EP1382698A1 - Knetprodukt aus Al-Cu-Mg-Legierung für das Strukturbauteil eines Flugzeugs - Google Patents

Knetprodukt aus Al-Cu-Mg-Legierung für das Strukturbauteil eines Flugzeugs Download PDF

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Publication number
EP1382698A1
EP1382698A1 EP03356108A EP03356108A EP1382698A1 EP 1382698 A1 EP1382698 A1 EP 1382698A1 EP 03356108 A EP03356108 A EP 03356108A EP 03356108 A EP03356108 A EP 03356108A EP 1382698 A1 EP1382698 A1 EP 1382698A1
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European Patent Office
Prior art keywords
alloy
product according
mpa
product
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EP03356108A
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English (en)
French (fr)
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EP1382698B1 (de
EP1382698B2 (de
Inventor
Timothy Warner
Ronan Dif
Bernard Bes
Hervé Ribes
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Constellium Issoire SAS
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Pechiney Rhenalu SAS
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Application filed by Pechiney Rhenalu SAS filed Critical Pechiney Rhenalu SAS
Priority to DE60300004T priority Critical patent/DE60300004T3/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/18—Alloys based on aluminium with copper as the next major constituent with zinc
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y10T428/12764—Next to Al-base component

Definitions

  • the invention relates to aircraft structural elements, in particular sheet metal for large commercial aircraft fuselage made from rolled, spun or forged alloy AlCuMg in the treated state by dissolving, quenching and cold work hardening, and having, compared to the products of the prior art used for the same application, an improved compromise between the different properties required.
  • the fuselage of commercial aircraft of large capacity is typically made of an AlCuMg alloy sheet skin, as well as longitudinal stiffeners and circumferential frames.
  • a type 2024 alloy is used which, according to the designation of the Aluminum Association or the standard EN 573-3, has the following chemical composition (% by weight): If ⁇ 0.5 Fe ⁇ 0.5 Cu: 3.8 - 4.9 Mg: 1.2-1.8 Mn: 0.3 - 0.9 Cr ⁇ 0.10 Zn ⁇ 0.25 Ti ⁇ 0.15.
  • Variants of this alloy are also used. These elements are asked structures a compromise between several properties such as: resistance mechanical (i.e. static mechanical characteristics), tolerance to damage (toughness and speed of fatigue cracking), fatigue resistance (especially oligocyclic), resistance to different forms of corrosion, fitness ability. In some cases, especially for airplanes supersonic, creep resistance can be critical.
  • US Patent 5,652,063 (Alcoa) relates to an aircraft structural element made from a composition alloy (% by weight): Cu: 4.85-5.3 Mg: 0.51-1.0 Mn: 0.4-0.8 Ag: 0.2 - 0.8 If ⁇ 0.1 Fe ⁇ 0.1 Zr ⁇ 0.25 with Cu / Mg between 5 and 9.
  • the sheet of this alloy in the T8 state has a yield strength> 77 ksi (531 MPa).
  • the alloy is particularly intended for supersonic aircraft.
  • the patent application EP 0 731 185 of the Applicant relates to an alloy, subsequently recorded under No. 2024A, of composition: Si ⁇ 0.25 Fe ⁇ 0.25 Cu: 3.5 - 5 Mg: 1 - 2 Mn ⁇ 0.55 with the relation: 0 ⁇ Mn-2Fe ⁇ 0.2
  • the thick plates in this alloy have both improved toughness and a reduced level of residual stresses, without loss on the other properties.
  • the alloy may also contain: Zr ⁇ 0.20% V ⁇ 0.20% Mn ⁇ 0.80% Ti ⁇ 0.05% Fe ⁇ 0.15% If ⁇ 0.10%.
  • the patent application EP 1 170 394 A2 (Alcoa) describes four AlCu-type alloys which have, respectively, the composition Cu 4.08, Mn 0.29, Mg 1.36, Zr 0.12, Fe 0.02, Si 0.01; Cu 4.33, Mn 0.30, Mg 1.38, Zr 0.10, Fe 0.01, Si 0.00; Cu 4.09, Mn 0.58, Mg 1.35, Zr 0.11, Fe 0.02, Si 0.01; and Cu 4.22, Mn 0.66, Mg 1.32, Zr 0.10, Fe 0.01, Si 0.01.
  • the patent teaches how to convert these products into sheets having an elongated grain structure, wherein the grains have a length to thickness ratio of greater than 4.
  • the present invention aims to obtain aircraft structural elements, and in particular fuselage elements made of AlCuMg alloy having, compared to the prior art, improved damage tolerance, mechanical resistance to less equal, an improved resistance to corrosion, and this without resorting to expensive and troublesome addition elements for recycling.
  • the subject of the invention is a wrought product, in particular a laminated, spun or forged product, made of an alloy of composition (% by weight): Cu 3.80-4.30, Mg 1.25-1.45, Mn 0.20-0.50, Zn 0.40-1.30, Zr ⁇ 0.05, Fe ⁇ 0.15, Si ⁇ 0.15, Ag ⁇ 0.01 other elements ⁇ 0.05 each and ⁇ 0.15 in total, remain Al, said product can be treated by dissolving, quenching, and cold working, with a permanent deformation of between 0.5% and 15%, preferably between 1% and 5%, and even more preferably between 1.5% and 3.5%.
  • Cold working can be obtained by controlled pulling and / or cold processing, for example rolling or drawing.
  • the invention also relates to a structural element for construction aeronautical equipment, in particular an aircraft fuselage element, manufactured from such an aircraft wrought product, and especially from such a rolled product.
  • the copper content of the alloy according to the invention is between 3.80 and 4.30 %, and preferably between 4.05 and 4.30%; so it's in the low half of the content range of alloy 2024, so as to limit the volume fraction residual coarse copper particles.
  • the interval of magnesium content which must be between 1.25 and 1.45% and preferably between 1.28 and 1.42%, is shifted downwards compared to that of 2024.
