US20120152415A1 - Aluminum copper lithium alloy with improved resistance under compression and fracture toughness - Google Patents

Aluminum copper lithium alloy with improved resistance under compression and fracture toughness Download PDF

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US20120152415A1
US20120152415A1 US13/328,872 US201113328872A US2012152415A1 US 20120152415 A1 US20120152415 A1 US 20120152415A1 US 201113328872 A US201113328872 A US 201113328872A US 2012152415 A1 US2012152415 A1 US 2012152415A1
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mpa
yield stress
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Armelle Danielou
Gaelle Pouget
Christophe Sigli
Timothy Warner
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Constellium Issoire SAS
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Constellium France SAS
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    • 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
    • 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

Definitions

  • the invention relates to aluminum-copper-lithium alloy products, and more particularly such products, their manufacturing processes and use, designed in particular for aeronautical and aerospace engineering.
  • Hat-rolled products made of aluminum alloy are developed to produce parts of high strength designed in particular for the aircraft and aerospace industry.
  • Aluminum alloys containing lithium are of great interest in this respect, because lithium can reduce the density of aluminum by 3% and increase the modulus of elasticity by 6% for each percent of added lithium weight.
  • their performance as compared to the other usual properties must attain that of alloys in regular use, in particular in terms of the compromise between static mechanical resistance properties (tensile and compression yield stress, ultimate tensile strength) and damage tolerance properties (fracture toughness, resistance to fatigue crack propagation), these properties being in general contradictory.
  • static mechanical resistance properties tensile and compression yield stress, ultimate tensile strength
  • damage tolerance properties fracture toughness, resistance to fatigue crack propagation
  • These alloys must also have sufficient corrosion resistance, be capable of being formed according to usual processes and have low residual stresses in order to be able to be integrally machined.
  • U.S. Pat. No. 5,032,359 describes a vast 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 resistance.
  • U.S. Pat. No. 5,455,003 describes a manufacturing process for Al—Cu—Li alloys which have improved mechanical resistance and fracture toughness at cryogenic temperature, in particular owing to appropriate working and aging.
  • U.S. Pat. No. 7,438,772 describes alloys including, expressed as a 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 a reduction in the balance between fracture toughness and mechanical resistance.
  • U.S. Pat. No. 7,229,509 describes an alloy including (% 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 describes alloys including (percentage by weight), 3.4 to 4.2% Cu, 0.9 to 1.4% Li, 0.3 to 0.7% 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 controlling the granular structure. This request also describes a manufacturing process for extruded products.
  • a first subject of the invention is a manufacturing process for a flat-rolled product made of an aluminum alloy in which the following operations are performed in succession:
  • a second subject of the invention is a flat-rolled product of thickness between 8 and 50 mm and of substantially unrecrystallized granular structure obtainable by the process according to the invention having at mid-thickness at least one of the following combinations of characteristics:
  • Another subject of the invention is a structural element for an airplane, preferably an upper wing skin, including a product according to the invention.
  • Still another subject of the invention is the use of a product according to the invention or a structural element according to the invention for aeronautical engineering.
  • FIG. 1 Example of an aging curve and determination of the slope of tangent P N .
  • FIG. 2 Change in the compression yield stress and the tensile yield stress with the permanent set during controlled stretching.
  • FIG. 3 Property compromise between the compression yield stress and fracture toughness for K app for alloys N° 2 to N° 5 in example 2.
  • All the indications concerning the chemical composition of the alloys are 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 as a percentage by weight is multiplied by 1.4.
  • Alloys are designated in conformity with the rules of The Aluminium Association, known to those skilled in the art. The density depends on the composition and is determined by calculation rather than by a method of weight measurement. The values are calculated in compliance with the procedure of The Aluminium Association, which is described on pages 2-12 and 2-13 of “Aluminum Standards and Data”. The definitions of the metallurgical states are indicated in European standard EN 515.
  • the tensile static mechanical characteristics in other words the ultimate tensile strength R m , the conventional yield stress at 0.2% of elongation R p0.2 and elongation at break A %, are determined by a tensile test according to standard EN ISO 6892-1, sampling and test direction being defined by standard EN 485-1.
