EP3007844B1 - Method for manufacturing a titanium-aluminium alloy part - Google Patents
Method for manufacturing a titanium-aluminium alloy part Download PDFInfo
- Publication number
- EP3007844B1 EP3007844B1 EP14734884.1A EP14734884A EP3007844B1 EP 3007844 B1 EP3007844 B1 EP 3007844B1 EP 14734884 A EP14734884 A EP 14734884A EP 3007844 B1 EP3007844 B1 EP 3007844B1
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- temperature
- mpa
- titanium
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- aluminum
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- 238000000034 method Methods 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 229910000838 Al alloy Inorganic materials 0.000 title description 4
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title description 3
- 239000000203 mixture Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 22
- 229910052782 aluminium Inorganic materials 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 19
- 238000002490 spark plasma sintering Methods 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 239000010955 niobium Substances 0.000 claims description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 16
- 229910052721 tungsten Inorganic materials 0.000 claims description 16
- 239000010937 tungsten Substances 0.000 claims description 16
- 229910052758 niobium Inorganic materials 0.000 claims description 15
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 15
- 239000010936 titanium Substances 0.000 claims description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 229910052702 rhenium Inorganic materials 0.000 claims description 9
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 51
- 239000000956 alloy Substances 0.000 description 51
- 230000008569 process Effects 0.000 description 29
- 239000000126 substance Substances 0.000 description 10
- 238000007711 solidification Methods 0.000 description 9
- 238000004663 powder metallurgy Methods 0.000 description 8
- 230000008023 solidification Effects 0.000 description 8
- 230000002093 peripheral effect Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004626 scanning electron microscopy Methods 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
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- 238000005245 sintering Methods 0.000 description 4
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- 238000005242 forging Methods 0.000 description 3
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- 230000007246 mechanism Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000037361 pathway Effects 0.000 description 3
- 229910021324 titanium aluminide Inorganic materials 0.000 description 3
- 229910000927 Ge alloy Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
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- 229910000601 superalloy Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- OQPDWFJSZHWILH-UHFFFAOYSA-N [Al].[Al].[Al].[Ti] Chemical compound [Al].[Al].[Al].[Ti] OQPDWFJSZHWILH-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
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Images
Classifications
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- 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
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B22F5/008—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of engine cylinder parts or of piston parts other than piston rings
-
- 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
- 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
-
- 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
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
- F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
- F01D5/12—Blades
- F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
- F01D5/00—Blades; Blade-carrying members; Heating, heat-insulating, cooling or antivibration means on the blades or the members
- F01D5/12—Blades
- F01D5/28—Selecting particular materials; Particular measures relating thereto; Measures against erosion or corrosion
- F01D5/288—Protective coatings for blades
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01L—CYCLICALLY OPERATING VALVES FOR MACHINES OR ENGINES
- F01L3/00—Lift-valve, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces; Parts or accessories thereof
- F01L3/02—Selecting particular materials for valve-members or valve-seats; Valve-members or valve-seats composed of two or more materials
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01L—CYCLICALLY OPERATING VALVES FOR MACHINES OR ENGINES
- F01L2303/00—Manufacturing of components used in valve arrangements
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05C—INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
- F05C2201/00—Metals
- F05C2201/02—Light metals
- F05C2201/021—Aluminium
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
- F05C—INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
- F05C2201/00—Metals
- F05C2201/02—Light metals
- F05C2201/025—Boron
Definitions
- the present invention relates to the manufacture of a titanium-aluminum alloy (TiAl) for use as a structural material for the production of a part, for example in the aeronautical sector for the manufacture of turbine blades for aircraft or helicopter engines, or in the automobile field for the manufacture of valves.
- TiAl titanium-aluminum alloy
- a problem that arises in this type of industry is related to the quality of materials used in particular for the manufacture of parts exposed to very high temperature and pressure constraints.
- TiAl alloys have been the subject of intensive research since the 1980s with the aim of replacing nickel-based monocrystalline superalloys used for over fifty years for turbine blades.
- TiAl alloys have the advantage of having a density half that of superalloys. Their use improves engine performance, reduces structural load, reduces noise, saves fuel and reduces greenhouse gas emissions.
- Today most engine manufacturers have integrated TiAl alloy turbine blades in their latest aircraft engines. Until now, all these blades have a chemical composition called GE type (46 to 48% aluminum, 2% niobium and 2% chromium, titanium balancing) and are developed by the foundry pathway, followed heat treatments.
- the casting channel on GE alloys allows the manufacture of blades for low pressure stages of an aircraft engine.
- a GE type alloy is creep efficient due to the presence of a predominantly or totally lamellar microstructure.
- the incorporation into stages of more constrained and warmer engines through the manufacture of blades made of more efficient materials, especially more resistant to oxidation where the introduction in larger quantities of elements such as niobium and / or refractory elements such as tungsten. Since these alloys doped with refractory elements are characterized in the foundry by a poor ductility resulting from a high resistance, it is not currently possible to use such blades at other stages of an aircraft engine.
- the microstructures of these TiAl alloys Due to a relatively complex equilibrium diagram, the microstructures of these TiAl alloys, which are determinant for the properties, are strongly dependent on the thermal history experienced by the alloy and the processing method used.
- biphasic ( ⁇ + ⁇ 2 ), duplex ( ⁇ + lamellar) and lamellar microstructures are obtained.
- the ⁇ phase is quadratic of L1 0 structure, the ⁇ phase being disordered hexagonal and the ordered ⁇ 2 hexagonal phase of DO 19 structure.
- the lamellar structure is obtained during the cooling of grains ⁇ .
- Solidification processes such as foundry or directed solidification allow the formation of columnar structures formed of elongate and lamellar grains with interfaces perpendicular to the longitudinal axis of the grains.
- Research shows that the most efficient microstructures are microstructures whose crystallographic grains have a size of a few tens of microns and are formed either exclusively or in a large proportion of lamellar grains. It has also been demonstrated that a small-grain lamellar microstructure obtained by a succession of heat treatments has a good mechanical strength and a ductility of the order of 5%, which is quite exceptional.
- Alloys containing niobium (called TNB: Ti-45Al- (5-10) Nb) were then developed, more particularly in connection with the forging process or for the manufacture of thin sheets.
- TNB Ti-45Al- (5-10) Nb
- the best creep results were obtained for extruded alloys containing carbon.
- the creep rate is 6.10 -9 s -1 at 500 MPa at 700 ° C., but the ductility of these alloys is on average 0.69%, with samples breaking at 0.34% deformation (Strength properties hardened high niobium containing titanium aluminide alloy, PAUL J, OEHRING M, HOPPE R, CALL F, Gamma Titanium Aluminides 2003, 403, TMS, 2003 ).
- ABB type US5,286,443 and US 5,207,982 and G4 alloys ( FR-2,732,038 ).
- ABB type alloys contain 2% by weight of tungsten and less than 0.5% of silicon and boron.
- One of the alloys of the ABB family of composition Ti-47Al-2W-0,5Si has been studied in detail. It has a fine microstructure formed of lamellar grains, feather structures and ⁇ zones and excellent resistance to creep but a very limited ductility.
- G4-type alloys contain 1% by weight of tungsten, 1% by weight of rhenium and 0.2% of silicon. These alloys exhibit excellent creep performance, as well as a reasonable ductility of 1.2% at 20 ° C.
- the strong interest of these alloys G4 comes from the fact that their mechanical properties are optimal in a simple structural state without homogenization treatment at very high temperature, unlike ABB type alloys.
- Line 7 of Table 1 gives the properties of alloys obtained by directed solidification: their microstructure is formed of elongated lamellar grains in the direction of solidification and with the interface planes parallel to this same direction.
- the Ti-46Al-1 Mo-0.5Si composition alloy has an elongation at break of more than 25% at room temperature and a creep resistance of 3.5.10 -10 s -1 at 750 ° C and 240 MPa .
- ARCAM powder metallurgy
- SPS synchronization for Spark Plasma Sintering
- French flash sintering a technique that allows like the SPS (acronym for Spark Plasma Sintering, called in French flash sintering) to give a complex shape to the part.
- Tensile test results show a ductility of the order of 1.2% and a yield strength of the order of 350 MPa, for GE-type alloys densified by this process.
