EP3080318B1 - Method for manufacturing products made of aluminium-copper-lithium alloy with improved fatigue properties and distributor for this method - Google Patents

Method for manufacturing products made of aluminium-copper-lithium alloy with improved fatigue properties and distributor for this method Download PDF

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Publication number
EP3080318B1
EP3080318B1 EP14828176.9A EP14828176A EP3080318B1 EP 3080318 B1 EP3080318 B1 EP 3080318B1 EP 14828176 A EP14828176 A EP 14828176A EP 3080318 B1 EP3080318 B1 EP 3080318B1
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Prior art keywords
weight
fabric
casting
dispenser
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German (de)
French (fr)
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EP3080318A2 (en
EP3080318B2 (en
Inventor
Armelle Danielou
Soizic BLAIS
Philippe Jarry
Olivier Ribaud
Bernard Valentin
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Constellium Issoire SAS
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Constellium Issoire SAS
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    • 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/057—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/14—Alloys based on aluminium with copper as the next major constituent with silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/21—Presses specially adapted for extruding metal
    • B21C23/212—Details
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
    • B22D11/003—Aluminium alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/0408—Moulds for casting thin slabs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/041—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds for vertical casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/059—Mould materials or platings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/10—Supplying or treating molten metal
    • B22D11/103—Distributing the molten metal, e.g. using runners, floats, distributors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/10—Supplying or treating molten metal
    • B22D11/11—Treating the molten metal
    • B22D11/116—Refining the metal
    • B22D11/119—Refining the metal by filtering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/002—Castings of light metals
    • B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/04—Casting aluminium or magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/18—Alloys based on aluminium with copper as the next major constituent with zinc
    • 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B2003/001—Aluminium or its alloys

Definitions

  • the invention relates to a distributor for the semi-continuous casting of aluminum alloy plates and a process for producing wrought aluminum-copper-lithium alloy products, intended in particular for aeronautical and aerospace construction.
  • Aluminum alloy rolled products are developed to produce structural elements for the aerospace industry and the aerospace industry in particular.
  • Aluminum - copper - lithium alloys are particularly promising for this type of product.
  • the specifications imposed by the aeronautical industry for fatigue performance are high.
  • Thick products made of Al-Cu-Li alloy are described in particular in the US2005 / 0006008 and US2009 / 0159159 .
  • a first object of the invention is a distributor for the semi-continuous casting of aluminum alloy plates according to claim 1.
  • Another object of the invention is a method of manufacturing an aluminum alloy product according to claim 7.
  • the static mechanical characteristics in tension in other words the tensile strength R m , the conventional yield stress at 0.2% elongation R p0.2 , and the elongation at break A% are determined by a tensile test according to standard NF EN ISO 6892-1, the sampling and the direction of the test being defined by the EN 485-1 standard.
  • the test conditions follow the ASTM E466 standard.
  • the logarithmic average of the results obtained on at least 4 test pieces is determined.
  • the Walker equation was used to determine a representative maximum stress value of 50% non-break at 100,000 cycles.
  • the IQF corresponding to the median is reported, ie 50% rupture per 100,000 cycles.
  • a thick wrought product is a product whose thickness is at least 6 mm.
  • the thickness of the products according to the invention is at least 80 mm and preferably at least 100 mm.
  • the thickness of the wrought products is at least 120 mm or preferably 140 mm.
  • the thickness of the thick products according to the invention is typically at most 240 mm, generally at most 220 mm and preferably at most 180 mm.
  • a sheet is according to the invention a laminated product of rectangular cross section whose uniform thickness is at least 6 mm and does not exceed 1 / 10th of the width.
  • a "structural element” or “structural element” of a mechanical construction is called a mechanical part for which the static and / or dynamic mechanical properties are particularly important for the performance of the structure, and for which a structural calculation is usually prescribed or realized. These are typically elements whose failure is likely to endanger the safety of said construction, its users, its users or others.
  • these structural elements include in particular the elements that make up the fuselage (such as the fuselage skin (fuselage skin), the stiffeners or stringers, the bulkheads (bulkheads), circumferential frames, wings (such as wing skin), stiffeners (stiffeners), ribs and spars) and tail fin consisting in particular of horizontal and vertical stabilizers (horizontal or vertical stabilizers), as well as the floor beams, the seat tracks and the doors.
  • the term "set of the casting plant” is here referred to as the set of devices making it possible to transform a metal in any form into a semi-product of raw form via the liquid phase.
  • a casting plant may include a number of devices such as one or more ovens required for melting the metal (“melting furnace”) and / or maintaining it (“holding furnace”) in temperature and / or preparation of the liquid metal and adjustment of the composition (“preparation furnace”), one or more tanks (or “pockets”) intended to carry out a treatment for the removal of impurities dissolved and / or suspended in the liquid metal this treatment may consist of filtering the liquid metal on a filter medium in a "filtration bag” or introducing into the bath a so-called “treatment” gas that can be inert or reactive in a “degassing bag", a device for solidification of the liquid metal (or “casting loom") by vertical semi-continuous casting by direct cooling in a casting well, which may comprise devices such as a mold (or “mold”) a liquid metal supply device (or “nozzle”) and a cooling system, these different furnaces, tanks and solidification devices being interconnected by transfer devices or channels called “chutes” in which the liquid metal can to be transported.
  • devices such
  • an alloy liquid metal bath comprising, in% by weight Cu: 2.0 - 6.0; Li: 0.5 - 2.0; Mg: 0-1.0; Ag: 0 - 0.7; Zn 0 - 1.0; and at least one member selected from Zr, Mn, Cr, Sc, Hf and Ti, the amount of said element, if selected, being from 0.05 to 0.20% by weight for Zr, 0.05 to 0 , 8% by weight for Mn, 0.05 to 0.3% by weight weight for Cr and Sc, 0.05 to 0.5% by weight for Hf and 0.01 to 0.15% by weight for Ti, Si ⁇ 0.1; Fe ⁇ 0.1; other ⁇ 0.05 each and ⁇ 0.15 in total, remains aluminum.
  • An advantageous alloy for the process according to the invention comprises, in% by weight, Cu: 3.0 - 3.9; Li: 0.7 - 1.3; Mg: 0.1 - 1.0, at least one element selected from Zr, Mn and Ti, the amount of said element, if selected, being from 0.06 to 0.15% by weight for Zr, 0, From 0.5 to 0.8% by weight for Mn and from 0.01 to 0.15% by weight for Ti; Ag: 0 - 0.7; Zn ⁇ 0.25; If ⁇ 0.08; Fe ⁇ 0.10; other ⁇ 0.05 each and ⁇ 0.15 in total, remains aluminum.
  • the copper content is at least 3.2% by weight.
  • the lithium content is preferably between 0.85 and 1.15% by weight and preferably between 0.90 and 1.10% by weight.
  • the magnesium content is preferably between 0.20 and 0.6% by weight.
  • the simultaneous addition of manganese and zirconium is generally advantageous.
  • the manganese content is between 0.20 and 0.50% by weight and the zirconium content is between 0.06 and 0.14% by weight.
  • the silver content is between 0.20 and 0.7% by weight. It is advantageous that the silver content is at least 0.1% by weight. In one embodiment of the invention the silver content is at least 0.20% by weight. Preferably, the silver content is at most 0.5% by weight. In one embodiment of the invention, the silver content is limited to 0.3% by weight.
  • the silicon content is at most 0.05% by weight and the iron content is at most 0.06% by weight.
  • the titanium content is between 0.01 and 0.08% by weight.
  • the zinc content is at most 0.15% by weight.
  • a preferred aluminum-copper-lithium alloy is AA2050 alloy. This liquid metal bath is prepared in a furnace of the casting plant. It is known, for example from US 5,415,220 using lithium-containing molten salts such as KCl / LiCl mixtures in the melting furnace to passivate the alloy as it is transferred to the casting plant.
  • molten salt containing lithium is not used throughout the casting installation.
  • no molten salt is used throughout the casting installation.
  • an oxygen content of less than 0.5% by volume and preferably less than 0.3% by volume is maintained.
  • the furnace or furnaces of the casting installation are induction furnaces.
  • the present inventors have found that this type of oven is advantageous despite the stirring generated by the induction heating.
  • This bath of liquid metal is then treated with a degassing bag and in a filtration bag so that its hydrogen content is less than 0.4 ml / 100g and preferably less than 0.35 ml / 100g .
  • the hydrogen content of the liquid metal is measured using a commercial apparatus such as the apparatus marketed under the tradename ALSCAN TM, known to those skilled in the art, the probe being maintained under a nitrogen sweep.
  • the oxygen content of the atmosphere in contact with the liquid metal bath in the melting furnace during the degassing steps, filtration is less than 0.5% by volume and preferably less than 0.3% by volume.
  • the oxygen content of the atmosphere in contact with the liquid metal bath is less than 0.5% by volume and preferably less than 0.3% by volume for the whole of the installation of casting.
  • the liquid metal bath is then solidified in the form of a plate.
  • a plate is an aluminum block of substantially parallelepiped shape, length L, width W and thickness T.
  • the atmosphere is controlled above the liquid surface during solidification.
  • An example of a device for controlling the atmosphere above the liquid surface during solidification is presented on the Figure 2 .
  • the liquid metal coming from a chute (63) is introduced into a nozzle (4) controlled by a stopper (8) which can move towards the up and down (81) in an ingot mold (31) placed on a false bottom (21).
  • the aluminum alloy is solidified by direct cooling (5).
  • the aluminum alloy (1) has at least one solid surface (11, 12, 13) and at least one liquid surface (14, 15).
  • An elevator (2) maintains the level of the liquid surface (14, 15) substantially constant.
  • a distributor (7) allows the distribution of the liquid metal.
  • a cover (62) covers the liquid surface.
  • the cover may include seals (61) for sealing with the casting table (32).
  • the liquid metal in the trough (63) can be advantageously protected by a cover (64).
  • An inert gas (9) is introduced into the chamber (65) defined between the cover and the pouring table.
  • the inert gas is advantageously chosen from rare gases, nitrogen and carbon dioxide or mixtures of these gases.
  • a preferred inert gas is argon.
  • the oxygen content is measured in the chamber (65) above the liquid surface. The flow of inert gas can be adjusted to achieve the desired oxygen content.
  • the suction of the pump (101) is such that the pressure in the enclosure (10) is lower than the pressure in the chamber (65), which can preferably be obtained by imposing a speed of the atmosphere through the open surfaces of the casting well of at least 2 m / s and preferably at least 2.5 m / s.
  • the pressure in the chamber (65) is close to atmospheric pressure and the pressure in the chamber (10) is lower than atmospheric pressure, typically 0.95 times the atmospheric pressure.
  • the chamber (65) is maintained, thanks to the devices described, with an oxygen content of less than 0.5% by volume and preferably less than 0.3% by volume.
  • An example of a dispenser (7) of the process according to the invention is presented on the figures 3 and 4 .
  • the dispenser according to the invention is made of fabric comprising essentially carbon, it comprises a lower face (76), a typically empty upper face defining the orifice through which the liquid metal is introduced (71) and wall of substantially rectangular section typically substantially constant and of height h typically substantially constant, the wall comprising two longitudinal parts parallel to the width W of the plate (720, 721) and two transverse portions parallel to the thickness T of the plate (730, 731), said transverse and longitudinal portions being formed of at least two tissues, a first substantially obturating tissue and semi-rigid (77) maintaining the shape of the dispenser during casting and a second non-sealing fabric (78) for passage and filtration of the liquid, said first and second fabric being bonded to each other without overlapping or overlapping and without interstices separating them, said first fabric continuously covering at least 30% of the area of said wall portions (720,721,730,731) and being positioned so that the liquid surface is in contact with him on the entire section of the dispenser.
  • the first and second fabrics being sewn together without overlapping or overlapping and without interstices separating them, i.e., in contact, the liquid metal can not pass through the first fabric and be deflected by the second fabric as is the case for example in a combo-bag as described in the application WO 99/44719 Fig 2 to 5 .
  • the dispenser is semi-rigid and does not deform substantially during casting.
  • the first fabric has a height, hl, measured from the upper face on the circumference of the wall (720, 721, 730, 731) such that h1 ⁇ 0.3 h and preferably h1 ⁇ 0, 5 h, where h denotes the total height of the distributor wall.
  • the liquid surface being in contact with said first liquid-sealing fabric passes through the dispenser only under the liquid surface in certain directions of each part of the wall.
  • the height immersed in the liquid wall metal (720, 721, 730, 731) of the distributor (7) covered by the first fabric is at least 20%, preferably 40% and preferably 60% of the height. total submerged wall.
  • the figure 4 represents the bottom and the longitudinal wall portions.
  • the bottom (76) is typically covered by the first and / or second fabric.
  • the first fabric is at least located in the central part of the bottom (76) along a length L1 and / or in the central part of the longitudinal parts (720) and (721) over the entire height h and over a length L2.
  • the surface portion covered by the first fabric is between 30 and 90% and preferably between 50 and 80% for the longitudinal portions (720) and (721), and / or between 30 and 70% and preferably between 40 and 60% for the side parts (730, 731) and / or between 30 and 100% and preferably between 50 and 80% for the bottom (76). It is advantageous that the length L1 of the first tissue located in the bottom (76) is greater than the length L2 of the first tissue located in the portion of the longitudinal walls (720) and (721) in contact with the bottom.
  • the present inventors believe that the geometry of the dispenser makes it possible in particular to improve the quality of the flow of the liquid metal, to reduce turbulence and to improve the temperature distribution.
  • the first fabric and the second fabric are advantageously obtained by weaving a yarn essentially comprising carbon.
  • the weaving of graphite yarn is particularly advantageous.
  • the tissues are typically sewn to each other. It is also possible instead of first and second fabrics to use a single diffuser fabric having at least two weaving areas, more or less dense. It is advantageous for the ease of weaving that the wire comprising carbon is coated with a layer facilitating sliding. This layer may for example comprise a fluorinated polymer such as Teflon or a polyamide such as xylon.
  • the first fabric is substantially obturant. Typically it is a fabric having mesh size of less than 0.5 mm, preferably less than 0.2 mm.
  • the second fabric is non-sealing and allows the passage of the molten metal. Typically, it is a fabric having mesh sizes of between 1 and 5 mm, preferably 2 to 4 mm.
  • the first tissue locally covers the second tissue, while being in intimate contact so as not to leave a gap between the two tissues.
  • the plate thus obtained is then transformed to obtain a wrought product.
  • the plate thus obtained is then homogenized before or after having been optionally machined to obtain a shape that can be deformed while hot.
  • the plate is machined in the form of a rolling plate so as to then be deformed to hot by rolling.
  • the plate is machined as a forging blank so as to be hot deformed by forging.
  • the plate is billet machined so as to be extrusion hot deformed.
  • the homogenization is carried out at a temperature between 470 and 540 ° C for a period of between 2 and 30 hours.
  • the shape thus homogenized is deformed hot and optionally cold so as to obtain a wrought product.
  • the heat-forming temperature is advantageously at least 350 ° C and preferably at least 400 ° C.
  • the rate of deformation hot and optionally cold that is to say the ratio between the difference between the initial thickness, before deformation but after the possible machining, and the final thickness and on the other hand, the initial thickness is less than 85% and preferably less than 80%.
  • the deformation rate during the deformation is less than 75% and preferably less than 70%.
  • the wrought product thus obtained is then dissolved and quenched.
  • the dissolution temperature is advantageously between 470 and 540 ° C and preferably between 490 and 530 ° C and the duration is adapted to the thickness of the product.
  • the wrought product thus solubilized is de-tensioned by plastic deformation with a deformation of at least 1%.
  • the income is made in one or more steps at a temperature advantageously between 130 and 160 ° C for a period of 5 to 60 hours.
  • a metallurgical state T8 such as in particular T851, T83, T84, or T85.
  • the wrought products obtained by the process according to the invention have advantageous properties.
  • the fatigue property is obtained for wrought products obtained by the process according to the invention, the thickness of which is at least 100 mm or preferably at least 120 mm or even at least 140 mm.
  • the products obtained by the process according to the invention have advantageous static mechanical characteristics.
  • wrought products whose thickness is at least 80 mm comprising in% by weight, Cu: 3.0 - 3.9; Li: 0.7 - 1.3; Mg: 0.1 - 1.0, at least one element selected from Zr, Mn and Ti, the amount of said element, if selected, being from 0.06 to 0.15% by weight for Zr, 0, From 0.5 to 0.8% by weight for Mn and from 0.01 to 0.15% by weight for Ti; Ag: 0 - 0.7; Zn ⁇ 0.25; If ⁇ 0.08; Fe ⁇ 0.10; other ⁇ 0.05 each and ⁇ 0.15 in total, remains aluminum, the yield strength measured at quarter thickness in the direction L is at least 450 MPa and preferably at least 470 MPa and / or the breaking strength measured is at least 480 MPa and preferably at least 500 MPa and / or the elongation is at least 5% and preferably at least 6%.
  • the wrought products obtained by the process according to the invention can advantageously be used to produce structural elements, preferably aircraft structural elements.
  • Preferred aircraft structural elements are spars, ribs or frames.
  • the invention is particularly advantageous for parts of complex shape obtained by integral machining, used in particular for the manufacture of aircraft wings and for any other use for which the properties of the products according to the invention are advantageous. .
  • AA2050 alloy plates were prepared. AA2050 alloy plates were cast by direct cooling vertical semi-continuous casting. The alloy was prepared in a melting furnace. For Examples 1 to 7, a KCL / LiCl mixture was used on the surface of the liquid metal in the melting furnace. For Examples 8 to 9 no salt was used in the melting furnace. For Examples 8 to 9 the atmosphere in contact with the liquid metal with an oxygen content of less than 0.3% by volume for the entire casting installation.
  • the casting installation included a hood disposed above the pouring well to limit the oxygen content.
  • an aspiration (101) was also used such that the pressure in the chamber (10) was lower than the pressure in the chamber (65) and such that the speed of the atmosphere through the open surfaces of the casting well was at least 2 m / s.
  • Oxygen content was measured with an oximeter during casting.
  • the hydrogen content in the liquid aluminum was measured using an Alscan TM type probe . under nitrogen sweep. Two types of liquid metal dispensers were used.
  • a first "Combo Bag” type dispenser as described, for example, in the Figures 2 to 6 international demand WO 99/44719 , which does not call into question the invention, but made of fabric comprising essentially carbon, referenced below “distributor A” and a second distributor as described figure 3 referenced below “distributor B” is made of graphite wire cloth.
  • the casting conditions of the various tests carried out are given in Table 1.
  • the plates were homogenized for 12 hours at 505 ° C., machined to a thickness of about 365 mm, hot-rolled to sheets with a final thickness of between 154 and 158 mm, dissolved at 504 ° C. , quenched and relieved by controlled traction with a permanent elongation of 3.5%.
  • the sheets thus obtained have an 18 hour income at 155 ° C.
  • Static mechanical properties and toughness were characterized at quarter-thickness. Static mechanical characteristics and toughness are given in Table 2.
  • Table 2 Mechanical characteristics Thickness [mm] Rm (L) Rp0.2 (L) Trial MPa MPa A% (L) 1 158 528 495 6.5 2 155 538 507 7.0 3 155 525 493 8.3 4 158 528 four hundred ninety seven 7.0 5 158 529 495 6.0 6 158 527 496 6.8 7 154 514 486 8.3 8 158 533 502 6.3 9 158 542 512 5.8
  • the fatigue properties were characterized on smooth test specimens and hole test specimens for some samples taken at mid-thickness.
  • the corresponding Wöhler curves are presented on the Figures 6a and 6b .
  • the IQF fatigue quality index was calculated.