  • the compression yield stress was measured at 0.2% of compression as per standard ASTM E9.
  • K Q The stress intensity factor
  • ASTM F 399 Standard ASTM E 399 gives the criteria which make it possible to determine whether K Q is a valid value of K 1C .
  • ASTM E 399 gives the criteria which make it possible to determine whether K Q is a valid value of K 1C .
  • the values of K Q obtained for various materials are comparable with each other insofar as the yield stresses of the material are of the same order of magnitude.
  • a plot of the stress intensity versus crack extension, known as the R curve, is determined according to ASTM standard E561.
  • the critical stress intensity factor K C in other words the intensity factor that makes the crack unstable, is calculated starting from the R curve.
  • the stress intensity factor K CO is also calculated by assigning the initial crack length to the critical load, at the beginning of the monotonous load. These two values are calculated for a test piece of the required shape.
  • K app denotes the K CO factor corresponding to the test piece that was used to make the R curve test.
  • “Structural element” of a mechanical construction here refers to 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 analysis is usually prescribed or performed. These are typically elements the failure of which is likely to endanger the safety of said construction, its users or others.
  • these structural elements include the parts which make up the fuselage (such as the fuselage skin, stringers, bulkheads, circumferential frames), the wings (such as the upper or lower wing skin, stringers or stiffeners, ribs and spars) and the tail unit, made up of horizontal and vertical stabilizers, as well as floor beams, seat tracks and doors.
  • a selected class of aluminum alloys which contain specific and critical quantities of lithium, copper, magnesium, silver and zirconium makes it possible to prepare, in certain transformation conditions, flat-rolled products having an improved compromise between fracture toughness, tensile yield stress and compression yield stress.
  • the present inventors noted that, surprisingly, it is possible to improve the compression yield stress for these alloys by choosing specific transformation process parameters, in particular during hot working and stress relieving by controlled stretching.
  • the copper content of the products according to the invention lies between 4.2 and 4.6% by weight. In an advantageous embodiment of the invention, the copper content is at least 4.3% by weight. A maximum copper content of 4.4% by weight is preferred.
  • the lithium content of the products according to the invention lies between 0.8% or 0.80% and 1.30% by weight and preferably 1.15% by weight.
  • the lithium content is at least 0.85% by weight.
  • a maximum lithium content of 0.95% by weight is preferred.
  • the increase in the copper content and, to a lesser extent, the lithium content contributes to improving static mechanical resistance; however, as copper has a detrimental effect in particular on density, it is preferable to limit the copper content to the preferred maximum value.
  • the increase in the lithium content has a favorable effect on density; however the present inventors noted that for alloys according to the invention, the preferred lithium content ranging between 0.85% and 0.95% by weight in an embodiment makes for an improved compromise between mechanical resistance (tensile yield stress and compression) and fracture toughness and, in addition, the fracture toughness attained for aging at the peak or close to the peak is higher.
  • the preferred lithium content ranges between 1.10% and 1.20% by weight, with preferably a magnesium content ranging between 0.50% or preferably 0.53% and 0.70% or preferably 0.65% by weight.
  • the magnesium content of the products according to the invention lies between 0.3% or 0.30% and 0.8 or 0.80% by weight.
  • the magnesium content is at least 0.40% or even 0.45% by weight, which simultaneously improves static mechanical resistance and fracture toughness.
  • the present inventors noted that the combination of a magnesium content ranging between 0.50% or preferably 0.53% and 0.70% or preferably 0.65% by weight and a lithium content ranging between 0.85% and 1.15% by weight and preferably between 0.85% and 0.95% by weight led to a compromise between mechanical resistance (tensile and compression yield stress) and particularly advantageous fracture toughness, while keeping an acceptable failure rate during the transformation, and thus satisfactory reliability of the manufacturing process.
  • the zirconium content lies between 0.05 and 0.18% by weight and preferably between 0.08 and 0.14% by weight. In an advantageous embodiment of the invention, the zirconium content is at least 0.11% by weight.
  • the manganese content lies between 0.0 and 0.5% by weight. In an advantageous embodiment of the invention, the manganese content is between 0.2 and 0.4% by weight. In another embodiment of the invention, the manganese content is lower than 0.1% by weight and preferably lower than 0.05% by weight, which makes it possible, for the products obtained by the process according to the invention, to decrease the quantity of insoluble metal phases and to improve damage tolerance still further.
