EP3223981B1 - Verfahren zur herstellung dreidimensionaler teile aus einer aluminium-titan-legierung - Google Patents

Verfahren zur herstellung dreidimensionaler teile aus einer aluminium-titan-legierung Download PDF

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Publication number
EP3223981B1
EP3223981B1 EP15817955.6A EP15817955A EP3223981B1 EP 3223981 B1 EP3223981 B1 EP 3223981B1 EP 15817955 A EP15817955 A EP 15817955A EP 3223981 B1 EP3223981 B1 EP 3223981B1
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Prior art keywords
pressure
sintering
sintering step
aluminum
powder
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English (en)
French (fr)
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EP3223981A1 (de
Inventor
Guillaume Fribourg
Jean-François CASTAGNE
Jean-Claude Bihr
Clément GILLOT
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Safran Aircraft Engines SAS
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Safran Aircraft Engines SAS
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    • 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
    • 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
    • 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
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B22F3/101—Changing atmosphere
    • 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
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • 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
    • 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 the general field of manufacturing processes for three-dimensional parts based on metal alloys.
  • titanium-based alloys are used for parts intended to be subjected to significant thermomechanical stresses and corrosive atmospheres. These alloys make it possible to reduce the mass of these parts and their use is therefore advantageous for reasons of cost and/or energy efficiency, as is the case for example in the aeronautical field.
  • the manufacture of titanium-based metal alloy parts is traditionally done by processes involving foundry or the electron beam melting technique or “Electron Beam Melting” (EBM).
  • EBM Electro Beam Melting
  • the manufacture of parts of complex geometry, such as a turbomachine blade, is difficult and requires significant processing and machining steps subsequent to the application of the aforementioned development processes. In particular, additional machining steps often result in a high scrap rate, which increases production costs.
  • MIM Metal Injection Molding
  • Such a method comprises a step of preparing an injection composition based on metal powder (for example a metal alloy) and at least one binder (for example a thermoplastic resin), a step of injecting the injection composition in a cavity of a mold for producing a blank of the part, a step of selective elimination of the binder present in the blank or debinding, for example using a solvent at a controlled temperature, and a step of sintering the metal powder in order to densify it.
  • metal powder for example a metal alloy
  • binder for example a thermoplastic resin
  • titanium-based alloy parts produced by traditional MIM processes often exhibit inhomogeneous mechanical properties and relatively significant oxidation, which reduces their service life.
  • the present invention aims to overcome the disadvantages of the MIM processes of the prior art by proposing a method of manufacturing a sintered three-dimensional part comprising a titanium-based alloy which makes it possible to compensate for undesirable modifications in the chemistry of the alloy and to obtain, consequently, parts of complex geometry presenting homogeneous mechanical properties.
  • Controlling the pressure during the first sintering step is necessary because it is necessary to ensure the densification of the part at a high temperature, while avoiding a significant change in the chemistry of the preform following the first sintering step. Also, by setting a first pressure greater than or equal to 1 mbar, this first pressure is greater than the saturated vapor pressure of the addition elements at the sintering temperature, which limits their evaporation and therefore changes in the chemistry of the part following the first sintering step.
  • the first pressure can be greater than or equal to 10 mbar.
  • the first pressure can be applied for a duration of, for example, between 1 hour and 24 hours.
  • the method further comprises, after the first sintering step, a second sintering step during which a second pressure is imposed, the second pressure being lower than the first pressure, the duration of application of the second pressure being chosen so that the content mass of aluminum and/or chromium in a 200 ⁇ m thick layer located on the surface of the preform does not vary by more than 5% in relative value following the second sintering step.
  • the second pressure is less than 1 mbar.
  • the second pressure may be less than or equal to 10 -1 mbar, less than or equal to 10 -2 mbar, or even less than or equal to 10 -3 mbar.
  • the second pressure is applied for a period of less than 5 hours, for example between 10 minutes and 5 hours.
  • the porosity of the preform obtained after the first sintering step is further reduced due to the evacuation of the gas present in the porosity.
