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EP1544316A2 - Thick sheet made of Al-Zn-Cu-Mg recrystallised alloy with low Zirconium content - Google Patents

Thick sheet made of Al-Zn-Cu-Mg recrystallised alloy with low Zirconium content Download PDF

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Publication number
EP1544316A2
EP1544316A2 EP04356197A EP04356197A EP1544316A2 EP 1544316 A2 EP1544316 A2 EP 1544316A2 EP 04356197 A EP04356197 A EP 04356197A EP 04356197 A EP04356197 A EP 04356197A EP 1544316 A2 EP1544316 A2 EP 1544316A2
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EP
European Patent Office
Prior art keywords
sheet
alloy
sheet according
mpa
low
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EP04356197A
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German (de)
French (fr)
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EP1544316B1 (en
EP1544316A3 (en
Inventor
David Dumont
Vic Dangerfield
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Constellium Issoire SAS
Constellium Rolled Products Ravenswood LLC
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Alcan Rhenalu SAS
Pechiney Rhenalu SAS
Pechiney Rolled Products LLC
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/10Alloys based on aluminium with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/053Changing 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 zinc as the next major constituent

Definitions

  • the present invention relates to sheet metal aluminum alloys of the Al-Zn-Cu-Mg type intended for manufacture of structural elements used in the aerospace industry.
  • patent EP 0 876 514 B1 describes a Thick Al-Zn-Cu-Mg alloy product with a fraction volume of recrystallized grains less than 35% between quarter and mid-thickness.
  • RPFF fatigue crack propagation
  • the present invention addresses the problem of knowing how to improve the resistance to the propagation of fatigue cracks in a thick alloy sheet Al-Zn-Cu-Mg.
  • a first object of the present invention is a thick sheet of Al-Zn-Cu-Mg alloy, comprising 0.04 to 0.09% by weight of Zr, said sheet having a from recrystallization greater than 35% to one quarter of thickness.
  • a second object is a manufacturing process a thick sheet of Al-Zn-Cu-Mg alloy comprising from 0.04 to 0.09% by weight of Zr, said process comprising hot rolling a blank of said sheet at a temperature of less than 420 ° C. This method makes it possible to obtain a sheet having a recrystallization greater than 35% to one quarter of thickness.
  • FIGS. 1 to 7 relate to certain aspects of the invention as described herein. They are purely illustrative and non-limiting.
  • Figure 1 shows the dimensions of specimens RPFF according to an embodiment of the present invention.
  • Figure 2 shows the test results of fatigue crack propagation (PFF) on a sheet of 856385) according to an embodiment of the present invention.
  • Figure 3 is a microscope characterization electronic scanning (SEM) of fracture surfaces of a reference material.
  • Figure 4 shows the results of PFF tests on a rolled sheet with an outlet temperature lower.
  • Figure 5 shows test results from PFF on a sheet with a lower Zr content.
  • Figure 6 shows a comparison of the path of the crack near the threshold for materials (a) and low Zr (b) according to a embodiment.
  • Figure 7 is a schematic representation of RPFF differences between reference materials and low Zr content according to one embodiment.
  • the fatigue strength is determined by a test according to ASTM E 466, and the fatigue crack growth rate (so-called da / dn test) according to ASTM E 647.
  • the curve R is determined according to ASTM standard 561. From the curve R, the critical stress intensity factor K c is calculated, ie the intensity factor which causes the instability of the crack.
  • the stress intensity factor K CO is also calculated by assigning to the critical load the initial length of the crack at the beginning of the monotonic loading. These two values are calculated for a specimen of the desired shape. K app designates the K CO corresponding to the specimen used to make the R curve test.
  • these structural elements include the elements that make up the fuselage (such as the fuselage skin (fuselage skin in English), stiffeners or fuselage stringers, the bulkheads (bulkheads), fuselage frames (circumferential frames), wings (such as the skin of wing (wing), stiffeners (stringers or stiffeners), ribs and spars) and the empennage composed in particular of stabilizers horizontal and vertical (horizontal or vertical stabilizers), as well as floor profiles (floor beams), seat tracks and doors.
  • fuselage such as the fuselage skin (fuselage skin in English), stiffeners or fuselage stringers, the bulkheads (bulkheads), fuselage frames (circumferential frames), wings (such as the skin of wing (wing), stiffeners (stringers or stiffeners), ribs and spars
  • the empennage composed in particular of stabilizers horizontal and vertical (horizontal or vertical stabilizers), as well as floor profiles (floor beams), seat tracks and doors.
  • the Zr content is between 0.05 and 0.07%.
  • Such an alloy can be cast in the form of a rolling plate, and can be processed according to the known processes in thick plates. These processes make always intervene at least one rolling pass at hot.
  • the sheet according to the invention is a strong plate (thick sheet), because the technical effect of the invention will be noticeable only for a sheet that is not completely recrystallized, whereas a thin sheet may be .
  • its thickness is at least 15 mm, and preferably at least 20 mm; its thickness can reach or exceed 100 mm.
  • the sheet according to the invention has a recrystallization rate at a quarter of the thickness (E / 4) greater than 35%, and preferably greater than 50%, but must not be completely recrystallized. As such, it is preferred that the recrystallization rate at E / 4 does not exceed 90%.
  • a sheet according to the invention in alloy according to one of the preferred embodiments (that is to say in alloy AA7040 or comprising from 5.8 to 6.8% of Zn, from 1.5 to 2.5% of Cu, from 1.5 to 2.5% Mg, from 0.04 to 0.09% of Zr) has a tenacity K IC (LT) > 30 MPa ⁇ m, and preferentially in addition a toughness K IC (TL ) > 25 MPa ⁇ m, and even more preferably in addition to these two previous values a toughness K IC (ST) > 25 MPa ⁇ m.
  • the sheet according to the invention can be manufactured by a process that includes hot rolling a roughing said sheet at a temperature which is less than 420 ° C. Then this sheet can be subjected to type T7651 treatment; this treatment includes an income.
  • the recrystallization rate itself has a low effect in areas near the threshold; the curves nominal values are slightly different because of a closure effect induced by the roughness, the path of the crack being more tortuous.
  • the recrystallized grains of the low-grade material Zr content are probably larger. It is suggested to laminate this material cold in order to obtain a microstructure comparable in terms of size of grain and then test its resistance to the fatigue crack propagation.
  • the sheets according to the invention can be used, especially in the form of thick plates, for the manufacture of structural elements for aeronautical construction.
  • the tests were performed with a cyclic load frequency of 35 Hz and a load ratio of 0.1.
  • the length of the fatigue cracks was continuously monitored using a compliance technique. It was also evaluated by optical observation of the surface of the test piece after polishing.
  • the fatigue crack propagation threshold stress intensity range, ⁇ K th is arbitrarily defined as the stress intensity coefficient range, ⁇ K, which corresponds to a fatigue crack propagation rate, da /. dN, 10 -10 m / cycle.
  • the tests were interrupted before the fracture in order to characterize the path of the rift.
  • the surface of the specimen is observed optically after acid attack (perpendicularly to the plan of propagation of the crack).
  • the surface morphologies after fracture were examined under a microscope scanning electronics. A correction due to the effect closure has been applied systematically in order to rationalize the observed differences.
  • Figure 2 shows the crack propagation of fatigue in the air through the reference material (% low recruits).
  • Figure 4 shows the crack propagation of fatigue (measured in the air) through a material rolled at a low rolling temperature (TL) (%) rec. high) in the L-T direction. This one was compared to the reference material (low recrystallization). All tests were conducted with a ratio of R load of 0.1.
  • This difference may be due to a roughness-induced closure effect in the ⁇ K range of 1.2 to 8 MPa m .
  • the path of the crack is more tortuous for the low Zr material (see Figure 6).
  • the fracture surfaces are mainly transgranular, as for the other two materials, and have a large amount of secondary cracks.
  • Figure 5 shows the crack propagation of fatigue in the air through the low material Zr content (% high recryst) in the L-T direction. Comparison with the reference material (% recrist. low). All tests were done with a ratio R load of 0.1.
  • Figure 6 shows a comparison of the path cracks near the threshold for materials reference (a) and low Zr (b) content. Samples tested in L-T orientation, at E / 4.
  • Figure 7 is a diagram of the differences of RPFF between reference materials and low Zr content. (Curve right: low material Zr content. Left curve: material of reference).