Description

Domaine de l'inventionField of the invention

L'invention concerne un distributeur destiné à la coulée semi-continue des plaques en alliage d'aluminium et un procédé de fabrication de produits corroyés alliages aluminium - cuivre - lithium, destinés notamment à la construction aéronautique et aérospatiale.The invention relates to a distributor for the semi-continuous casting of aluminum alloy plates and a process for producing wrought aluminum-copper-lithium alloy products, intended in particular for aeronautical and aerospace construction.

Etat de la techniqueState of the art

Des produits laminés en alliage d'aluminium sont développés pour produire des éléments structuraux destinés notamment à l'industrie aéronautique et à l'industrie aérospatiale.Aluminum alloy rolled products are developed to produce structural elements for the aerospace industry and the aerospace industry in particular.

Les alliages aluminium - cuivre - lithium sont particulièrement prometteurs pour fabriquer ce type de produit. Les spécifications imposées par l'industrie aéronautique pour la tenue en fatigue sont élevées. Pour les produits épais elles sont particulièrement difficiles à atteindre. En effet compte tenu des épaisseurs possibles des plaques coulées, la réduction d'épaisseur par déformation à chaud est assez faible et par conséquent les sites liés à la coulée sur lesquels s'initient les fissures de fatigue ne voient pas leur taille réduite au cours de la déformation à chaud.Aluminum - copper - lithium alloys are particularly promising for this type of product. The specifications imposed by the aeronautical industry for fatigue performance are high. For thick products they are particularly difficult to reach. Indeed, given the possible thicknesses of the cast slabs, the thickness reduction by hot deformation is quite low and therefore the sites related to the casting on which the fatigue cracks are initiated do not see their reduced size during hot deformation.

