Classifications

• • 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
• • 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
• • 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
• • 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
• • 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 process for manufacturing aluminum-copper-lithium alloy products, in particular such products intended for aeronautical and aerospace construction.
• Aluminum alloy products are developed to produce high-strength parts for the aerospace industry and the aerospace industry in particular.
• Aluminum alloys containing lithium are very interesting in this respect, since lithium can reduce the density of aluminum by 3% and increase the modulus of elasticity by 6% for each weight percent of lithium added.
• their performance compared with the other properties of use must reach that of the alloys commonly used, in particular in terms of a compromise between the static mechanical strength properties (yield strength in tension and in compression, breaking strength) and the properties of damage tolerance (toughness, fatigue crack propagation resistance), these properties being in general antinomic.
• the elastic limit in compression and the toughness in plane stress are essential properties. These mechanical properties must also preferably be stable over time and have good thermal stability, that is to say, not be significantly modified by aging at the temperature of use.
• alloys must also have sufficient corrosion resistance, be able to be shaped according to the usual methods and have low residual stresses so that they can be machined integrally. Finally, they must be able to be obtained by robust manufacturing processes, in particular, the properties must be able to be obtained on industrial tools for which it is difficult to guarantee a temperature homogeneity to a few degrees for large parts.
• No. 5,032,359 discloses a broad family of aluminum-copper-lithium alloys in which the addition of magnesium and silver, in particular between 0.3 and 0.5 percent by weight, makes it possible to increase the mechanical strength.
• No. 5,455,003 discloses a process for manufacturing Al-Cu-Li alloys which have improved mechanical strength and toughness at cryogenic temperature, in particular through proper work-hardening and tempering.
• US Pat. No. 7,438,772 describes alloys comprising, in percentage by weight, Cu: 3-5, Mg: 0.5-2, Li: 0.01-0.9 and discourages the use of higher lithium content because of degradation of the compromise between toughness and mechanical strength.
• US Pat. No. 7,229,509 discloses an alloy comprising (% by weight): (2,5-5,5) Cu (0,1-2,5) Li (0.2-1.0) Mg (0) 2-0, 8) Ag, (0.2-0.8) Mn, 0.4 max Zr or other grain refining agents such as Cr, Ti, Hf, Sc, V.
• US Patent Application 2009/142222 A1 discloses alloys comprising (in% by weight), 3.4 to 4.2% Cu, 0.9 to 1.4% Li, 0.3 to 0.7%. of Ag, 0.1 to 0.6% Mg, 0.2 to 0.8% Zn, 0.1 to 0.6% Mn and 0.01 to 0.6% of at least one element. for the control of the granular structure. This application also describes a process for manufacturing spun products.
• the patent application WO2009 / 036953 relates to an aluminum alloy product for the structural elements having a chemical composition comprising, by weight Cu of 3.4 to 5.0, Li of 0.9 to 1.7 g / l of O , 2 to 0.8, Ag from about 0.1 to 0.8, Mn from 0.1 to 0.9, Zn to 1.5, and one or more elements selected from the group consisting of: Zr about 0.05 to 0.3, Cr 0.05 to 0.3, Ti about 0.03 to 0.3, Sc about 0.05 to 0.4, Hf about 0.05 to 0.4), Fe ⁇ 0.15, Si ⁇ 0, 5, normal and unavoidable impurities.
• the patent application WO 2012/085359 A2 relates to a process for producing aluminum-based alloy rolled products comprising 4.2 to 4.6% by weight of Cu, 0.8 to 1.30% by weight of Li 0.3 to 0.8% by weight of Mg, 0.05 to 0.18% by weight of Zr, 0.05 to 0.4% by weight of Ag, 0.0 to 0.5% by weight, weight of Mn, at most 0.20% by weight of Fe + Si, less than 0.20% by weight of Zn, at least one element selected from Cr, Se, Hf and Ti, the amount of said element, if is selected, being from 0.05 to 0.3% by weight for Cr and for Se, 0.05 to 0.5% by weight for Hf and from 0.01 to 0.15% by weight for Ti, the others elements at most 0.05% by weight each and 0, 15% by weight in total, the aluminum residue, comprising the stages of production, casting, homogenization, rolling with a temperature above 400 ° C, dissolution, quenching , traction between 2 and 3.5% and income.