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Metal Rolling (AREA)
  • Heat Treatment Of Steel (AREA)
  • Conductive Materials (AREA)
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Abstract

The sheet of AlZnCuMg alloy also contains zirconium, with its components having the following percentage weights: Zn 5.8 - 6.8; Cu 1.5 - 2.5; Mg 1.5 - 2.5; and Zr 0.04 - 0.09; and aluminum and minor impurities the remainder. The sheet, which can be made with higher zirconium contents and in thicknesses up to at least 16 mm, is produced by hot laminating a blank at a temperature below 420 degrees C.

Description

DOMAINE DE L'INVENTIONFIELD OF THE INVENTION

La présente invention concerne les tôles en alliages d'aluminium de type Al-Zn-Cu-Mg destinées à la fabrication d'éléments de structure utilisés dans l'industrie aéronautique ou spatiale.The present invention relates to sheet metal aluminum alloys of the Al-Zn-Cu-Mg type intended for manufacture of structural elements used in the aerospace industry.

ETAT DE LA TECHNIQUESTATE OF THE ART

Des travaux considérables ont été menés au cours des dernières décennies en vue d'améliorer les propriétés des alliages de la série 7xxx, et plus particulièrement leur compromis résistance / ténacité. A titre d'exemple, le brevet EP 0 876 514 B1 décrit un produit épais en alliage Al-Zn-Cu-Mg avec une fraction volumique de grains recristallisés inférieure à 35% entre le quart et la mi-épaisseur. Toutefois, les relations de la microstructure avec leur résistance à la propagation des fissures de fatigue (RPFF) restent à éclaircir.Considerable work has been done during recent decades in order to improve the properties of 7xxx series alloys, and more especially their resistance / toughness compromise. By way of example, patent EP 0 876 514 B1 describes a Thick Al-Zn-Cu-Mg alloy product with a fraction volume of recrystallized grains less than 35% between quarter and mid-thickness. However, relationships of microstructure with their resistance to fatigue crack propagation (RPFF) remain at lighten.

La présente invention aborde de problème de savoir comment améliorer la résistance à la propagation de fissures de fatigue dans une tôle épaisse en alliage Al-Zn-Cu-Mg.The present invention addresses the problem of knowing how to improve the resistance to the propagation of fatigue cracks in a thick alloy sheet Al-Zn-Cu-Mg.

OBJETS DE L'INVENTIONOBJECTS OF THE INVENTION

Un premier objet de la présente invention est une tôle épaisse en alliage Al-Zn-Cu-Mg, comprenant de 0,04 à 0,09% en poids de Zr, ladite tôle présentant un taux de recristallisation supérieur à 35% à un au quart de l'épaisseur.A first object of the present invention is a thick sheet of Al-Zn-Cu-Mg alloy, comprising 0.04 to 0.09% by weight of Zr, said sheet having a from recrystallization greater than 35% to one quarter of thickness.

Un deuxième objet est un procédé de fabrication d'une tôle épaisse en alliage Al-Zn-Cu-Mg, comprenant de 0,04 à 0,09% en poids de Zr, ledit procédé comprenant le laminage à chaud d'une ébauche de ladite tôle à une température qui est inférieure à 420°C. Ce procédé permet d'obtenir une tôle présentant un taux de recristallisation supérieur à 35% à un au quart de l'épaisseur.A second object is a manufacturing process a thick sheet of Al-Zn-Cu-Mg alloy comprising from 0.04 to 0.09% by weight of Zr, said process comprising hot rolling a blank of said sheet at a temperature of less than 420 ° C. This method makes it possible to obtain a sheet having a recrystallization greater than 35% to one quarter of thickness.