- a disadvantage related to this route is a loss of aluminum (typically 2 at% Al) during melting while the aluminum concentration is very critical for the properties.
- the implementation of this method also requires a vacuum chamber, which results in a high industrial cost.
- the present invention aims to overcome the disadvantages of the prior art. Its purpose is in particular to provide the means for producing a part exhibiting advantageous mechanical properties making it possible in particular to meet the needs of engine manufacturers for aeronautics by having a yield point of about 400 MPa at 0.2% ambient temperature at 0.2%. and an elongation at break of the order of 1.5%, and creep at 700 ° C - 300 MPa and at 750 ° C - 200 MPa, a time before rupture of at least 400 hours.
- the present invention aims to provide a part with excellent properties including the point of view of the ductility at room temperature and the hot resistance.
- the term "piece” here means any product obtained by the present invention and intended to be used subsequently as a blank for a mechanical part, as a mechanical part (turbine blade, valve, etc.) or part of mechanical part (valve head, ...) or several mechanical parts (realization of several blades or valves or any set of mechanical parts, including complex mechanical parts).
- a pellet, a block, a bar or any other basic element that can be used for machining a mechanical component are here also considered to be one piece.
- the method according to the invention is also intended to obtain a part having a high homogeneity of microstructures and therefore excellent reproducibility of mechanical properties.
- the present invention will provide a method characterized by a low cost and robustness of the means for its implementation.
- the method according to the invention will also advantageously offer a high speed of elaboration and will allow the manufacture of the part without subsequent heat treatment, thus offering the possibility of directly manufacturing blade preforms and thus limiting the machining.
- the present invention therefore proposes to combine in a completely novel manner a titanium-aluminum alloy, having a particular chemical composition, with a flash sintering (or SPS) manufacturing process.
- a flash sintering (or SPS) manufacturing process is a process that makes it possible to obtain parts with mechanical characteristics that largely meet the requirements of the engine manufacturers in the aeronautical industry.
- the chemical composition of the material used in the process according to the invention is based on elements which are relatively inexpensive such as tungsten.
- the TiAl alloys conventionally manufactured by the foundry process are much less efficient in terms of the ductility / creep resistance compromise and the reproducibility of the microstructures than the alloys obtained by a process according to the present invention.
- this path (foundry) requires to apply to the alloys heat treatments and material machining more important than for the SPS channel.
- the use of the powder metallurgy (PW) pathway associated with that of flash sintering makes it possible here to refine and homogenize the microstructures for the alloys selected by the present invention and allows them to be used at the highest temperatures in the field. 'use.
- the electric current can pass directly into the powder material and / or into the tooling and thus causes an increase in the temperature of the material.
- the metal alloy part (PF) obtained at the end of the process according to the invention contains heavy elements in an amount of less than 5 atomic% and boron in a very small amount (0.05 to 1.5 atomic%), which makes it possible to obtain a lamellar microstructure with small grains resistant to creep.
- Another advantage of the present invention lies in the fact that it is not it is not necessary to systematically obtain low-aluminum grades to, for example, promote ⁇ -solidification, since the alloy obtained at the end of the process contains boron in order to obtain a fine microstructure with equiaxed grains. An originality compared to existing alloys is thus to be able to offer a rich aluminum grade which also has an interest in ductility and resistance to oxidation.
- the chemical composition-densification coupling by Spark Plasma Sintering makes it possible to obtain an alloy having a particular microstructure with exceptional mechanical properties. It is formed of small lamellar grains, surrounded by peripheral ⁇ zones. It is the combination of this method with the claimed chemical composition that makes it possible to obtain a piece with qualities far superior to those of the alloy parts of the prior art. In fact, a part with the same chemical composition as the one claimed but which would be produced by powder metallurgy (PW) in combination with the conventional hot isostatic compaction (DUC) process would not have exceptional properties. which confirms the original character obtained thanks to the method according to the invention.
- PW powder metallurgy
- DUC hot isostatic compaction
- the method thus defined according to the present invention makes it possible to limit the magnification of the grains, to obtain a thin lamellar microstructure, to have a ⁇ phase intrinsically resistant to heat and at ambient temperature, to have good reproducibility of the mechanical properties as well as a very good compromise between ductility at room temperature and resistance to creep at high temperature.
- the material used in the context of the process according to the invention has the following composition in atomic percentage: 49.92% of titanium, 48.00% of aluminum, 2.00% of tungsten, 0.08% boron.
- a pressure of between 80 and 120 MPa is applied during step b).
- the pressure increases gradually during step b) over a period of less than 5 minutes.
- the temperature increases from 80 to 120 ° C / min.
- step c the temperature is maintained at the plateau for two minutes.
- the method according to the present invention is particularly advantageously used for the manufacture of a turbine blade preform and / or a turbocharger turbine wheel and / or a valve (or at least one valve head) and / or a piston pin.
- Alloys of small-grain lamellar structure are thus obtained by a simple SPS cycle according to the present invention.
- the SPS cycle used in the context of the invention is based on the process described in the international application WO 2012/131625 wherein a uniaxial pressure is applied, directly or via force transmission parts, by means of at least two pistons (P1, P2) sliding towards one another inside a matrix, said pistons and / or said force transmission parts having bearing surfaces in contact with the constituent material and cooperating with each other to define the shape of the part to be manufactured.
- P1, P2 pistons sliding towards one another inside a matrix
- said pistons and / or said force transmission parts having bearing surfaces in contact with the constituent material and cooperating with each other to define the shape of the part to be manufactured.
- the device has the advantage of allowing the manufacture of complex shaped metal parts. However, it is possible to envisage using a different device allowing the implementation of an SPS method for the implementation of the present invention.
- the rise in temperature can be obtained by direct passage of the current in the powder material or by passing the current in the matrix which exchanges the heat with the powder material. After about 2 minutes of maintaining the bearing temperature (1355 ° C), the pressure and the heating are cut off. In less than 30 minutes, the densification test is complete and the sample available. It should be noted that figure 1 illustrates in particular measured temperatures that are lower than the core temperature of the material but the temperature difference between the measured temperature and the temperature in the material is known because it can be calibrated.
- the alloy constituting the part obtained has a microstructure illustrated on the Figure 2 which presents images in scanning electron microscopy at different magnifications. It is formed of lamellar grains surrounded by ⁇ -phase peripheral zones containing phase B2 precipitates, with a strong white contrast. The lamellar grains have an average size of 30 ⁇ m. The peripheral ⁇ zones are elongated (a few microns). In the lamellar zones, we observe low contrast ribbons (noted BO on the figure 2d ) which are borides.
- the Figure 3 presents the same area observed under the microscope at scanning and transmission electron microscope.
- the lamellar zones generally have a classic appearance: they are formed of lamellae of average width 0.15 ⁇ m and separated by very straight interfaces. The proportion of ⁇ 2 phase in these lamellar zones is about 10%.
- the Figure 4 shows in detail a peripheral zone, where one observes the extension of the ⁇ phase in the joints between lamellar grains.
- the Figure 5 shows local analyzes of chemical composition by EDS-MEB. It is measured that the tungsten is distributed fairly homogeneously in all phases, which is quite unexpected because the B2 and ⁇ 2 phases are supposed to accept larger proportions.
- the Figures 6 and 7 illustrate the exceptional mechanical properties of this alloy by showing tensile curves at room temperature and creep curves at 700 ° C at 300 MPa.
- two curves obtained for samples extracted from different SPS pellets were represented.
- the second test was stopped at 1.5% in order to study the microstructure of deformation by electron microscopy and to try to explain the good creep behavior.
- the superposition of the curves illustrates the high reproducibility of the mechanical properties of the samples obtained by the SPS process.
- the tensile curve at room temperature gives: elongation at break of 1.6%, a yield strength of 496 MPa and a breaking strength of 646 MPa. In creep at 700 ° C.
- the secondary velocity is 3.7 10 -9 s -1 and the duration before rupture is 4076 hours, which is exceptional.
- the creep rate at 750 ° C. was measured. It is 2.3 10 -9 s -1 at 120 MPa and 5.8 10 -9 s -1 at 200 MPa, values which confirm the excellent creep resistance of the parts obtained according to the present invention.
