassen sich ähnlich wie vergleichbare Bauteile aus anderen Hochtemperaturlegierungen, beispielsweise auf Ni - , Fe - oder Co - Basis, sowohl schmelzmetallurgisch als auch pulvermetallurgisch herstellen.Components made of TiAl alloys can be produced similarly to comparable components from other high - temperature alloys, for example based on Ni, Fe or Co, both by melt metallurgy and powder metallurgy.

Bei der schmelzmetallurgischen Herstellung wird die Legierung, die für die Herstellung des Bauteils verwendet wird, in Form einer Schmelze bereitgestellt und diese wird in einer Form abgegossen. Der gegossene Werkstoff muss üblicherweise geeigneten Umformungen und/oder Wärmebehandlungen unterzogen werden, um das Gussgefüge zu zerstören und eine gewünschte Mikrostruktur des Werkstoffs einzustellen. Das entsprechende Bauteil kann dann durch geeignete Nachbearbeitung, beispielsweise durch spanabhebende, mechanische Bearbeitung oder elektrochemische Bearbeitung in die gewünschte Form gebracht werden.In melt metallurgy production, the alloy used to make the component is provided in the form of a melt and is poured off in a mold. The cast material must usually be subjected to suitable forming and / or heat treatments to destroy the cast structure and to set a desired microstructure of the material. The corresponding component can then be brought into the desired shape by suitable post-processing, for example by machining, mechanical processing or electrochemical machining.

Bei der pulvermetallurgischen Herstellung umfassen die Herstellungsschritte zusätzlich oder alternativ zu den einzelnen Schritten der schmelzmetallurgischen Herstellung den Einsatz von Pulvermaterialien, um beispielsweise durch mechanisches Legieren eine gewünschte Zusammensetzung des Werkstoffs zu erzeugen. Ein Beispiel für die Herstellung eines Gegenstands aus einer TiAl - Legierung unter Verwendung von Pulvermaterialien ist in der US 5,424,027 beschrieben.In the production of powder metallurgy, the manufacturing steps additionally or alternatively to the individual steps of the fusion metallurgical production include the use of powder materials in order to produce a desired composition of the material, for example by mechanical alloying. An example of the production of a TiAl alloy article using powder materials is shown in U.S.P. US 5,424,027 described.

Gemäß diesem Dokument werden Gegenstände aus TiAl - Legierungen mit 50 at.% Aluminium sowie Legierungen mit 48 at.% Aluminium und 1 at.% Niob, 48 at.% Aluminium, 2 at.% Niob und 2 at.% Chrom sowie 48 at.% Aluminium, 1 at.% Niob und 1 at.% Vanadium und 48 at.% Aluminium, 3 at.% Niob, 2 at.% Chrom und 1 at.% Mangan sowie Rest jeweils Titan dadurch hergestellt, dass ein entsprechend vorlegiertes TiAl - Pulver in eine geeignete Form eingefüllt wird, um anschließend heißisostatisch gepresst zu werden. Nach dem heißisostatischen Pressen wird der Werkstoff einer Warmumformung unterzogen, um eine feine, gleichmäßige und isotrope Mikrostruktur einzustellen.According to this document, articles made of TiAl alloys containing 50 at.% Aluminum and alloys containing 48 at.% Aluminum and 1 at.% Niobium, 48 at.% Aluminum, 2 at.% Niobium and 2 at.% Chromium and 48 at % Aluminum, 1 at.% Niobium and 1 at.% Vanadium and 48 at.% Aluminum, 3 at.% Niobium, 2 at.% Chromium and 1 at.% Manganese and the remainder titanium in each case produced by a correspondingly pre-alloyed TiAl powder is poured into a suitable mold for subsequent hot isostatic pressing. After hot isostatic pressing, the material undergoes hot working to set a fine, uniform and isotropic microstructure.

Für eine Warmumformung, die sowohl bei einer schmelzmetallurgischen Herstellung als auch bei der pulvermetallurgischen Herstellung gemäß der US 5,424,027 durchgeführt werden kann bzw. zur Erzielung bestimmter Eigenschaften durchgeführt werden muss, ist ein hoher Aufwand bezüglich der Warmumformungsschritte erforderlich. Außerdem ist bei einer derartigen Herstellung ein hoher Materialverbrauch gegeben, da eine endkonturnahe Herstellung, beispielsweise durch endkonturnahes Gießen, nicht möglich ist. In diesem Zusammenhang ergibt sich dann ein weiterer, erhöhter Aufwand für die spannabhebende bzw. elektrochemische Formgebung des Bauteils.For hot forming, both in a melt metallurgical production as well as in the powder metallurgical production according to the US 5,424,027 can be carried out or must be carried out to achieve certain properties, a high cost of the hot forming steps is required. In addition, in such a production, a high material consumption is given because a near-net shape production, for example by near-net shape casting, is not possible. In this context, then results in a further, increased effort for the Spannabhebende or electrochemical shaping of the component.

Das Dokument JP 2008208432 A offenbart eine pulvermetallurgische Herstellung eines Bauteils aus einem TiAl - Werkstoff durch heißisostatisches Pressen. Auch in den Dokumenten US 5 768 679 A und JP 2006 009 062 A werden Verfahren zur Herstellung von Bauteilen aus TiAl - Werkstoffen beschrieben, bei denen die Formgebung durch heißisostatisches Pressen (HIP) erfolgt, wobei nach der Formgebung eine Wärmebehandlung des Bauteils vorgenommen wird.The document JP 2008208432 A discloses a powder metallurgical production of a component from a TiAl material by hot isostatic pressing. Also in the documents US 5,768,679 A and JP 2006 009 062 A German: v3.espacenet.com/textdoc? DB = EPODOC & ... PN = EP0056537 Processes for the production of components made of TiAl materials, in which the shaping is carried out by hot isostatic pressing (HIP), are carried out after the shaping of a heat treatment of the component.