  • the manganese is maintained between 0.20 and 0.50%, preferably between 0.30 and 0.50, and more preferably between 0.35 and 0.48%.
  • the implementation of the invention does not require significant addition of zirconium at a content greater than 0.05%.
  • the present invention requires careful control of the zinc content, the alloy being discharged into copper, magnesium and manganese.
  • the zinc content must be between 0.40 and 1.30%, preferably between 0.50 and 1.10%, and still between more preferably between 0.50 and 0.70%.
  • the zinc content at least equal to (1.2Cu - 0.3Mg + 0.3Mn - 3.75).
  • the silicon and iron contents are each kept below 0.15%, and preferably below 0.10%, to have good toughness.
  • this is only in very cases (depending on the type of alloy and the intended application) that the gain in damage tolerance related to the use of aluminum containing less than 0.06 % iron and silicon each is large enough to be valued.
  • the implementation of the present invention does not require that the content of iron and silicon less than 0.06% each, because in the selected composition range, the Damage tolerance is very good.
  • the alloy contains no silver addition, nor any other element likely to increase the production cost of the alloy and to pollute the other alloys produced on the same site by recycling manufacturing scrap.
  • the preferred method of manufacture comprises casting of plates, in the case where the product to be made is a rolled sheet, or billets in the case where it is a spun section or a forged part.
  • the plate or the billet is scalped, then homogenized between 450 and 500 ° C.
  • the hot transformation is then carried out by rolling, spinning or forging, optionally completed by a cold transformation step.
  • the laminated, spun or forged half-product is then dissolved between 480 and 505 ° C., so that this dissolution is as complete as possible, that is to say that the maximum of potentially soluble phases , in particular the precipitates Al 2 Cu and Al 2 CuMg, are effectively put back in solution.
  • the quality of the dissolution can be assessed by differential enthalpy analysis (AED) by measuring the specific energy using the area of the peak on the thermogram. This specific energy must preferably be less than 2 J / g.
  • AED differential enthalpy analysis
  • This hardening cold can be a controlled pull with a permanent elongation between 1 and 5% bringing the product to a T351 state. Controlled traction with a permanent elongation of between 1.5% and 3.5%. It can also be a cold rolling by rolling in the case of sheets or by drawing in the case profiles, with a permanent elongation of up to 15%, bringing the in the T39 state, or in the T3951 state if the rolling or drawing is combined with the traction.
  • the product finally undergoes natural aging at room temperature.
  • the final microstructure is in general largely recrystallized, with grains relatively thin and fairly equiaxed.
  • the product according to the present invention is well suited for use as an aircraft structural element, for example as a fuselage skin element, and especially as an element for the fuselage skin panel (skin).
  • These sheets preferably plated, have a thickness of between 1 and 16 mm, and have good resistance to intergranular corrosion and corrosion on riveted assembly. They have a breaking strength in the L direction and / or TL direction greater than 430 MPa, and preferably greater than 440 MPa, and a yield strength in the L and / or TL direction greater than 300 MPa, and preferably greater than 320. MPa.
  • the sheet according to the invention may be a sheet plated with at least one face with an alloy of the 1xxx series, and preferably with an alloy selected from the group consisting of alloys 1050, 1070, 1300 and 1145.
  • plated sheets according to the invention which are particularly resistant to corrosion by galvanic coupling. in a riveted assembly. More particularly, plated sheets which exhibit a galvanic corrosion current of less than 4 ⁇ A / cm 2 , and preferably less than 2.5 ⁇ A / cm 2 , for exposure of up to 200 hours, during corrosion tests in a riveted assembly, placing the core alloy in a non-deaerated solution containing 0.06 M NaCl and the plating alloy in a 0.02 M AlCl 3 solution deaerated by nitrogen sparging.
  • N0, N1, N2 and N3 alloys were developed with chemical composition was in accordance with the invention.
  • the liquid metal was first treated in the furnace maintaining by injection of gas using a rotor of a type known under the brand IRMA, and then in a pocket of type known as Alpur.
  • the refining has been done online, that is to say between the holding oven and the Alpur pocket, with wire AT5B (0.7 kg / t for N0, N1 and N3, 0.3 kg / t for N2).
  • 3.0 plates were cast m length and section 1450 mm x 377 mm (except for N3: section 1450 x 446 mm). They were relaxed for 10h at 350 ° C.
  • alloy plating 1050 corresponds to about 2% of thickness.
  • alloys E and F For the alloys according to the prior art (alloys E and F), the plates have been heated to around 450 ° C, then hot-rolled at the reversing mill up to a thickness of about 20 mm. The resulting strips were rolled on a tandem rolling mill with three cages up to a final thickness close to 5 mm, then wound (at temperatures of 320 ° C and 260 ° C, respectively for alloys F and E). In the case of alloy F, the coil thus obtained was laminated to cold to a thickness of 3.2 mm.