- the ductility obtained could be explained by: i) the presence of peripheral ⁇ zones that accept a fairly large amount of deformation, ii) the characteristics of the lamellar zones (fairly large lamella size) which are also deformable and iii) the small size lamellar grains which limit the formation of internally constraining stacks causing rupture.
- the exceptional resistance to creep could be explained by the resistance of the lamellar structure and the good dispersion of tungsten in the matrix ⁇ which is deformed. It seems that the characteristic dimensions of the microstructure obtained at the end of the process according to the invention, namely the size of the grains and the width of the lamellae, are close to the ideal so that at the same time the dislocations do not move. not too easily by involving diffusion and that there are enough interfaces and grain boundaries to hinder the movement of dislocations.
- a metal alloy part could be manufactured.
- This part had characteristics going beyond the characteristics corresponding to the aforementioned requirements for turbine blades of an aircraft engine (elastic limit of about 400 MPa at 0.2% at room temperature and an elongation at break of the order of 1.5%, and creep at 700 ° C - 300 MPa and at 750 ° C - 200 MPa, a break-up time of at least 400 hours) and even largely fulfilled all required specifications.
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Description
La présente invention concerne la fabrication d'un alliage en titane-aluminium (TiAl) en vue de son utilisation comme matériau de structure pour la réalisation d'une pièce, par exemple dans le secteur aéronautique pour la fabrication d'aubes de turbine pour des moteurs d'avion ou d'hélicoptère, ou bien dans le domaine automobile pour la fabrication de soupapes.The present invention relates to the manufacture of a titanium-aluminum alloy (TiAl) for use as a structural material for the production of a part, for example in the aeronautical sector for the manufacture of turbine blades for aircraft or helicopter engines, or in the automobile field for the manufacture of valves.
Un problème qui se pose dans ce type d'industrie est lié à la qualité des matériaux utilisés notamment pour la fabrication des pièces exposées à de très fortes contraintes de température et de pression.A problem that arises in this type of industry is related to the quality of materials used in particular for the manufacture of parts exposed to very high temperature and pressure constraints.
Les alliages TiAl sont l'objet de recherches intensives depuis les années 80 dans le but de remplacer les superalliages monocristallins à base nickel utilisés depuis plus de cinquante ans pour les aubes de turbine. Les alliages TiAl ont l'avantage d'avoir une densité moitié moindre que celle des superalliages. Leur utilisation permet l'amélioration du rendement des moteurs, l'allègement des structures, la réduction des émissions sonores, des économies de carburant et la diminution des émissions de gaz à effet de serre. Aujourd'hui la plupart des motoristes ont intégré des aubes de turbine en alliage TiAl dans leurs derniers moteurs d'avion. Jusqu'à présent, toutes ces aubes ont une composition chimique dite de type GE (46 à 48 % d'aluminium, 2 % de niobium et 2 % de chrome, le titane faisant la balance) et sont élaborées par la voie fonderie, suivie de traitements thermiques.TiAl alloys have been the subject of intensive research since the 1980s with the aim of replacing nickel-based monocrystalline superalloys used for over fifty years for turbine blades. TiAl alloys have the advantage of having a density half that of superalloys. Their use improves engine performance, reduces structural load, reduces noise, saves fuel and reduces greenhouse gas emissions. Today most engine manufacturers have integrated TiAl alloy turbine blades in their latest aircraft engines. Until now, all these blades have a chemical composition called GE type (46 to 48% aluminum, 2% niobium and 2% chromium, titanium balancing) and are developed by the foundry pathway, followed heat treatments.
La voie fonderie sur des alliages de type GE permet la fabrication d'aubes pour des étages basse pression d'un moteur d'avion. Un alliage de type GE est performant en fluage grâce à la présence d'une microstructure majoritairement ou totalement lamellaire. Or, l'incorporation dans des étages des moteurs plus contraints et plus chauds passe par la fabrication d'aubes faites de matériaux plus performants, en particulier plus résistants en oxydation d'où l'introduction en plus grande quantité d'éléments comme le niobium et/ou d'éléments réfractaires comme le tungstène. Étant donné que ces alliages dopés en éléments réfractaires se caractérisent en fonderie par une ductilité médiocre résultant d'une haute résistance, il n'est pas possible actuellement d'utiliser de telles aubes à d'autres étages d'un moteur d'avion.The casting channel on GE alloys allows the manufacture of blades for low pressure stages of an aircraft engine. A GE type alloy is creep efficient due to the presence of a predominantly or totally lamellar microstructure. However, the incorporation into stages of more constrained and warmer engines through the manufacture of blades made of more efficient materials, especially more resistant to oxidation where the introduction in larger quantities of elements such as niobium and / or refractory elements such as tungsten. Since these alloys doped with refractory elements are characterized in the foundry by a poor ductility resulting from a high resistance, it is not currently possible to use such blades at other stages of an aircraft engine.
En raison d'un diagramme d'équilibre relativement complexe, les microstructures de ces alliages TiAl qui sont déterminantes pour les propriétés, sont fortement dépendantes de l'histoire thermique subie par l'alliage et du procédé d'élaboration utilisé. Pour des températures de traitement thermique croissantes et pour des compositions classiques décrites par un diagramme binaire, des microstructures biphasées (γ+α2), duplex (γ + lamellaire) et lamellaires sont obtenues. La phase γ est quadratique de structure L10, la phase α étant hexagonale désordonnée et la phase α2 hexagonale ordonnée de structure DO19. La structure lamellaire s'obtient lors du refroidissement de grains α.Due to a relatively complex equilibrium diagram, the microstructures of these TiAl alloys, which are determinant for the properties, are strongly dependent on the thermal history experienced by the alloy and the processing method used. For increasing heat treatment temperatures and for conventional compositions described by a binary diagram, biphasic (γ + α 2 ), duplex (γ + lamellar) and lamellar microstructures are obtained. The γ phase is quadratic of L1 0 structure, the α phase being disordered hexagonal and the ordered α 2 hexagonal phase of DO 19 structure. The lamellar structure is obtained during the cooling of grains α.
Des procédés de solidification tels que la fonderie ou la solidification dirigée permettent la formation de structures colonnaires formées de grains allongés et lamellaires avec des interfaces perpendiculaires à l'axe longitudinal des grains. Il ressort des travaux de recherche que les microstructures les plus performantes sont des microstructures dont les grains cristallographiques ont une taille de quelques dizaines de microns et sont formés soit exclusivement, soit en forte proportion de grains lamellaires. Il a en outre été démontré qu'une microstructure lamellaire à petits grains obtenue par une succession de traitements thermiques possède une bonne résistance mécanique et une ductilité de l'ordre de 5%, ce qui est assez exceptionnel.Solidification processes such as foundry or directed solidification allow the formation of columnar structures formed of elongate and lamellar grains with interfaces perpendicular to the longitudinal axis of the grains. Research shows that the most efficient microstructures are microstructures whose crystallographic grains have a size of a few tens of microns and are formed either exclusively or in a large proportion of lamellar grains. It has also been demonstrated that a small-grain lamellar microstructure obtained by a succession of heat treatments has a good mechanical strength and a ductility of the order of 5%, which is quite exceptional.
Une des difficultés rencontrées pour obtenir une microstructure lamellaire résulte du fait qu'il faut franchir le transus α du diagramme d'équilibre (situé aux alentours de 1325-1350°C selon la composition chimique de l'alliage) alors que toute incursion dans ce domaine α provoque un grossissement des grains qui dépassent très rapidement la centaine de microns.One of the difficulties encountered in obtaining a lamellar microstructure results from the fact that it is necessary to cross the transus α of the equilibrium diagram (located around 1325-1350 ° C. according to the chemical composition of the alloy) while any incursion into this α-domain causes a magnification of grains that exceed very quickly the hundred microns.
En ce qui concerne la tenue au fluage des alliages TiAl aux températures d'utilisation (700-800°C), il a été montré que la diffusion joue un rôle important dans le déplacement des dislocations par des mécanismes de montée et donc qu'une trop grande proportion de joints de grains ou d'interfaces est préjudiciable à la tenue au fluage car ces joints ou interfaces facilitent la diffusion par la présence de lacunes.With respect to the creep resistance of TiAl alloys at operating temperatures (700-800 ° C), diffusion has been shown to play an important role in the dislocation displacement by ascending mechanisms and therefore Too large a proportion of grain boundaries or interfaces is detrimental to creep resistance because these seals or interfaces facilitate diffusion by the presence of gaps.