OFFENBARUNG DER ERFINDUNGDISCLOSURE OF THE INVENTION AUFGABE DER ERFINDUNGOBJECT OF THE INVENTION

Es ist deshalb Aufgabe der vorliegenden Erfindung ein Verfahren zur Herstellung eines Bauteils aus einer Hochtemperaturlegierung, insbesondere einer TiAl - Legierung anzugeben, mit welchem effizient unter Reduzierung des Aufwands gegenüber dem Stand der Technik ein Bauteil gefertigt werden kann, wobei der Werkstoff des Bauteils eine optimale Mikrostruktur, insbesondere eine homogene und gleichmäßige Gefügestruktur aufweisen soll, sodass das Bauteil ebenfalls gleichmäßige mechanische Eigenschaften aufweist. Das entsprechende Verfahren soll einfach und zuverlässig durchführbar sein und reproduzierbar geeignete Mikrostrukturen bei Hochtemperaturlegierungen und insbesondere TiAl-Legierungen einstellen lassen, die die erforderlichen Eigenschaften insbesondere für Bauteile von Strömungsmaschinen bereitstellen.It is therefore an object of the present invention to provide a method for producing a component from a high-temperature alloy, in particular a TiAl alloy, with which a component can be manufactured efficiently while reducing the expenditure compared to the prior art, wherein the material of the component has an optimum microstructure , in particular, should have a homogeneous and uniform microstructure, so that the Component also has uniform mechanical properties. The corresponding method should be simple and reliable feasible and can be set reproducibly suitable microstructures in high-temperature alloys and in particular TiAl alloys that provide the necessary properties, especially for components of turbomachinery.

TECHNISCHE LÖSUNGTECHNICAL SOLUTION

Diese Aufgabe wird gelöst durch ein Verfahren mit den Merkmalen des Anspruchs 1. Vorteilhafte Ausgestaltungen sind Gegenstand der abhängigen Ansprüche.This object is achieved by a method having the features of claim 1. Advantageous embodiments are the subject of the dependent claims.

Gemäß der vorliegenden Erfindung wird vorgeschlagen, ein Bauteil, insbesondere ein Bauteil für eine Strömungsmaschine, wie eine stationäre Gasturbine oder ein Flugtriebwerk, aus einer TiAl - Legierung dadurch herzustellen, dass zunächst ein Pulver aus der gewünschten Legierung hergestellt wird, dieses Pulver in eine Kapsel eingefüllt wird, deren Form der Form des herzustellenden Bauteils weitgehend entspricht, und diese Kapseln mit dem eingefüllten Pulver heißisostatisch zu pressen und einer Wärmebehandlung zu unterziehen, sodass nach dem Entfernen der Kapsel und der Nachbearbeitung des Bauteils zur Herstellung der endgültigen Kontur durch Materialabtrag das fertige Bauteil vorliegt.According to the present invention, it is proposed to produce a component, in particular a component for a turbomachine, such as a stationary gas turbine or an aircraft engine, from a TiAl alloy by first producing a powder of the desired alloy, filling this powder into a capsule is whose shape largely corresponds to the shape of the component to be manufactured, and hot isostatically press these capsules with the filled powder and subjected to a heat treatment, so that after removal of the capsule and the post-processing of the component to produce the final contour by material removal the finished component ,

Durch das erfindungsgemäße Verfahren lässt sich eine Warmumformung bzw. ein Schmieden des Werkstoffs vermeiden, sodass der Aufwand bei der Herstellung reduziert werden kann. Gleichzeitig kann jedoch eine homogene, gleichmäßige Mikrostruktur ohne Seigerungen und Ausscheidungsvergröberungen hergestellt werden, die günstige mechanische Eigenschaften des eingesetzten Werkstoffs für den Einsatz in Strömungsmaschinen liefert.By means of the method according to the invention, hot working or forging of the material can be avoided so that the outlay on manufacture can be reduced. At the same time, however, it is possible to produce a homogeneous, uniform microstructure without segregation and precipitation coarsening, which provides favorable mechanical properties of the material used for use in turbomachinery.

Durch die Verwendung einer endkonturnahen Kapsel, die also die Form des herzustellenden Bauteils berücksichtigt bzw. dieser angenähert ist, lassen sich aufwändige Nachbearbeitungen mit der Entfernung eines großen Volumens überschüssigen Materials durch Materialabtrag vermeiden, sodass der Materialeinsatz und der dadurch verbundene Aufwand verringert werden können. Die endkonturnahe Form der Kapsel muss somit lediglich die nachfolgenden Bearbeitungsschritte berücksichtigen, bei denen jedoch keine umfangreiche Formänderung des Bauteils mehr stattfindet, wie dies beispielsweise bei einer erforderlichen Warmumformung der Fall wäre. Beispielsweise kann lediglich ein geringes Aufmaß zur endgültigen Form bzw. Kontur des herzustellenden Bauteils vorgesehen werden, welches herstellungsbedingte Abweichungen beim heißisostatischen Pressen, der Wärmebehandlung oder dem Entfernen der Kapsel Rechnung trägt, sodass durch den anschließenden Materialabtrag die gewünschte Form des Bauteils erhalten werden kann.By using a near-net shape capsule, which takes into account or approximates the shape of the component to be produced, elaborate rework can be avoided by removing a large volume of excess material by removing material, so that the use of materials and the associated effort can be reduced. The close-to-net shape of the capsule therefore only has to take into account the subsequent processing steps in which, however, no extensive change in shape of the component takes place, as would be the case, for example, with a required hot forming. For example, only a slight oversize to the final shape or contour of the component to be produced can be provided, which variations due to production in hot isostatic pressing, heat treatment or removal the capsule takes into account so that the desired shape of the component can be obtained by the subsequent material removal.

Durch die Verwendung von Pulver kann eine feine Mikrostruktur mit kleiner, homogen verteilter Korngröße und homogener Elementverteilung erzielt werden, da beispielsweise keine Texturen durch Schmiedeprozesse eingebracht werden und das Pulver sehr gut im Vakuum und unter Schutzgas handhabbar ist und somit in entsprechender Reinheit eingesetzt und verarbeitet werden kann. Dabei kann zum Erreichen eines geringen Anteils an Verunreinigungen, beispielsweise Sauerstoffkontaminationen, eine Verarbeitung unter Schutzgas vorgenommen werden.By using powder, a fine microstructure with a small, homogeneously distributed particle size and homogeneous element distribution can be achieved since, for example, no textures are introduced by forging processes and the powder is very easy to handle under vacuum and under protective gas and thus used and processed in appropriate purity can. In this case, to achieve a small proportion of impurities, for example, oxygen contamination, processing under inert gas can be made.

