EP2990141A1 - Procédé de fabrication de composants en Titanaluminide (TiAI) - Google Patents

Procédé de fabrication de composants en Titanaluminide (TiAI) Download PDF

Info

Publication number
EP2990141A1
EP2990141A1 EP14182981.2A EP14182981A EP2990141A1 EP 2990141 A1 EP2990141 A1 EP 2990141A1 EP 14182981 A EP14182981 A EP 14182981A EP 2990141 A1 EP2990141 A1 EP 2990141A1
Authority
EP
European Patent Office
Prior art keywords
capsule
powder
component
alloy
heat treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP14182981.2A
Other languages
German (de)
English (en)
Other versions
EP2990141B1 (fr
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
Original Assignee
MTU Aero Engines AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by MTU Aero Engines AG filed Critical MTU Aero Engines AG
Priority to EP14182981.2A priority Critical patent/EP2990141B1/fr
Priority to ES14182981T priority patent/ES2728527T3/es
Priority to US14/838,802 priority patent/US10029309B2/en
Publication of EP2990141A1 publication Critical patent/EP2990141A1/fr
Application granted granted Critical
Publication of EP2990141B1 publication Critical patent/EP2990141B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/009Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine components other than turbine blades
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D29/00Removing castings from moulds, not restricted to casting processes covered by a single main group; Removing cores; Handling ingots
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00Casting ingots, e.g. from ferrous metals
    • B22D7/005Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/04Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine blades
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • C22C1/0458Alloys based on titanium, zirconium or hafnium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/047Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00Electrolytic stripping of metallic layers or coatings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2202/00Treatment under specific physical conditions
    • B22F2202/13Use of plasma
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00Metallic composition of the powder or its coating
    • B22F2301/20Refractory metals
    • B22F2301/205Titanium, zirconium or hafnium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes 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.
  • 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 may be subjected to a heat treatment, in particular a multi-stage heat treatment, in which a solution annealing, a high-temperature annealing and an aging annealing can be performed in this order according to the powder material used.
  • a heat treatment in particular a multi-stage heat treatment, in which a solution annealing, a high-temperature annealing and an aging annealing can be performed in this order according to the powder material used.
  • a heat treatment in particular a multi-stage heat treatment, in which a solution annealing, a high-temperature annealing and an aging annealing can be performed in this order according to the powder material used.
  • solution annealing may be performed at a temperature up to 1400 ° C for 15 to 45 minutes.
  • the high-temperature annealing may be performed at a temperature of 1100 ° C to 1300 ° C, and an aging annealing may be performed 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 can be 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.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Powder Metallurgy (AREA)
EP14182981.2A 2014-09-01 2014-09-01 Procédé de fabrication de composants en Titanaluminide (TiAI) Not-in-force EP2990141B1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP14182981.2A EP2990141B1 (fr) 2014-09-01 2014-09-01 Procédé de fabrication de composants en Titanaluminide (TiAI)
ES14182981T ES2728527T3 (es) 2014-09-01 2014-09-01 Procedimiento de fabricación de componentes de TiAl
US14/838,802 US10029309B2 (en) 2014-09-01 2015-08-28 Production process for TiAl components

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP14182981.2A EP2990141B1 (fr) 2014-09-01 2014-09-01 Procédé de fabrication de composants en Titanaluminide (TiAI)

Publications (2)

Publication Number Publication Date
EP2990141A1 true EP2990141A1 (fr) 2016-03-02
EP2990141B1 EP2990141B1 (fr) 2019-04-03

Family

ID=51453656

Family Applications (1)

Application Number Title Priority Date Filing Date
EP14182981.2A Not-in-force EP2990141B1 (fr) 2014-09-01 2014-09-01 Procédé de fabrication de composants en Titanaluminide (TiAI)

Country Status (3)

Country Link
US (1) US10029309B2 (fr)
EP (1) EP2990141B1 (fr)
ES (1) ES2728527T3 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3450056A1 (fr) * 2017-09-01 2019-03-06 MTU Aero Engines GmbH Procédé de fabrication d'un composant d'aluminiure de titane à noyau dur et composant fabriqué selon ledit procédé
DE102018208709A1 (de) 2018-06-04 2019-12-05 MTU Aero Engines AG Kapsel zur Herstellung eines Bauteils für eine Strömungsmaschine, Verfahren zur Herstellung eines Bauteils für eine Strömungsmaschine und Bauteil für eine Strömungsmaschine