Depuis les années 90, de nombreuses études d'alliages TiAl de compositions chimiques variées et élaborés par diverses filières de mise en oeuvre ont été publiées. Parfois, plusieurs voies d'élaboration (fusion, fonderie, forgeage, métallurgie des poudres ou MdP) ont été appliquées à certaines de ces nuances (Microstructure and déformation of two-phase γ-titanium aluminides,
Après des travaux préliminaires sur des alliages binaires ne contenant que du titane et de l'aluminium, la communauté a concentré ses efforts sur des nuances de type GE se caractérisant par des teneurs en aluminium entre 46 et 48% at. et par un ajout de 2% de niobium et de 2% de chrome. Des recherches ont été entreprises sur ce type d'alliage GE en comparant les deux voies fonderie et métallurgie des poudres qui possédaient respectivement des microstructures quasi-lamellaires texturées et duplex. Les deux premières lignes du tableau 1 résument les propriétés de ces alliages. On constate que la ductilité de ces deux alliages est faible et que seul l'alliage élaboré par la voie fonderie a une tenue au fluage correcte.After preliminary work on binary alloys containing only titanium and aluminum, the community focused its efforts on GE-type grades with aluminum contents between 46 and 48% at. and by adding 2% of niobium and 2% of chromium. Research was carried out on this type of GE alloy by comparing the two foundry and powder metallurgy paths, which respectively possessed textured quasi-lamellar and duplex microstructures. The first two rows of Table 1 summarize the properties of these alloys. It can be seen that the ductility of these two alloys is low and that only the alloy produced by the foundry channel has a correct creep resistance.
Des alliages contenant du niobium (appelés TNB : Ti-45Al-(5-10)Nb) ont ensuite été développés, plus particulièrement en liaison avec le procédé de forgeage ou pour la fabrication de tôles minces. Sur les matériaux massifs, les meilleurs résultats en fluage ont été obtenus pour des alliages extrudés contenant du carbone. Par exemple la vitesse de fluage est de 6.10-9 s-1 sous 500 MPa à 700°C mais la ductilité de ces alliages est en moyenne de 0,69%, avec des échantillons cassant à 0,34% de déformation (Strength properties of a précipitation hardened high niobium containing titanium aluminide alloy,
Des recherches se sont orientées vers des alliages contenant des éléments lourds en s'appuyant sur deux idées : la mise en oeuvre de la solidification β qui pourrait permettre la réduction de la taille des grains et la réduction de la mobilité des dislocations à haute température par interaction de ces éléments avec les dislocations. C'est le cas des alliages dit de type ABB (brevets
Un des alliages de la famille ABB de composition Ti-47Al-2W-0,5Si a été étudié en détail. Il possède une microstructure fine formée de grains lamellaires, de structures plumeaux et de zones γ et une excellente tenue au fluage mais une ductilité très limitée. Quant aux alliages de type G4, ils contiennent 1% atomique de tungstène , 1% atomique de rhénium et 0,2% de silicium. Ces alliages présentent une excellente performance en fluage, ainsi qu'une ductilité raisonnable de 1,2% à 20°C. Le fort intérêt de ces alliages G4 provient du fait que leurs propriétés mécaniques sont optimales dans un état structural simple sans traitement d'homogénéisation à très haute température, contrairement aux alliages de type ABB. Il s'avère que les structures de fonderie, de nature assez tortueuse avec notamment l'imbrication des nombreuses dendrites de solidification, contribuent de façon marquée au gain de propriétés mécaniques. Une proportion assez similaire en rhénium et tungstène est d'ailleurs recommandée, étant donné qu'en cours de solidification le rhénium est rejeté dans les zones interdendritiques alors que le tungstène ségrége plutôt au coeur des dendrites.One of the alloys of the ABB family of composition Ti-47Al-2W-0,5Si has been studied in detail. It has a fine microstructure formed of lamellar grains, feather structures and γ zones and excellent resistance to creep but a very limited ductility. G4-type alloys contain 1% by weight of tungsten, 1% by weight of rhenium and 0.2% of silicon. These alloys exhibit excellent creep performance, as well as a reasonable ductility of 1.2% at 20 ° C. The strong interest of these alloys G4 comes from the fact that their mechanical properties are optimal in a simple structural state without homogenization treatment at very high temperature, unlike ABB type alloys. It turns out that foundry structures, quite tortuous nature including the interweaving of many solidification dendrites, contribute significantly to the gain of mechanical properties. A fairly similar proportion of rhenium and tungsten is recommended, since during solidification the rhenium is rejected in the interdendritic zones while the tungsten rather segregates in the heart of the dendrites.
Certains alliages présentent des propriétés exceptionnelles mais celles-ci sont obtenues par des procédés complexes et difficilement industrialisables à un coût concurrentiel. La ligne 7 du tableau 1 donne les propriétés d'alliages obtenus par solidification dirigée : leur microstructure est formée de grains lamellaires allongés selon la direction de solidification et avec les plans d'interface parallèles à cette même direction. L'alliage de composition Ti-46AI-1 Mo-0,5Si possède un allongement à rupture de plus de 25% à la température ambiante et une résistance au fluage de 3,5.10-10 s-1 sous 750°C et 240 MPa.Some alloys have exceptional properties but these are obtained by complex processes and difficult to industrialize at a competitive cost.
Enfin, une autre voie de métallurgie des poudres fait l'objet de travaux récents. Un procédé appelé ARCAM consiste en la fusion de poudres par un faisceau d'électrons, technique qui permet comme le SPS (acronyme anglais de Spark Plasma Sintering, appelé en français frittage flash) de donner une forme complexe à la pièce. Des résultats d'essais de traction montrent une ductilité de l'ordre de 1,2% et une limite d'élasticité de l'ordre de 350 MPa, pour des alliages de type GE densifié par ce procédé. Un inconvénient lié à cette voie réside en une perte en aluminium (typiquement 2 at%Al) au cours de la fusion alors que la concentration en aluminium est très critique pour les propriétés. La mise en oeuvre de ce procédé exige également une enceinte sous vide, ce qui aboutit à un coût industriel élevé.Finally, another path of powder metallurgy is the subject of recent work. A process called ARCAM consists of the melting of powders by an electron beam, a technique that allows like the SPS (acronym for Spark Plasma Sintering, called in French flash sintering) to give a complex shape to the part. Tensile test results show a ductility of the order of 1.2% and a yield strength of the order of 350 MPa, for GE-type alloys densified by this process. A disadvantage related to this route is a loss of aluminum (typically 2 at% Al) during melting while the aluminum concentration is very critical for the properties. The implementation of this method also requires a vacuum chamber, which results in a high industrial cost.
La présente invention vise à pallier les inconvénients de l'art antérieur. Elle a notamment pour but de fournir les moyens de réaliser une pièce présentant des propriétés mécaniques intéressantes permettant notamment de répondre aux besoins des motoristes pour l'aéronautique en ayant à température ambiante une limite d'élasticité d'environ 400 MPa à 0,2 % et un allongement à la rupture de l'ordre de 1,5%, et en fluage à 700 °C - 300 MPa et à 750 °C - 200 MPa, une durée avant rupture d'au moins 400 heures. Ainsi, la présente invention a pour but de fournir une pièce avec d'excellentes propriétés notamment du point de vue de la ductilité à la température ambiante et de la résistance à chaud.The present invention aims to overcome the disadvantages of the prior art. Its purpose is in particular to provide the means for producing a part exhibiting advantageous mechanical properties making it possible in particular to meet the needs of engine manufacturers for aeronautics by having a yield point of about 400 MPa at 0.2% ambient temperature at 0.2%. and an elongation at break of the order of 1.5%, and creep at 700 ° C - 300 MPa and at 750 ° C - 200 MPa, a time before rupture of at least 400 hours. Thus, the present invention aims to provide a part with excellent properties including the point of view of the ductility at room temperature and the hot resistance.