• the patent application US2012 / 0225271 A1 concerns wrought products with a thickness of at least 12.7 mm containing 3.00 to 3.80% by weight of Cu, from 0.05 to 0.35 by weight% of Mg, from 0.975 to 1.385 wt% of Li, wherein -0.3 Mg-0.l5Cu +1, 65 ⁇ Li ⁇ -0.3 Mg-O.l5Cu +1, 85, from 0.05 to 0 50% by weight.
• % of at least one grain structure control element wherein the grain structure control element is selected from the group consisting of Zr, Sc, Cr, V, Hf, other land elements Rare, and combinations thereof, up to 1.0% by weight% Zn, up to 1.0% by weight% Mn, up to 0.12% by weight% Si, up to 0%. , By weight% Fe, up to 0.15% by weight% Ti, up to 0.10 weight. % of other elements with a total not exceeding 0.35% by weight.
• Application WO 2013/169901 discloses alloys comprising, in percentage by weight, 3.5 to 4.4% Cu, 0.65 to 1.15% Li, 0.1 to 1.0% Ag, 0.45 to 0.75% Mg, 0.45 to 0.75% Zn and 0.05 to 0.50% of at least one element for controlling the granular structure.
• the alloys advantageously have a Zn to Mg ratio of between 0.60 and 1.67.
• a first object of the invention is a method of manufacturing an aluminum alloy product in which, successively,
• an aluminum-based liquid metal bath comprising 3.5 to 4.7% by weight of Cu; 0.6 to 1.2% by weight of Li; 0.2 to 0.8% by weight of Mg; 0.1 to 0.2% by weight of Zr; 0.0 to 0.3% by weight of Ag; 0.0 to 0.8% by weight of Zn; 0.0 to 0.5% by weight of Mn; not more than 0.20% by weight of Fe + Si; optionally an element selected from Cr, Se, Hf and V, the quantity of said element, if it is chosen, being from 0.05 to 0.3% by weight for Cr and for Se, 0.05 to 0.5% by weight for Hf and for V; other elements not exceeding 0.05% by weight each and 0.15% by weight in total and remaining aluminum;
• Another subject of the invention is a product that can be obtained by the process according to the invention and that it is a laminated product with a thickness of between 8 and 50 mm and having, at half thickness,
• Yet another object is an aircraft structural element, preferably an extrados wing wing element, comprising a product according to the invention.
• Figure 1 Compromise between the toughness K aPP LT and the compressive yield strength Rc p o.2 L of the alloys of Example 1.
• FIG. 2 Graph representing the difference between the value of K aPP (LT) measured according to the alloys of example 1 and the value calculated according to the formula -0.5 R cp o, 2 (L) + 386 as a function of the conventional yield strength R P o.2 measured in the longitudinal direction of the product.
• Figure 3 Compromise between the toughness Kapp LT and the yield strength in compression Rc p o . 2 L alloys of Example 2.
• FIG. 4 Graph representing the difference between the Ka PP (LT) value measured according to the alloys of Example 2 and the value calculated according to the formula -0.5 R cp o, 2 (L) + 375 as a function of the conventional yield strength R p o.2 measured in the longitudinal direction of the product.
• the static mechanical characteristics in tension in other words the tensile strength R m , the conventional yield stress at 0.2% elongation R P o, 2, and the elongation at break A%, are determined by a tensile test according to standard NF EN ISO 6892-1 (2016), the sampling and the direction of the test being defined by standard EN 485 (2016).
• R PO , 2 (L) means R p o, 2 measured in the longitudinal direction.
• the yield strength in compression Rc p o, 2 was measured at 0.2% compression according to ASTM E9-09 (2016).
• Rc p o, 2 (L) means Rc p o, 2 measured in the longitudinal direction.
• the stress intensity factor (Kic) is determined according to ASTM E 399 (2012).
• ASTM E 399 (2012) provides the criteria for determining whether KQ is a valid Kic value. For a given specimen geometry, the KQ values obtained for different materials are comparable to each other as long as the elasticity limits of the materials are of the same order of magnitude. Unless otherwise specified, the definitions of EN 12258 (2012) apply.
• the values of the apparent tensile strength factor (K aPP ) and the tensile stress intensity factor (K c ) are as defined in ASTM E561. Curved line giving the effective stress intensity factor as a function of the effective crack extension, known as the R curve, is determined according to ASTM E 561 (ASTM E 561-10-2).