Le lithium étant particulièrement oxydable, la coulée des alliages aluminium-cuivre-lithium génère d'une manière générale des sites d'initiation de fissure en fatigue plus nombreux que pour les alliages de type 2XXX sans lithium ou 7XXX. Ainsi les solutions habituellement trouvées pour l'obtention de produits laminés épais en alliages de type 2XXX sans lithium ou 7XXX ne permettent pas d'obtenir des propriétés en fatigue suffisantes pour les alliages aluminium - cuivre - lithium.Since lithium is particularly oxidizable, the casting of aluminum-copper-lithium alloys generally generates more fatigue crack initiation sites than for 2XXX lithium-free or 7XXX-type alloys. Thus the solutions usually found for obtaining thick rolled products of 2XXX type alloys without lithium or 7XXX do not make it possible to obtain sufficient fatigue properties for aluminum-copper-lithium alloys.

Des produits épais en alliage Al-Cu-Li sont notamment décrits dans les demandes US2005/0006008 et US2009/0159159 .Thick products made of Al-Cu-Li alloy are described in particular in the US2005 / 0006008 and US2009 / 0159159 .

Dans la demande WO2012/ll0717 , il est proposé pour améliorer les propriétés, notamment en fatigue, des alliages d'aluminium contenant en particulier au moins 0,1 % de Mg et/ou 0,1 % de Li de réaliser lors de la coulée un traitement ultrason. Cependant ce type de traitement reste difficile à effectuer pour les quantités nécessaires à la fabrication de tôles épaisses.In the request WO2012 / ll0717 it is proposed to improve the properties, especially in fatigue, aluminum alloys containing in particular at least 0.1% Mg and / or 0.1% Li to perform during casting an ultrasound treatment. However, this type of treatment remains difficult to perform for the quantities necessary for the manufacture of thick plates.

Dans la demande US5383986 , il est proposé pour améliorer les propriétés mécaniques d'un alliage Al-Cu-Li de réaliser après mise en solution trempe du produit, une traction comprise entre 1 et 20% suivie d'un revenu.In the request US5383986 it is proposed to improve the mechanical properties of an Al-Cu-Li alloy to achieve after solution quenching of the product, a traction of between 1 and 20% followed by income.

Dans la demande US2009/0142222 , il est proposé pour obtenir un excellent compromis de propriétés, en particulier la fatigue, d'utiliser un alliage extrudé consistant essentiellement en 3.4-4.2 pds% Cu; 0.9-1.4 pds% Li; 0.3-0.7 pds% Ag; 0.1-0.6 pds% Mg; 0.2-0.8 pds% Zn; 0.1-0.6 pds% Mn et 0.01-0.06 pds % d'au moins un élément influant sur la taille de grain ; le reste consistant en l'aluminium et d'éventuelles impuretés.In the request US2009 / 0142222 it is proposed to obtain an excellent compromise of properties, in particular fatigue, of using an extruded alloy consisting essentially of 3.4-4.2 wt% Cu; 0.9-1.4 wt% Li; 0.3-0.7 wt% Ag; 0.1-0.6 wt% Mg; 0.2-0.8 wt% Zn; 0.1-0.6 wt% Mn and 0.01-0.06 wt% of at least one element affecting grain size; the rest consisting of aluminum and possible impurities.

Il existe un besoin pour des produits épais en alliage aluminium - cuivre - lithium présentant des propriétés améliorées par rapport à celles des produits connus, en particulier en termes de propriétés en fatigue tout en ayant des propriétés de ténacité et des propriétés de résistance mécanique statique avantageuses. Par ailleurs il existe un besoin pour un procédé simple et économique d'obtention de ces produits.There is a need for thick aluminum-copper-lithium alloy products having improved properties over those of the known products, particularly in terms of fatigue properties while having advantageous toughness properties and static strength properties. . Moreover, there is a need for a simple and economical method of obtaining these products.

Objet de l'inventionObject of the invention

Un premier objet de l'invention est un distributeur destiné à la coulée semi-continue de plaques en alliage d'aluminium selon la revendication 1.A first object of the invention is a distributor for the semi-continuous casting of aluminum alloy plates according to claim 1.

Un autre objet de l'invention est un procédé de fabrication d'un produit en alliage d'aluminium selon la revendication 7.Another object of the invention is a method of manufacturing an aluminum alloy product according to claim 7.

Description des figuresDescription of figures

  • La Figure 1 est le schéma des éprouvettes utilisées pour les essais en fatigue lisse (Fig 1a) et en fatigue à trou (Fig 1b). Les dimensions sont données en mm.The Figure 1 is the diagram of the specimens used for the smooth fatigue tests ( Fig 1a ) and in hole fatigue ( Fig 1b ). Dimensions are given in mm.
  • La Figure 2 est un schéma général du dispositif de solidification utilisé dans un mode de réalisation de l'invention.The Figure 2 is a general diagram of the solidification device used in one embodiment of the invention.
  • La Figure 3 est un schéma général du distributeur utilisé dans le procédé selon l'invention.The Figure 3 is a general scheme of the dispenser used in the process according to the invention.
  • La Figure 4 présente des représentations du fond et des parties latérales et longitudinales de la paroi du distributeur selon un mode de réalisation de l'invention.The Figure 4 presents representations of the bottom and the lateral and longitudinal parts of the distributor wall according to one embodiment of the invention.
  • La Figure 5 montre la relation entre la performance en fatigue lisse et la teneur en hydrogène du bain de métal liquide lors de la solidification (Fig 5a) ou la teneur en oxygène mesurée au-dessus de la surface liquide lors de la solidification (Fig. 5b).The Figure 5 shows the relationship between the smooth fatigue performance and the hydrogen content of the liquid metal bath during solidification ( Fig 5a ) or the oxygen content measured above the liquid surface during solidification ( Fig. 5b ).
  • La Figure 6 montre les courbes de Wöhler obtenues avec les essais 3, 7 et 8 dans la direction L-T (Figure 6a) et T-L (figure 6b).The Figure 6 shows the Wöhler curves obtained with tests 3, 7 and 8 in the LT direction ( Figure 6a ) and TL ( figure 6b ).
Description de l'inventionDescription of the invention

Sauf mention contraire, toutes les indications concernant la composition chimique des alliages sont exprimées comme un pourcentage en poids basé sur le poids total de l'alliage. L'expression 1,4 Cu signifie que la teneur en cuivre exprimée en % en poids est multipliée par 1,4. La désignation des alliages se fait en conformité avec les règlements de The Aluminium Association, connus de l'homme du métier. Sauf mention contraire les définitions des états métallurgiques indiquées dans la norme européenne EN 515 s'appliquent.Unless stated otherwise, all the information concerning the chemical composition of the alloys is expressed as a percentage by weight based on the total weight of the alloy. The expression 1.4 Cu means that the copper content expressed in% by weight is multiplied by 1.4. The designation of alloys is in accordance with the regulations of The Aluminum Association, known to those skilled in the art. Unless otherwise stated, the definitions of the metallurgical states given in the European standard EN 515 apply.

Les caractéristiques mécaniques statiques en traction, en d'autres termes la résistance à la rupture Rm, la limite d'élasticité conventionnelle à 0,2% d'allongement Rp0,2, et l'allongement à la rupture A%, sont déterminés par un essai de traction selon la norme NF EN ISO 6892-1, le prélèvement et le sens de l'essai étant définis par la norme EN 485-1. Les propriétés en fatigue sur éprouvettes lisses sont mesurées à l'air ambiant à une contrainte d'amplitude maximale de 242 MPa, une fréquence de 50 Hz, un rapport de contrainte R = 0,1, sur des éprouvettes telles que représentées sur la Figure la, prélevées à mi-largeur et à mi-épaisseur des tôles dans la direction TL. Les conditions de test obéissent à la norme ASTM E466. On détermine la moyenne logarithmique des résultats obtenus sur au moins 4 éprouvettes.The static mechanical characteristics in tension, in other words the tensile strength R m , the conventional yield stress at 0.2% elongation R p0.2 , and the elongation at break A% are determined by a tensile test according to standard NF EN ISO 6892-1, the sampling and the direction of the test being defined by the EN 485-1 standard. The fatigue properties on smooth specimens are measured in ambient air at a maximum amplitude stress of 242 MPa, a frequency of 50 Hz, a stress ratio R = 0.1, on specimens as shown in FIG. la, taken at mid-width and at mid-thickness of the sheets in the direction TL. The test conditions follow the ASTM E466 standard. The logarithmic average of the results obtained on at least 4 test pieces is determined.

Les propriétés en fatigue sur éprouvettes à trou sont mesurées à l'air ambiant pour des niveaux de contrainte variables, à une fréquence de 50 Hz, un rapport de contrainte R = 0,1, sur des éprouvettes telles que représentées sur la Figure 1b, Kt = 2,3, prélevées au centre et à mi-épaisseur des tôles dans la direction L-T et T-L. L'équation de Walker a été utilisée pour déterminer une valeur de contrainte maximale représentative de 50 % de non rupture à 100 000 cycles. Pour ce faire un indice de qualité fatigue (IQF) est calculé pour chaque point de la courbe de Wöhler avec la formule IQF = σ max N 0 N 1 / n

Figure imgb0001
où σmax est la contrainte maximale appliquée à un échantillon donné, N est le nombre de cycles jusqu'à la rupture, No est égale à 100 000 et n = -4,5. On rapporte l'IQF correspondant à la médiane, soit 50% rupture pour 100 000 cycles.The fatigue properties on hole specimens are measured in the ambient air for variable stress levels, at a frequency of 50 Hz, a stress ratio R = 0.1, on specimens as shown in FIG. Figure 1b , Kt = 2,3, taken at the center and at mid-thickness of the sheets in the direction LT and TL. The Walker equation was used to determine a representative maximum stress value of 50% non-break at 100,000 cycles. To do this a fatigue quality index (IQF) is calculated for each point of the Wöhler curve with the formula IQF = σ max NOT 0 NOT 1 / not
Figure imgb0001
 where σ max is the maximum stress applied to a given sample, N is the number of cycles to failure, No is equal to 100,000 and n = -4.5. The IQF corresponding to the median is reported, ie 50% rupture per 100,000 cycles.

Dans le cadre de l'invention, un produit corroyé épais est un produit dont l'épaisseur est au moins 6 mm. De préférence l'épaisseur des produits selon l'invention est au moins 80 mm et de manière préférée au moins 100 mm. Dans un mode de réalisation de l'invention l'épaisseur des produits corroyés est au moins 120 mm ou de préférence 140 mm. L'épaisseur des produits épais selon l'invention est typiquement au plus de 240 mm, généralement au plus de 220 mm et préférentiellement au plus de 180 mm.In the context of the invention, a thick wrought product is a product whose thickness is at least 6 mm. Preferably the thickness of the products according to the invention is at least 80 mm and preferably at least 100 mm. In one embodiment of the invention the thickness of the wrought products is at least 120 mm or preferably 140 mm. The thickness of the thick products according to the invention is typically at most 240 mm, generally at most 220 mm and preferably at most 180 mm.