Pour la présente invention, on entend ici par pièce tout produit obtenu par la présente invention et destiné à être utilisé par la suite comme ébauche d'une pièce mécanique, comme pièce mécanique (aube de turbine, soupape, ...) ou partie de pièce mécanique (tête de soupape, ...) ou bien encore plusieurs pièces mécaniques (réalisation de plusieurs aubes ou soupapes ou tout ensemble de pièces mécaniques, notamment pièces mécaniques complexes). Une pastille, un bloc, une barre ou tout autre élément de base pouvant servir pour la réalisation par usinage d'un composant mécanique sont ici aussi considérés comme étant chacun une pièce.For the present invention, the term "piece" here means any product obtained by the present invention and intended to be used subsequently as a blank for a mechanical part, as a mechanical part (turbine blade, valve, etc.) or part of mechanical part (valve head, ...) or several mechanical parts (realization of several blades or valves or any set of mechanical parts, including complex mechanical parts). A pellet, a block, a bar or any other basic element that can be used for machining a mechanical component are here also considered to be one piece.
Le procédé selon l'invention vise en outre à obtenir une pièce présentant une grande homogénéité des microstructures et par conséquent une excellente reproductibilité des propriétés mécaniques.The method according to the invention is also intended to obtain a part having a high homogeneity of microstructures and therefore excellent reproducibility of mechanical properties.
Avantageusement, la présente invention fournira un procédé caractérisé par un faible coût et par une robustesse des moyens permettant sa mise en oeuvre.Advantageously, the present invention will provide a method characterized by a low cost and robustness of the means for its implementation.
Le procédé selon l'invention offrira avantageusement également une grande rapidité d'élaboration et permettra la fabrication de la pièce sans traitement thermique ultérieur, offrant alors la possibilité de fabriquer directement des préformes d'aubes et donc de limiter l'usinage.The method according to the invention will also advantageously offer a high speed of elaboration and will allow the manufacture of the part without subsequent heat treatment, thus offering the possibility of directly manufacturing blade preforms and thus limiting the machining.
À cet effet la présente invention propose un procédé de fabrication par frittage flash d'une pièce (PF) en alliage métallique, comportant l'application simultanée d'une pression uniaxiale et d'un courant électrique à un outillage contenant un matériau constitutif pulvérulent répondant à la composition suivante en pourcentage atomique :
- 42 à 49 % d'aluminium,
- 0,05 à 1,5 % de bore,
- 0,2% minimum d'au moins un élément choisi parmi le tungstène, le rhénium et le zirconium
éventuellement 0 à 5 % d'un ou plusieurs éléments choisis parmi le chrome, le niobium, le molybdène, le silicium et le carbone,- du titane faisant la balance et la totalité des éléments hors aluminium et titane étant comprise
entre 0,25 et 12 %.
- 42 to 49% aluminum,
- 0.05 to 1.5% boron,
- 0.2% minimum of at least one element selected from tungsten, rhenium and zirconium
- optionally 0 to 5% of one or more elements selected from chromium, niobium, molybdenum, silicon and carbon,
- titanium balancing and all the elements except aluminum and titanium being between 0.25 and 12%.
La présente invention propose donc de combiner de manière tout à fait originale un alliage à base de titane et d'aluminium, présentant une composition chimique particulière, avec un procédé de fabrication par frittage flash (ou SPS). De façon surprenante, le procédé ci-dessus permet d'obtenir des pièces avec des caractéristiques mécaniques répondant largement aux exigences des motoristes dans l'aéronautique.The present invention therefore proposes to combine in a completely novel manner a titanium-aluminum alloy, having a particular chemical composition, with a flash sintering (or SPS) manufacturing process. Surprisingly, the above process makes it possible to obtain parts with mechanical characteristics that largely meet the requirements of the engine manufacturers in the aeronautical industry.
La composition chimique du matériau utilisé dans le procédé selon l'invention est basée sur des éléments qui sont relativement peu coûteux tel que le tungstène.The chemical composition of the material used in the process according to the invention is based on elements which are relatively inexpensive such as tungsten.
Les alliages TiAl classiquement fabriqués par la voie fonderie sont beaucoup moins performants en termes de compromis ductilité/tenue au fluage et de reproductibilité des microstructures que des alliages obtenus par un procédé selon la présente invention. De plus, cette voie (fonderie) nécessite d'appliquer aux alliages des traitements thermiques et un usinage de matière plus important que pour la voie SPS.The TiAl alloys conventionally manufactured by the foundry process are much less efficient in terms of the ductility / creep resistance compromise and the reproducibility of the microstructures than the alloys obtained by a process according to the present invention. In addition, this path (foundry) requires to apply to the alloys heat treatments and material machining more important than for the SPS channel.
L'utilisation de la voie de la métallurgie des poudres (MdP) associée à celle du frittage flash permet ici d'affiner et d'homogénéiser les microstructures pour les alliages sélectionnés par la présente invention et permet leur mise en oeuvre aux plus hautes températures d'utilisation. Le courant électrique peut passer directement dans le matériau pulvérulent et/ou dans l'outillage et provoque ainsi une augmentation de la température du matériau.The use of the powder metallurgy (PW) pathway associated with that of flash sintering makes it possible here to refine and homogenize the microstructures for the alloys selected by the present invention and allows them to be used at the highest temperatures in the field. 'use. The electric current can pass directly into the powder material and / or into the tooling and thus causes an increase in the temperature of the material.
Les autres voies envisagées comme le forgeage et la fusion de poudres par faisceau d'électrons n'ont pour l'instant pas abouti à la fabrication d'aubes et à la production conjointe d'un alliage aussi performant que celui obtenu à l'issue du procédé selon la présente invention.The other channels envisaged, such as forging and melting of powders by electron beam, have so far not resulted in the manufacture of blades and the joint production of an alloy as efficient as that obtained at the end of the process according to the present invention.
La pièce (PF) en alliage métallique obtenue à l'issue du procédé selon l'invention contient des éléments lourds dans une quantité inférieure à 5% atomique et du bore en très faible quantité (0,05 à 1,5 % atomique), ce qui permet d'obtenir une microstructure lamellaire à petits grains résistante en fluage. Un autre avantage de la présente invention réside dans le fait qu'il n'est pas nécessaire d'aller chercher systématiquement des nuances à faible teneur en aluminium pour, par exemple, favoriser la solidification β, puisque l'alliage obtenu à l'issue du procédé contient du bore pour permettre l'obtention d'une microstructure fine avec des grains équiaxes. Une originalité par rapport aux alliages existants est ainsi de pouvoir proposer une nuance riche en aluminium qui a par ailleurs un intérêt pour la ductilité et la tenue à l'oxydation.The metal alloy part (PF) obtained at the end of the process according to the invention contains heavy elements in an amount of less than 5 atomic% and boron in a very small amount (0.05 to 1.5 atomic%), which makes it possible to obtain a lamellar microstructure with small grains resistant to creep. Another advantage of the present invention lies in the fact that it is not it is not necessary to systematically obtain low-aluminum grades to, for example, promote β-solidification, since the alloy obtained at the end of the process contains boron in order to obtain a fine microstructure with equiaxed grains. An originality compared to existing alloys is thus to be able to offer a rich aluminum grade which also has an interest in ductility and resistance to oxidation.
Le couplage composition chimique - densification par Spark Plasma Sintering selon la présente invention permet d'obtenir un alliage présentant une microstructure particulière aux propriétés mécaniques exceptionnelles. Elle est formée de petits grains lamellaires, entourés de zones γ périphériques. C'est bien la combinaison de ce procédé avec la composition chimique revendiquée qui permet d'obtenir une pièce dotée de qualités bien supérieures à celles des pièces en alliage de l'art antérieur. En effet, une pièce présentant la même composition chimique que celle qui est revendiquée mais qui serait élaborée par la voie de la métallurgie de poudre (MdP) combinée au procédé conventionnel de compaction isostatique à chaud (CIC) ne présenterait pas de propriétés exceptionnelles, ce qui confirme le caractère original obtenu grâce au procédé selon l'invention.The chemical composition-densification coupling by Spark Plasma Sintering according to the present invention makes it possible to obtain an alloy having a particular microstructure with exceptional mechanical properties. It is formed of small lamellar grains, surrounded by peripheral γ zones. It is the combination of this method with the claimed chemical composition that makes it possible to obtain a piece with qualities far superior to those of the alloy parts of the prior art. In fact, a part with the same chemical composition as the one claimed but which would be produced by powder metallurgy (PW) in combination with the conventional hot isostatic compaction (DUC) process would not have exceptional properties. which confirms the original character obtained thanks to the method according to the invention.