  • Sheet metal was cut, put in solution in a salt bath oven at a temperature of 498.5 ° C for a duration of 30 minutes (sheet metal E thickness 5 mm) or 25 min (sheet F thickness 3.2 mm), then completed (wrinkling followed by controlled traction with permanent elongation included between 1.5 and 3%).
  • the N0 plate has undergone the following homogenization cycle: 8h at 495 ° C + 12h at 500 ° C (nominal values) while alloys N1, N2 and N3 have been homogenized for 12 hours at 500 ° C.
  • the plates After reheating (about 18 hours at 425-445 ° C), the plates were hot-rolled (inlet temperature: 413 ° C) to a thickness of about 90 mm.
  • the N0 band thus obtained was cut in half in the direction perpendicular to the rolling direction. There were thus obtained two bands, labeled N01 and N02. These strips were rolled on a tandem hot rolling mill 3 cages to a final thickness of 6 mm (winding temperature about 320 - 325 ° C).
  • N1 and N3 alloy plate and one N3 alloy plate were hot rolled at 5.5 mm before being cold rolled to the final thickness of 3.2 mm, and another N1 alloy plate. was hot rolled at 4.5 mm before being cold rolled to the final thickness of 1.6 mm.
  • An N2 alloy plate was hot rolled to a final thickness of 6 mm (tandem winding temperature 270 ° C).
  • the coil N01 has not undergone any other rolling pass, while the coil N02 was cold rolled to a final thickness of 3.2 mm.
  • the plates once cut were dissolved in a salt bath oven (thickness 6 mm: 60 minutes at 500 ° C., thickness 3.2 mm: 40 minutes at 500 ° C.; thickness 1, 6 mm: 30 minutes at 500 ° C) followed by quenching with water to about 23 ° C. After quenching, the sheets have undergone wrinkling and pulling with elongation cumulative standing between 1.5 and 3.5%. The waiting time between quenching and wrinkling did not exceed 6 hours.
  • the tensile strength R m (in MPa), the conventional yield stress at 0.2% elongation R p0.2 (in MPa) and the elongation at break A (in%) were measured by a tensile test according to EN 10002-1.
  • the product according to the invention therefore has a better breaking strength in the case of a cracked panel.
  • the plates of 2024 in particular for ⁇ K ⁇ 20 MPa ⁇ m, exhibit a cracking rate two to three times higher than for the product according to the invention. The latter therefore allows longer inspection intervals (to mass given structure) or reductions in the inspection interval structure fixed.
  • the breaking K values for a limiting load greater than 200 MPa are greater than about 120 MPa ⁇ m for the described R curves, with apparent K (K r ) greater than about 110 MPa m.
  • K r apparent K
  • the dimensioning portion of the curve R consists of points corresponding to a static crack advance ⁇ a eff of more than 20 mm.
  • the corrosion resistance of the sheets has also been characterized.
  • the alloy according to the invention shows intrinsically, that is to say after displacement by machining, resistance to intergranular corrosion, measured according to ASTM standard G 110, substantially comparable to that of the reference 2024.
  • the test consists in measuring the current which is established naturally between the anode (alloy of plating placed in a cell containing a solution of AlCl 3 (0,02 M, deaerated by sparging of nitrogen)) and the cathode (alloy core placed in a cell containing a solution of NaCl (0.06 M, aerated)), a salt bridge ensuring the electrolytic contact between the two cells. Both elements (veneer and core) have the same surface (2.54 cm 2 ). The coupling current densities are recorded throughout the duration of the test. It is observed that the current reaches a plateau after about 55 hours and hardly changes during the tests (200 hours or 15 days, depending on the sample). The results are summarized in Table 6.
  • state F From hot-rolled and possibly cold-rolled sheets (state F) of the alloy according to the invention (see example 1), several other metallurgical states were developed in the form of a size of 600 mm (L-direction) x 160 mm (TL direction) x thickness.
  • the marks ending in A, D, F and I correspond to T351 states.
  • the different samples were characterized by tensile tests (L and TL directions) as well as toughness tests.
  • the tenacity was first evaluated in the TL and LT directions using the maximum stress R e (in MPa) and the flow energy E ec according to the Kahn test.
  • the stress Kahn is equal to the ratio of the maximum load F max that the specimen can withstand on the section of the specimen (product of the thickness B by the width W).
  • the flow energy is determined as the area under the force-displacement curve up to the maximum force F max supported by the specimen.
  • the test is described in the article "Kahn-Type Tear Test and Crack Toughness of Aluminum Alloy Sheet", published in the journal Materials Research & Standards, April 1964, p. 151- 155.
  • the sample used for the test of tenacity Kahn is described, for example, in the "Metals Handbook", 8 th Edition, vol. 1, American Society for Metals, pp. 241-242.
  • the tenacity was also approached for sheets of thickness 6 mm, using a curve-type test R, in the TL direction, but on smaller specimens than that described in Example 1.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Heat Treatment Of Steel (AREA)
  • Metal Rolling (AREA)
  • Conductive Materials (AREA)
  • Powder Metallurgy (AREA)
  • Laminated Bodies (AREA)
  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
EP03356108A 2002-07-11 2003-07-09 Knetprodukt aus Al-Cu-Mg-Legierung für das Strukturbauteil eines Flugzeugs Expired - Lifetime EP1382698B2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE60300004T DE60300004T3 (de) 2002-07-11 2003-07-09 Knetprodukt aus Al-Cu-Mg-Legierung für das Strukturbauteil eines Flugzeugs