Das oben beschriebene Herstellungsverfahren kann insbesondere für TiAl - Legierungen und insbesondere hochlegierte TiAl - Legierungen und/oder TiAl - Legierungen mit hohen Al - Gehalten, beispielsweise mit Al - Gehalten von mehr als 30 at.% Al, insbesondere mehr als 45 at.% Al, vorzugsweise mehr als 50 at.% und bis zu 60 at.% Al oder mehr eingesetzt werden, da bei diesen Legierungen die Ausbildung von fein verteilten Ausscheidungen und einer feinkörnigen, homogenen Mikrostruktur mit dem vorliegenden Verfahren günstig zu erzielen ist.The production method described above can be used in particular for TiAl alloys and in particular highly alloyed TiAl alloys and / or TiAl alloys with high Al contents, for example with Al contents of more than 30 at.% Al, in particular more than 45 at.% Al , preferably more than 50 at.% And up to 60 at.% Al or more are used, since in these alloys, the formation of finely divided precipitates and a fine-grained, homogeneous microstructure with the present method is to achieve low.

Bei der Herstellung des Pulvers für den Einsatz bei dem vorliegenden Verfahren können verschiedene Ausgangsmaterialien Verwendung finden, wie beispielsweise Pulver aus den einzelnen, zu legierenden Elementen oder zu recycelndes Pulver oder Pulver aus Masteralloys, also Legierungen, die Teile der späteren Legierungszusammensetzung umfassen. Die Ausgangsmaterialien können zu Presslingen gepresst werden, welche dann für das Erschmelzen der Legierung eingesetzt werden können.In the preparation of the powder for use in the present process, various starting materials may be used, such as powder of the individual elements to be alloyed or powder or powder of master alloys to be recycled, that is, alloys comprising parts of the later alloy composition. The starting materials can be pressed into compacts, which can then be used for melting the alloy.

Das Erschmelzen der Legierung kann durch einmaliges oder mehrmaliges Plasma - Lichtbogen - Schmelzen (PAM plasma arc melting), Vakuum - Lichtbogen - Schmelzen (VAR vacuum arc remelting) oder Vakuum - Induktions - Schmelzen (VIM vacuum induction melting) erfolgen. Beim Erschmelzen der TiAl - Legierung kann bereits eine mögliche Verarmung der Legierung bei der Herstellung und Verarbeitung, beispielsweise durch Abbrand von Elementen, wie z.B. Aluminium, beim Verdüsen berücksichtigt werden und somit die Legierungszusammensetzung entsprechend angepasst werden, also beispielsweise mit einem höheren Al - Anteil versehen werden.The melting of the alloy can be carried out by single or multiple plasma arc melting (PAM), vacuum arc melting (VAR) or vacuum induction melting (VIM). Upon melting of the TiAl alloy, even a possible depletion of the alloy during manufacture and processing, for example by burning off of elements such as e.g. Aluminum, are taken into account during atomization and thus the alloy composition are adjusted accordingly, so for example, be provided with a higher Al - share.

Das Pulver kann direkt aus der entsprechenden Schmelze oder nach erneutem Aufschmelzen nach einem zwischenzeitlichen Abgießen der Schmelze aus einem Schmelzbad oder aus einem zwischenzeitlich abgegossenem Ingot durch Verdüsen hergestellt werden. Als Verfahren können das Vakuum - Inertgas - Zerstäuben (VIG vacuum inert gas atomization), das Plasma - Schmelzen - Induktionsführungs - Zerstäuben (PIGA plasma melting induction guiding atomization) oder die Elektroden - Induktions - Zerstäubung (EIGA electrode induction gas atomization) eingesetzt werden.The powder can directly from the corresponding melt or after reflowing after an intermediate casting of the melt from a molten bath or from a meanwhile poured ingot can be produced by spraying. As the method, the vacuum inert gas atomization (VIG), the plasma melting induction induction atomization (PIGA) or the electrode induction gas atomization (EIGA) can be used.

Das Pulver kann weiterhin einem zusätzlichen Reinigungsprozess unterzogen werden, um beispielsweise die Sauerstoffbelegung der Pulveroberfläche zu reduzieren und somit die Sauerstoffkontamination des eingesetzten Werkstoffs für die Bauteilherstellung zu reduzieren sowie organische und/oder anorganische Verunreinigungen zu verringern oder zu beseitigen. Außerdem kann bei dem Reinigungsprozess eine Bearbeitung der Pulverpartikel dahingehend erfolgen, dass eine sphärische Partikelform eingestellt und/oder die Größe der Partikel (Korngröße) beeinflusst wird. Beispielsweise kann dies in einem Plasmareinigungsprozess erfolgen, bei dem die Pulverpartikel in ein Plasma eingebracht werden, sodass Kontaminationen entfernt werden und sich die Oberflächenform der Partikel einer Kugelform annähern kann.The powder may also be subjected to an additional purification process, for example, to reduce the oxygen occupancy of the powder surface and thus to reduce the oxygen contamination of the material used for component manufacturing and to reduce or eliminate organic and / or inorganic impurities. In addition, during the cleaning process, the powder particles can be processed to set a spherical particle shape and / or to influence the size of the particles (grain size). For example, this can be done in a plasma cleaning process in which the powder particles are introduced into a plasma so that contaminants can be removed and the surface shape of the particles can approach a spherical shape.

Das hergestellte Pulver kann entsprechend der Partikelgröße klassifiziert werden und es können ein oder mehrere Pulverfraktionen für die weitere Herstellung des Bauteils ausgewählt werden. Die Fraktionierung kann vor oder nach dem Reinigungsprozess durchgeführt werden, wobei eine Reinigung vor der Fraktionierung bevorzugt ist, da durch eine Plasma - Reinigung die Größe der Partikel verändert werden kann.The produced powder can be classified according to the particle size and one or more powder fractions can be selected for the further production of the component. Fractionation may be carried out before or after the purification process, with purification prior to fractionation being preferred, as the size of the particles may be altered by plasma purification.