Le procédé ainsi défini selon la présente invention permet de limiter le grossissement des grains, d'obtenir une microstructure lamellaire fine, d'avoir une phase γ intrinsèquement résistante à chaud et à température ambiante, d'avoir une bonne reproductibilité des propriétés mécaniques ainsi qu'un très bon compromis entre ductilité à température ambiante et tenue en fluage à haute température.The method thus defined according to the present invention makes it possible to limit the magnification of the grains, to obtain a thin lamellar microstructure, to have a γ phase intrinsically resistant to heat and at ambient temperature, to have good reproducibility of the mechanical properties as well as a very good compromise between ductility at room temperature and resistance to creep at high temperature.
De préférence, le matériau utilisé dans le cadre du procédé selon l'invention comprend au moins un des éléments suivants dans les proportions définies ci-après :
- 0,2 à 4 % de tungstène,
- 0,2 à 4 % de rhénium,
- 0,2 à 5 % de zirconium,
- 0 à 3 % de chrome,
- 0 à 5 % de niobium,
- 0 à 5 % de molybdène,
- 0 à 2 % de silicium,
- 0 à 1 % de carbone.
- 0.2 to 4% of tungsten,
- 0.2 to 4% rhenium,
- 0.2 to 5% zirconium,
- 0 to 3% chromium,
- 0 to 5% of niobium,
- 0 to 5% molybdenum,
- 0 to 2% silicon,
- 0 to 1% carbon.
Dans un mode particulier de réalisation, le matériau utilisé dans le cadre du procédé selon l'invention répond à la composition suivante en pourcentage atomique : 49,92% de titane, 48,00% d'aluminium, 2,00% de tungstène, 0,08% de bore.In a particular embodiment, the material used in the context of the process according to the invention has the following composition in atomic percentage: 49.92% of titanium, 48.00% of aluminum, 2.00% of tungsten, 0.08% boron.
De manière préférée, le procédé selon la présente invention comprend les étapes suivantes :
- a) Sélectionner une composition choisie parmi les compositions définies ci-dessus pour la présente invention,
- b) Appliquer une pression supérieure à 30 MPa et augmenter la température progressivement jusqu'à un palier situé entre 1200 et 1400 °C.
- c) Maintenir la température au palier pendant au moins une minute,
- d) Ramener la température et la pression aux conditions ambiantes.
- a) Selecting a composition chosen from the compositions defined above for the present invention,
- b) Apply pressure above 30 MPa and increase the temperature gradually to a plateau between 1200 and 1400 ° C.
- (c) Maintain the temperature at the landing for at least one minute,
- d) Reduce the temperature and pressure to ambient conditions.
Dans un mode particulier de réalisation du procédé selon l'invention, une pression comprise entre 80 et 120 MPa est appliquée au cours de l'étape b). De manière préférée, la pression augmente progressivement au cours de l'étape b) sur une période inférieure à 5 minutes.In a particular embodiment of the method according to the invention, a pressure of between 80 and 120 MPa is applied during step b). Preferably, the pressure increases gradually during step b) over a period of less than 5 minutes.
Dans un autre mode particulier de réalisation du procédé selon l'invention, toujours au cours de l'étape b), la température augmente de 80 à 120°C/min.In another particular embodiment of the method according to the invention, still during step b), the temperature increases from 80 to 120 ° C / min.
De préférence, au cours de l'étape c), la température est maintenue au palier pendant deux minutes.Preferably, during step c), the temperature is maintained at the plateau for two minutes.
Le procédé selon la présente invention est utilisé de manière particulièrement avantageuse pour la fabrication d'une préforme d'aube de turbine et/ou d'une roue de turbine de turbocompresseur et/ou d'une soupape (ou tout du moins d'une tête de soupape) et/ou d'un axe de piston.The method according to the present invention is particularly advantageously used for the manufacture of a turbine blade preform and / or a turbocharger turbine wheel and / or a valve (or at least one valve head) and / or a piston pin.
D'autres caractéristiques et avantages de l'invention apparaîtront encore à la lecture de la description qui va suivre. Celle-ci est purement illustrative et doit être lue en regard des
- La
figure 1 illustre une évolution de la pression et de la température mesurées en fonction du temps pendant un cycle SPS mis en oeuvre selon l'invention, - La
figure 2 illustre des images obtenues par MEB (acronyme de Microscopie Électronique à Balayage) d'une microstructure d'une pièce issue du procédé selon l'invention à différents grandissements, - La
figure 3 illustre une large zone d'une microstructure d'une pièce issue du procédé selon l'invention étudiée en MEB et MET (acronyme de Microscopie Électronique en Transmission), - La
figure 4 illustre une zone γ périphérique contenant des précipités de phase B2 entre des grains lamellaires observés par MET de la microstructure d'une pièce issue du procédé selon l'invention, - La
figure 5 illustre des analyses chimiques locales par EDS-MEB (pour spectroscopie de rayons X à dispersion d'énergie - Microscopie Électronique à Balayage) d'une pièce issue du procédé selon l'invention, - La
figure 6 illustre des courbes de traction à température ambiante obtenues dans deux échantillons de l'alliage obtenus par procédé selon l'invention, et - La
figure 7 illustre des courbes de fluage obtenues à 700 °C sous 300 MPa dans deux échantillons de l'alliage obtenus par procédé selon l'invention.
- The
figure 1 illustrates a change in pressure and temperature measured as a function of time during an SPS cycle implemented according to the invention, - The
figure 2 illustrates images obtained by SEM (acronym for Scanning Electron Microscopy) of a microstructure of a part resulting from the process according to the invention at different magnitudes, - The
figure 3 illustrates a large area of a microstructure of a part resulting from the process according to the invention studied in SEM and MET (acronym for Electron Microscopy in Transmission), - The
figure 4 illustrates a peripheral γ zone containing phase B2 precipitates between lamellar grains observed by TEM of the microstructure of a part resulting from the process according to the invention, - The
figure 5 illustrates local chemical analyzes by EDS-MEB (for energy dispersive X-ray spectroscopy - Scanning Electron Microscopy) of a part resulting from the process according to the invention, - The
figure 6 illustrates room temperature tensile curves obtained in two samples of the alloy obtained by the process according to the invention, and - The
figure 7 illustrates creep curves obtained at 700 ° C. under 300 MPa in two samples of the alloy obtained by the process according to the invention.
Il est proposé ici de manière originale de réaliser une pièce en alliage à base de titane et d'aluminium par un procédé connu sous le nom SPS (acronyme anglais de Spark Plasma Sintering, appelé en français frittage flash) à partir d'un matériau constitutif pulvérulent. L'alliage utilisé répond à la composition en pourcentage atomique suivante :
- 42 à 49 % d'aluminium,
- 0,05 à 1,5 % de bore,
- 0,2% minimum d'au moins un élément choisi parmi le tungstène, le rhénium et le zirconium,
éventuellement 0 à 5 % d'un ou plusieurs éléments choisis parmi le chrome, le niobium, le molybdène, le silicium et le carbone, du titane faisant la balance et la totalité des éléments hors aluminium et titane étant compriseentre 0,25 et 12 %.
- 42 to 49% aluminum,
- 0.05 to 1.5% boron,
- 0.2% minimum of at least one element selected from tungsten, rhenium and zirconium,
- optionally 0 to 5% of one or more elements selected from chromium, niobium, molybdenum, silicon and carbon, titanium balancing and all the elements excluding aluminum and titanium being between 0.25 and 12 %.