BREVE DESCRIPTION DES FIGURESBRIEF DESCRIPTION OF THE FIGURES

Les figures illustrent un mode de réalisation actuellement préféré de l'invention et, ensemble avec la description générale donnée ci-dessus et la description détaillée du mode de réalisation préféré donnée ci-après, ils servent à expliquer les principes de l'invention.The figures illustrate an embodiment currently preferred of the invention and together with the general description given above and the detailed description of the preferred embodiment given below, they serve to explain the principles of the invention.

Les figures 1 à 7 concernent certains aspects de l'invention telle qu'elle est décrite ici. Elles sont purement illustratives et non limitatives.Figures 1 to 7 relate to certain aspects of the invention as described herein. They are purely illustrative and non-limiting.

La figure 1 montre les dimensions d'éprouvettes RPFF selon un mode de réalisation de la présente invention.Figure 1 shows the dimensions of specimens RPFF according to an embodiment of the present invention.

La figure 2 montre les résultats d'essais de propagation de fissure de fatigue (PFF) sur une tôle de référence (n° 856385) selon un mode de réalisation de la présente invention.Figure 2 shows the test results of fatigue crack propagation (PFF) on a sheet of 856385) according to an embodiment of the present invention.

La figure 3 est une caractérisation au microscope électronique à balayage (MEB) de surfaces de fracture d'un matériau de référence. Figure 3 is a microscope characterization electronic scanning (SEM) of fracture surfaces of a reference material.

La figure 4 montre les résultats d'essais de PFF sur une tôle laminée avec une température de sortie plus basse.Figure 4 shows the results of PFF tests on a rolled sheet with an outlet temperature lower.

La figure 5 montre des résultats d'essais de PFF sur une tôle avec une teneur en Zr plus faible.Figure 5 shows test results from PFF on a sheet with a lower Zr content.

La figure 6 montre une comparaison du cheminement de la fissure au voisinage du seuil pour des matériaux de référence (a) et à faible teneur en Zr (b) selon un mode de réalisation.Figure 6 shows a comparison of the path of the crack near the threshold for materials (a) and low Zr (b) according to a embodiment.

La figure 7 est une représentation schématique des différences de RPFF entre les matériaux de référence et à faible teneur en Zr selon un mode de réalisation.Figure 7 is a schematic representation of RPFF differences between reference materials and low Zr content according to one embodiment.

TERMINOLOGIETERMINOLOGY

Sauf mention contraire, toutes les indications relatives à la composition chimique des alliages sont exprimées en pourcent massique. La désignation des alliages suit les règles de The Aluminum Association, connues de l'homme du métier. Les états métallurgiques sont définis dans la norme européenne EN 515. La composition chimique d'alliages d'aluminium normalisés est définie par exemple dans la norme EN 573-3. Sauf mention contraire, les caractéristiques mécaniques statiques, c'est-à-dire la résistance à la rupture Rm, la limite élastique Rp0,2, et l'allongement à la rupture A, sont déterminées par un essai de traction selon la norme EN 10002-1, l'endroit et le sens du prélèvement des éprouvettes étant définis dans la norme EN 485-1. La résistance à la fatigue est déterminée par un essai selon ASTM E 466, et la vitesse de propagation de fissures en fatigue (essai dit da/dn) selon ASTM E 647. La courbe R est déterminée selon la norme ASTM 561. A partir de la courbe R, on calcule le facteur d'intensité de contrainte critique Kc , c'est à dire le facteur d'intensité qui provoque l'instabilité de la fissure. On calcule également le facteur d'intensité de contrainte KCO, en affectant à la charge critique la longueur initiale de la fissure, au début du chargement monotone. Ces deux valeurs sont calculées pour une éprouvette de forme voulue. Kapp désigne le KCO correspondant à l'éprouvette ayant servi à faire le test de courbe R.Unless stated otherwise, all the information relating to the chemical composition of the alloys is expressed in percent by weight. The designation of the alloys follows the rules of The Aluminum Association, known to those skilled in the art. The metallurgical states are defined in the European standard EN 515. The chemical composition of standardized aluminum alloys is defined for example in the standard EN 573-3. Unless otherwise stated, the static mechanical characteristics, ie the breaking strength R m , the yield stress R p0,2 , and the elongation at break A, are determined by a tensile test according to EN 10002-1 standard, the location and direction of specimen collection being defined in EN 485-1. The fatigue strength is determined by a test according to ASTM E 466, and the fatigue crack growth rate (so-called da / dn test) according to ASTM E 647. The curve R is determined according to ASTM standard 561. From the curve R, the critical stress intensity factor K c is calculated, ie the intensity factor which causes the instability of the crack. The stress intensity factor K CO is also calculated by assigning to the critical load the initial length of the crack at the beginning of the monotonic loading. These two values are calculated for a specimen of the desired shape. K app designates the K CO corresponding to the specimen used to make the R curve test.

Sauf mention contraire, les définitions de la norme européenne EN 12258-1 s'appliquent. Cette norme définit notamment une tôle épaisse (ou tôle forte) comme une tôle ayant une épaisseur supérieure à 6 mm. E désigne ici l'épaisseur des tôles.Unless otherwise specified, the definitions of the standard European standard EN 12258-1 apply. This standard defines especially a thick plate (or strong plate) as a sheet having a thickness greater than 6 mm. E designates here the thickness of the sheets.

On appelle ici « élément de structure » ou « élément structural » d'une construction mécanique une pièce mécanique dont la défaillance est susceptible de mettre en danger la sécurité de ladite construction, de ses utilisateurs, des 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.Here we call "element of structure" or "element structural "of a one-piece mechanical mechanically whose failure is likely to endanger the security of the said construction, its users, its users or others. For a airplane, these structural elements include the elements that make up the fuselage (such as the fuselage skin (fuselage skin in English), stiffeners or fuselage stringers, the bulkheads (bulkheads), fuselage frames (circumferential frames), wings (such as the skin of wing (wing), stiffeners (stringers or stiffeners), ribs and spars) and the empennage composed in particular of stabilizers horizontal and vertical (horizontal or vertical stabilizers), as well as floor profiles (floor beams), seat tracks and doors.