Die Fraktionierung kann mit verschiedenen bekannten Verfahren durchgeführt werden und insbesondere ist eine zweistufige Fraktionierung möglich, bei der z.B. zunächst mittels einer Zentrifuge eine Vorfraktionierung erfolgt und anschließend in einem zweiten Schritt durch Sieben und/oder Sichten eine Hauptfraktion erzeugt wird. Für die Herstellung eines feinkörnigen TiAl - Werkstoffs können insbesondere Pulverfraktionen mit durchschnittlichen oder maximalen Partikelgrößen ≤ 125µm im Durchmesser oder entsprechend der maximalen Erstreckung ausgewählt werden.The fractionation may be carried out by various known methods, and in particular, a two-stage fractionation is possible wherein e.g. First, a prefractionation takes place by means of a centrifuge, and then, in a second step, a main fraction is produced by sieving and / or sifting. For the production of a fine-grained TiAl material, in particular powder fractions with average or maximum particle sizes ≤ 125 μm in diameter or corresponding to the maximum extent can be selected.

Die Kapsel, in die das Pulver für das nachfolgende heiß - isostatische Pressen eingefüllt wird, kann aus einem Blech aus einem ähnlichen Material wie das Pulver gefertigt werden, insbesondere aus dem Basis - Material des eingesetzten Pulvers, also beispielsweise einer Legierung mit dem gleichen Hauptbestandteil. Bei Verwendung einer TiAl - Legierung zur Herstellung des Bauteils kann die Kapsel mit beispielsweise 1 bis 3 mm, vorzugsweise 2 bis 3 mm, Wandstärke aus Titan oder einer Titan - Legierung gebildet sein.The capsule into which the powder is filled for the subsequent hot isostatic pressing can be made of a sheet of a material similar to the powder, in particular of the base material of the powder used, that is, for example, an alloy having the same main constituent. When using a TiAl alloy for production of the component, the capsule may be formed with, for example, 1 to 3 mm, preferably 2 to 3 mm, wall thickness of titanium or a titanium alloy.

Darüber hinaus kann die Kapsel aus mindestens zwei Formteilen gebildet sein, die zum Verschließen der Kapsel miteinander verbunden werden können, beispielsweise durch Schweißen unter Schutzgas.In addition, the capsule can be formed from at least two mold parts, which can be connected together to close the capsule, for example by welding under inert gas.

Die Formteile der Kapsel können aus tiefgezogenen Blechen des entsprechenden Kapselmaterials gebildet sein, sodass eine der Form des herzustellenden Bauteils ähnliche Kontur der Kapsel in einfacher Weise hergestellt werden kann. Wie bereits vorher erwähnt, kann die Kontur bzw. Form der Kapsel mit einem gewissen Aufmaß ausgebildet sein, welches die Formänderungen beim anschließenden heißisostatischen Pressen und den Wärmebehandlungen berücksichtigt bzw. eine nachgeschalteten Nachbearbeitung durch Materialabtrag erlaubt, die die Möglichkeit gibt, die exakte gewünschte Form des Bauteils zu erzeugen.The molded parts of the capsule can be formed from deep-drawn sheets of the corresponding capsule material, so that a contour of the capsule which is similar to the shape of the component to be produced can be produced in a simple manner. As already mentioned above, the contour or shape of the capsule can be formed with a certain allowance, which takes into account the shape changes in the subsequent hot isostatic pressing and the heat treatments or allows a subsequent post-processing by material removal, which gives the possibility of the exact desired shape of the To produce component.

Das Einfüllen des Pulvers in die Kapsel kann unter Schutzgas erfolgen, um so die Belastung mit Kontaminationen weiter zu verringern. Insbesondere kann das Einfüllen des Pulvers in die Kapsel direkt im Anschluss an die Reinigung unter Vakuum oder Schutzgas erfolgen, sodass das Pulver nicht mehr der Umgebungsatmosphäre ausgesetzt wird.The filling of the powder in the capsule can be done under inert gas, so as to further reduce the burden of contamination. In particular, the filling of the powder into the capsule can take place directly after the cleaning under vacuum or inert gas, so that the powder is no longer exposed to the ambient atmosphere.

Zusätzlich kann die befüllte, aber noch nicht verschlossene Kapsel - oder alternativ auch das Pulver vor dem Abfüllen in die Kapsel - einer Wärmebehandlung unter Vakuum (Reinigungswärmebehandlung) ausgesetzt werden, um eine weitere Reinigung des Pulvermaterials durch Verdampfen bzw. Ausgasen zu bewirken. Beispielsweise kann die Wärmebehandlung bei einer Temperatur im Bereich von 200°C bis 500°C, vorzugsweise zwischen 440°C und 460°C bei Vakuum mit einem Druck ≤10-3 mbar , insbesondere ≤10-5 mbar oberhalb des Pulvers durchgeführt werden. Damit lässt sich beispielsweise der Sauerstoffgehalt bei der Herstellung eines Bauteils aus einer TiAl - Legierung auf einem Bereich ≤ 600 ppm verringern.In addition, the filled but not yet sealed capsule - or alternatively the powder prior to filling into the capsule - can be subjected to a heat treatment under vacuum (cleaning heat treatment) to effect further purification of the powder material by evaporation or outgassing. For example, the heat treatment at a temperature in the range of 200 ° C to 500 ° C, preferably between 440 ° C and 460 ° C under vacuum with a pressure ≤10 -3 mbar, in particular ≤10 -5 mbar above the powder can be performed. Thus, for example, the oxygen content in the production of a component made of a TiAl alloy can be reduced to a range of ≦ 600 ppm.