  • the conditions of the second sintering stage are optimal for evacuating the gas from the porosity, they are also favorable to the evaporation of the addition elements within the alloy which can lead to a modification of its chemistry, particularly on the surface of the preform. It is therefore desirable to limit the duration of this second sintering step. This limitation of duration is possible in the present invention because the densification of the preform has already been advanced during the first sintering step without affecting its chemistry. The duration of the second sintering step can then be significantly reduced so as not to unduly affect the chemistry of the alloy while being useful for evacuating the gas present in the porosity of the preform and thus improving the densification obtained.
  • the duration of application of the second pressure is determined so that the mass contents of addition elements (such as aluminum and/or chromium) on the surface of the preform do not vary by more than 5% in relative value. following the second sintering stage.
  • ICP plasma torch spectrometry
  • EDX energy dispersive analysis
  • WDS analysis wavelength dispersive
  • XRF X-ray fluorescence spectrometry
  • the method further comprises, after the second sintering step, a third sintering step during which a third pressure is imposed, the third pressure being greater at the second pressure, and which may for example be greater than or equal to 1 mbar.
  • the third sintering step makes it possible to complete the densification of the part, for example if too many addition elements have evaporated and the desired densification is not achieved.
  • the duration of this third step therefore depends on the progress of the densification of the preform at the end of the second sintering step.
  • the duration of this third step can be, for example, between 10 minutes and 10 hours.
  • the invention also relates to the manufacturing process described above in which the manufactured part is a turbomachine blade.
  • the aluminum mass content of the titanium-based alloy powder is greater than 10% before the first sintering step.
  • the titanium-based alloy powder has the following mass contents of elements before the first sintering step: between 32% and 33.5% aluminum, between 4.5% and 5.1% niobium , and between 2.4% and 2.7% chromium.
  • the titanium-based alloy powder has the following mass contents of elements before the first sintering step: between 28.12% and 29.12% aluminum, between 8.56% and 9.56% aluminum. niobium, and between 1.84% and 2.84% molybdenum.
  • the titanium-based alloy powder has the following mass contents of elements before the first sintering step: between 5.4% and 6.6% aluminum, and between 3.6% and 4.4%. % vanadium.
  • one of the steps of a MIM process consists of injecting under pressure into a cavity of a mold an injection composition comprising a powder of a metal alloy and a binder.
  • the alloy powder may preferably be a titanium and aluminum alloy powder.
  • the alloys described above can be used.
  • the powder is preferably in the form of substantially spherical grains.
  • the powder preferably has a grain size (d 90 ) less than or equal to 150 ⁇ m. In other words, if we consider the size distribution of the grains making up the powder, 90% of the grains have a size less than or equal to 150 ⁇ m.
  • the binder may, in a manner known per se, comprise a compound chosen from: paraffins, thermoplastic resins, agar gel, cellulose, polyethylene, polyethylene glycol, polypropylene, stearic acid, polyoxymethylene, etc. . and their mixtures.
  • a mode of implementing a method according to the invention comprises the following steps.
  • An injection composition is prepared (step E10) from an alloy powder as described above and a binder.
  • the injection composition can typically consist of alloy powder between 50% and 70% by volume, and 30% to 50% by volume of binder.
  • the injection composition can first be mixed at a temperature between 150°C and 200°C under a neutral atmosphere for example, and will be injected at this temperature.
  • the injection mold 1 generally consists of two parts 14, 16 forming a cavity 12 having the shape of the part to be manufactured.
  • the injection mold advantageously has several injection points 18a, 18b, 18c which allow injection into several parts of the cavity 12 of the mold 1.
  • injection is carried out at pressures which can vary from 400 bars to 800 bars.
  • step E20 The injection is then carried out (step E20) in the injection mold 1 which is temperature regulated, between 30°C and 70°C for example, so that the injection composition becomes plastic to form a blank of the piece to be made.
  • the blank thus produced is said to be in a “green” or plastic state.
  • the blank is then demolded (step E30), and possibly machined in the green state (step E40) to remove burrs or carrots from the injection points which could have appeared during demoulding.
  • the next step consists of selectively eliminating the binder present in the blank thus formed.