  • the silver content lies between 0.05% and 0.5% by weight. In an advantageous embodiment of the invention, the silver content is between 0.10 and 0.40% by weight.
  • the addition of silver helps to improve the compromise of the mechanical properties of the products obtained by the process according to the invention.
  • the sum of the iron content and the silicon content is at the most 0.20% by weight.
  • the iron and silicon contents are each at the most 0.08% by weight.
  • the iron and silicon contents are at the most 0.06% and 0.04% by weight respectively.
  • a controlled and limited iron and silicon content helps to improve the compromise between mechanical resistance and damage tolerance.
  • the alloy also contains at least one element which may contribute to the control of grain size chosen from Cr, Sc, Hf and Ti, the quantity of the element, if it is chosen, being from 0.05 to 0.3% by weight for Cr and Sc, 0.05 to 0.5% by weight for Hf and from 0.01 to 0.15% by weight for Ti.
  • it is chosen to add between 0.01 and 0.10% by weight of titanium and to limit the Cr, Sc and Hf content to 0.05% by weight maximum, as these elements can have a detrimental effect, in particular on density and are added only to further help obtain a primarily unrecrystallized structure if necessary.
  • Zinc is an undesirable impurity, in particular because of its contribution to the density of the alloy.
  • the zinc content is lower than 0.20% by weight, preferably Zn ⁇ 0.15% by weight and preferably still Zn ⁇ 0.05% by weight.
  • the zinc content is advantageously lower than 0.04% by weight.
  • the elements added that contribute to increasing density such as Cu, Zn, Mn and Ag are minimized and the elements that contribute to decreasing the density such as Li and Mg are maximized in order to reach a density of less than 2.73 g/cm 3 and preferably less than 2.70 g/cm 3 .
  • the manufacturing process for the products according to the invention includes the steps of production, casting, homogenization, rolling at a temperature higher than 400° C., solution hardening, quenching, stretching between 2 and 3.5% and aging.
  • a molten metal bath is produced in order to obtain an aluminum alloy composed according to the invention.
  • the molten metal bath is then cast in the form of rolling slab.
  • the rolling slab is then homogenized in order to reach a temperature ranging between 450° C. and 550° and preferably between 480 and 530° C. for a length of time ranging between 5 and 60 hours.
  • the homogenization treatment can be carried out in one or more steps.
  • the rolling slab After homogenization, the rolling slab is in general cooled down to room temperature before being preheated ready for hot rolling.
  • the aim of the pre-heating is to reach a temperature making it possible to maintain a temperature of at least 400° C. and preferably of at least 420° C. during hot rolling.
  • Intermediate reheating is carried out if during hot rolling the temperature decreases excessively.
  • Hot rolling is carried out down to a thickness ranging preferably between 8 and 50 mm and preferably between 12 and 40 mm.
  • the product so obtained is then solution heat treated by thermal treatment making it possible to reach a temperature ranging between 490 and 530° C. for 15 min to 8 hours, then quenched typically with water at room temperature or preferably with cold water.
  • the product then undergoes controlled stretching with a permanent set of 2 to 3.5% and preferably 2.0% to 3.0%. Controlled stretching with a maximum permanent set of approximately 2.5% is preferred.
  • the present inventors noted that, surprisingly, the compression yield stress decreases with the increasing permanent sets during controlled stretching while the yield stress under traction increases in these conditions. There is therefore an optimal permanent set by controlled stretching making it possible to obtain a high compression yield stress while maintaining a sufficient tensile yield stress.
  • the permanent set by controlled stretching is selected so as to obtain a compression yield stress at least equal to the tensile yield stress.
  • the effect of the rate of permanent set on the compression yield stress is specific to flat-rolled products; tests on extruded products showed that such an effect is not observed in this case.
  • Known steps such as rolling, flattening, straightening or shaping may optionally be performed after solution heat treatment and quenching and before or after controlled stretching.
  • a cold rolling step of at least 7% and preferably at least 9% and at the most 15% is carried out after solution heat treatment and quenching and before controlled stretching. But especially given the cost of the additional cold rolling step, it is advantageous in another embodiment to realize directly controlled stretching after solution treatment and quenching.
  • Aging is performed in which the product reaches a temperature ranging between 130 and 170° C. and preferably between 150 and 160° C. for 5 to 100 hours and preferably from 10 to 70 hours. Aging may be performed in one or more steps.
  • the yield stress increases with the duration of aging at a given temperature up to a maximum value known as the hardening peak or “peak”, then decreases with aging time.