Die Abkühlung der Oberfläche der Kapsel mit dem eingefüllten Pulver nach der Reinigungswärmebehandlung kann mit einer Abkühlrate von 25°C/min bis 35°C/min, vorzugsweise bei 30°C/min bis zu einer Temperatur von 120°C oder darunter, insbesondere auf 100°C, unter Vakuum durchgeführt werden, wobei anschließend das Verschließen der Kapsel beispielsweise durch Verschweißen unter Schutzgas erfolgen kann. Durch die schnelle Abkühlung kann das herrschende Vakuum verbessert, also niedrigere Drücke erzeugt werden, sodass die Reinigung des Pulvers weiter verbessert werden kann. Beispielsweise kann sich das Vakuum von 10-3 mbar auf 10-4 mbar verbessern.The cooling of the surface of the capsule with the filled powder after the cleaning heat treatment can at a cooling rate of 25 ° C / min to 35 ° C / min, preferably at 30 ° C / min up to a temperature of 120 ° C or below, in particular 100 ° C, are carried out under vacuum, wherein subsequently the closure of the capsule can be done for example by welding under inert gas. Rapid cooling can improve the prevailing vacuum, allowing lower pressures to be generated and cleaning of the powder can be further improved. For example, the vacuum can improve from 10 -3 mbar to 10 -4 mbar.

Um die Schrumpfung und den Verzug kontrollieren zu können, kann das Pulver in der Kapsel durch mechanische Anregung, wie Vibration, Rütteln, Klopfen oder dergleichen verdichtet werden. Die Kapsel kann dabei noch offen oder verschlossenen sein, wobei bei einer offenen Kapsel die mechanische Verdichtung unter Vakuum erfolgen kann.In order to control shrinkage and distortion, the powder in the capsule may be densified by mechanical stimulation such as vibration, vibration, tapping or the like. The capsule can still be open or closed, wherein in an open capsule, the mechanical compression can be carried out under vacuum.

Die so vorbereitete Kapsel kann bei Temperaturen im Bereich von 1100°C bis 1400°C, insbesondere 1150°C bis 1300°C bei einem Druck von 100 bis 250 MPa für eine Zeitdauer von zwei bis sechs Stunden heißisostatisch gepresst werden, sodass sich ein kompaktierter Materialblock in einer endkonturnahen Form des Bauteils ergibt.The thus prepared capsule can be hot isostatically pressed at temperatures in the range of 1100 ° C to 1400 ° C, especially 1150 ° C to 1300 ° C at a pressure of 100 to 250 MPa for a period of two to six hours, so that a compacted Material block in a near-net shape of the component results.

Die endkonturnahe Form kann so gewählt werden, dass das hergestellte Bauteil den Anforderungen der Herstellung von net - shape - Bauteilen oder near - net - shape - Bauteilen entspricht. Beispielsweise kann die heißisostatisch gepresste Kapsel ein Übermaß gegenüber dem fertigen Bauteil von 0,5 mm bis 5 mm, insbesondere 0,5 mm oder 1 mm bis 2 mm (net shape) oder 2 mm bis 5 mm (near net shape) plus jeweils der entsprechenden Kapseldicke aufweisen.The shape close to the final contour can be chosen such that the manufactured component meets the requirements of the production of net - shape components or near - net - shape components. For example, the hot isostatically pressed capsule may have an oversize of the finished component of 0.5 mm to 5 mm, in particular 0.5 mm or 1 mm to 2 mm (net shape) or 2 mm to 5 mm (near net shape) plus the respective have corresponding capsule thickness.

Nach dem heißisostatischen Pressen wird die Kapsel einer mehrstufigen Wärmebehandlung unterzogen, bei der entsprechend dem eingesetzten Pulvermaterial eine Lösungsglühung, eine Hochtemperaturglühung und eine Auslagerungsglühung in dieser Reihenfolge durchgeführt wird.After the hot isostatic pressing, the capsule is subjected to a multi-stage heat treatment in which solution annealing, high-temperature annealing and aging annealing are performed in this order according to the powder material used.

Bei der Verwendung einer TiAl - Legierung wird eine Lösungsglühung bei einer Temperatur bis zu 1400°C für 15 bis 45 Minuten durchgeführt. Die Hochtemperaturglühung wird bei einer Temperatur von 1100°C bis 1300°C durchgeführt und eine Auslagerungsglühung erfolgt bei einer Temperatur von 850°C bis 1100°C für sechs bis hundert Stunden.When using a TiAl alloy, solution annealing is carried out at a temperature up to 1400 ° C for 15 to 45 minutes. The high-temperature annealing is carried out at a temperature of 1100 ° C to 1300 ° C and an aging annealing is carried out at a temperature of 850 ° C to 1100 ° C for six to one hundred hours.

Die Aufheiz - und/oder Abkühlraten für die Wärmebehandlung können in Abhängigkeit der Größe und/oder der Form des Bauteils gewählt werden, wobei beispielsweise für größere Bauteile eher geringere Aufheiz - und/oder Abkühlraten gewählt werden, während für kleine Bauteile größere Aufheiz - und/oder Abkühlraten realisiert werden können. Außerdem können die Aufheiz - und/oder Abkühlraten so bestimmt werden, dass möglichst kein Verzug des Bauteils stattfindet.The heating and / or cooling rates for the heat treatment can be selected as a function of the size and / or the shape of the component, whereby, for example, relatively lower heating and / or cooling rates are selected for larger components, while for small components greater heating and / or or cooling rates can be realized. In addition, you can the heating and / or cooling rates are determined so that as far as possible no distortion of the component takes place.

Nach der Wärmebehandlung wird die Kapsel entfernt, und zwar beispielsweise durch chemisches Beizen, elektrochemische Bearbeitung, Strahlen mit Partikeln, insbesondere mit Kunststoffgranulat und/oder spanabhebende mechanische Bearbeitung, wie Fräsen oder Schleifen. Danach kann die Nachbearbeitung der äußeren Form (Kontur) des Bauteils durch mechanische, spannabhebende Bearbeitung, insbesondere durch Fräsen, Schleifen, Polieren etc. und/oder elektrochemische Bearbeitung erfolgen.After the heat treatment, the capsule is removed, for example by chemical pickling, electrochemical machining, blasting with particles, in particular with plastic granules and / or machining, such as milling or grinding. Thereafter, the post-processing of the outer shape (contour) of the component by mechanical, spannabhebende processing, in particular by milling, grinding, polishing, etc. and / or electrochemical machining done.