  • step E50 also called “debinding”
  • step E50 makes it possible to obtain a powder which has the shape of the part to be manufactured from a blank of the part in the green state.
  • Selective removal of the binder may include dissolving the binder by treatment with a solvent.
  • the selective removal of the binder can be carried out entirely or finalized thermally. In this case, it can be carried out in a sintering chamber so as not to move the powder between the step of selective elimination of the binder present in the blank and the first sintering step.
  • the sintering chamber Prior to introducing the powder into the sintering chamber, the sintering chamber was purged and decontaminated by cycles pumping under vacuum, for example under reduced pressure of argon or dihydrogen. Indeed, it is necessary to be under a neutral or reducing atmosphere during sintering to avoid oxidation of the elements present in the alloy.
  • the sintering step (step E60) is carried out in a sintering chamber, in which a sintering temperature is imposed gradually.
  • the sintering temperature is of the order of 80% to 90% of the solidus temperature of the alloy present in the powder to be sintered and ramps from 0.10°C/minute to 20° C/minute allows you to gradually reach this temperature.
  • a first sintering step (step E601) is carried out by subjecting the powder to a first pressure, of neutral or reducing atmosphere (under argon or dihydrogen for example), greater than or equal to 1 mbar, for example greater than or equal to 10 mbar.
  • a first pressure of neutral or reducing atmosphere (under argon or dihydrogen for example), greater than or equal to 1 mbar, for example greater than or equal to 10 mbar.
  • addition compounds such as chromium and/or aluminum is negligible throughout the duration of the first sintering stage in which this first pressure is applied.
  • the densification of the preform is carried out while avoiding a modification of the chemistry of the powder on the surface of the preform by evaporation of the addition elements.
  • Partial sintering is carried out during the first sintering step and then a second sintering step is carried out.
  • the preform is subjected to a second pressure, lower than the first, which is imposed in the sintering chamber for a determined duration (step E602).
  • this second pressure is to evacuate the gas present in the porosity of the preform to increase its densification.
  • the duration of application of the second pressure is limited in order to minimize the evaporation of the addition elements such as aluminum and/or chromium from the surface of the preform.
  • a treatment is carried out to evacuate the gas present in the porosity. generated during sintering without significantly affecting the composition of the preform, particularly on its surface.
  • evaporation on the surface of the preform is meant the evaporation of the addition elements in a layer of characteristic thickness (generally of the order of 200 ⁇ m) on the surface of the preform.
  • the evacuation of the gas present in the porosity will be more effective and the densification faster, but the evaporation of the addition elements on the surface of the preform will be even more important.
  • the evacuation of the gas present in the porosity will be longer and the densification more limited, but the evaporation of the addition elements on the surface of the preform will be less.
  • the duration of application of the second pressure will be adapted to minimize the relative variation in the mass content of aluminum and/or chromium on the surface of the preform following the second sintering step, preferably to less than 5%, more preferably less than 3%, even more preferably less than 1%.
  • the mass content of aluminum and/or chromium on the surface of the preform does not preferentially vary by more than 5% in relative value following the second sintering step, more preferably by 3%, even more preferably 1%.
  • step E603 After the second sintering step, it is possible to carry out a third sintering step (step E603) during which a third pressure greater than the second pressure is imposed.
  • This third pressure can for example be greater than or equal to 1 mbar.
  • the preform is cooled by temperature reduction ramps, for example by 0.1° C/minute at 60°C/minute, in order to optimize the microstructure of the part.
  • the final part is obtained from the preform which will have undergone finishing treatments (step E70), known per se, such as hot isostatic compression to finalize the densification of the part, additional heat treatments to optimize the microstructure, surface treatments by machining or polishing, etc.
  • finishing treatments known per se, such as hot isostatic compression to finalize the densification of the part, additional heat treatments to optimize the microstructure, surface treatments by machining or polishing, etc.
  • the method of the invention is particularly suitable for the manufacture of a blade 2 of a turbomachine, comprising for example a foot 22, a blade 24 and a head 26, like that illustrated very schematically on the Figure 3 .
  • the first example describes a method of manufacturing a blade 2 made of titanium alloy of the TiAl6-V4 type by a method according to the invention.