• the critical stress intensity factor Kc in other words the intensity factor that makes the crack unstable, is calculated from the curve R.
• the stress intensity factor Kco is also calculated by assigning the length initial crack at the beginning of the monotonic load, at the critical load. These two values are calculated for a specimen of the required form.
• K aPP represents the Kco factor corresponding to the specimen that was used to perform the R curve test.
• K ef r represents the Kc factor corresponding to the specimen that was used to perform the R curve test.
• 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 the elements that make up the fuselage (such as fuselage skin, fuselage skin in English), stiffeners or stringers, bulkheads, fuselage (circumferential ffames), wings (such as upper or lower wing skin, stringers or stiffeners), ribs and spars) and composite empennage including horizontal and vertical stabilizers (horizontal or vertical stabilizers), as well as floor beams, seat tracks and doors.
• fuselage such as fuselage skin, fuselage skin in English
• stiffeners or stringers such as upper or lower wing skin, stringers or stiffeners
• ribs and spars composite empennage including horizontal and vertical stabilizers (horizontal or vertical stabilizers), as well as floor beams, seat tracks and doors.
• a selected class of aluminum alloys containing in particular specific and critical quantities of lithium, copper, magnesium and zirconium makes it possible, under certain processing conditions, to produce products, particularly laminated products, having an improved compromise between toughness, yield strength in tension and in compression.
• the present inventors have found that, surprisingly, it is possible to improve the properties of use for the products made from these alloys, in particular those making the products suitable for the preparation of structural elements in the aeronautical and aerospace.
• the products according to the invention are particularly well suited to the development of extrados elements of aircraft wings since they have a compromise limit of elasticity in compression Rc p o, 2 (L) - toughness Kapp (LT) particularly improved.
• the invention relates in particular to a manufacturing method in which an alloy comprising 3.5 to 4.7% by weight of Cu is prepared; 0.6 to 1.2% by weight of Li; 0.2 to 0.8% by weight of Mg; 0.1 to 0.2% by weight of Zr; 0.0 to 0.3% by weight of Ag; 0.0 to 0.8% by weight of Zn; 0.0 to 0.5% by weight of Mn; not more than 0.20% by weight of Fe + Si; optionally an element selected from Cr, Se, Hf and V, the quantity of said element, if it is chosen, being from 0.05 to 0.3% by weight for Cr and for Se, 0.05 to 0.5% by weight for Hf and for V; other elements at most 0.05% by weight each and 0.15% by weight in total, is introduced a refining, poured in a raw form, homogenized, deformed hot, dissolved, quenched, deforms cold and produces an income, wherein the refining contains TiC particles and / or the cold deformation is between 8 to 16%.
• the copper content of the products according to the invention is between 3.5 and 4.7% by weight, preferably between 4.0 and 4.6% by weight. In a particularly advantageous embodiment, the copper content is between 4.1 and 4.5% by weight, preferably between 4.2 and 4.4% by weight.
• the increase in the copper content contributes to an improvement of the elastic limit in tension and in compression. However, the copper, in excessively high quantity, induces a reduction in the toughness in Kapp plane stress.
• the lithium content of the products according to the invention is between 0.6 and 1, 2% by weight.
• the lithium content is between 0.8 and 1.0% by weight; preferably between 0.85 and 0.95% by weight.
• the increase in the lithium content has a favorable effect on the density, however the present inventors have found that for the alloys according to the invention, the selected lithium content makes it possible to improve the compromise between mechanical strength, in particular the limit of elasticity in traction and in compression, and tenacity. Too high a lithium content can lead to a degradation of toughness.
• the magnesium content of the products according to the invention is between 0.2% and 0.8% by weight.
• the magnesium content is at least 0.3% or even 0.4% or 0.5% by weight, which simultaneously improves static mechanical strength and toughness.
• the magnesium content is less than 0.7% by weight or even 0.65% by weight. Indeed, a high magnesium content can induce a degradation of the tenacity.
• the alloy may contain zinc up to 0.8% by weight.
• the Zn content is between 0.05 and 0.6% by weight, preferably 0.2 and 0.5% by weight and, more preferably, between 0.30 and 0.40. % in weight.
• the alloy contains less than 0.05% by weight of Zn, preferably less than 0.02% by weight.
• the alloy may also contain up to 0.3% by weight of silver.
• the alloy comprises more than 0.05% by weight, preferably more than 0.1% and even more preferably 0.2 to 0.3% by weight of Ag.