DESCRIPTION DETAILLEEDETAILED DESCRIPTION

La présente invention peut s'appliquer aux alliages de type Al-Zn-Cu-Mg, c'est-à-dire aux alliages d'aluminium qui comprennent les éléments d'alliage Zn, Cu et Mg, et notamment aux alliages de type Al-Zn-Cu-Mg de la série 7xxx, et de préférence aux alliages comprenant (en % en poids) :

  • de 5,8 à 6,8% de Zn
  • de 1,5 à 2,5% de Cu
  • de 1,5 à 2,5% de Mg
  • de 0,04 à 0,09% de Zr
  • le reste étant de l'aluminium et des impuretés mineures, avec, de préférence, une teneur résiduelle en fer inférieure à 0,09%, et une teneur résiduelle en silicium inférieure à 0,07%. Un autre alliage auquel la présente invention peut être appliquée avantageusement est l'alliage AA7040.
  • The present invention can be applied to alloys of the Al-Zn-Cu-Mg type, that is to say to aluminum alloys which comprise the alloy elements Zn, Cu and Mg, and in particular to alloys of the type Al-Zn-Cu-Mg of the 7xxx series, and preferably to alloys comprising (in% by weight):
  • from 5.8 to 6.8% of Zn
  • 1.5 to 2.5% Cu
  • 1.5 to 2.5% Mg
  • from 0.04 to 0.09% of Zr
  • the balance being aluminum and minor impurities, preferably with a residual iron content of less than 0.09%, and a residual silicon content of less than 0.07%. Another alloy to which the present invention can be advantageously applied is AA7040 alloy.
  • Dans une réalisation préférée, la teneur en Zr est comprise entre 0,05 à 0,07%.In a preferred embodiment, the Zr content is between 0.05 and 0.07%.

    Un tel alliage peut être coulé sous forme d'une plaque de laminage, et peut être transformé selon les procédés connus en tôles épaisses. Ces procédés font toujours intervenir au moins une passe de laminage à chaud.Such an alloy can be cast in the form of a rolling plate, and can be processed according to the known processes in thick plates. These processes make always intervene at least one rolling pass at hot.

    La tôle selon l'invention est une tôle forte (tôle épaisse), car l'effet technique de l'invention ne sera perceptible que pour une tôle qui n'est pas complètement recristallisée, alors qu'une tôle mince risque de l'être. Avantageusement, son épaisseur est d'au moins 15 mm, et préférentiellement d'au moins 20 mm ; son épaisseur peut atteindre ou dépasser 100 mm. La tôle selon l'invention présente un taux de recristallisation au quart de l'épaisseur (E/4) supérieur à 35%, et préférentiellement supérieur à 50%, mais ne doit pas être totalement recristallisée. A ce titre, on préfère que le taux de recristallisation à E/4 ne dépasse pas 90%. La vitesse de propagation des fissures de fatigue dans une tôle selon l'invention est inférieure à 10-4 mm/cycle à ΔK = 10 MPa m pour un essai effectué à R = 0,1 dans le sens L-T à l'endroit E/4.The sheet according to the invention is a strong plate (thick sheet), because the technical effect of the invention will be noticeable only for a sheet that is not completely recrystallized, whereas a thin sheet may be . Advantageously, its thickness is at least 15 mm, and preferably at least 20 mm; its thickness can reach or exceed 100 mm. The sheet according to the invention has a recrystallization rate at a quarter of the thickness (E / 4) greater than 35%, and preferably greater than 50%, but must not be completely recrystallized. As such, it is preferred that the recrystallization rate at E / 4 does not exceed 90%. The speed of propagation of the fatigue cracks in a sheet according to the invention is less than 10 -4 mm / cycle at ΔK = 10 MPa m for a test performed at R = 0,1 in the LT direction at the E / 4 location.

    Une tôle selon l'invention en alliage selon un des mode de réalisation préférentiels (c'est-à-dire en alliage AA7040 ou comportant de 5,8 à 6,8% de Zn, de 1,5 à 2,5% de Cu, de 1,5 à 2,5% de Mg, de 0,04 à 0,09% de Zr) a une ténacité KIC(L-T) > 30 MPa√m, et préférentiellement en plus une ténacité KIC(T-L) > 25 MPa√m, et encore plus préférentiellement en plus de ces deux valeurs précédentes une ténacité KIC(S-T) > 25 MPa√m.A sheet according to the invention in alloy according to one of the preferred embodiments (that is to say in alloy AA7040 or comprising from 5.8 to 6.8% of Zn, from 1.5 to 2.5% of Cu, from 1.5 to 2.5% Mg, from 0.04 to 0.09% of Zr) has a tenacity K IC (LT) > 30 MPa√m, and preferentially in addition a toughness K IC (TL ) > 25 MPa√m, and even more preferably in addition to these two previous values a toughness K IC (ST) > 25 MPa√m.

    La tôle selon l'invention peut être fabriquée par un procédé qui comprend le laminage à chaud d'une ébauche de ladite tôle à une température qui est inférieure à 420°C. Ensuite, cette tôle peut être soumise à un traitement de type T7651 ; ce traitement comprend un revenu. The sheet according to the invention can be manufactured by a process that includes hot rolling a roughing said sheet at a temperature which is less than 420 ° C. Then this sheet can be subjected to type T7651 treatment; this treatment includes an income.

    Dans le cadre de la présente invention, un matériau de référence en alliage AA7040 présentant un taux de recristallisation de 20% a été comparé à deux autres matériaux hautement recristallisés (60%) :

    • Tôle laminée à une température plus basse, inférieure à 420°C, de préférence allant de 300°C à 419°C, de façon plus préférentielle allant de 305°C à 350°C et dans certains cas d'environ 315°C.
    • Tôle avec une teneur en Zr plus faible : 0,06 au lieu de 0,11% en poids.
    In the context of the present invention, an AA7040 alloy reference material having a recrystallization rate of 20% has been compared to two other highly recrystallized materials (60%):
    • Sheet rolled at a lower temperature, below 420 ° C, preferably from 300 ° C to 419 ° C, more preferably from 305 ° C to 350 ° C and in some cases about 315 ° C.
    • Sheet with a lower Zr content: 0.06 instead of 0.11% by weight.