  • the aging curve is the change in yield stress according to the equivalent duration of aging at 155° C.
  • An example of an aging curve is given in FIG. 1 .
  • the yield stress of a point N of the aging curve is close to the yield stress at the peak if the absolute value of slope P N is at the most 3 MPa/h.
  • an under-aged state is a state for which P N is positive and an over-aged state is a state for which P N is negative.
  • T in Kelvin
  • T ref is a reference temperature fixed at 428 K.
  • t i is expressed in hours.
  • the tensile or compression yield stress can be used to determine whether aging makes it possible to reach a state close to the peak; the results are, however, not necessarily identical. Within the framework of the invention, it is preferred to use the values of compression yield stress to optimize aging.
  • the clearly under-aged states correspond to compromises between the static mechanical resistance (Rp 0.2 R m ) and damage tolerance (fracture toughness, resistance to spreading of fatigue cracks) of more interest than at the peak and, a fortiori, beyond the peak.
  • Rp 0.2 R m static mechanical resistance
  • damage tolerance fracture toughness, resistance to spreading of fatigue cracks
  • a temper essentially under-aged close to the peak of the compression yield i.e. a temper essentially under-aged with the conditions of time and temperature equivalent to those of a point N of the aging curve under compression at 155° C. such that the tangent to the aging curve at this point has a slope P N , expressed in MPa/h, such that ⁇ 1 ⁇ P N ⁇ 3 and preferably ⁇ 0.5 ⁇ P N ⁇ 2.3.
  • the flat-rolled products obtained by the process according to the invention have, for a thickness ranging between 8 and 50 mm, at mid-thickness at least one of the following combinations of characteristics:
  • Airplane structural elements according to the invention include products according to the invention.
  • a preferred airplane structural element is an upper wing skin.
  • the use of a structural element incorporating at least one product according to the invention or manufactured from such a product is advantageous, in particular for aeronautical engineering.
  • the products according to the invention are particularly advantageous for the production of airplane upper wing skins.
  • the slab was homogenized at about 500° C. for about 20 hours.
  • the slab was hot rolled at a temperature greater than 445° C. to obtain plates of thickness 25 mm.
  • the plates were solution heat treated at approximately 510° C., for 5 hours and quenched with water at 20° C.
  • the plates were then stretched with a permanent elongation ranging between 2% and 6%.
  • the plates underwent single-step aging of 40 hours at 155° C. for 2 and 3% stretching, 30 hours for 4% and 20 hours for 6%, this aging making it possible to attain a tensile yield stress and compression at the peak or close to the peak.
  • Samples were taken at mid-thickness to measure the static mechanical characteristics under stretching and compression, together with fracture toughness K Q .
  • the structure of the plates obtained was primarily unrecrystallized.
  • the unrecrystallized granular structure content at mid-thickness was 90%.
  • FIG. 2 presents the changes in tensile yield stress and compression as a function of permanent elongation during controlled stretching.
  • a favorable compromise is obtained between the compression yield stress and the tensile yield stress. So under these conditions, the compression yield stress is higher than the tensile yield stress, the tensile yield stress remaining higher than 620 MPa.
  • the slabs were homogenized by a two-step treatment of 8 hours at 500° C. followed by 12 hours at 510° C., then surface-machined. After homogenization, the slabs were hot rolled to obtain plates with a thickness of 9.4 mm, with intermediate reheating if the temperature decreased to less than 400° C. The plates were solution heat treated for 5 hours at approximately 510° C., quenched with cold water and stretched with a permanent elongation of 3%.
  • the structure of the plates obtained was primarily unrecrystallized.
  • the uncrystallized granular structure content at mid-thickness was 90%.
  • FIG. 3 illustrates the compromise obtained between the compression yield stress and fracture toughness K app .
  • the combination of the preferred composition (Alloy N° 3) with the process according to the invention gives, in particular for a 50-hour aging at 155° C., the most favorable aging from the point of view of thermal stability, a particularly favorable compromise between compression yield stress, tensile yield stress and fracture toughness.
  • the slab was homogenized at about 500° C. for about 30 hours.
  • the slab was hot rolled at a temperature greater than 400° C. to obtain plates of thickness 25 mm.
  • the plates were solution heat treated at approximately 510° C. for 5 hours and quenched with water at 20° C. The plates were then stretched with a permanent elongation of 2% or 3%.
  • the plates underwent single-step aging of 10 h to 30 h at 155° C. Samples were taken at mid-thickness to measure the static mechanical characteristics under stretching and compression, together with fracture toughness K Q .
  • the structure of the plates obtained was primarily unrecrystallized.
  • the unrecrystallized granular structure content at mid-thickness was higher than 90%.