Ce matériau contient des éléments lourds dans une quantité inférieure à 5% atomique et du bore en très faible quantité (0,05 à 1,5 %). De préférence, il comprend, outre le titane, l'aluminium et le bore, au moins un des éléments suivants dans les proportions définies ci-après :
- 0,2 à 4 % de tungstène,
- 0,2 à 4 % de rhénium,
- 0,2 à 5 % de zirconium,
- 0 à 3 % de chrome,
- 0 à 5 % de niobium,
- 0 à 5 % de molybdène,
- 0 à 2 % de silicium,
- 0 à 1 % de carbone.
- 0.2 to 4% of tungsten,
- 0.2 to 4% rhenium,
- 0.2 to 5% zirconium,
- 0 to 3% chromium,
- 0 to 5% of niobium,
- 0 to 5% molybdenum,
- 0 to 2% silicon,
- 0 to 1% carbon.
De manière encore préférée, il répond à la composition suivante Ti49,92Al48W2B0,08.More preferably, it has the following composition Ti 49.92 Al 48 W 2 B 0.08 .
Des alliages de structure lamellaire à petits grains sont ainsi obtenus par un cycle SPS simple selon la présente invention. Le cycle SPS utilisé dans le cadre de l'invention est basé sur le procédé décrit dans la demande internationale
Le dispositif présente l'avantage de permettre la fabrication de pièces métalliques de forme complexes. Toutefois, on peut envisager d'utiliser un dispositif différent permettant la mise en oeuvre d'un procédé SPS pour la mise en oeuvre de la présente invention.The device has the advantage of allowing the manufacture of complex shaped metal parts. However, it is possible to envisage using a different device allowing the implementation of an SPS method for the implementation of the present invention.
Jusqu'à présent, un procédé SPS, pour une pièce de géométrie simple ou complexe, n'a jamais été utilisé avec un matériau répondant à la composition telle que définie plus haut. Cette combinaison d'un procédé de fabrication avec un alliage particulier permet de réaliser de façon surprenante une pièce en alliage métallique présentant des propriétés mécaniques exceptionnelles comme illustré ci-après.So far, an SPS process, for a piece of simple or complex geometry, has never been used with a material meeting the composition as defined above. This combination of a manufacturing method with a particular alloy makes it possible surprisingly to produce a metal alloy piece having exceptional mechanical properties as illustrated below.
Il est proposé d'utiliser le dispositif présenté et revendiqué dans le document
L'alliage constituant la pièce obtenue présente une microstructure illustrée sur la
La
La
Le mécanisme de formation de cette microstructure n'est pas complètement clair car le diagramme d'équilibre correspondant à cette composition n'est pas connu complètement. Des travaux sont en cours sur ce mécanisme de formation. Toutefois, il semble que la montée en température à 1355°C permette le franchissement du transus α. Cependant, soit parce qu'il n'existe pas pour cette composition de domaine monophasé α, soit parce que la cinétique de transformation est trop lente, il est probable qu'il subsiste à 1355°C des zones β en périphérie des grains α. La limitation du grossissement des grains α est donc due non seulement au bore mais peut-être aussi à la présence de cette phase résiduelle. Lors du refroidissement deux transformations se produisent : la transformation lamellaire qui est facilitée par la présence de borure et la transformation des zones périphériques β en γ + B2.The mechanism of formation of this microstructure is not completely clear because the equilibrium diagram corresponding to this composition is not completely known. Work is in progress on this training mechanism. However, it seems that the rise in temperature to 1355 ° C allows the crossing of the transus α. However, either because it does not exist for this one-phase domain composition α, or because the kinetics of transformation is too slow, it is likely that there remain at 1355 ° C zones β periphery of α grains. The limitation of the magnification of α grains is therefore due not only to boron but possibly also to the presence of this residual phase. During cooling two transformations occur: the lamellar transformation which is facilitated by the presence of boride and the transformation of the peripheral zones β into γ + B2.
Les
Les tableaux ci-dessous résument des résultats obtenus grâce à la présente invention avec la composition Ti49,92Al48W2B0,08 en matière de traction et de fluage.The tables below summarize the results obtained with the present invention with the composition Ti 49.92 Al 48 W 2 B 0.08 in terms of traction and creep.
Ces excellents résultats permettent à l'homme du métier de mieux appréhender l'intérêt de la présente invention pour des applications à hautes températures.These excellent results allow the skilled person to better understand the interest of the present invention for high temperature applications.
La ductilité obtenue pourrait s'expliquer par : i) la présence de zones γ périphériques qui acceptent une quantité de déformation assez importante, ii) les caractéristiques des zones lamellaires (taille des lamelles assez importante) qui sont également déformables et iii) la taille réduite des grains lamellaires qui limite la formation d'empilements générateurs de contraintes internes provoquant la rupture. L'exceptionnelle tenue au fluage pourrait s'expliquer par la résistance de la structure lamellaire et la bonne dispersion du tungstène dans la matrice γ qui se déforme. Il semble que les dimensions caractéristiques de la microstructure obtenue à l'issue du procédé selon l'invention, à savoir la taille des grains et la largeur des lamelles, soient proches de l'idéal pour qu'à la fois les dislocations ne se déplacent pas trop facilement en mettant en jeu de la diffusion et qu'il y ait suffisamment d'interfaces et de joints de grains pour faire obstacle au mouvement des dislocations.The ductility obtained could be explained by: i) the presence of peripheral γ zones that accept a fairly large amount of deformation, ii) the characteristics of the lamellar zones (fairly large lamella size) which are also deformable and iii) the small size lamellar grains which limit the formation of internally constraining stacks causing rupture. The exceptional resistance to creep could be explained by the resistance of the lamellar structure and the good dispersion of tungsten in the matrix γ which is deformed. It seems that the characteristic dimensions of the microstructure obtained at the end of the process according to the invention, namely the size of the grains and the width of the lamellae, are close to the ideal so that at the same time the dislocations do not move. not too easily by involving diffusion and that there are enough interfaces and grain boundaries to hinder the movement of dislocations.
À l'issue du procédé selon l'invention, une pièce en alliage métallique a pu être fabriquée. Cette pièce présentait des caractéristiques allant au-delà des caractéristiques correspondant aux besoins mentionnés précédemment pour des aubes de turbine d'un moteur d'avion (limite d'élasticité d'environ 400 MPa à 0,2 % à la température ambiante et un allongement à la rupture de l'ordre de 1,5%, et en fluage à 700 °C - 300 MPa et à 750 °C - 200 MPa, une durée avant rupture d'au moins 400 heures) et remplissait même largement l'ensemble des spécifications requises.At the end of the process according to the invention, a metal alloy part could be manufactured. This part had characteristics going beyond the characteristics corresponding to the aforementioned requirements for turbine blades of an aircraft engine (elastic limit of about 400 MPa at 0.2% at room temperature and an elongation at break of the order of 1.5%, and creep at 700 ° C - 300 MPa and at 750 ° C - 200 MPa, a break-up time of at least 400 hours) and even largely fulfilled all required specifications.
Bien entendu, la présente invention ne se limite pas à la forme de réalisation préférée décrite ci-dessus à titre d'exemple non limitatif et aux variantes de réalisation évoquées. Elle concerne également toute variante de réalisation à la portée de l'homme du métier dans le cadre des revendications ci-après.Of course, the present invention is not limited to the preferred embodiment described above by way of non-limiting example and the variants mentioned. It also relates to any embodiment within the scope of the skilled person within the scope of the claims below.
Claims (12)
- Method for manufacturing a metal alloy part (PF) by spark plasma sintering, comprising the simultaneous application of a uniaxial pressure and of an electric current to an equipment containing a powder component material that has the following composition in atomic percentages:- 42 to 49 % aluminum,- 0.05 to 1.5% boron,- at least 0.2% of at least one element selected from tungsten, rhenium and zirconium,- optionally 0 to 5 % of one or more elements selected from chromium, niobium, molybdenum, silicon and carbon,- the balance being titanium and the total of the elements without aluminum and titanium being between 0.25 and 12 %.
- Method according to claim 1, characterized in that the material comprises at least one of the following elements in the proportions defined below:- 0.2 to 4 % tungsten,- 0.2 to 4 % rhenium,- 0.2 to 5 % zirconium,- 0 to 3 % chromium,- 0 to 5 % niobium,- 0 to 5 % molybdenum,- 0 to 2 % silicon,- 0 to 1 % carbon.