Sauf mention contraire, les définitions de la norme EN 12258 s'appliquent. Notamment, une tôle est selon l'invention un produit laminé de section transversale rectangulaire dont l'épaisseur uniforme est au moins de 6 mm et n'excède pas 1/10ème de la largeur.
On appelle ici « élément de structure » ou « élément structural » d'une construction mécanique une pièce mécanique pour laquelle les propriétés mécaniques statiques et/ou dynamiques sont particulièrement importantes pour la performance de la structure, et pour laquelle un calcul de structure est habituellement prescrit ou réalisé. Il s'agit typiquement d'éléments dont la défaillance est susceptible de mettre en danger la sécurité de ladite construction, de ses utilisateurs, de ses usagers ou d'autrui. Pour un avion, ces éléments de structure comprennent notamment les éléments qui composent le fuselage (tels que la peau de fuselage (fuselage skin en anglais), les raidisseurs ou lisses de fuselage (stringers), les cloisons étanches (bulkheads), les cadres de fuselage (circumferential frames), les ailes (tels que la peau de voilure (wing skin), les raidisseurs (stringers ou stiffeners), les nervures (ribs) et longerons (spars)) et l'empennage composé notamment de stabilisateurs horizontaux et verticaux (horizontal or vertical stabilisers), ainsi que les profilés de plancher (floor beams), les rails de sièges (seat tracks) et les portes.
On appelle ici « ensemble de l'installation de coulée » l'ensemble des dispositifs permettant de transformer un métal sous forme quelconque en demi-produit de forme brute en passant par la phase liquide. Une installation de coulée peut comprendre de nombreux dispositifs tels que un ou plusieurs fours nécessaires à la fusion du métal (« four de fusion ») et/ou à son maintien (« four de maintien ») en température et/ou à des opérations de préparation du métal liquide et d'ajustement de la composition (« four d'élaboration »), une ou plusieurs cuves (ou « poches ») destinées à effectuer un traitement d'élimination des impuretés dissoutes et/ou en suspension dans le métal liquide, ce traitement pouvant consister à filtrer le métal liquide sur un média filtrant dans une « poche de filtration » ou à introduire dans le bain un gaz dit « de traitement » pouvant être inerte ou réactif dans une « poche de dégazage », un dispositif de solidification du métal liquide (ou « métier de coulée »), par coulée semi-continue verticale par refroidissement direct dans un puits de coulée, pouvant comprendre des dispositifs tels que un moule (ou « lingotière ») un dispositif d'approvisionnement du métal liquide (ou «busette ») et un système de refroidissement, ces différents fours, cuves et dispositifs de solidification étant reliés entre eux par des dispositifs de transfert ou chenaux appelés « goulottes » dans lesquels le métal liquide peut être transporté.Unless otherwise specified, the definitions of EN 12258 apply. In particular, a sheet is according to the invention a laminated product of rectangular cross section whose uniform thickness is at least 6 mm and does not exceed 1 / 10th of the width.
Here, a "structural element" or "structural element" of a mechanical construction is called a mechanical part for which the static and / or dynamic mechanical properties are particularly important for the performance of the structure, and for which a structural calculation is usually prescribed or realized. These are typically elements whose failure is likely to endanger the safety of said construction, its users, its users or others. For an aircraft, these structural elements include in particular the elements that make up the fuselage (such as the fuselage skin (fuselage skin), the stiffeners or stringers, the bulkheads (bulkheads), circumferential frames, wings (such as wing skin), stiffeners (stiffeners), ribs and spars) and tail fin consisting in particular of horizontal and vertical stabilizers (horizontal or vertical stabilizers), as well as the floor beams, the seat tracks and the doors.
The term "set of the casting plant" is here referred to as the set of devices making it possible to transform a metal in any form into a semi-product of raw form via the liquid phase. A casting plant may include a number of devices such as one or more ovens required for melting the metal ("melting furnace") and / or maintaining it ("holding furnace") in temperature and / or preparation of the liquid metal and adjustment of the composition ("preparation furnace"), one or more tanks (or "pockets") intended to carry out a treatment for the removal of impurities dissolved and / or suspended in the liquid metal this treatment may consist of filtering the liquid metal on a filter medium in a "filtration bag" or introducing into the bath a so-called "treatment" gas that can be inert or reactive in a "degassing bag", a device for solidification of the liquid metal (or "casting loom") by vertical semi-continuous casting by direct cooling in a casting well, which may comprise devices such as a mold (or "mold") a liquid metal supply device (or "nozzle") and a cooling system, these different furnaces, tanks and solidification devices being interconnected by transfer devices or channels called "chutes" in which the liquid metal can to be transported.

Les présents inventeurs ont constaté que de manière surprenante on peut obtenir des produits corroyés épais en alliage aluminium cuivre lithium présentant une performance en fatigue améliorée en préparant ces tôles à l'aide du procédé suivant.
Dans une première étape on élabore un bain de métal liquide en alliage comprenant, en % en poids Cu: 2,0 - 6,0; Li : 0,5 - 2,0 ; Mg : 0- 1,0 ; Ag: 0 - 0,7 ; Zn 0 - 1,0 ; et au moins un élément choisi parmi Zr, Mn, Cr, Sc, Hf et Ti, la quantité dudit élément, s'il est choisi, étant de 0,05 à 0,20 % en poids pour Zr, 0,05 à 0,8 % en poids pour Mn, 0,05 à 0,3 % en poids pour Cr et pour Sc, 0,05 à 0,5 % en poids pour Hf et de 0,01 à 0,15 % en poids pour Ti, Si ≤ 0,1 ; Fe ≤ 0,1; autres ≤ 0,05 chacun et ≤ 0,15 au total, reste aluminium.
Un alliage avantageux pour le procédé selon l'invention comprend, en % en poids, Cu : 3,0 - 3,9 ; Li : 0,7 - 1,3 ; Mg : 0,1 - 1,0, au moins un élément choisi parmi Zr, Mn et Ti, la quantité dudit élément, s'il est choisi, étant de 0,06 à 0,15 % en poids pour Zr, 0,05 à 0,8 % en poids pour Mn et de 0,01 à 0,15 % en poids pour Ti; Ag: 0 - 0,7 ; Zn ≤ 0,25 ; Si ≤ 0,08 ; Fe ≤ 0,10 ; autres ≤ 0,05 chacun et ≤ 0,15 au total, reste aluminium.
Avantageusement la teneur en cuivre est au moins de 3,2 % en poids. La teneur en lithium est de préférence comprise entre 0,85 et 1,15 % en poids et de préférence entre 0,90 et 1,10 % en poids. La teneur en magnésium est de préférence comprise entre 0,20 et 0,6 % en poids. L'addition simultanée de manganèse et de zirconium est généralement avantageuse. De façon préférée la teneur en manganèse est comprise entre 0,20 et 0,50 % en poids et la teneur en zirconium est comprise entre 0,06 et 0,14 % en poids. Avantageusement la teneur en argent est comprise entre 0,20 et 0,7 % en poids. Il est avantageux que la teneur en argent soit au moins 0,1 % en poids. Dans un mode de réalisation de l'invention la teneur en argent est au moins 0,20 % en poids. Préférentiellement la teneur en argent est au plus 0,5 % en poids. Dans un mode de réalisation de l'invention la teneur en argent est limitée à 0,3 % en poids. Préférentiellement la teneur en silicium est au plus de 0,05 % en poids et la teneur en fer est au plus de 0,06 % en poids. Avantageusement la teneur en titane est comprise entre 0,01 et 0,08 % en poids. Dans un mode de réalisation de l'invention la teneur en zinc est au plus de 0,15 % en poids.
Un alliage aluminium-cuivre-lithium préféré est l'alliage AA2050.
Ce bain de métal liquide est préparé dans un four de l'installation de coulée. Il est connu, par exemple de US 5,415,220 d'utiliser des sels fondus contenant du lithium tels que des mélanges KCl/LiCl dans le four de fusion pour passiver l'alliage lors de son transfert vers l'installation de coulée. Les présents inventeurs ont cependant obtenu d'excellentes propriétés de fatigue pour des tôles épaisses sans utiliser de sel fondu contenant du lithium dans le four de fusion, mais en maintenant dans ce four une atmosphère pauvre en oxygène et pensent que la présence de sel dans le four de fusion pourrait avoir dans certains cas un effet néfaste sur les propriétés en fatigue des produits corroyés épais. Avantageusement, on n'utilise pas de sel fondu contenant du lithium dans l'ensemble de l'installation de coulée. Dans un mode de réalisation avantageux on n'utilise pas de sel fondu dans l'ensemble de l'installation de coulée. Préférentiellement on maintient dans le ou les fours de l'installation de coulée une teneur en oxygène inférieure à 0,5 % en volume et de préférence inférieure à 0,3 % en volume. Cependant on peut tolérer une teneur en oxygène d'au moins 0,05 % en volume et même d'au moins 0,1 % en volume dans le ou les fours de l'installation de coulée, ce qui est avantageux notamment pour les aspects économiques du procédé. Avantageusement le ou les fours de l'installation de coulée sont des fours à induction. Les présents inventeurs ont constaté que ce type de four est avantageux malgré le brassage généré par le chauffage par induction.
Ce bain de métal liquide est ensuite traité avec dans une poche de dégazage et dans une poche de filtration de façon notamment à ce que sa teneur en hydrogène soit inférieure à 0,4 ml/100g et de préférence inférieure à 0,35 ml/100g. La teneur en hydrogène du métal liquide est mesurée à l'aide d'un appareillage commercial tel que l'appareil commercialisé sous la marque ALSCAN™, connu de l'homme du métier, la sonde étant maintenue sous un balayage d'azote. Avantageusement la teneur en oxygène de l'atmosphère en contact avec le bain de métal liquide dans le four de fusion lors des étapes de dégazage, filtration est inférieure à 0,5 % en volume et de préférence inférieure à 0,3 % en volume. De préférence, la teneur en oxygène de l'atmosphère en contact avec le bain de métal liquide est inférieure est inférieure à 0,5 % en volume et de préférence inférieure à 0,3 % en volume pour l'ensemble de l'installation de coulée. Cependant on peut tolérer une teneur en oxygène d'au moins 0,05 % en volume et même d'au moins 0,1 % en volume pour l'ensemble de l'installation de coulée ce qui est avantageux notamment pour les aspects économiques du procédé.The present inventors have found that, surprisingly, thick wrought products of copper lithium aluminum alloy with improved fatigue performance can be obtained by preparing these sheets by the following method.
In a first step, an alloy liquid metal bath comprising, in% by weight Cu: 2.0 - 6.0; Li: 0.5 - 2.0; Mg: 0-1.0; Ag: 0 - 0.7; Zn 0 - 1.0; and at least one member selected from Zr, Mn, Cr, Sc, Hf and Ti, the amount of said element, if selected, being from 0.05 to 0.20% by weight for Zr, 0.05 to 0 , 8% by weight for Mn, 0.05 to 0.3% by weight weight for Cr and Sc, 0.05 to 0.5% by weight for Hf and 0.01 to 0.15% by weight for Ti, Si ≤ 0.1; Fe ≤ 0.1; other ≤ 0.05 each and ≤ 0.15 in total, remains aluminum.
An advantageous alloy for the process according to the invention comprises, in% by weight, Cu: 3.0 - 3.9; Li: 0.7 - 1.3; Mg: 0.1 - 1.0, at least one element selected from Zr, Mn and Ti, the amount of said element, if selected, being from 0.06 to 0.15% by weight for Zr, 0, From 0.5 to 0.8% by weight for Mn and from 0.01 to 0.15% by weight for Ti; Ag: 0 - 0.7; Zn ≤ 0.25; If ≤ 0.08; Fe ≤ 0.10; other ≤ 0.05 each and ≤ 0.15 in total, remains aluminum.
Advantageously, the copper content is at least 3.2% by weight. The lithium content is preferably between 0.85 and 1.15% by weight and preferably between 0.90 and 1.10% by weight. The magnesium content is preferably between 0.20 and 0.6% by weight. The simultaneous addition of manganese and zirconium is generally advantageous. Preferably, the manganese content is between 0.20 and 0.50% by weight and the zirconium content is between 0.06 and 0.14% by weight. Advantageously, the silver content is between 0.20 and 0.7% by weight. It is advantageous that the silver content is at least 0.1% by weight. In one embodiment of the invention the silver content is at least 0.20% by weight. Preferably, the silver content is at most 0.5% by weight. In one embodiment of the invention, the silver content is limited to 0.3% by weight. Preferably, the silicon content is at most 0.05% by weight and the iron content is at most 0.06% by weight. Advantageously, the titanium content is between 0.01 and 0.08% by weight. In one embodiment of the invention, the zinc content is at most 0.15% by weight.
A preferred aluminum-copper-lithium alloy is AA2050 alloy.
This liquid metal bath is prepared in a furnace of the casting plant. It is known, for example from US 5,415,220 using lithium-containing molten salts such as KCl / LiCl mixtures in the melting furnace to passivate the alloy as it is transferred to the casting plant. The present inventors, however, have obtained excellent fatigue properties for thick plates without using molten salt containing lithium in the melting furnace, but maintaining in this furnace a low oxygen atmosphere and believe that the presence of salt in the furnace Melting furnace could have in some cases a detrimental effect on the fatigue properties of thick wrought products. Advantageously, molten salt containing lithium is not used throughout the casting installation. In an advantageous embodiment, no molten salt is used throughout the casting installation. Preferably, in the furnace or furnaces of the casting installation, an oxygen content of less than 0.5% by volume and preferably less than 0.3% by volume is maintained. However, it is possible to tolerate an oxygen content of at least 0.05% by volume and even at least 0.1% by volume in the furnace (s) of the casting plant, which is advantageous in particular for the aspects process economics. Advantageously, the furnace or furnaces of the casting installation are induction furnaces. The present inventors have found that this type of oven is advantageous despite the stirring generated by the induction heating.
This bath of liquid metal is then treated with a degassing bag and in a filtration bag so that its hydrogen content is less than 0.4 ml / 100g and preferably less than 0.35 ml / 100g . The hydrogen content of the liquid metal is measured using a commercial apparatus such as the apparatus marketed under the tradename ALSCAN ™, known to those skilled in the art, the probe being maintained under a nitrogen sweep. Advantageously, the oxygen content of the atmosphere in contact with the liquid metal bath in the melting furnace during the degassing steps, filtration is less than 0.5% by volume and preferably less than 0.3% by volume. Preferably, the oxygen content of the atmosphere in contact with the liquid metal bath is less than 0.5% by volume and preferably less than 0.3% by volume for the whole of the installation of casting. However, it is possible to tolerate an oxygen content of at least 0.05% by volume and even at least 0.1% by volume for the entire casting plant, which is advantageous especially for the economic aspects of the casting. process.