• the maximum content of Ag is 0.27% by weight.
• the Ag content is 0.1 to 0.27 wt% and / or the Zn content is 0.2 to 0.40 wt%.
• the alloy may also contain up to 0.5% by weight of manganese.
• the manganese content is between 0.05 and 0.4% by weight.
• the manganese content is between 0.2 and 0.37% by weight and preferably between 0.25 and 0.35% by weight.
• the manganese content is between 0.1 and 0.2% by weight and preferably between 0.10 and 0.20% by weight.
• Mn makes it possible in particular to obtain a high tenacity. However, if the Mn content is too high, the fatigue life can be significantly reduced.
• the Zr content of the alloy is between 0.1 and 0.2% by weight. In an advantageous embodiment, the Zr content is between 0.10 and 0.15% by weight, preferably between 0.1 and 0.14% by weight.
• the alloy also contains titanium, the Ti content is between 0.01 and 0.15% by weight, preferably between 0.02 and 0.08% by weight.
• the refiner introduced into the aluminum alloy bath contains TiC type particles.
• the formula has the formula A1T i x C y that is also written AT x C y where x and y are the contents of Ti and C in% by weight for 1% by weight of Al, and x / y> 4.
• the present inventors have found that, in the particular case of the present alloy, the presence in the refining and therefore in the alloy of TiC particles at the origin of a particular refining of the alloy during casting (AlTiC refining), provides a product with an optimized compromise of properties.
• AlTiC refining the presence of TiC particles in the refining yarn and in the alloy of one embodiment of the process of the present invention makes it possible to improve the compromise between the Ka PP LT toughness and the yield strength in R compression. c p0.2 L.
• the sum of the iron content and the silicon content is at most 0.20% by weight.
• the iron and silicon contents are each at most 0.08% by weight.
• the iron and silicon contents are at most 0.06% and 0.04% by weight, respectively.
• a controlled and limited iron and silicon content contributes to the improvement of the compromise between mechanical resistance and damage tolerance.
• the alloy may also contain at least one element that can contribute to the control of the grain size chosen from Cr, Se, Hf and V, the quantity of said element, if it is chosen, being from 0.05 to 0.3% by weight for Cr and Se and 0.05 to 0.5% by weight for Hf and for V.
• the density increasing additive elements such as Cu, Zn, Mn and Ag are minimized and the density reducing elements such as Li and Mg are maximized to a density of 2.73 or lower. g / cm 3 and preferably less than or equal to 2.72 g / cm 3 .
• the content of the other elements is not more than 0.05% by weight each and 0.15% by weight in total.
• the other elements are typically unavoidable impurities.
• the manufacturing process of the products according to the invention comprises the steps of production, casting, introduction of a refining, homogenization, hot deformation, dissolution and quenching, cold deformation and tempering.
• a bath of liquid metal is produced so as to obtain an aluminum alloy of composition according to the invention.
• a refining so that the Ti content is between 0.01 to 0.15% by weight, optionally refining contains T iC type particles.
• the Ti content is between 0.02 and 0.08% by weight, preferably between 0.03 and 0.06% by weight.
• the refining contains TiC type particles.
• the refining agent containing TiC-type particles is introduced in a form and quantity such that an identical amount of TiC to that added with a refining AT3C0.15 at a rate of 2 to 5 kg / t of alloy of aluminum is added.
• the refining containing T iC type particles is introduced in the form of AT3C0.15 at a rate of 2 to 5 kg / t of aluminum alloy.
• the bath of liquid metal is then cast as a raw form, preferably in the form of a rolling plate.
• the raw form is then homogenized so as to reach a temperature of between 450 ° C. and 550 ° C. and preferably between 480 ° C. and 530 ° C. for a period of between 5 and 60 hours.
• the homogenization treatment can be carried out in one or more stages.
• the raw form is generally cooled to room temperature before being preheated for hot deformation.
• the hot deformation may in particular be extrusion or hot rolling. Preferably, it is a hot rolling step.
• the hot rolling is carried out to a thickness of preferably between 8 and 50 mm and preferably between 15 and 40 mm.
• the product thus obtained is then put in solution by heat treatment to reach a temperature between 490 and 530 ° C for 15 min to 8 h, and then typically quenched with water at room temperature.
• the product then undergoes a cold deformation with a cold deformation of 2 to 16%.