Auf dem so hergestellten Bauteil können verschiedene Funktionsschichten aufgebracht werden, wie beispielsweise Verschleißschutzschichten, Korosionsschutzschichten, Oxidationsschutzschichten und dergleichen.Various functional layers can be applied to the component produced in this way, for example wear protection layers, corrosion protection layers, oxidation protection layers and the like.

Während des Verfahrens können das Bauteil und/oder das Material bzw. der Werkstoff, aus dem das Bauteil hergestellt ist, charakterisiert werden, insbesondere durch zerstörungsfreie Verfahren, wie beispielsweise durch Röntgendiffraktometrie.During the process, the component and / or the material or the material of which the component is made can be characterized, in particular by non-destructive methods, such as, for example, by X-ray diffractometry.

Unter einer TiAl - Legierung wird gemäß der vorliegenden Erfindung ein Werkstoff verstanden wird, der als Hauptbestandteile Titan und Aluminium aufweist. Unter Hauptbestandteile werden diejenigen Elemente verstanden, deren Anteil in at.% oder Gew.% der größte ist, also bei einer TiAl - Legierung Titan und Aluminium als Elemente mit den größten Anteilen in at.% oder Gew.% in der Legierung vorliegen. Bei einer TiAl - Legierung, die gemäß dem vorliegenden Verfahren zu einem Bauteil verarbeitet wird, kann es sich insbesondere um eine hochlegierte TiAl - Legierung handeln, die insbesondere für hohe Temperaturen z. B. als Schaufelwerkstoff für Strömungsmaschinen eingesetzt werden kann. Entsprechend können chemische Elemente wie Niob, Molybdän, Wolfram, Kobalt, Chrom, Vanadium, Zirkon, Silizium, Kohlenstoff, Erbium, Gadolinium, Hafnium, Yttrium und Bor enthalten sein.Under a TiAl - alloy is understood according to the present invention, a material having as main constituents of titanium and aluminum. Main constituents are understood to mean those elements whose proportion in at.% Or wt.% Is the largest, ie in the case of a TiAl alloy titanium and aluminum as elements having the largest proportions in at.% Or wt.% In the alloy. In the case of a TiAl alloy which is processed into a component according to the present method, it can be, in particular, a high-alloy TiAl alloy, which is particularly suitable for high temperatures, for example. B. can be used as a blade material for turbomachinery. Accordingly, chemical elements such as niobium, molybdenum, tungsten, cobalt, chromium, vanadium, zirconium, silicon, carbon, erbium, gadolinium, hafnium, yttrium and boron may be included.

AUSFÜHRUNGSBEISPIELEmbodiment

Weitere Vorteile, Kennzeichen und Merkmale der vorliegenden Erfindung werden bei der nachfolgenden detaillierten Beschreibung eines Ausführungsbeispiels deutlich. Allerdings ist die Erfindung nicht auf dieses Ausführungsbeispiel beschränkt.Further advantages, characteristics and features of the present invention will become apparent in the following detailed description of an embodiment. However, the invention is not limited to this embodiment.

Nach einem Ausführungsbeispiel wird mit dem erfindungsgemäßen Verfahren eine Laufschaufel eines Flugtriebwerks aus einer hochlegierten TiAl - Legierung gebildet, wobei zunächst in einem ersten Schritt ein Pressling aus Pulvern der einzelnen zu legierenden Elemente und/oder von sogenannten Masteralloys gepresst wird. Außerdem kann der Pressling Titanschwamm enthalten (Verfahrensschritt I).According to one exemplary embodiment, the method according to the invention forms a rotor blade of an aircraft engine made of a highly alloyed TiAl alloy, wherein first in a first step, a compact of powders of the individual elements to be alloyed and / or of so-called master alloys is pressed. In addition, the compact may contain titanium sponge (step I).

Der Pressling wird anschließend (Verfahrensschritt II) durch einen einmaligen Plasma - Lichtbogen - Schmelzvorgang aufgeschmolzen, sodass sich eine Legierungsschmelze ergibt. Diese wird zunächst abgegossen und anschließend in einem dritten Verfahrensschritt (Verfahrensschritt III) für die Pulverherstellung ein zweites Mal aufgeschmolzen, um eine Gasverdüsung aus dem Schmelzbad vornehmen zu können. Die Gasverdüsung aus dem Schmelzbad kann durch VIGA oder PIGA-Verfahren erfolgen, wobei durch die Gasverdüsung möglichst sphärische Pulverpartikel erzeugt werden sollen.The compact is subsequently melted (method step II) by a single plasma arc melting process, so that an alloy melt results. This is first poured off and then melted a second time in a third process step (process step III) for powder production in order to make a gas atomization from the molten bath can. The gas atomization from the molten bath can be carried out by VIGA or PIGA process, whereby as spherical as possible powder particles are to be produced by the gas atomization.

In einem vierten Verfahrensschritt (Verfahrensschritt IV) werden aus dem erzeugten Pulver die für die Weiterverarbeitung gewünschten Partikelgrößenfraktionen ausgewählt, beispielsweise Partikelgrößenfraktionen mit maximalen oder durchschnittlichen Durchmessern der Partikel im Bereich von 15 bis 150µm oder vorzugsweise 45 bis 125µm. Bei dem gewählten Ausführungsbeispiel wird die Partikelgröße ≤125µm gehalten, um ein feinkörniges Gefüge zu erzielen.In a fourth method step (method step IV), the particle size fractions desired for further processing are selected from the powder produced, for example particle size fractions with maximum or average diameters of the particles in the range from 15 to 150 μm or preferably 45 to 125 μm. In the chosen embodiment, the particle size ≤125μm is maintained in order to achieve a fine-grained structure.

In einem fünften Verfahrensschritt (Verfahrensschritt V) wird die gewählte Pulverfraktion in ein Plasma eingegeben, sodass durch das Plasma eine Reinigung der Pulverpartikel und eine sphärische Ausbildung der Pulverpartikel erfolgt. Durch das Plasma wird beispielsweise die Sauerstoffbelegung an der Pulveroberfläche reduziert und die Oberflächenform einer Kugelform angenähert.In a fifth method step (method step V), the selected powder fraction is introduced into a plasma, so that the plasma cleans the powder particles and forms a spherical formation of the powder particles. For example, the plasma reduces the oxygen occupancy of the powder surface and approximates the surface shape to a spherical shape.