Le bain de métal liquide est ensuite solidifié sous forme de plaque. Une plaque est un bloc d'aluminium de forme substantiellement parallélépipédique, de longueur L, de largeur W et d'épaisseur T. On contrôle l'atmosphère au-dessus de la surface liquide lors de la solidification. Un exemple de dispositif permettant de contrôler l'atmosphère au-dessus de la surface liquide lors de la solidification est présenté sur la Figure 2.
Dans cet exemple de dispositif approprié, le métal liquide provenant d'une goulotte (63) est introduit dans une busette (4) contrôlée par une quenouille (8) pouvant se déplacer vers le haut et vers le bas (81), dans une lingotière (31) placée sur un faux fond (21). L'alliage d'aluminium est solidifié par refroidissement direct (5). L'alliage d'aluminium (1) a au moins une surface solide (11, 12, 13) et au moins une surface liquide (14, 15). Un ascenseur (2) permet de maintenir le niveau de la surface liquide (14, 15) sensiblement constant. Un distributeur (7) permet la répartition du métal liquide. Un couvercle (62) recouvre la surface liquide. Le couvercle peut comprendre des joints (61) pour assurer une étanchéité avec la table de coulée (32). Le métal liquide dans la goulotte (63) peut être avantageusement protégé par un couvercle (64). Un gaz inerte (9) est introduit dans la chambre (65) définie entre le couvercle et la table de coulée. Le gaz inerte est avantageusement choisi parmi les gaz rares, l'azote et le dioxyde de carbone ou des mélanges de ces gaz. Un gaz inerte préféré est l'argon. La teneur en oxygène est mesurée dans la chambre (65) au-dessus de la surface liquide. Le débit de gaz inerte peut être ajusté pour atteindre la teneur en oxygène désirée. Cependant il est avantageux de maintenir une aspiration suffisante dans le puits de coulée (10) grâce à une pompe (101). En effet les présents inventeurs ont constaté qu'il n'existe pas en général une étanchéité suffisante entre la lingotière (31) et le métal solidifié (5) ce qui conduit à une diffusion de l'atmosphère du puits de coulée (10) vers la chambre (65). Avantageusement l'aspiration de la pompe (101) est telle que la pression dans l'enceinte (10) soit inférieure à la pression dans la chambre (65), ce qui est peut être obtenu de préférence en imposant une vitesse de l'atmosphère au travers des surfaces ouvertes du puits de coulée d'au moins de 2 m/s et de préférence d'au moins de 2,5 m/s. Typiquement la pression dans la chambre (65) est proche de la pression atmosphérique et la pression dans l'enceinte (10) est inférieure à la pression atmosphérique, typiquement 0,95 fois la pression atmosphérique. Dans le cadre du procédé selon l'invention, on maintient dans la chambre (65), grâce aux dispositifs décrits, une teneur en oxygène inférieure à 0,5 % en volume et de préférence inférieure à 0,3 % en volume.
Un exemple de distributeur (7) du procédé selon l'invention est présenté sur les figures 3 et 4. Le distributeur selon l'invention est réalisé en tissu comprenant essentiellement du carbone, il comprend une face inférieure (76), une face supérieure typiquement vide définissant l'orifice par lequel le métal liquide est introduit (71) et paroi de section substantiellement rectangulaire typiquement substantiellement constante et de hauteur h typiquement substantiellement constante, la paroi comprenant deux parties longitudinales parallèles à la largeur W de la plaque (720, 721) et deux parties transversales parallèles à l'épaisseur T de la plaque (730, 731) lesdites parties transversales et longitudinales étant formées d'au moins deux tissus, un premier tissu sensiblement obturant et semi-rigide (77) assurant le maintien de la forme du distributeur pendant la coulée et un second tissu non obturant (78) permettant le passage et la filtration du liquide, lesdits premier et deuxième tissu étant liés l'un à l'autre sans recouvrement ou avec recouvrement et sans interstice les séparant, ledit premier tissu couvrant de façon continue au moins 30 % de la surface desdites parties de paroi (720,721, 730, 731) et étant positionné de manière à ce que la surface liquide soit en contact avec lui sur l'ensemble de la section du distributeur. Les premier et deuxième tissus étant cousus l'un à l'autre sans recouvrement ou avec recouvrement et sans interstice les séparant, c'est-à-dire en contact, le métal liquide ne peut pas traverser le premier tissu et être dévié par le second tissu comme c'est le cas par exemple dans un combo-bag tel que décrit dans la demande WO 99/44719 Fig 2 à 5. Grâce au maintien assuré par le premier tissu, le distributeur est semi-rigide et ne se déforme pas sensiblement lors de la coulée. Dans une réalisation avantageuse le premier tissu a une hauteur, hl, mesurée à partir de la face supérieure sur la circonférence de la paroi (720, 721, 730, 731) telle que h1 ≥ 0,3 h et de préférence h1 ≥ 0,5 h, où h désigne la hauteur totale de la paroi du distributeur.The liquid metal bath is then solidified in the form of a plate. A plate is an aluminum block of substantially parallelepiped shape, length L, width W and thickness T. The atmosphere is controlled above the liquid surface during solidification. An example of a device for controlling the atmosphere above the liquid surface during solidification is presented on the Figure 2 .
In this example of suitable device, the liquid metal coming from a chute (63) is introduced into a nozzle (4) controlled by a stopper (8) which can move towards the up and down (81) in an ingot mold (31) placed on a false bottom (21). The aluminum alloy is solidified by direct cooling (5). The aluminum alloy (1) has at least one solid surface (11, 12, 13) and at least one liquid surface (14, 15). An elevator (2) maintains the level of the liquid surface (14, 15) substantially constant. A distributor (7) allows the distribution of the liquid metal. A cover (62) covers the liquid surface. The cover may include seals (61) for sealing with the casting table (32). The liquid metal in the trough (63) can be advantageously protected by a cover (64). An inert gas (9) is introduced into the chamber (65) defined between the cover and the pouring table. The inert gas is advantageously chosen from rare gases, nitrogen and carbon dioxide or mixtures of these gases. A preferred inert gas is argon. The oxygen content is measured in the chamber (65) above the liquid surface. The flow of inert gas can be adjusted to achieve the desired oxygen content. However, it is advantageous to maintain sufficient suction in the casting well (10) by means of a pump (101). Indeed the present inventors have found that there is generally no sufficient seal between the mold (31) and the solidified metal (5) which leads to a diffusion of the atmosphere of the casting well (10) to the room (65). Advantageously, the suction of the pump (101) is such that the pressure in the enclosure (10) is lower than the pressure in the chamber (65), which can preferably be obtained by imposing a speed of the atmosphere through the open surfaces of the casting well of at least 2 m / s and preferably at least 2.5 m / s. Typically the pressure in the chamber (65) is close to atmospheric pressure and the pressure in the chamber (10) is lower than atmospheric pressure, typically 0.95 times the atmospheric pressure. In the context of the process according to the invention, the chamber (65) is maintained, thanks to the devices described, with an oxygen content of less than 0.5% by volume and preferably less than 0.3% by volume.
An example of a dispenser (7) of the process according to the invention is presented on the figures 3 and 4 . The dispenser according to the invention is made of fabric comprising essentially carbon, it comprises a lower face (76), a typically empty upper face defining the orifice through which the liquid metal is introduced (71) and wall of substantially rectangular section typically substantially constant and of height h typically substantially constant, the wall comprising two longitudinal parts parallel to the width W of the plate (720, 721) and two transverse portions parallel to the thickness T of the plate (730, 731), said transverse and longitudinal portions being formed of at least two tissues, a first substantially obturating tissue and semi-rigid (77) maintaining the shape of the dispenser during casting and a second non-sealing fabric (78) for passage and filtration of the liquid, said first and second fabric being bonded to each other without overlapping or overlapping and without interstices separating them, said first fabric continuously covering at least 30% of the area of said wall portions (720,721,730,731) and being positioned so that the liquid surface is in contact with him on the entire section of the dispenser. The first and second fabrics being sewn together without overlapping or overlapping and without interstices separating them, i.e., in contact, the liquid metal can not pass through the first fabric and be deflected by the second fabric as is the case for example in a combo-bag as described in the application WO 99/44719 Fig 2 to 5 . Thanks to the maintenance provided by the first fabric, the dispenser is semi-rigid and does not deform substantially during casting. In an advantageous embodiment, the first fabric has a height, hl, measured from the upper face on the circumference of the wall (720, 721, 730, 731) such that h1 ≥ 0.3 h and preferably h1 ≥ 0, 5 h, where h denotes the total height of the distributor wall.