  • TiAl6-V4 grade 23 titanium alloy
  • binder consisting in particular of paraffin wax, poly(ethylene-vinyl acetate) and stearic acid.
  • the injection composition is produced (step E10) by mixing the alloy powder with the binder under Argon, at a temperature of 120° C. for 2 hours.
  • the injection composition is injected into the cavity 12 of the injection mold 1 (step E20).
  • the blank of blade 2 in the green state is then demolded (step E30) and machined in the green state (step E40) to remove the burrs due to the injection.
  • the blade blank is placed in a hexane bath at 40°C for 10 hours to remove the binder by dissolution (step E50).
  • the step of selective elimination of the binder continues in a sintering chamber, in which the blank partially removed from the binder will have been placed, carrying out heat treatments to eliminate the last traces of binder.
  • the sintering step (step E60) is initiated by raising the temperature in the sintering chamber to 1350°C.
  • step E601 The pressure inside the enclosure is then adjusted to 10 mbar for 2 hours to carry out a first sintering step (step E601).
  • the preform is cooled then extracted from the sintering chamber to undergo conventional finishing treatments (step E70).
  • the second example describes a method of manufacturing a blade 2 of titanium alloy of the TiAl 48-2-2 type by another method according to the invention.
  • binder mainly made up of polyethylene and polyethylene glycol.
  • the injection composition is produced (step E10) by mixing the alloy powder with the binder, at a temperature of 170°C.
  • the injection composition is injected into the cavity 12 of the injection mold 1 (step E20) regulated at 40°C and in which a vacuum has been created.
  • the blank of blade 2 in the green state is then demolded (step E30) and machined in the green state (step E40) to remove the burrs due to the injection.
  • the blade blank is placed in a water bath at 75°C for 24 hours to remove the binder by dissolution (step E50).
  • the step of selective elimination of the binder continues in a sintering chamber in which the blank partially removed from the binder will have been placed, carrying out heat treatments to eliminate the last traces of binder.
  • the sintering step (step E60) is initiated by raising the temperature in the sintering chamber to 1410°C.
  • the pressure inside the enclosure is adjusted to 1 mbar for 6 hours to carry out a first sintering step (step E601).
  • a second sintering step is carried out (step E602) by lowering the pressure to 10 -1 mbar in the enclosure for 30 minutes.
  • the preform is cooled then extracted from the sintering chamber to undergo conventional finishing treatments (step E70).

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Claims (8)

  1. Verfahren zur Herstellung eines gesinterten dreidimensionalen Teils, das eine Legierung auf Titanbasis beinhaltet, wobei das Verfahren die folgenden Schritte beinhaltet:
    - Zubereiten einer Einspritzzusammensetzung, die ein Bindemittel und ein Pulver einer Legierung auf Titanbasis umfasst, die Aluminium und/oder Chrom als Zusatzelement beinhaltet (Schritt E10),
    - Einspritzen der Einspritzzusammensetzung in einen Hohlraum (12) einer Form (1), um einen Rohling des zu bildenden Teils zu erhalten (Schritt E20),
    - selektives Entfernen des Bindemittels, das in dem Rohling vorhanden ist (Schritt E50),
    - einen ersten Schritt des Sinterns des Pulvers der Legierung auf Titanbasis (Schritt E601), wobei das Pulver während des ersten Sinterschritts einem ersten Druck größer als oder gleich 1 mbar ausgesetzt ist, um eine Vorform des Teils aus gesintertem Legierungspulver zu erhalten, und
    - einen zweiten Sinterschritt, der nach dem ersten Sinterschritt durchgeführt wird, bei dem ein zweiter Druck ausgeübt wird (Schritt E602), wobei der zweite Druck weniger als der erste Druck beträgt, wobei die Dauer der Ausübung des zweiten Drucks so gewählt ist, dass der Massegehalt an Aluminium und/oder Chrom in einer Schicht mit einer Dicke von 200 µm, die sich auf der Oberfläche der Vorform befindet, um nicht mehr als 5 % im relativen Wert nach dem zweiten Sinterschritt variiert, wobei der zweite Druck weniger als 1 mbar ist, und wobei der zweite Druck während einer Dauer von weniger als 5 Stunden ausgeübt wird.