- Method according to claim 1 or 2, characterized in that the material has the following composition in atomic percentages: 49.92% titanium, 48.00% aluminum, 2.00% tungsten, 0.08% boron.
- Method according to one of claims 1 to 3 characterized in that the method comprises the following steps:a) Select a composition defined in claims 1 to 3,b) Apply pressure greater than 30 MPa and progressively increase the temperature to a target between 1200 and 1400 °C.c) Maintain the target temperature for at least one minute.d) Return the temperature and pressure to ambient conditions.
- Method according to claim 4, characterized in that pressure between 80 and 120 MPa is applied during step b).
- Method according to claim 4 or 5, characterized in that the pressure progressively increases over a period of less than 5 minutes during step b).
- Method according to any one of claims 4 to 6, characterized in that, during step b), the temperature increases from 80 to 120°C/min except for the last three minutes before the target temperature, when the rate is reduced between 10 and 40 °C/min.
- Method according to any one of claims 4 to 7, characterized in that during step c), the temperature is maintained at the target for two minutes.
- Utilization of the method according to any one of the previous claims to manufacture a turbine blade.
- Utilization of the method according to any one of claims 1 to 8 to manufacture an internal combustion engine valve.
- Utilization of the method according to any one of claims 1 to 8 to manufacture a turbocharger turbine wheel.
- Utilization of the method according to any one of claims 1 to 8 to manufacture a piston pin.
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| PL14734884T PL3007844T3 (en) | 2013-06-11 | 2014-06-11 | Method for manufacturing a titanium-aluminium alloy part |
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| FR1355393A FR3006696B1 (en) | 2013-06-11 | 2013-06-11 | PROCESS FOR MANUFACTURING A TITANIUM ALUMINUM ALLOY PIECE |
| PCT/FR2014/051419 WO2014199082A1 (en) | 2013-06-11 | 2014-06-11 | Method for manufacturing a titanium-aluminium alloy part |
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| EP3007844A1 EP3007844A1 (en) | 2016-04-20 |
| EP3007844B1 true EP3007844B1 (en) | 2017-08-16 |
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| US (1) | US10183331B2 (en) |
| EP (1) | EP3007844B1 (en) |
| JP (1) | JP6445542B2 (en) |
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| CN (1) | CN105451915B (en) |
| FR (1) | FR3006696B1 (en) |
| MX (1) | MX2015017070A (en) |
| PL (1) | PL3007844T3 (en) |
| WO (1) | WO2014199082A1 (en) |
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| CN104550956A (en) * | 2015-01-20 | 2015-04-29 | 哈尔滨工业大学 | Component preparation method through beta-gamma titanium-aluminum alloy prealloy powder spark plasma sintering |
| KR20180112071A (en) * | 2016-04-20 | 2018-10-11 | 아르코닉 인코포레이티드 | HCP materials consisting of aluminum, titanium, and zirconium, and products made therefrom |
| CN107058799B (en) * | 2017-01-22 | 2019-09-20 | 康硕电气集团有限公司 | A kind of rhenium-containing 3D printing titanium-based alloy material and preparation method thereof |
| US11229950B2 (en) | 2017-04-21 | 2022-01-25 | Raytheon Technologies Corporation | Systems, devices and methods for spark plasma sintering |
| CN108856708B (en) * | 2017-05-09 | 2020-08-04 | 中国航空制造技术研究院 | TiAl-based material with gradient structure and manufacturing method thereof |
| KR102010306B1 (en) * | 2017-11-03 | 2019-08-13 | (주)차세대소재연구소 | Aluminum-Titanium Different Functionally Graded Composite Materials and Manufacturing method thereof |
| EP3575016A1 (en) * | 2018-06-01 | 2019-12-04 | Siemens Aktiengesellschaft | Improvements relating to the manufacture of superalloy components |
| JP7233659B2 (en) * | 2019-03-18 | 2023-03-07 | 株式会社Ihi | Titanium aluminide alloy material for hot forging, method for forging titanium aluminide alloy material, and forged body |
| FR3105048B1 (en) * | 2019-12-20 | 2022-08-05 | Safran | MANUFACTURING SOLUTION FOR A MONOBLOC BLADE DISC |
| CN112756624A (en) * | 2020-12-11 | 2021-05-07 | 丹阳层现三维科技有限公司 | Method for reducing cracks in selective laser melting printing titanium-aluminum alloy |
| CN116607048A (en) * | 2022-02-09 | 2023-08-18 | 中国科学院金属研究所 | Gamma-TiAl alloy for precision casting and preparation method thereof |
| PL440911A1 (en) | 2022-04-11 | 2023-10-16 | Kghm Polska Miedź Spółka Akcyjna | Three-component titanium alloy, method of its production and application |
| CN115404381B (en) * | 2022-09-14 | 2023-06-30 | 西北工业大学 | TiAl alloy sheet and low-cost rolling method thereof |
| CN115466867B (en) * | 2022-09-14 | 2023-05-05 | 西北工业大学 | TiAl alloy capable of improving uniform deformation capacity and preparation method thereof |
| CN115627386B (en) * | 2022-11-07 | 2023-10-24 | 西北工业大学 | TiAlRe alloy suitable for rolling deformation and rolling method thereof |
| CN115976367A (en) * | 2023-02-17 | 2023-04-18 | 浙江工业大学 | Rhenium alloying titanium-aluminum alloy and preparation method thereof |
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| DE59106459D1 (en) | 1990-05-04 | 1995-10-19 | Asea Brown Boveri | High temperature alloy for machine components based on doped titanium aluminide. |
| JP2743720B2 (en) | 1992-07-03 | 1998-04-22 | トヨタ自動車株式会社 | Method for producing TiB2 dispersed TiAl-based composite material |
| JPH0892602A (en) * | 1994-09-28 | 1996-04-09 | Toyo Alum Kk | Titanium-aluminium intermetallic compound powder and its sintered compact |
| FR2732038B1 (en) | 1995-03-24 | 1997-06-06 | Onera (Off Nat Aerospatiale) | INTERMETALLIC ALLOY BASED ON TITANIUM ALUMINIURE FOR FOUNDRY |
| CN100425722C (en) * | 2005-11-30 | 2008-10-15 | 济南大学 | Method for improving property of TiAI intermetallic compound based composite material |
| CN100496815C (en) * | 2007-01-31 | 2009-06-10 | 哈尔滨工业大学 | TiAl-base composite material enhanced by three-dimensional network Ti2AlC and manufacturing method thereof |
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| CN102492871A (en) * | 2011-12-19 | 2012-06-13 | 武汉理工大学 | TiAl intermetallic compound-based solid seif-lubricating composite material and preparation method thereof |
| CN102888549A (en) * | 2012-10-19 | 2013-01-23 | 武汉理工大学 | TiAl-C-Ag-Ti2AlC-TiC self-lubricating composite material and preparation method thereof |
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2013
- 2013-06-11 FR FR1355393A patent/FR3006696B1/en not_active Expired - Fee Related
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2014
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- 2014-06-11 EP EP14734884.1A patent/EP3007844B1/en not_active Not-in-force
- 2014-06-11 US US14/897,877 patent/US10183331B2/en active Active
- 2014-06-11 MX MX2015017070A patent/MX2015017070A/en unknown
- 2014-06-11 JP JP2016518568A patent/JP6445542B2/en not_active Expired - Fee Related
- 2014-06-11 WO PCT/FR2014/051419 patent/WO2014199082A1/en active Application Filing
Non-Patent Citations (1)
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2014199082A1 (en) | 2014-12-18 |
| US20160121400A1 (en) | 2016-05-05 |
| FR3006696B1 (en) | 2015-06-26 |
| PL3007844T3 (en) | 2018-02-28 |
| MX2015017070A (en) | 2016-08-03 |
| EP3007844A1 (en) | 2016-04-20 |
| CN105451915A (en) | 2016-03-30 |
| KR20160033096A (en) | 2016-03-25 |
| US10183331B2 (en) | 2019-01-22 |
| JP2016526602A (en) | 2016-09-05 |
| JP6445542B2 (en) | 2018-12-26 |
| FR3006696A1 (en) | 2014-12-12 |
| CN105451915B (en) | 2018-01-02 |
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