    Le taux de recristallisation lui-même a un faible effet dans les régions voisines du seuil ; les courbes nominales sont légèrement différentes à cause d'un effet de fermeture induit par la rugosité, le cheminement de la fissure étant plus tortueux.The recrystallization rate itself has a low effect in areas near the threshold; the curves nominal values are slightly different because of a closure effect induced by the roughness, the path of the crack being more tortuous.

    En outre, une différence intéressante a été observée par les présents inventeurs lors de la comparaison du matériau de référence et de matériaux à faible teneur en Zr. Ces derniers présentent des taux de propagation de fissures significativement moindres sur une plage de ΔK étendue : de 8 à 20 MPa m , où aucun effet de fermeture n'est observé. Cette différence pourrait être due à un effet intrinsèque de la microstructure du matériau à faible teneur en Zr. Ce comportement est schématisé sur la figure 7.In addition, an interesting difference has been observed by the present inventors in comparison of the reference material and low Zr materials. The latter have significantly lower crack propagation rates over an extended ΔK range: from 8 to 20 MPa m , where no closing effect is observed. This difference could be due to an intrinsic effect of the microstructure of the low Zr material. This behavior is shown schematically in Figure 7.

    Les grains recristallisés du matériau à faible teneur en Zr sont probablement plus grands. Il est suggéré de laminer ce matériau à froid afin d'obtenir une microstructure comparable en termes de taille de grain et ensuite de tester sa résistance à la propagation de fissure de fatigue. The recrystallized grains of the low-grade material Zr content are probably larger. It is suggested to laminate this material cold in order to obtain a microstructure comparable in terms of size of grain and then test its resistance to the fatigue crack propagation.

    Les tôles selon l'invention peuvent être utilisées, notamment sous forme de tôles épaisses, pour la fabrication d'éléments de structure pour construction aéronautique.The sheets according to the invention can be used, especially in the form of thick plates, for the manufacture of structural elements for aeronautical construction.

    La présente invention est illustrée par les exemples qui suivent. Ils ne limitent pas la présente invention.The present invention is illustrated by the examples that follow. They do not limit this invention.

    EXEMPLESEXAMPLES 1)Procédure expérimentale1) Experimental procedure A) MatériauA) Material

    Toutes les éprouvettes ont été prélevées dans des tôles d'alliage 7040 de 100 mm d'épaisseur qui ont été transformées sur un équipement industriel. Les numéros de chaque tôle et leur composition chimique correspondante sont indiqués dans le tableau 1, leurs propriétés mécaniques dans le tableau 2 et leurs taux de recristallisation et leurs conditions de transformation dans le tableau 3 : Composition chimique Tôle n° Si Fe Cu Mg Zn Ti Zr 856385 0,035 0,072 1,72 1,89 6,37 0,039 0,111 859188 0,029 0,059 1,59 1,87 6,39 0,021 0,060 859198 0,031 0,063 1,60 1,91 6,36 0,038 0,113 Propriétés mécaniques KIC [MPa m ] Rés. à la traction [MPa] Tôle n° L-T T-L S-L L LT ST 856385 28,8 24,2 26,9 506 501 490 859188 31,6 26,6 26,8 508 504 475 859198 28,3 25,1 25,8 492 492 466 Taux de recristallisation et caractéristiques de transformation Matériau Tôle n° % recrist. Principales caractéristiques E/4 E/2 % recrist. faible (référence) 856385 20% 17% Température de laminage typique (sortie environ 430°C) et taux de Zr typique 0,11% % recrist. élevé 859198 60% 55% Température de sortie de laminage plus basse : 315°C, Zr typique 859188 60% 58% Teneur en Zr moindre : 0,06%, température de laminage typique (sortie à environ 455°C) All the samples were taken from 7040 alloy sheets 100 mm thick which were processed on industrial equipment. The numbers of each sheet and their corresponding chemical composition are shown in Table 1, their mechanical properties in Table 2 and their recrystallization rates and their transformation conditions in Table 3: Chemical composition Sheet no. Yes Fe Cu mg Zn Ti Zr 856385 0,035 0,072 1.72 1.89 6.37 0,039 0.111 859188 0,029 0.059 1.59 1.87 6.39 0,021 0,060 859198 0.031 0.063 1.60 1.91 6.36 0,038 0.113 Mechanical properties K IC [MPa m ] Res. with traction [MPa] Sheet no. LT TL SL The LT ST 856385 28.8 24.2 26.9 506 501 490 859188 31.6 26.6 26.8 508 504 475 859198 28.3 25.1 25.8 492 492 466 Recrystallization rate and transformation characteristics Material Sheet no. % recrist. Main characteristics E / 4 E / 2 % recrist. low (reference) 856385 20% 17% Typical rolling temperature (output about 430 ° C) and typical Zr rate 0.11% % recrist. Student 859198 60% 55% Lower rolling output temperature: 315 ° C, typical Zr 859188 60% 58% Lower Zr content: 0.06%, typical rolling temperature (output at about 455 ° C)

    Les taux de recristallisation (% recrist.) ont été mesurés par analyse d'images sur des micrographies. La tôle n° 856385 était représentative d'une production industrielle courante et elle peut généralement être considérée comme étant une référence : chimie et transformation standard. Dans le but d'étudier l'influence du taux de recristallisation sur la RPFF, la tôle 856385 a été comparée avec deux autres plaques dont les pourcentages de recristallisation sont significativement plus élevés :

    • La tôle n° 859198 a été laminée à une température plus basse. Ce laminage modifié s'est traduit par une énergie accumulée plus élevée et donc a favorisé une recristallisation plus marquée au cours du traitement thermique en solution ultérieur ;
    • La tôle n° 859188 avait une plus faible teneur en zirconium et donc une quantité de dispersoïdes plus faible pour inhiber la cristallisation par ancrage aux limites de grains.
    Recrystallization rates (% recrist) were measured by image analysis on micrographs. Sheet No. 856385 was representative of current industrial production and can generally be considered as a reference: standard chemistry and processing. In order to study the influence of the recrystallization rate on the RPFF, the 856385 sheet was compared with two other plates whose recrystallization percentages are significantly higher:
    • Sheet No. 859198 was rolled at a lower temperature. This modified lamination resulted in a higher accumulated energy and thus favored a more marked recrystallization during the heat treatment in the subsequent solution;
    • Sheet No. 859188 had a lower zirconium content and thus a lower amount of dispersoid to inhibit grain boundary anchoring crystallization.