Das so gereinigte Pulver wird unter Schutzgas, beispielsweise Helium oder Argon in Kapseln aus Titan eingefüllt (Verfahrensschritt VI), die beispielsweise eine Wandstärke von 1 bis 2 mm aufweisen, und entsprechend der Form des herzustellenden Bauteils beispielsweise aus zwei tiefgezogenen Titan-Blechen geformt sind. Bei dem Titanmaterial, das für die Kapseln verwendet wird, kann es sich um sogenanntes Titan Grade I Material handeln.The thus purified powder is filled under protective gas, for example helium or argon in capsules made of titanium (step VI), for example, have a wall thickness of 1 to 2 mm, and are formed according to the shape of the component to be produced, for example, two deep-drawn titanium sheets. The titanium material used for the capsules may be so-called titanium grade I material.

Vor dem Verschließen der Kapsel durch Zusammenschweißen der Kapselteile im neunten Verfahrensschritt wird in einem siebten Verfahrensschritt (Verfahrensschritt VII) eine weitere Reinigung des Materials durchgeführt, indem die mit Pulver gefüllte, aber noch nicht verschlossene Kapsel unter Vakuumbedingungen bei einem Druck von ≤10-3 mbar, insbesondere ≤10-5 mbar bei Temperaturen bis 450°C ausgeheizt wird, damit weitere Verunreinigungen durch Verdampfen verflüchtigen. Auf diese Weise lässt sich beispielsweise der Sauerstoffgehalt ≤600 ppm einstellen. Von der Ausheiztemperatur kann die weiterhin unter Vakuum gehaltene Kapsel auf 120°C oder 100°C abgekühlt werden, wobei eine Abkühlrate von 30°C/min gewählt werden kann (Verfahrensschritt VIII).Before sealing the capsule by welding together the capsule parts in the ninth step, a further purification of the material is carried out in a seventh process step (step VII) by the powder-filled, but not yet sealed capsule under vacuum conditions at a pressure of ≤10 -3 mbar , in particular ≤10 -5 mbar is heated at temperatures up to 450 ° C, so that further impurities volatilize by evaporation. In this way, for example, the oxygen content ≤600 ppm can be set. From the baking temperature, the capsule, which is furthermore kept under vacuum, can be cooled to 120 ° C. or 100 ° C., wherein a cooling rate of 30 ° C./min can be selected (method step VIII).

Im neunten Verfahrensschritt (Verfahrensschritt IX) wird die Kapsel durch Verschweißen verschlossen, sodass im zehnten Verfahrensschritt (Verfahrensschritt X) die Kapsel mit dem darin eingeschlossenen Pulver heißisostatisch gepresst werden kann und zwar bei einem Druck im Bereich von 100 bis 240 MPa und einer Temperatur im Bereich von 1150°C bis 1400°C für eine Zeitdauer von zwei bis sechs Stunden.In the ninth process step (process step IX), the capsule is closed by welding, so that in the tenth process step (process step X) the capsule can be hot isostatically pressed with the powder enclosed therein at a pressure in the range of 100 to 240 MPa and a temperature in the range from 1150 ° C to 1400 ° C for a period of two to six hours.

Nach dem heißisostatischen Pressen (Verfahrensschritt X) schließt sich als elfter Verfahrensschritt (Verfahrensschritt XI) eine mehrstufige Wärmebehandlung an, mit deren Hilfe die Mikrostruktur des Bauteils eingestellt werden kann. Zunächst erfolgt ein Lösungsglühen bei 1400°C oder knapp darunter für eine Zeitdauer von 15 bis 45 Minuten. Danach wird eine Hochtemperaturglühung bei 1100°C bis 1300°C durchgeführt und zum Abschluss erfolgt eine Auslagerungsglühung bei 850°C bis 1100°C für eine Zeitdauer von sechs bis hundert Stunden. Danach ist das Bauteil bezüglich des Werkstoffgefüges fertiggestellt und es müssen lediglich noch abschließende Arbeiten bezüglich der Formgebung des Bauteils durchgeführt werden.After hot isostatic pressing (process step X), the eleventh process step (process step XI) is followed by a multi-stage heat treatment, with the aid of which the microstructure of the component can be adjusted. First, a solution heat treatment at 1400 ° C or just below for a period of 15 to 45 minutes. Thereafter, a high-temperature annealing is carried out at 1100 ° C to 1300 ° C, and finally, an aging annealing is carried out at 850 ° C to 1100 ° C for a period of six to one hundred hours. Thereafter, the component is finished with respect to the material structure and it only need to be done final work on the shape of the component.

Hierzu wird in einem zwölften Verfahrensschritt (Verfahrensschritt XII) die Kapsel entfernt, und zwar durch Abbeizen der Außenschicht und/oder elektrochemische Bearbeitung, Strahlen mit Partikeln, insbesondere Kunststoffpartikeln, und/oder durch mechanische Bearbeitung, wie Fräsen, Schleifen oder dergleichen.For this purpose, the capsule is removed in a twelfth method step (method step XII), namely by pickling the outer layer and / or electrochemical machining, blasting with particles, in particular plastic particles, and / or by mechanical processing, such as milling, grinding or the like.

In einem dreizehnten Verfahrensschritt (Verfahrensschritt XIII) wird nunmehr durch mechanische, insbesondere spanabhebende Bearbeitung das überschüssige Material von dem Bauteil entfernt, beispielsweise durch Fräsen, Schleifen, Polieren und dergleichen. Alternativ kann der Materialabtrag auch durch elektrochemische Bearbeitung erfolgen, sodass das Endmaß eingestellt wird.In a thirteenth method step (method step XIII), the excess material is now removed from the component by mechanical, in particular machining, for example by milling, grinding, polishing and the like. Alternatively, the material removal can also be done by electrochemical machining, so that the final dimension is set.