La surface liquide étant en contact avec ledit premier tissu obturant le métal liquide ne traverse le distributeur que sous la surface liquide dans certaines directions de chaque partie de la paroi. De préférence la hauteur immergée dans le métal liquide de paroi (720, 721, 730, 731) du distributeur (7) couverte par le premier tissu est au moins égale à 20 %, préférentiellement 40 % et de manière préférée 60 % de la hauteur totale de paroi immergée.
La figure 4 représente le fond et les parties de paroi longitudinales. Le fond (76) est typiquement couvert par le premier et/ou le second tissu. Avantageusement le premier tissu est au moins situé dans la partie centrale du fond (76) sur une longueur L1 et/ou dans la partie centrale des parties longitudinales (720) et (721) sur l'ensemble de la hauteur h et sur une longueur L2.The liquid surface being in contact with said first liquid-sealing fabric passes through the dispenser only under the liquid surface in certain directions of each part of the wall. Preferably the height immersed in the liquid wall metal (720, 721, 730, 731) of the distributor (7) covered by the first fabric is at least 20%, preferably 40% and preferably 60% of the height. total submerged wall.
The figure 4 represents the bottom and the longitudinal wall portions. The bottom (76) is typically covered by the first and / or second fabric. Advantageously, the first fabric is at least located in the central part of the bottom (76) along a length L1 and / or in the central part of the longitudinal parts (720) and (721) over the entire height h and over a length L2.

Avantageusement, la portion de surface couverte par le premier tissu est comprise entre 30 et 90 % et de préférence entre 50 et 80 % pour les parties longitudinales (720) et (721), et/ou entre 30 et 70 % et de préférence entre 40 et 60 % pour les parties latérales (730, 731) et/ou entre 30 et 100 % et de préférence entre 50 et 80 % pour le fond (76).
Il est avantageux que la longueur L1 de premier tissu situé dans le fond (76) soit supérieure à la longueur L2 de premier tissu situé dans la partie des parois longitudinales (720) et (721) en contact avec le fond.
Les présents inventeurs pensent que la géométrie du distributeur permet notamment d'améliorer la qualité du flux du métal liquide, de réduire les turbulences et d'améliorer la distribution de température.
Le premier tissu et le deuxième tissu sont avantageusement obtenus par tissage d'un fil comprenant essentiellement du carbone. Le tissage de fil graphite est particulièrement avantageux. Les tissus sont typiquement cousus l'un à l'autre. Il est possible également en lieu et place d'un premier et deuxième tissus d'utiliser un tissu diffuseur unique présentant au moins deux zones de tissage, plus ou moins denses.
Il est avantageux pour la facilité du tissage que le fil comprenant du carbone soit revêtu d'une couche facilitant le glissement. Cette couche peut par exemple comprendre un polymère fluoré tel que le Teflon ou une polyamide telle que le xylon.
Le premier tissu est sensiblement obturant. Typiquement il s'agit d'un tissu présentant des mailles de dimension inférieure à 0,5 mm, de préférence inférieure à 0,2 mm. Le second tissu est non obturant et permet le passage du métal en fusion. Typiquement, il s'agit d'un tissu présentant des mailles de dimension comprise entre 1 et 5 mm, de préférence de 2 à 4 mm. Dans un mode de réalisation de l'invention le premier tissu recouvre localement le second tissu, tout en étant en contact intime de façon à ne pas laisser d'interstice entre les deux tissus.Advantageously, the surface portion covered by the first fabric is between 30 and 90% and preferably between 50 and 80% for the longitudinal portions (720) and (721), and / or between 30 and 70% and preferably between 40 and 60% for the side parts (730, 731) and / or between 30 and 100% and preferably between 50 and 80% for the bottom (76).
It is advantageous that the length L1 of the first tissue located in the bottom (76) is greater than the length L2 of the first tissue located in the portion of the longitudinal walls (720) and (721) in contact with the bottom.
The present inventors believe that the geometry of the dispenser makes it possible in particular to improve the quality of the flow of the liquid metal, to reduce turbulence and to improve the temperature distribution.
The first fabric and the second fabric are advantageously obtained by weaving a yarn essentially comprising carbon. The weaving of graphite yarn is particularly advantageous. The tissues are typically sewn to each other. It is also possible instead of first and second fabrics to use a single diffuser fabric having at least two weaving areas, more or less dense.
It is advantageous for the ease of weaving that the wire comprising carbon is coated with a layer facilitating sliding. This layer may for example comprise a fluorinated polymer such as Teflon or a polyamide such as xylon.
The first fabric is substantially obturant. Typically it is a fabric having mesh size of less than 0.5 mm, preferably less than 0.2 mm. The second fabric is non-sealing and allows the passage of the molten metal. Typically, it is a fabric having mesh sizes of between 1 and 5 mm, preferably 2 to 4 mm. In one embodiment of the invention the first tissue locally covers the second tissue, while being in intimate contact so as not to leave a gap between the two tissues.

Avantageusement la plaque ainsi obtenue est ensuite transformée pour obtenir un produit corroyé.
La plaque ainsi obtenue est ensuite homogénéisée avant ou après avoir optionnellement été usinée pour obtenir une forme pouvant être déformée à chaud. Dans un mode de réalisation, la plaque est usinée sous forme de plaque de laminage de façon à ensuite être déformée à chaud par laminage. Dans un autre mode de réalisation, la plaque est usinée sous forme de d'ébauche de forge de façon à ensuite être déformée à chaud par forgeage. Dans encore une autre mode de réalisation la plaque est usinée sous forme de billettes de façon à ensuite être déformée à chaud par extrusion. De préférence l'homogénéisation est réalisée à une température comprise entre 470 et 540°C pendant une durée comprise entre 2 et 30 heures.Advantageously, the plate thus obtained is then transformed to obtain a wrought product.
The plate thus obtained is then homogenized before or after having been optionally machined to obtain a shape that can be deformed while hot. In one embodiment, the plate is machined in the form of a rolling plate so as to then be deformed to hot by rolling. In another embodiment, the plate is machined as a forging blank so as to be hot deformed by forging. In yet another embodiment the plate is billet machined so as to be extrusion hot deformed. Preferably the homogenization is carried out at a temperature between 470 and 540 ° C for a period of between 2 and 30 hours.

On déforme à chaud et optionnellement à froid ladite forme ainsi homogénéisée pour obtenir un produit corroyé. La température de déformation à chaud est avantageusement au moins 350°C et de préférence au moins 400 °C. Le taux de déformation à chaud et optionnellement à froid, c'est-à-dire le rapport entre d'une part la différence entre l'épaisseur initiale, avant déformation mais après l'éventuel usinage, et l'épaisseur finale et d'autre part l'épaisseur initiale est inférieur à 85% et de préférence inférieur à 80 %. Dans un mode de réalisation lequel le taux de déformation lors de la déformation est inférieur à 75% et de préférence inférieur à 70 %.
Le produit corroyé ainsi obtenu est ensuite mis en solution et trempé. La température de mise en solution est avantageusement comprise entre 470 et 540°C et de préférence entre 490 et 530 °C et la durée est adaptée à l'épaisseur du produit.
Optionnellement on détensionne ledit produit corroyé ainsi mis en solution par déformation plastique avec une déformation d'au moins 1%. Dans le cas des produits laminés il est avantageux de détensionner par traction contrôlée ledit produit corroyé ainsi mis en solution avec un allongement permanent d'au moins 1% et de préférence compris entre 2 et 5%.
Enfin on fait subir un revenu au produit ainsi mis en solution et optionnellement détensionné. Le revenu est effectué en un ou plusieurs paliers à une température avantageusement comprise entre 130 et 160 °C pendant une durée de 5 à 60 heures. De préférence on obtient à l'issue du revenu un état métallurgique T8, tel que notamment T851, T83, T84, ou T85.
Les produits corroyés obtenus par le procédé selon l'invention présentent des propriétés avantageuses.
La moyenne logarithmique de fatigue des produits corroyés dont l'épaisseur est au moins 80 mm, obtenus par le procédé selon l'invention, mesurée à mi-épaisseur dans la directionThe shape thus homogenized is deformed hot and optionally cold so as to obtain a wrought product. The heat-forming temperature is advantageously at least 350 ° C and preferably at least 400 ° C. The rate of deformation hot and optionally cold, that is to say the ratio between the difference between the initial thickness, before deformation but after the possible machining, and the final thickness and on the other hand, the initial thickness is less than 85% and preferably less than 80%. In one embodiment, the deformation rate during the deformation is less than 75% and preferably less than 70%.
The wrought product thus obtained is then dissolved and quenched. The dissolution temperature is advantageously between 470 and 540 ° C and preferably between 490 and 530 ° C and the duration is adapted to the thickness of the product.
Optionally, the wrought product thus solubilized is de-tensioned by plastic deformation with a deformation of at least 1%. In the case of rolled products, it is advantageous to detension by controlled traction said wrought product thus put into solution with a permanent elongation of at least 1% and preferably between 2 and 5%.
Finally, we make an income to the product thus put in solution and optionally relieved. The income is made in one or more steps at a temperature advantageously between 130 and 160 ° C for a period of 5 to 60 hours. Preferably one obtains at the end of the income a metallurgical state T8, such as in particular T851, T83, T84, or T85.
The wrought products obtained by the process according to the invention have advantageous properties.
The logarithmic fatigue mean of the wrought products whose thickness is at least 80 mm, obtained by the method according to the invention, measured at mid-thickness in the direction