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016224532A1 (de) * 2016-12-08 2018-06-14 MTU Aero Engines AG Hochtemperaturschutzschicht für Titanaluminid-Legierungen
KR102197604B1 (ko) * 2017-11-24 2021-01-05 한국재료연구원 고온 특성이 우수한 3d 프린팅용 타이타늄-알루미늄계 합금 및 이의 제조방법
CN108115365A (zh) * 2017-12-20 2018-06-05 西安西工大超晶科技发展有限责任公司 一种钛铝合金铸锭的包套开坯锻造成型工艺
CN110586948A (zh) * 2019-09-09 2019-12-20 中国人民解放军第五七一九工厂 航空发动机低成本双性能粉末涡轮盘的制备方法
CN111455203A (zh) * 2020-05-28 2020-07-28 陕西工业职业技术学院 一种3D打印制粉用TiAl棒材的制备方法
CN113664199A (zh) * 2021-08-20 2021-11-19 西安欧中材料科技有限公司 航空发动机涡轮叶片热等静压近净成型方法
CN114921735B (zh) * 2022-06-02 2022-11-18 中国航发北京航空材料研究院 改善铸造用高Nb-TiAl合金力学性能的热调控方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5098484A (en) * 1991-01-30 1992-03-24 The United States Of America As Represented By The Secretary Of The Air Force Method for producing very fine microstructures in titanium aluminide alloy powder compacts
US5424027A (en) 1993-12-06 1995-06-13 The United States Of America As Represented By The Secretary Of The Air Force Method to produce hot-worked gamma titanium aluminide articles
JP2008208432A (ja) * 2007-02-27 2008-09-11 Kinzoku Giken Kk TiAl金属間化合物基合金の粉末焼結体の製造方法

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4094672A (en) * 1975-12-22 1978-06-13 Crucible Inc. Method and container for hot isostatic compacting
US4834942A (en) * 1988-01-29 1989-05-30 The United States Of America As Represented By The Secretary Of The Navy Elevated temperature aluminum-titanium alloy by powder metallurgy process
US5768679A (en) * 1992-11-09 1998-06-16 Nhk Spring R & D Center Inc. Article made of a Ti-Al intermetallic compound
JP3459138B2 (ja) * 1995-04-24 2003-10-20 日本発条株式会社 TiAl系金属間化合物接合体およびその製造方法
DE10355036A1 (de) * 2003-11-25 2005-06-23 Mtu Aero Engines Gmbh Verfahren zur Herstellung einer Schutzschicht, Schutzschicht und Bauteil mit einer solchen Schutzschicht
JP4384557B2 (ja) * 2004-06-23 2009-12-16 新日鉄マテリアルズ株式会社 チタンアルミ金属間化合物製精密機械装置用部材の製造方法及び精密機械装置用部材
US20060083653A1 (en) * 2004-10-20 2006-04-20 Gopal Das Low porosity powder metallurgy produced components
US20130248061A1 (en) * 2012-03-23 2013-09-26 General Electric Company Methods for processing titanium aluminide intermetallic compositions
US20160138423A1 (en) * 2013-03-15 2016-05-19 Rolls-Royce North American Technologies, Inc. Titanium-aluminide components

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5098484A (en) * 1991-01-30 1992-03-24 The United States Of America As Represented By The Secretary Of The Air Force Method for producing very fine microstructures in titanium aluminide alloy powder compacts
US5424027A (en) 1993-12-06 1995-06-13 The United States Of America As Represented By The Secretary Of The Air Force Method to produce hot-worked gamma titanium aluminide articles
JP2008208432A (ja) * 2007-02-27 2008-09-11 Kinzoku Giken Kk TiAl金属間化合物基合金の粉末焼結体の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3450056A1 (fr) * 2017-09-01 2019-03-06 MTU Aero Engines GmbH Procédé de fabrication d'un composant d'aluminiure de titane à noyau dur et composant fabriqué selon ledit procédé
DE102018208709A1 (de) 2018-06-04 2019-12-05 MTU Aero Engines AG Kapsel zur Herstellung eines Bauteils für eine Strömungsmaschine, Verfahren zur Herstellung eines Bauteils für eine Strömungsmaschine und Bauteil für eine Strömungsmaschine

Also Published As

Publication number Publication date
EP2990141B1 (fr) 2019-04-03
US10029309B2 (en) 2018-07-24
US20160059312A1 (en) 2016-03-03
ES2728527T3 (es) 2019-10-25