    Tous les échantillons ont été testés dans le revenu T7651. Les trois tôles ont des propriétés mécaniques statiques et des propriétés de ténacité comparables. En outre, les taux de recristallisation ont été déterminés par analyse d'images avec le logiciel Imagetool™. Les mesures micrographiques ont été effectuées dans les plans L-ST après attaque à l'acide chromique. La précision de cette caractérisation est voisine de 2%.All samples were tested in the T7651 income. The three sheets have properties static mechanics and toughness properties comparable. In addition, recrystallization rates were determined by image analysis with the Imagetool ™ software. Micrographic measurements have were made in the L-ST plans after attack at chromic acid. The precision of this characterization is close to 2%.

    B) Caractérisation mécaniqueB) Mechanical characterization

    Une caractérisation des caractéristiques mécaniques statiques (Rp0.2, Rm, A) et de la ténacité a été effectuée. Des mesures du taux de propagation de fissure de fatigue (RPFF) ont été effectuées dans l'air suivant ASTM E647, dont le protocole est incorporé dans son entièreté aux présentes à titre de référence, avec des éprouvettes CT50 (voir la figure 1). Ces essais ont été réalisés dans les orientations L-T et T-L pour les trois matériaux, les éprouvettes étant prélevées à E/4. Le matériau de référence a été testé également à E/2 dans l'orientation L-T.A characterization of the static mechanical characteristics (R p0.2 , R m , A) and toughness was performed. Fatigue crack propagation rate (RPFF) measurements were made in the air according to ASTM E647, the protocol of which is incorporated in its entirety herein by reference, with CT50 specimens (see FIG. 1). These tests were carried out in the LT and TL orientations for the three materials, the specimens being taken at E / 4. The reference material was also tested at E / 2 in the LT orientation.

    Les tests ont été réalisés avec une fréquence de charge cyclique de 35 Hz et un ratio de charge de 0,1. La longueur des fissures de fatigue a été contrôlée en continu en utilisant une technique de compliance. Elle a également été évaluée par une observation optique de la surface de l'éprouvette après un polissage. La plage d'intensité de contrainte de seuil de propagation de fissure de fatigue, ΔKth, est définie arbitrairement comme étant la plage de coefficient d'intensité de contrainte, ΔK, qui correspond à un taux de propagation de fissure de fatigue, da/dN, de 10-10 m/cycle. The tests were performed with a cyclic load frequency of 35 Hz and a load ratio of 0.1. The length of the fatigue cracks was continuously monitored using a compliance technique. It was also evaluated by optical observation of the surface of the test piece after polishing. The fatigue crack propagation threshold stress intensity range, ΔK th , is arbitrarily defined as the stress intensity coefficient range, ΔK, which corresponds to a fatigue crack propagation rate, da /. dN, 10 -10 m / cycle.

    Les tests ont été interrompus avant la fracture finale afin de caractériser le cheminement de la fissure. Pour cela, la surface de l'éprouvette est observée optiquement après attaque acide (perpendiculairement au plan de propagation de la fissure). Après les essais de PFF, les morphologies de surface après fracture ont été examinées au microscope électronique à balayage. Une correction due à l'effet de fermeture a été appliquée systématiquement afin de rationaliser les différences observées.The tests were interrupted before the fracture in order to characterize the path of the rift. For this, the surface of the specimen is observed optically after acid attack (perpendicularly to the plan of propagation of the crack). After the PFF tests, the surface morphologies after fracture were examined under a microscope scanning electronics. A correction due to the effect closure has been applied systematically in order to rationalize the observed differences.

    2) Résultats2) Results A) Matériau de référenceA) Reference material

    La figure 2 montre la propagation de fissure de fatigue dans l'air à travers le matériau de référence (% recrist. faible). (a) Influence de l'emplacement de l'échantillon (E/2 par rapport à E/4), (b) Influence de l'orientation de l'échantillon (L-T par rapport à T-L), les courbes marquées "effectives" tiennent compte de la correction de l'effet de fermeture. Tous les essais ont été réalisés avec un ratio de charge R de 0,1.Figure 2 shows the crack propagation of fatigue in the air through the reference material (% low recruits). (a) Influence of the location of the sample (E / 2 with respect to E / 4), (b) Influence of the orientation of the sample (L-T with respect to T-L), the marked "effective" curves take into account the correction of the closing effect. All tests have were made with a load ratio R of 0.1.

    Aucun effet significatif de l'orientation ou de l'emplacement de l'échantillon n'a été observé sur la figure 2. A l'échelle macroscopique, le cheminement de la fissure semble être très régulier et peu tortueux dans les trois cas. Les surfaces de fracture présentent des comportements comparables (voir la figure 3) : la fracture a un cheminement principalement trans-granulaire avec un grand nombre de facettes. Certaines décohésions de constituants intermétalliques grossiers et de limites de grains ont également été observées. Les cheminements des fissures dans les régions voisines du seuil étaient en outre plus plats, avec des facettes plus grandes.No significant effect of orientation or the location of the sample was observed on the Figure 2. At the macroscopic scale, the path of the crack seems to be very regular and not very tortuous in all three cases. Fracture surfaces present comparable behaviors (see Figure 3): fracture has a predominantly trans-granular path with a lot of facets. Some decohesions of coarse intermetallic constituents and grain boundaries were also observed. Crack paths in neighboring regions the threshold were also flatter, with facets bigger.