TL sur éprouvettes lisses selon la Figure la à une contrainte d'amplitude maximale de 242 MPa, une fréquence de 50 Hz, un rapport de contrainte R = 0,1 est au moins 250 000 cycles, avantageusement la propriété en fatigue est obtenue pour les produits corroyés obtenus par le procédé selon l'invention dont l'épaisseur est au moins 100 mm ou de préférence au moins 120 mm ou même au moins 140 mm.
Les produits corroyés selon l'invention d'épaisseur au moins 80 mm présentent également des propriétés en fatigue avantageuse pour des éprouvettes à trou, ainsi l'indice de qualité fatigue IQF obtenu sur des éprouvettes à trou Kt = 2,3 selon la Figure 1b à une fréquence de 50 Hz à l'air ambiant avec une valeur R = 0,1 est au moins 180 MPa et de préférence est au moins 190 MPa dans le sens T-L.
De plus les produits obtenus par le procédé selon l'invention ont des caractéristiques mécaniques statiques avantageuses. Ainsi pour les produits corroyés dont l'épaisseur est au moins 80 mm comprenant en % en poids, Cu : 3,0 - 3,9 ; Li : 0,7 - 1,3 ; Mg : 0,1 - 1,0, au moins un élément choisi parmi Zr, Mn et Ti, la quantité dudit élément, s'il est choisi, étant de 0,06 à 0,15 % en poids pour Zr, 0,05 à 0,8 % en poids pour Mn et de 0,01 à 0,15 % en poids pour Ti,; Ag : 0 - 0,7 ; Zn ≤ 0,25 ; Si ≤ 0,08 ; Fe ≤ 0,10 ; autres ≤ 0,05 chacun et ≤ 0,15 au total, reste aluminium, la limite d'élasticité mesurée à quart épaisseur dans le sens L est au moins 450 MPa et de préférence au moins 470 MPa et/ou la résistance à la rupture mesurée est au moins 480 MPa et de préférence au moins 500 MPa et/ou l'allongement est au moins 5% et de préférence au moins 6%.
Les produits corroyés obtenus par le procédé selon l'invention peuvent de manière avantageuse être utilisées pour réaliser des éléments de structure, de préférence des éléments de structure d'avion. Des éléments de structure d'avion préférés sont les longerons, nervures ou un cadres. L'invention est particulièrement avantageuse pour des pièces de forme complexe obtenues par usinage intégral, utilisées en particulier pour la fabrication d'ailes d'avion ainsi que pour n'importe quel autre usage pour lequel les propriétés des produits selon l'invention sont avantageuses.TL on smooth test pieces according to Figure la at a maximum amplitude stress of 242 MPa, a frequency of 50 Hz, a stress ratio R = 0.1 is at least 250 000 cycles, advantageously the fatigue property is obtained for wrought products obtained by the process according to the invention, the thickness of which is at least 100 mm or preferably at least 120 mm or even at least 140 mm.
The wrought products according to the invention having a thickness of at least 80 mm also have advantageous fatigue properties for hole-shaped specimens, thus the fatigue quality index IQF obtained on specimens with a hole Kt = 2.3 according to the Figure 1b at a frequency of 50 Hz to ambient air with a value R = 0.1 is at least 180 MPa and preferably is at least 190 MPa in the TL direction.
In addition, the products obtained by the process according to the invention have advantageous static mechanical characteristics. Thus for wrought products whose thickness is at least 80 mm comprising in% by weight, Cu: 3.0 - 3.9; Li: 0.7 - 1.3; Mg: 0.1 - 1.0, at least one element selected from Zr, Mn and Ti, the amount of said element, if selected, being from 0.06 to 0.15% by weight for Zr, 0, From 0.5 to 0.8% by weight for Mn and from 0.01 to 0.15% by weight for Ti; Ag: 0 - 0.7; Zn ≤ 0.25; If ≤ 0.08; Fe ≤ 0.10; other ≤ 0.05 each and ≤ 0.15 in total, remains aluminum, the yield strength measured at quarter thickness in the direction L is at least 450 MPa and preferably at least 470 MPa and / or the breaking strength measured is at least 480 MPa and preferably at least 500 MPa and / or the elongation is at least 5% and preferably at least 6%.
The wrought products obtained by the process according to the invention can advantageously be used to produce structural elements, preferably aircraft structural elements. Preferred aircraft structural elements are spars, ribs or frames. The invention is particularly advantageous for parts of complex shape obtained by integral machining, used in particular for the manufacture of aircraft wings and for any other use for which the properties of the products according to the invention are advantageous. .

ExempleExample

Dans cet exemple, on a préparé des tôles fortes en alliage AA2050. Des plaques en alliage AA2050 ont été coulées par coulée semi-continue verticale à refroidissement direct. L'alliage a été préparé dans un four de fusion. Pour les exemples 1 à 7 on a utilisé un mélange KCL/LiCl en surface du métal liquide dans le four de fusion. Pour les exemples 8 à 9 on n'a pas utilisé de sel dans le four de fusion. Pour les exemples 8 à 9 l'atmosphère en contact avec le métal liquide avec une teneur en oxygène inférieure à 0,3 % en volume pour l'ensemble de l'installation de coulée. L'installation de coulée comprenait un capot disposé au-dessus du puits de coulée permettant de limiter la teneur en oxygène. Pour les essais 8 et 9 on avait en plus utilisé une aspiration (101) telle que la pression dans l'enceinte (10) était inférieure à la pression dans la chambre (65) et telle que la vitesse de l'atmosphère au travers des surfaces ouvertes du puits de coulée était au moins de 2 m/s. La teneur en oxygène a été mesurée à l'aide d'un oxymètre lors de la coulée. Par ailleurs, la teneur en hydrogène dans l'aluminium liquide a été mesurée à l'aide d'une sonde de type Alscan™.sous balayage d'azote. Deux types de distributeurs de métal liquide ont été utilisés. Un premier distributeur de type « Combo Bag » tel que décrit par exemple dans les Figures 2 à 6 de la demande internationale WO 99/44719 , qui ne remet pas en cause l'invention, mais réalisé en tissu comprenant essentiellement du carbone, référencé ci-dessous « distributeur A » et un second distributeur tel que décrit figure 3 référencé ci-dessous « distributeur B » est réalisé en tissu de fil de graphite.
Les conditions de coulée des différents essais réalisés sont données dans le tableau 1. Table 1 - Conditions de coulée pour les différents essais Essai H2 [ml/100g] O2 mesuré au dessus du puits de coulée (% en volume) Distributeur 1 0,41 0,3 A 2 0,43 0,1 A 3 0,37 0,1 A 4 0,33 0,1 A 5 0,35 0,4 A 6 0,38 0,3 A 7 0,47 0,7 B 8 0,34 0,1 B 9 0,29 0,1 B In this example, AA2050 alloy plates were prepared. AA2050 alloy plates were cast by direct cooling vertical semi-continuous casting. The alloy was prepared in a melting furnace. For Examples 1 to 7, a KCL / LiCl mixture was used on the surface of the liquid metal in the melting furnace. For Examples 8 to 9 no salt was used in the melting furnace. For Examples 8 to 9 the atmosphere in contact with the liquid metal with an oxygen content of less than 0.3% by volume for the entire casting installation. The casting installation included a hood disposed above the pouring well to limit the oxygen content. For tests 8 and 9, an aspiration (101) was also used such that the pressure in the chamber (10) was lower than the pressure in the chamber (65) and such that the speed of the atmosphere through the open surfaces of the casting well was at least 2 m / s. Oxygen content was measured with an oximeter during casting. In addition, the hydrogen content in the liquid aluminum was measured using an Alscan ™ type probe . under nitrogen sweep. Two types of liquid metal dispensers were used. A first "Combo Bag" type dispenser as described, for example, in the Figures 2 to 6 international demand WO 99/44719 , which does not call into question the invention, but made of fabric comprising essentially carbon, referenced below "distributor A" and a second distributor as described figure 3 referenced below "distributor B" is made of graphite wire cloth.
The casting conditions of the various tests carried out are given in Table 1. Table 1 - Casting conditions for different tests Trial H2 [ml / 100g] O2 measured above casting well (% by volume) Distributor 1 0.41 0.3 AT 2 0.43 0.1 AT 3 0.37 0.1 AT 4 0.33 0.1 AT 5 0.35 0.4 AT 6 0.38 0.3 AT 7 0.47 0.7 B 8 0.34 0.1 B 9 0.29 0.1 B

Les plaques ont été homogénéisées 12 heures à 505°C, usinées jusqu'à une épaisseur d'environ 365 mm, laminées à chaud jusqu'à des tôles d'épaisseur finale comprise entre 154 et 158 mm, mises en solution à 504 °C, trempées et détensionnée par traction contrôlée avec un allongement permanent de 3,5%. Les tôles ainsi obtenues ont subi un revenu de 18 heures à 155 °C.The plates were homogenized for 12 hours at 505 ° C., machined to a thickness of about 365 mm, hot-rolled to sheets with a final thickness of between 154 and 158 mm, dissolved at 504 ° C. , quenched and relieved by controlled traction with a permanent elongation of 3.5%. The sheets thus obtained have an 18 hour income at 155 ° C.

Les propriétés mécaniques statiques et de ténacité ont été caractérisées à quart-épaisseur. Les caractéristiques mécaniques statiques et la ténacité sont données dans le Tableau 2. Tableau 2 Caractéristiques mécaniques Epaisseur [mm] Rm (L) Rp0,2 (L) Essai MPa MPa A % (L) 1 158 528 495 6,5 2 155 538 507 7,0 3 155 525 493 8,3 4 158 528 497 7,0 5 158 529 495 6,0 6 158 527 496 6,8 7 154 514 486 8,3 8 158 533 502 6,3 9 158 542 512 5,8 Static mechanical properties and toughness were characterized at quarter-thickness. Static mechanical characteristics and toughness are given in Table 2. Table 2 Mechanical characteristics Thickness [mm] Rm (L) Rp0.2 (L) Trial MPa MPa A% (L) 1 158 528 495 6.5 2 155 538 507 7.0 3 155 525 493 8.3 4 158 528 four hundred ninety seven 7.0 5 158 529 495 6.0 6 158 527 496 6.8 7 154 514 486 8.3 8 158 533 502 6.3 9 158 542 512 5.8