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US13/328,872 2010-12-20 2011-12-16 Aluminum copper lithium alloy with improved resistance under compression and fracture toughness Abandoned US20120152415A1 (en)

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US201061424970P 2010-12-20 2010-12-20
FR1004962 2010-12-20
FR1004962A FR2969177B1 (fr) 2010-12-20 2010-12-20 Alliage aluminium cuivre lithium a resistance en compression et tenacite ameliorees
US13/328,872 US20120152415A1 (en) 2010-12-20 2011-12-16 Aluminum copper lithium alloy with improved resistance under compression and fracture toughness

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EP (1) EP2655680B1 (fr)
CN (2) CN108048717A (fr)
BR (1) BR112013015531B1 (fr)
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FR3080861B1 (fr) 2018-05-02 2021-03-19 Constellium Issoire Procede de fabrication d'un alliage aluminium cuivre lithium a resistance en compression et tenacite ameliorees
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FR3007423A1 (fr) * 2013-06-21 2014-12-26 Constellium France Element de structure extrados en alliage aluminium cuivre lithium
US11472532B2 (en) 2013-06-21 2022-10-18 Constellium Issoire Extrados structural element made from an aluminium copper lithium alloy
WO2015011346A1 (fr) * 2013-06-21 2015-01-29 Constellium France Elément de structure extrados en alliage aluminium cuivre lithium
EP3080317B1 (fr) 2013-12-13 2018-09-19 Constellium Issoire Produits en alliage d'aluminium - cuivre - lithium à propriétés en fatigue améliorées et procédé de sa productuion
US10689739B2 (en) 2013-12-13 2020-06-23 Constellium Issoire Aluminium-copper-lithium alloy products with improved fatigue properties
WO2015086921A3 (fr) * 2013-12-13 2015-08-20 Constellium France Produits en alliage d'aluminium - cuivre - lithium à propriétés en fatigue améliorées
RU2674789C1 (ru) * 2013-12-13 2018-12-13 Констеллиум Иссуар Изделия из алюминиево-медно-литиевого сплава с улучшенными усталостными свойствами
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FR3014905A1 (fr) * 2013-12-13 2015-06-19 Constellium France Produits en alliage d'aluminium-cuivre-lithium a proprietes en fatigue ameliorees
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RU2716722C2 (ru) * 2014-10-26 2020-03-16 КАЙЗЕР АЛЮМИНУМ ФАБРИКЕЙТЕД ПРОДАКТС, ЭлЭлСи Алюминиево-литиевые сплавы с высокой прочностью, высокой деформируемостью и низкой стоимостью
EP3384061B1 (fr) 2015-12-04 2020-02-05 Constellium Issoire Alliage aluminium cuivre lithium à resistance mécanique et tenacité ameliorées
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EP3526358B1 (fr) 2016-10-17 2020-07-22 Constellium Issoire Toles minces en alliage aluminium-magnesium-scandium pour applications aerospatiales
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US20200165707A1 (en) * 2017-06-06 2020-05-28 Constellium Issoire Aluminum alloy comprising lithium with improved fatigue properties
CN108570579A (zh) * 2018-04-11 2018-09-25 上海交通大学 一种含钪铸造铝锂合金及其制备方法
EP3788178B1 (fr) 2018-05-02 2022-08-17 Constellium Issoire Alliage aluminium cuivre lithium a resistance en compression et tenacite ameliorees
WO2021101485A3 (fr) * 2019-11-19 2021-07-29 Gazi Universitesi Procédé de traitement thermomécanique de renforcement de l'alliage aa7075-t651 pendant un traitement thermique rra
CN111020322A (zh) * 2019-12-10 2020-04-17 江苏豪然喷射成形合金有限公司 一种高强高韧航天用铝锂合金板材及制造方法
CN115433888A (zh) * 2022-08-18 2022-12-06 哈尔滨工业大学（深圳） 一种铝锂合金中厚板的形变热处理方法
CN117187642A (zh) * 2023-11-03 2023-12-08 中铝材料应用研究院有限公司 一种超高强高韧Al-Cu-Li-Mg-Zn-Mn-Zr合金板材及其制备方法和应用

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BR112013015531A2 (pt) 2017-05-09
CA2821663C (fr) 2018-10-30
WO2012085359A2 (fr) 2012-06-28
EP2655680A2 (fr) 2013-10-30
BR112013015531B1 (pt) 2018-09-18
CN108048717A (zh) 2018-05-18
DE11808899T1 (de) 2014-01-02
FR2969177B1 (fr) 2012-12-21
FR2969177A1 (fr) 2012-06-22

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