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0208737A FR2842212B1 (fr) 2002-07-11 2002-07-11 Element de structure d'avion en alliage a1-cu-mg
FR0208737 2002-07-11

Publications (3)

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EP1382698A1 true EP1382698A1 (de) 2004-01-21
EP1382698B1 EP1382698B1 (de) 2004-05-26
EP1382698B2 EP1382698B2 (de) 2013-01-09

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US (2) US7294213B2 (de)
EP (1) EP1382698B2 (de)
AT (1) ATE267885T1 (de)
DE (1) DE60300004T3 (de)
ES (1) ES2220902T5 (de)
FR (1) FR2842212B1 (de)

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WO2008003503A2 (en) * 2006-07-07 2008-01-10 Aleris Aluminum Koblenz Gmbh Method of manufacturing aa2000 - series aluminium alloy products
US7883591B2 (en) 2004-10-05 2011-02-08 Aleris Aluminum Koblenz Gmbh High-strength, high toughness Al-Zn alloy product and method for producing such product
US8608876B2 (en) 2006-07-07 2013-12-17 Aleris Aluminum Koblenz Gmbh AA7000-series aluminum alloy products and a method of manufacturing thereof
US8877123B2 (en) 2007-03-14 2014-11-04 Aleris Aluminum Koblenz Gmbh Al—Cu alloy product suitable for aerospace application
CN104451298A (zh) * 2014-11-19 2015-03-25 无锡鸿声铝业有限公司 一种改进的2024铝合金
CN104711498A (zh) * 2013-12-13 2015-06-17 天津大学 高强度铝合金二次拉伸成型中表面橘皮效应的控制方法
US10472707B2 (en) 2003-04-10 2019-11-12 Aleris Rolled Products Germany Gmbh Al—Zn—Mg—Cu alloy with improved damage tolerance-strength combination properties