Similar Documents

Publication Publication Date Title
EP2990141B1 (fr) Procédé de fabrication de composants en Titanaluminide (TiAI)
EP3069802B1 (fr) Procédé de production d'un composant en matériau composite doté d'une matrice en métal et de phases intercalaires inter-métalliques
DE60033018T2 (de) Verfahren zur herstellung von metallprodukten, wie bleche durch kaltverformung und flashalterung
EP1718777B1 (fr) Procede pour produire un alliage de molybdene
WO2021004579A1 (fr) Alliage à base de nickel pour poudre et procédé de fabrication d'une poudre
DE2125562C3 (de) Verfahren zur pulvermetallurgischen Herstellung dichter Körper aus Nickel-Superlegierungen
EP2200768B1 (fr) PROCÉDÉ DE FABRICATION DE SEMI-PRODUITS À PARTIR D'ALLIAGES NiTi À MÉMOIRE DE FORME
DE1901766A1 (de) Verfahren zum Herstellen eines verdichteten Gegenstandes aus Pulver,insbesondere aus Metallpulver
EP2185738B1 (fr) Fabrication d'alliages a base d'aluminures de titane
EP0686443A1 (fr) Procédé de fabrication de pièces coulées d'un métal réactif et moule réutilisable pour la mise en oeuvre de la méthode
DE2445462B2 (de) Verwendung einer Nickellegierung
DE102012206125A1 (de) Verfahren zur Herstellung von Niederdruckturbinenschaufeln aus TiAl
DE2542094A1 (de) Metallpulver, verfahren zur behandlung losen metallpulvers und verfahren zur herstellung eines verdichteten presslings
DE2351846A1 (de) Metallpulversinterverfahren
EP3249064A1 (fr) Fabrication additive de composants haute temperature en tial
DE2326284A1 (de) Werkstueck aus einer verdichteten superlegierung auf ni-basis
DE4219469A1 (de) Hohen Temperaturen aussetzbares Bauteil, insbesondere Turbinenschaufel, und Verfahren zur Herstellung dieses Bauteils
EP3269838A1 (fr) Alliage tial thermostable et procédé de production associé et composant constitué d'un alliage tial correspondant
EP1568486A1 (fr) Procédé de fabrication de demi-produits et pièces contenant des alliages d'aluminure de titane et produits ainsi obtenus
EP3994289A1 (fr) Alliage à base de nickel pour poudre et procédé de fabrication d'une poudre
DE4219470A1 (de) Bauteil für hohe Temperaturen, insbesondere Turbinenschaufel, und Verfahren zur Herstellung dieses Bauteils
EP1647606B1 (fr) Alliage de nickel résistant à l'usure et a dureté élevée, et son utilisation comme un outil à haute température
DE2200670B2 (fr)
DE2522636A1 (de) Verfahren zur herstellung eines im gefuege grobkoernigen koerpers aus einer superlegierung und nach dem verfahren hergestellter koerper
EP3015199A2 (fr) Procede de fabrication d'un alliage cible resistant a de hautes temperatures, dispositif, alliage et composant correspondant

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

17P Request for examination filed

Effective date: 20160831

RBV Designated contracting states (corrected)

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

17Q First examination report despatched

Effective date: 20180605

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

RIC1 Information provided on ipc code assigned before grant

Ipc: C22F 1/18 20060101ALI20181108BHEP

Ipc: B22F 5/00 20060101AFI20181108BHEP

Ipc: C22C 1/04 20060101ALI20181108BHEP

Ipc: C25F 5/00 20060101ALI20181108BHEP

Ipc: B22F 3/15 20060101ALI20181108BHEP

Ipc: C22C 14/00 20060101ALI20181108BHEP

Ipc: B22D 7/00 20060101ALI20181108BHEP

Ipc: B22D 29/00 20060101ALI20181108BHEP

Ipc: B22F 5/04 20060101ALI20181108BHEP

Ipc: C22C 1/02 20060101ALI20181108BHEP

Ipc: B22F 3/24 20060101ALI20181108BHEP

Ipc: B22F 9/08 20060101ALI20181108BHEP

INTG Intention to grant announced

Effective date: 20181207

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 1115111

Country of ref document: AT

Kind code of ref document: T

Effective date: 20190415

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 502014011288

Country of ref document: DE

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: GERMAN

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20190403

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2728527

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20191025

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190703

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190803

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190703

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190704

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190803

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 502014011288

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

26N No opposition filed

Effective date: 20200106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190901

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190901

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190930

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190930

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20190930

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190930

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20200921

Year of fee payment: 7

Ref country code: GB

Payment date: 20200923

Year of fee payment: 7

Ref country code: DE

Payment date: 20200924

Year of fee payment: 7

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 1115111

Country of ref document: AT

Kind code of ref document: T

Effective date: 20190901

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190901

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20201016

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20140901

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 502014011288

Country of ref document: DE

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20210901

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190403

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210901

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210930

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20220401

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20221028

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210902