    Voir la figure 3, qui montre la caractérisation au MEB de surfaces de fracture du matériau de référence, testé dans le sens L-T à E/4 (ΔK = 6 MPa√m, da/dN = 1,6 · 10-8 m/cycle).See Figure 3, which shows the SEM characterization of fracture surfaces of the reference material, tested in the LT to E / 4 direction (ΔK = 6 MPa√m, da / dN = 1.6 · 10 -8 m / h). cycle).

    B) Matériau laminé à basse températureB) Low temperature laminated material

    La figure 4 montre la propagation de fissure de fatigue (mesurée dans l'air) à travers un matériau laminé à une température de laminage (TL) faible (% recrist. élevé) dans le sens L-T. Celui-ci a été comparé au matériau de référence (% recrist. faible). Tous les essais ont été réalisés avec un ratio de charge R de 0,1.Figure 4 shows the crack propagation of fatigue (measured in the air) through a material rolled at a low rolling temperature (TL) (%) rec. high) in the L-T direction. This one was compared to the reference material (low recrystallization). All tests were conducted with a ratio of R load of 0.1.

    Une légère différence a été observée en comparant les courbes nominales des matériaux de référence et à TL faible dans la région voisine du seuil. Cette différence a disparu avec la prise en compte de la correction de fermeture (voir les courbes « effectives » sur la figure 4). Nous pouvons donc expliquer la légère différence nominale par un effet de fermeture induit par la rugosité (cheminement plus tortueux de la fissure).A slight difference was observed when comparing the nominal curves of the reference materials and to Low TL in the region near the threshold. This difference disappeared with the consideration of the closing correction (see the curves "Effective" in Figure 4). We can therefore explain the slight nominal difference by an effect of Closure induced by roughness (more tortuous crack).

    C) Matériau à faible teneur en ZrC) Low Zr material

    Les résultats des essais de PFF sur la plaque ayant une plus faible teneur en Zr sont présentés sur la figure 5. Les taux de propagation de fissures sont plus faibles, comparés à ceux du matériau de référence, dans une plage de ΔK étendue : 4 à 20 MPa√m.The results of the PFF tests on the plate having a lower Zr content are shown on Figure 5. Crack propagation rates are lower, compared to those of the reference material, in a range of ΔK extended: 4 to 20 MPa√m.

    Cette différence peut vraisemblablement être due à un effet de fermeture induit par la rugosité dans la plage de ΔK de 1,2 à 8 MPa m . En effet, le cheminement de la fissure est plus tortueux pour le matériau à faible teneur en Zr (voir la figure 6). Les surfaces de fracture sont principalement transgranulaires, comme pour les deux autres matériaux, et présentent une grande quantité de fissures secondaires.This difference may be due to a roughness-induced closure effect in the ΔK range of 1.2 to 8 MPa m . Indeed, the path of the crack is more tortuous for the low Zr material (see Figure 6). The fracture surfaces are mainly transgranular, as for the other two materials, and have a large amount of secondary cracks.

    Toutefois, aucun effet de fermeture n'est mis en évidence dans la plage de ΔK de 8 à 20 MPa m : les courbes nominales et « effectives » se superposent. Ceci tend à montrer que la différence par rapport au matériau de référence dans cette plage de ΔK est due à un effet intrinsèque de la microstructure du matériau à faible teneur en Zr. Une schématisation de ce comportement est présentée sur la figure 7.However, no closure effect is demonstrated in the ΔK range of 8 to 20 MPa m : the nominal and "effective" curves are superimposed. This tends to show that the difference from the reference material in this ΔK range is due to an intrinsic effect of the microstructure of the low Zr material. A schematization of this behavior is presented in Figure 7.

    Un comportement comparable est observé dans l'orientation T-L. Les différences sont toutefois plus petites.Comparable behavior is observed in T-L orientation. The differences are however more small.

    La figure 5 montre la propagation de fissure de fatigue dans l'air à travers le matériau à faible teneur en Zr (% recrist. élevé) dans le sens L-T. Comparaison avec le matériau de référence (% recrist. faible). Tous les essais ont été réalisés avec un ratio de charge R de 0,1.Figure 5 shows the crack propagation of fatigue in the air through the low material Zr content (% high recryst) in the L-T direction. Comparison with the reference material (% recrist. low). All tests were done with a ratio R load of 0.1.

    La figure 6 montre une comparaison du cheminement des fissures au voisinage du seuil pour les matériaux de référence (a) et à faible teneur en Zr (b). Echantillons testés dans l'orientation L-T, à E/4.Figure 6 shows a comparison of the path cracks near the threshold for materials reference (a) and low Zr (b) content. Samples tested in L-T orientation, at E / 4.

    La figure 7 est une schématisation des différences de RPFF entre les matériaux de référence et à faible teneur en Zr. (Courbe de droite : matériau à faible teneur en Zr. Courbe de gauche : matériau de référence).Figure 7 is a diagram of the differences of RPFF between reference materials and low Zr content. (Curve right: low material Zr content. Left curve: material of reference).

    La présente invention permet entre autres de comprendre les effets du taux de recristallisation sur la résistance à la propagation des fissures de fatigue, dans le cas particulier de l'alliage 7040. Pour cela, un matériau de référence ayant un taux de recristallisation de 20% a été comparé avec deux autres matériaux hautement recristallisés (60%). Les matériaux ont été traités comme suit :

  • · Plaque laminée à une température plus basse, soit environ 315°C au lieu de 420°C,
  • · Plaque avec une teneur en Zr plus faible : 0,06 au lieu de 0,11% en poids.
  • The present invention makes it possible, inter alia, to understand the effects of the recrystallization rate on the resistance to the propagation of fatigue cracks, in the particular case of alloy 7040. For this purpose, a reference material having a recrystallization rate of 20% has been compared with two other highly recrystallized materials (60%). The materials were treated as follows:
  • · Plate rolled at a lower temperature, about 315 ° C instead of 420 ° C,
  • · Plate with a lower Zr content: 0.06 instead of 0.11% by weight.
  • On peut conclure en premier lieu que le taux de recristallisation lui-même a un effet minime dans les régions voisines du seuil : les courbes nominales sont légèrement différentes à cause d'un effet de fermeture induit par la rugosité. Le cheminement de la fissure est en effet plus tortueux.It can first be concluded that the rate of recrystallization itself has a minimal effect in regions close to the threshold: the nominal curves are slightly different due to a closing effect induced by roughness. The path of the crack is indeed more tortuous.