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DE112009002512B4 (de) 2008-10-10 2023-03-23 Gkn Sinter Metals, Llc. Mengenchemieformulierung für Pulvermetall-Aluminiumlegierung
CN102292463A (zh) 2009-01-22 2011-12-21 美铝公司 改良的包含钒的铝-铜合金
MX341354B (es) 2011-09-16 2016-08-17 Ball Corp Recipientes extruidos por impacto a partir de chatarra de aluminio reciclada.
CN102732849A (zh) * 2012-06-29 2012-10-17 武汉理工大学 镁合金与铝合金表面改性处理及高强连接的方法
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US11072844B2 (en) 2016-10-24 2021-07-27 Shape Corp. Multi-stage aluminum alloy forming and thermal processing method for the production of vehicle components
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GB1133113A (en) * 1965-02-05 1968-11-06 Aluminum Co Of America Improvements in forged aluminium base alloy members
US3826688A (en) * 1971-01-08 1974-07-30 Reynolds Metals Co Aluminum alloy system
EP0473122A1 (de) * 1990-08-27 1992-03-04 Aluminum Company Of America Blech aus einer Aluminiumlegierung mit guter Beständigkeit gegen Beschädigung für Flugzeugblech
EP0731185A1 (de) * 1995-03-10 1996-09-11 Pechiney Rhenalu Aluminium-Kupfer-Magnesiumbleche mit niedrigen Restspannungen
EP1045043A1 (de) * 1999-04-12 2000-10-18 Pechiney Rhenalu Verfahren zur Herstellung von Formteilen aus Aluminiumlegierung vom Typ 2024

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10472707B2 (en) 2003-04-10 2019-11-12 Aleris Rolled Products Germany Gmbh Al—Zn—Mg—Cu alloy with improved damage tolerance-strength combination properties
US7883591B2 (en) 2004-10-05 2011-02-08 Aleris Aluminum Koblenz Gmbh High-strength, high toughness Al-Zn alloy product and method for producing such product
WO2008003503A2 (en) * 2006-07-07 2008-01-10 Aleris Aluminum Koblenz Gmbh Method of manufacturing aa2000 - series aluminium alloy products
WO2008003503A3 (en) * 2006-07-07 2008-02-21 Aleris Aluminum Koblenz Gmbh Method of manufacturing aa2000 - series aluminium alloy products
US8002913B2 (en) 2006-07-07 2011-08-23 Aleris Aluminum Koblenz Gmbh AA7000-series aluminum alloy products and a method of manufacturing thereof
US8088234B2 (en) 2006-07-07 2012-01-03 Aleris Aluminum Koblenz Gmbh AA2000-series aluminum alloy products and a method of manufacturing thereof
US8608876B2 (en) 2006-07-07 2013-12-17 Aleris Aluminum Koblenz Gmbh AA7000-series aluminum alloy products and a method of manufacturing thereof
US8877123B2 (en) 2007-03-14 2014-11-04 Aleris Aluminum Koblenz Gmbh Al—Cu alloy product suitable for aerospace application
EP2121997B2 (de) † 2007-03-14 2016-08-24 Aleris Aluminum Koblenz GmbH Al-cu-legierungsprodukt, das für die luft- und raumfahrtanwendung geeignet ist
CN104711498A (zh) * 2013-12-13 2015-06-17 天津大学 高强度铝合金二次拉伸成型中表面橘皮效应的控制方法
CN104711498B (zh) * 2013-12-13 2016-09-07 天津大学 高强度铝合金二次拉伸成型中表面橘皮效应的控制方法
CN104451298A (zh) * 2014-11-19 2015-03-25 无锡鸿声铝业有限公司 一种改进的2024铝合金

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US20080210350A1 (en) 2008-09-04
FR2842212B1 (fr) 2004-08-13
EP1382698B1 (de) 2004-05-26
EP1382698B2 (de) 2013-01-09
ATE267885T1 (de) 2004-06-15
ES2220902T5 (es) 2013-05-09
US20040086418A1 (en) 2004-05-06
DE60300004D1 (de) 2004-07-01
DE60300004T2 (de) 2005-01-20
FR2842212A1 (fr) 2004-01-16
US7294213B2 (en) 2007-11-13
DE60300004T3 (de) 2013-06-20
ES2220902T3 (es) 2004-12-16
US7993474B2 (en) 2011-08-09

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