Les propriétés en fatigue ont été caractérisées sur des éprouvettes lisses et sur des éprouvettes à trou pour certains échantillons prélevées à mi-épaisseur.
Pour les caractérisations de fatigue lisse, quatre éprouvettes, dont le schéma est donné en
Figure la, ont été testées à mi-épaisseur et mi-largeur dans le sens TL, les conditions de test étant σ = 242 MPa, R = 0,1. Certains tests ont été arrêtés après 200 000 cycles et d'autres tests ont été arrêtés après 300 000 cycles.
Pour les caractérisations de fatigue à trou, on a utilisé l'éprouvette reproduite sur la Figure 1b, dont la valeur Kt est 2,3. Les éprouvettes ont été testées à une fréquence de 50 Hz à l'air ambiant avec une valeur R = 0,1. Les courbes de Wöhler correspondantes sont présentées sur les Figures 6a et 6b. On a calculé l'indice de qualité de fatigue IQF. Tableau 3 - Résultats des essais en fatigue Essai Résultats de fatigue lisse (nombre de cycles) Résultats de fatigue à trou IQF (MPa), 50% rupture pour 100 000 cycles Eprouvette 1 Eprouvette 2 Eprouvette 3 Eprouvette 4 Moyenne lo garithmique L-T T-L 1 101423 101761 116820 118212 109263 2 102570 140030 152120 178860 140600 3 112453 163422 152620 167113 147138 175 152 4 101900 110300 139400 144100 122580 5 93400 105000 112600 129900 109439 6 114000 116500 188100 195000 148564 7 192300 >200000 189600 >200000 >195400 183 168 8 >300000 >300000 >300000 >300000 >300000 186 196 9 >300000 >300000 >300000 >300000 >300000 The fatigue properties were characterized on smooth test specimens and hole test specimens for some samples taken at mid-thickness.
For the characterizations of smooth fatigue, four specimens, whose schema is given in
Figure la, were tested at mid-thickness and half-width in the TL direction, the test conditions being σ = 242 MPa, R = 0.1. Some tests were stopped after 200,000 cycles and other tests were stopped after 300,000 cycles.
For hole-type fatigue characterization, the test piece reproduced on the Figure 1b whose K t value is 2.3. The test pieces were tested at a frequency of 50 Hz in the air ambient with a value R = 0.1. The corresponding Wöhler curves are presented on the Figures 6a and 6b . The IQF fatigue quality index was calculated. Table 3 - Fatigue Test Results Trial Smooth fatigue results (number of cycles) IQF (MPa) hole fatigue results, 50% rupture per 100,000 cycles Test tube 1 Test tube 2 Test tube 3 Test tube 4 Average garithmic lo LT TL 1 101423 101761 116820 118212 109263 2 102570 140030 152120 178860 140600 3 112453 163422 152620 167113 147138 175 152 4 101900 110300 139400 144100 122580 5 93400 105000 112600 129900 109439 6 114000 116500 188100 195000 148564 7 192300 > 200000 189600 > 200000 > 195400 183 168 8 > 300000 > 300000 > 300000 > 300000 > 300000 186 196 9 > 300000 > 300000 > 300000 > 300000 > 300000

La combinaison d'une teneur en hydrogène inférieure à 0,4 ml/100g d'une teneur en oxygène mesurée au-dessus de la surface liquide inférieure à 0,3 % en volume et du distributeur B permet d'atteindre un excellent niveau de performance en fatigue. Ces résultats sont présentés sur la Figure 5. Tableau 3 - Résultats des essais en fatigue Essai Résultats de fatigue lisse (nombre de cycles) Résultats de fatigue à trou IQF (MPa), 50% rupture pour 100 000 cycles Eprouvette 1 Eprouvette 2 Eprouvette 3 Eprouvette 4 Moyenne logarithmique L-T T-L 1 101423 101761 116820 118212 109263 2 102570 140030 152120 178860 140600 3 112453 163422 152620 167113 147138 175 152 4 101900 110300 139400 144100 122580 5 93400 105000 112600 129900 109439 6 114000 116500 188100 195000 148564 7 192300 >200000 189600 >200000 >195400 183 168 8 >300000 >300000 >300000 >300000 >300000 186 196 9 >300000 >300000 >300000 >300000 >300000 The combination of a hydrogen content of less than 0.4 ml / 100g of an oxygen content measured above the liquid surface of less than 0.3% by volume and of the distributor B makes it possible to achieve an excellent level of fatigue performance. These results are presented on the Figure 5 . Table 3 - Fatigue Test Results Trial Smooth fatigue results (number of cycles) IQF (MPa) hole fatigue results, 50% rupture per 100,000 cycles Test tube 1 Test tube 2 Test tube 3 Test tube 4 Logarithmic average LT TL 1 101423 101761 116820 118212 109263 2 102570 140030 152120 178860 140600 3 112453 163422 152620 167113 147138 175 152 4 101900 110300 139400 144100 122580 5 93400 105000 112600 129900 109439 6 114000 116500 188100 195000 148564 7 192300 > 200000 189600 > 200000 > 195400 183 168 8 > 300000 > 300000 > 300000 > 300000 > 300000 186 196 9 > 300000 > 300000 > 300000 > 300000 > 300000

La combinaison d'une teneur en hydrogène inférieure à 0,4 ml/100g d'une teneur en oxygène mesurée au-dessus de la surface liquide inférieure à 0,3 % en volume et du distributeur B permet d'atteindre un excellent niveau de performance en fatigue. Ces résultats sont présentés sur la Figure 5.The combination of a hydrogen content of less than 0.4 ml / 100g of an oxygen content measured above the liquid surface of less than 0.3% by volume and of the distributor B makes it possible to achieve an excellent level of fatigue performance. These results are presented on the Figure 5 .

Claims (13)

  1. Dispenser used for semi-continuous casting of aluminium alloy slabs made of fabric comprising essentially carbon, having a lower face (76), an upper face defining the opening through which the molten metal is introduced (71) and a wall of substantially rectangular section, the wall comprising two longitudinal portions parallel with width W (720, 721) and two transverse portions parallel with thickness T (730, 731), said transverse and longitudinal portions being formed from at least two fabrics, a first fabric having mesh sizes of less than 0.5 mm and semi-rigid (77) ensuring that the dispenser keeps its shape during casting, and a second non-sealing fabric (78) allowing the passage and filtration of liquid, said first and second fabrics being bonded to each other without overlap or with overlap and no gap separating them, said first fabric continuously covering at least 30% of the surface of said wall portions (720, 721, 730, 731) and being positioned so that the liquid surface is in contact therewith over the entire section,
  2. Dispenser according to claim 1 characterized in that the first fabric has a height h1 as measured from the upper face on the circumference of the wall (720, 721, 730, 731) such that h1 ≥ 0.3 h and preferably h1 ≥ 0.5 h, where h is the total height of the wall of the dispenser.
  3. Dispenser according to claim 1 or claim 2 characterized in that the section of the wall changes linearly as a function of height h, typically so that the surface of the lower face (76) of the dispenser is higher or lower by at most 10% than the surface of the upper face (71) of the dispenser .
  4. Dispenser according to any one of claims 1 to 3, characterized in that the surface area covered by the first fabric is between 30 and 90% and
    preferably between 50 and 80% for the longitudinal portions (720) and (721), and/or between 30 and 70% and preferably between 40 and 60% for the lateral portions (730, 731) and/or between 30 and 100% and preferably between 50 and 80% for the base (76).
  5. Dispenser according to any of claims 1 to 4 characterized in that length L1 of the first fabric located in the base (76) is greater than length L2 of the first fabric in the portion of the longitudinal walls (720) and (721) in contact with the base.
  6. Dispenser according to any of claims 1 to 5 characterized in that the first fabric has a mesh size of less than 0.2 mm and/or the second fabric is non-sealing and allows molten metal to pass through, typically having a mesh size of between 1 and 5 mm, preferably 2 to 4 mm.
  7. Method of manufacturing an aluminium alloy wrought product comprising steps in which
    (a) a bath of molten alloy metal is prepared comprising, as a percentage by weight, Cu: 2.0 - 6.0; Li: 0.5 - 2.0, Mg: 0 - 1.0; Ag: 0 - 0.7; Zn 0 - 1.0; and at least one element selected from Zr, Mn, Cr, Sc, Hf and Ti, the amount of said element, if selected, being 0.05 to 0.20 by weight for Zr, 0.05 to 0.8% by weight for Mn, 0.05 to 0.3 by weight for Cr and for Sc, 0.05 to 0.5 by weight Hf and 0.01 to 0.15% by weight for Ti, Si ≤ 0.1; Fe ≤ 0.1; others ≤ 0.05 each and ≤ 0.15 in total, the rest aluminium,
    (b) said alloy is cast by semi-continuous vertical casting to obtain a slab of thickness T and width W so that upon solidification,
    - the hydrogen content of said molten metal bath (1) is less than 0.4 ml/100g,
    - the oxygen content measured above the liquid surface (14,15) is less than 0.5% by volume,
    - the dispenser used (7) for casting is a dispenser according to any one of claims 1 to 6.
    (c) said slab is homogenized before or after optionally machining it to get a shape that can be hot-worked
    (d) said shape, homogenized in this way, is hot worked and optionally cold worked to obtain a wrought product,
    (e) said wrought product undergoes solution heat treatment and quenching,
    (f) optionally said wrought product that has undergone solution heat treatment is stress-relieved by plastic deformation with a deformation of at least 1 %.
    (g) said solution heat-treated and optionally stress-relieved product is subjected to ageing.
  8. Method according to claim 7 wherein the oxygen content of the atmosphere in contact with the liquid metal bath in the melting furnace during the degassing step, filtration is less than 0.5% by volume and preferably wherein the oxygen content of the atmosphere in contact with the liquid metal bath is less than 0.5% by volume for the entire casting facility.
  9. Method according to either of claims 7 or 8 wherein a lid (62) covers the liquid surface during solidification (14,15), said lid preferably comprising seals (61) to ensure pressure tightness with the casting table (32) and wherein an inert gas (9) is introduced into the chamber (65) defined between the lid and the casting table and wherein suction is maintained in the casting pit (10) by means of a pump (101), preferably so that the pressure within the containment (10) is less than the pressure in the chamber (65).
  10. Method according to any of claims 7 to 9 in which a molten salt containing lithium is not used throughout the entire casting facility.
  11. Method according to any of claims 7 to 10 in which said hot and/or cold working is performed by extrusion, rolling and/or forging.
  12. Method according to any of claims 7 to 11 in which the deformation ratio during step (d) is lower than 85% and preferably lower than 80%.
  13. Method according to any of claims 1 to 8 in which the alloy comprises, as a percentage by weight, Cu: 3.0 - 3.9; Li: 0.7 - 1.3, Mg: 0.1 to 1.0, at least one element selected from Zr, Mn and Ti, the amount of said element, if selected, is from 0.06 to 0.15 by weight for Zr, 0.05 to 0.8 by weight for Mn and 0.01 to 0.15% by weight for Ti; Ag: 0 - 0.7; Zn ≤ 0.25; Si ≤ 0.08; Fe ≤ 0.10; others ≤ 0.05 each and ≤ 0.15 in total.
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JP2017507240A (en) 2017-03-16
CA2932989C (en) 2021-10-26
US20160237532A1 (en) 2016-08-18
JP6683611B2 (en) 2020-04-22
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BR112016012288A8 (en) 2020-05-05
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EP3080318B2 (en) 2023-09-13
WO2015086922A2 (en) 2015-06-18
EP3080317A2 (en) 2016-10-19
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DE14825363T1 (en) 2017-01-12
CN105814222B (en) 2019-07-23
BR112016012288B1 (en) 2021-05-04
CN105814222A (en) 2016-07-27
CN106170573B (en) 2018-12-21
FR3014905A1 (en) 2015-06-19
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WO2015086922A3 (en) 2015-08-27
CA2932989A1 (en) 2015-06-18

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