Die eingestellte Mikrostruktur des Bauteils lässt sich durch Röntgendiffraktometrie und sonstige zerstörungsfreie Prüfverfahren überprüfen. Des Weiteren können auf dem Bauteil erforderliche Schichten, wie Korrosionsschutzschichten, Oxidationsschutzschichten, Verschleißschutzschichten und dergleichen abgeschieden werden.The set microstructure of the component can be checked by X-ray diffractometry and other nondestructive testing methods. Furthermore, required on the component layers such as corrosion protection layers, oxidation protection layers, wear protection layers and the like can be deposited.

Obwohl die vorliegende Erfindung anhand des Ausführungsbeispiels detailliert beschrieben worden ist, ist die Erfindung nicht auf dieses Ausführungsbeispiel beschränkt, sondern vielmehr können Abänderungen in der Weise vorgenommen werden, dass einzelne Merkmale weggelassen oder andersartige Kombinationen von Merkmalen verwirklicht werden, solange der Schutzbereich der beigefügten Ansprüche nicht verlassen wird.Although the present invention has been described in detail with reference to the embodiment, the invention is not limited to this embodiment, but modifications may be made such that individual features are omitted or other combinations of features are realized unless the scope of the appended claims will leave.

Claims (17)

  1. Method for producing a component, in particular a component for a turbomachine, made of a TiAl alloy, which method comprises the following steps in the given sequence:
    - producing a powder from the TiAl alloy;
    - producing a capsule, the shape of which corresponds to the shape of the component to be produced;
    - pouring the powder into the capsule and sealing said capsule;
    - hot-isostatically pressing the capsule together with the powder;
    - heat-treating the hot-isostatically pressed capsule, wherein the heat treatment comprises, in the given sequence:
    - solution annealing at a temperature of up to 1400°C for 15 to 45 min;
    - high-temperature annealing at a temperature of from 1100°C to 1300°C for 15 to 120 min; and
    - precipitation annealing at a temperature of from 850°C to 1100°C for 6 to 100 h;
    - removing the capsule;
    - finishing the contour of the component by removing material.
  2. Method according to claim 1, characterized in that the production of the powder comprises at least one of the following steps, preferably all the steps in the given sequence:
    • pressing starting materials or smelting master alloys which consist of or comprise the components to be alloyed;
    • smelting the alloy by single or repeated plasma arc melting (PAM) or vacuum arc remelting (VAR) or vacuum induction melting (VIM);
    • atomizing the alloy to produce the powder from a molten bath or by means of a cast ingot, in particular using one of the methods which comprise vacuum inert gas atomization (VIGA), plasma melting induction guiding atomization (PIGA), electrode induction gas atomization (EIGA), and plasma rotating electrode process (PREP);
    • classifying powder fractions and selecting one or more powder fractions having average or maximum particle sizes of less than or equal to 150 µm, in particular less than or equal to 125 µm, in diameter or maximum extension, in particular particles having maximum or average diameters of the particle in the range of from 15 to 150 µm or preferably 45 to 125 µm; and
    • cleaning the powder in a plasma cleaning process.
  3. Method according to either of the preceding claims, characterized in that the capsule is formed of titanium or a Ti alloy.
  4. Method according to any of the preceding claims, characterized in that the capsule is formed of at least two shaped parts, which are in particular welded together, preferably under protective gas.
  5. Method according to any of the preceding claims, characterized in that the capsule is formed with a machining allowance with respect to the component to be produced.
  6. Method according to any of the preceding claims, characterized in that the powder is poured in under protective gas or under vacuum.
  7. Method according to any of the preceding claims, characterized in that the powder before it is filled into the capsule, or the filled but not yet sealed capsule, is subjected to heat treatment under vacuum, in particular heat treatment at a temperature in the range of from 200°C to 500°C, preferably between 440°C and 460°C, and to a pressure of less than or equal to 10-3 mbar, in particular less than or equal to 10-5 mbar.
  8. Method according to claim 7, characterized in that, after the heat treatment, the cooling takes place at a cooling rate of from 25°C/min to 35°C/min, in particular 30°C/min, to a temperature of 120°C or less, in particular 100°C or less.
  9. Method according to any of the preceding claims, characterized in that the packing density of the powder in the capsule is increased by mechanical agitation before or after the sealing.
  10. Method according to any of the preceding claims, characterized in that the hot-isostatic pressing takes place in the temperature range of from 1100°C to 1400°C, in particular 1150°C to 1300°C, at a pressure of from 100 to 250 MPa for a period of from 2 to 6 h.
  11. Method according to any of the preceding claims, characterized in that a net-shape component or near-net-shape component is produced by the hot-isostatic pressing.
  12. Method according to any of the preceding claims, characterized in that the capsule is removed by chemical pickling, electrochemical machining and/or mechanical machining.
  13. Method according to any of the preceding claims, characterized in that the contour is finished by mechanical material removal, in particular milling, and/or by electrochemical machining.
  14. Method according to any of the preceding claims, characterized in that the component is provided with suitable functional coatings.
  15. Method according to any of the preceding claims, characterized in that the component and/or the material from which the component has been produced is characterized, in particular by X-ray diffraction.
  16. Method according to any of the preceding claims, characterized in that the alloy comprises one or more constituents from the group which contains Nb, Mo, W, Co, Cr, V, Zr, Si, C, Er, Gd, Hf, Y and B.
  17. Method according to any of the preceding claims, characterized in that, in addition to the main constituents Ti and Al, the alloy contains the following elements in the specified proportions and is preferably, with the exception of unavoidable impurities, formed of said elements: W 0 to 3 at.%; and/or Si 0.2 to 0.35 at.%; and/or C 0 to 0.6 at.%; and/or Zr 0 to 6 at.%; and/or Y 0 to 0.5 at.%; and/or Hf 0 to 0.3 at.%; and/or Er 0 to 0.5 at.%; and/or Gd 0 to 0.5 at.%; and/or B 0 to 0.2 at.%; and/or Nb 4 to 25 at.%; and/or Mo 1 to 10 at.%; and/or W 0.5 to 3 at.%; and/or Co 0.1 to 10 at.%; and/or Cr 0.5 to 3 at.%; and/or V 0.5 to 10 at.%.
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