    En outre, une différence intéressante a été mise en évidence en comparant un matériau de référence et un matériau à faible teneur en Zr. Ce dernier présente un taux de propagation de fissure significativement moindre sur une plage de ΔK étendue : de 8 à 20 MPa m où aucun effet de fermeture n'est observé. Cette différence pourrait être due à un effet intrinsèque de la microstructure du matériau à faible teneur en Zr.In addition, an interesting difference has been demonstrated by comparing a reference material and a low Zr material. The latter has a significantly lower crack propagation rate over an extended ΔK range: from 8 to 20 MPa m where no closing effect is observed. This difference could be due to an intrinsic effect of the microstructure of the low Zr material.

    Claims (12)

    Tôle d'épaisseur supérieure à 6 mm en alliage Al-Zn-Cu-Mg, comprenant de 0,04 à 0,09% en poids de Zr, ladite tôle présentant un taux de recristallisation supérieur à 35% au quart de l'épaisseur.Sheet of thickness greater than 6 mm alloy Al-Zn-Cu-Mg, comprising from 0.04 to 0.09% by weight of Zr, said sheet having a recrystallization rate greater than 35% to one quarter of the thickness. Tôle selon la revendication 1, comprenant (en % en poids) : de 5,8 à 6,8% de Zn de 1,5 à 2,5% de Cu de 1,5 à 2,5% de Mg de 0,04 à 0,09% de Zr le reste étant de l'aluminium et des impuretés mineures.Sheet according to claim 1, comprising (in% by weight): from 5.8 to 6.8% of Zn 1.5 to 2.5% Cu 1.5 to 2.5% Mg from 0.04 to 0.09% of Zr the rest being aluminum and minor impurities. Tôle selon la revendication 1, caractérisée en ce qu'elle est en alliage AA7040.Sheet according to Claim 1, characterized in that it is made of AA7040 alloy. Tôle selon l'une quelconque des revendications 1 à 3, dans laquelle le Zr est présent en une quantité comprise entre 0,05 à 0,07% en poids.Sheet according to any one of the claims 1 to 3, wherein the Zr is present in a quantity from 0.05 to 0.07% by weight. Tôle selon l'une quelconque des revendications 1 à 4, présentant un taux de recristallisation supérieur à 50% au quart de l'épaisseur.Sheet according to any one of the claims 1 to 4, having a recrystallization rate greater than 50% to one quarter of the thickness. Tôle selon l'une quelconque des revendications 1 à 5, dans laquelle la vitesse de propagation des fissures de fatigue est inférieure à 10-4 mm/cycle à ΔK = 10 MPa m pour un essai effectué à R = 0,1 dans le sens L-T à l'emplacement E/4.Sheet according to any one of Claims 1 to 5, in which the speed of propagation of the fatigue cracks is less than 10 -4 mm / cycle at ΔK = 10 MPa m for a test performed at R = 0,1 in the LT direction at the E / 4 location. Tôle selon une quelconque des revendications 2 à 5, caractérisée en ce que KIC(L-T) > 30 MPa√m.Sheet according to any one of claims 2 to 5, characterized in that K IC (LT) > 30 MPa√m. Tôle selon la revendication 7, caractérisée en ce que KIC(T-L) > 25 MPa√, et préférentiellement caractérisée en plus en ce que KIC(S-L) > 25 MPa√m.Sheet according to claim 7, characterized in that K IC (TL) > 25 MPa√, and preferentially further characterized in that K IC (SL) > 25 MPa√m. Tôle selon une quelconque des revendications 1 à 8, caractérisée en ce que son épaisseur est d'au moins 15 mm.Sheet according to any one of claims 1 to 8, characterized in that its thickness is at least 15 mm. Procédé de fabrication d'une tôle selon l'une quelconque des revendications 1 à 9, comprenant le laminage à chaud d'une ébauche de ladite tôle à une température qui est inférieure à 420°C.Method of manufacturing a sheet according to one any of claims 1 to 9, including the hot rolling of a blank of said sheet to a temperature which is below 420 ° C. Procédé selon la revendication 10, dans lequel tôle est soumise à un revenu de type T7651.The process of claim 10 wherein sheet metal is subject to a T7651 type income. Utilisation d'une tôle selon une quelconque des revendications 1 à 9 ou d'une tôle issue du procédé selon la revendication 10 ou 11 pour la fabrication d'éléments de structure pour construction aéronautique.Use of a sheet according to any one Claims 1 to 9 or a sheet produced by the process according to claim 10 or 11 for the manufacture structural elements for aircraft construction.
    EP04356197A 2003-12-16 2004-12-15 Thick sheet made of Al-Zn-Cu-Mg recrystallised alloy with low Zirconium content Active EP1544316B1 (en)

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    CONNOLLY B J; KOUL M G; MORAN A L: "Comparison study of stress corrosion crack growth rates for AA7XXX alloys as a function of bulk aqueous chloride concentrations" CORROSION, vol. 61, no. 10, 2005, pages 976-986, XP009080831 20051000 *
    CONNOLY B J; DEFFENBAUGH K L; MORAN A L: "Environmentally assisted crack growth rates of high-strength aluminum alloys" JOM., vol. 55, 2003, pages 49-52, XP001249177 US *

    Cited By (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    US7520945B2 (en) 2003-12-16 2009-04-21 Alcan Rhenalu Recrystallized Al-Zn-Cu-Mg plate with low zirconium
    US10301710B2 (en) 2005-01-19 2019-05-28 Otto Fuchs Kg Aluminum alloy that is not sensitive to quenching, as well as method for the production of a semi-finished product

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    ES2383528T3 (en) 2012-06-21
    ATE548476T1 (en) 2012-03-15
    US7520945B2 (en) 2009-04-21
    EP1544316B1 (en) 2012-03-07
    US20050167016A1 (en) 2005-08-04
    EP1544316A3 (en) 2007-05-09

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