• the cold deformation is a controlled traction with a permanent deformation of 2 to 6%, preferably of 2.0% to 4.0%.
• said product is cold deformed with a cold deformation ratio of between 8 and 16%.
• the cold deformation is carried out in two steps: the product is first cold rolled with a thickness reduction ratio of between 8 and 12%, preferably 9 and 11%, and subsequently controlled tractionning with a permanent deformation of between 0.5 and 4%, preferably between 0.5 and 2%.
• the product is then subjected to a tempering step carried out by heating at a temperature between 130 and 170 ° C and preferably between 140 and 160 ° C for 5 to 100 hours and preferably from 10 to 70h.
• the tempering is carried out at a temperature of between 140 and 155 ° C., preferably between 145 and 150 ° C., preferably for 18 to 22 hours.
• the process according to the invention makes it possible to obtain an advantageous product.
• the specific and critical contents of the alloy of the present invention associated with a particular manufacturing process make it possible to achieve excellent properties.
• the product according to the invention is advantageously a laminated product having a thickness of between 8 and 50 mm and having, at mid-thickness,
• the product according to the invention is a laminated product with a thickness of between 8 and 50 mm and having, at mid-thickness,
• Rc p o , 2 (L) expressed in MPa the yield strength in compression measured at 0.2% compression according to ASTM E9 (2016)
• the inventors have found that surprisingly the combination of the introduction into the liquid metal bath of an affine containing TiC-type particles so that the Ti content is between 0.01 to 0.15 % by weight and cold deformation after dissolution with a degree of cold deformation of between 8 to 16% is advantageous.
• this combination makes it possible to obtain for a laminate product with a thickness of between 8 and 50 mm, at mid-thickness.
• the combination comprising the introduction into the liquid metal bath of an affine containing TiC type particles so that the Ti content is between 0.01 to 0.15% by weight and a cold deformation after dissolving with a cold deformation ratio of between 8 and 16% makes it possible to obtain for a rolled product with a thickness between 8 and 50 mm, at mid-thickness,
• R p 0.2 (L) the conventional yield strength at 0.2% elongation measured in the longitudinal direction of the product, determined by a tensile test according to NF EN ISO 6892-1 (2016).
• the alloy products according to the invention allow in particular the manufacture of structural elements, in particular of aircraft structural elements.
• the preferred aircraft structure element is an extrados wing wing component.
• the plates were homogenized at about 50 ° C.
• the homogenized plates were hot-rolled at an inlet temperature of approximately 450 ° C. and an outlet temperature of approximately 390 ° C. to obtain 28 mm thick plates for each alloy.
• the sheets were put in solution. at about 510 ° C for 3h, quenched with water at 20 ° C.
• One sheet of each alloy 1 and 2 was then cold rolled with a reduction rate of thickness 10% (condition "LAF 10%) followed by traction with a permanent elongation of about 1%.
• For each alloy another sheet was also tractionned with a permanent deformation of 3% without prior cold rolling.
• the plates experienced a single-stage income as indicated in Table 2.
• FIG. 2 represents the difference between the measured value of Kapp (LT) and the value calculated according to the formula "-0.5 R cp o, 2 (L) + 386" as a function of the yield strength R p o. 2 (L) conventionally measured in the longitudinal direction L of the product.
• the plates were homogenized at about 510 ° C. After homogenization, the plates were hot-rolled to obtain sheets having a thickness of 25 mm. The sheets were dissolved for 5 h at approximately 510 ° C., quenched with cold water. One plate of each alloy was cold rolled with a thickness reduction ratio of 10% (condition "LAF 10%"), followed by traction with a permanent elongation of about 1.2%. Another plate of each alloy has been traced with permanent elongation without prior cold rolling being performed. The values of the permanent elongations are shown in Table 4.
• the plates were then subjected to an income of between 10 h and 25 h at 155 ° C as indicated in Table 2.
• Samples were taken at mid-thickness to measure the static mechanical characteristics in tension, in compression as well as the tenacity in Ka PP (LT) plane stress.
• FIG. 4 represents the difference between the measured value of Kapp (LT) and the value calculated according to the formula -0.5 RcpO, 2 (L) + 375 as a function of the conventional yield strength Rp0.2 measured in the direction longitudinal L of the product .
• Table 4 Income conditions and mechanical properties obtained for alloy sheets 3, 4 and 5.

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