  2. Verfahren nach Anspruch 1, das ferner nach dem zweiten Sinterschritt einen dritten Sinterschritt, bei dem ein dritter Druck ausgeübt wird (Schritt E603), beinhaltet, wobei der dritte Druck größer als der zweite Druck ist.
  3. Verfahren nach Anspruch 2, wobei der dritte Druck größer als oder gleich 1 mbar ist.
  4. Verfahren nach einem der Ansprüche 1 bis 3, wobei das erhaltene Teil eine Turbinenschaufel (2) ist.
  5. Verfahren nach einem der Ansprüche 1 bis 4, wobei der Massegehalt an Aluminium des Legierungspulvers vor dem ersten Sinterschritt mehr als 10 % beträgt.
  6. Verfahren nach einem der Ansprüche 1 bis 5, wobei das Legierungspulver vor dem ersten Sinterschritt die folgenden Massegehalte an Elementen aufweist:
    zwischen 32 % und 33,5 % Aluminium,
    zwischen 4,5 % und 5,1 % Niob und
    zwischen 2,4 % und 2,7 % Chrom.
  7. Verfahren nach einem der Ansprüche 1 bis 5, wobei das Legierungspulver vor dem ersten Sinterschritt die folgenden Massegehalte an Elementen aufweist:
    zwischen 28,12 % und 29,12 % Aluminium,
    zwischen 8,56 % und 9,56 % Niob und
    zwischen 1,84 % und 2,84 % Molybdän.
  8. Verfahren nach einem der Ansprüche 1 bis 4, wobei das Legierungspulver vor dem ersten Sinterschritt die folgenden Massegehalte an Elementen aufweist:
    zwischen 5,4 % und 6,6 % Aluminium und
    zwischen 3,6 % und 4,4 % Vanadium.
EP15817955.6A 2014-11-25 2015-11-24 Verfahren zur herstellung dreidimensionaler teile aus einer aluminium-titan-legierung Active EP3223981B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1461443A FR3028784B1 (fr) 2014-11-25 2014-11-25 Procede de fabrication de pieces tridimensionnelles en alliage d'aluminium et de titane, et aube de turbomachine obtenue par un tel procede
PCT/FR2015/053187 WO2016083724A1 (fr) 2014-11-25 2015-11-24 Procede de fabrication de pieces tridimensionnelles en alliage d'aluminium et de titane

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EP3223981A1 EP3223981A1 (de) 2017-10-04
EP3223981B1 true EP3223981B1 (de) 2024-01-17

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US10934847B2 (en) * 2016-04-14 2021-03-02 Mitsubishi Power, Ltd. Steam turbine rotor blade, steam turbine, and method for manufacturing steam turbine rotor blade
CN108588482A (zh) * 2018-07-16 2018-09-28 宝鸡钛程压力容器设备制造有限公司 一种3d打印钛合金粉末的配方及制备方法
FR3086566B1 (fr) * 2018-10-02 2022-05-27 Norimat Procede de fabrication de piece de forme complexe par frittage sous pression a partir d'une preforme
FR3096912B1 (fr) * 2019-06-07 2021-10-29 Safran Aircraft Engines Procédé de fabrication de pièce de turbomachine par moulage MIM
FR3099717B1 (fr) * 2019-08-06 2022-06-10 Safran Aircraft Engines Procédé de fabrication d’une pièce métallique
FR3132912A1 (fr) * 2022-02-22 2023-08-25 Safran Aircraft Engines Poudre d’alliage, procédé de fabrication d’une pièce à base de cet alliage et pièce ainsi obtenue.

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FR3028784A1 (fr) 2016-05-27
CN107002178A (zh) 2017-08-01
WO2016083724A1 (fr) 2016-06-02
CN107002178B (zh) 2019-11-01
US20170321303A1 (en) 2017-11-09
FR3028784B1 (fr) 2019-05-10
EP3223981A1 (de) 2017-10-04

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