EP2171114B1 - Extrudierte produkte in der aluminiumlegierung al-mn mit erhöhter mechanischer festigkeit - Google Patents

Extrudierte produkte in der aluminiumlegierung al-mn mit erhöhter mechanischer festigkeit Download PDF

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Publication number
EP2171114B1
EP2171114B1 EP08835982.3A EP08835982A EP2171114B1 EP 2171114 B1 EP2171114 B1 EP 2171114B1 EP 08835982 A EP08835982 A EP 08835982A EP 2171114 B1 EP2171114 B1 EP 2171114B1
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Prior art keywords
weight
product according
tube
alloy
mpa
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EP08835982.3A
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English (en)
French (fr)
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EP2171114A1 (de
Inventor
Bruce Morere
Annabelle Bigot
Jérôme PIGNATEL
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Constellium Issoire SAS
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Constellium Issoire SAS
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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
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
    • F28F21/08—Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
    • 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
    • Y10T428/12292—Workpiece with longitudinal passageway or stopweld material [e.g., for tubular stock, etc.]

Definitions

  • the invention relates to spun aluminum alloy products Al-Mn (3000 series according to the nomenclature of the Aluminum Association) with improved mechanical strength, in particular tubes intended in particular for pipes or heat exchangers for the automotive industry. .
  • HFCs HydroFluoroCarbures
  • An air conditioner using CO2 as a refrigerant gas is based on gas compression and expansion.
  • a compressor compresses CO2 at high pressure and it then goes into a gas cooler (traditionally called a condenser, but in which condensation does not occur when the refrigerant is CO2), then in an internal heat exchanger (which allows heat exchanges with the low pressure zone).
  • the CO2 which is still gaseous, then passes into a regulator from which a liquid flows out which allows the cooling of the passenger compartment by passing through an evaporator.
  • the low pressure gas is then accumulated before circulating in the internal heat exchanger and back into the compressor for a new cycle.
  • the spun aluminum products can be used for the manufacture of heat exchangers (gas cooler, evaporator) and / or for the realization of the pipes allowing the refrigerant to circulate between the various elements of the cooling circuit.
  • CO2 as a refrigerant is made difficult by the pressure at which it must be used. Indeed, the critical temperature of CO2 is lower than that of HFC-134a and its critical pressure is higher which forces the air conditioning system to operate at higher pressures and temperatures than those currently used, whether in the high pressure part or the low pressure part of the circuit.
  • the materials used in the air conditioning circuit must therefore be stronger than current materials while maintaining at least equivalent performance in terms of manufacturing, shaping, assembly and corrosion resistance.
  • the CO2 thus needs to be compressed at high pressures of the order of 100 to 200 bar. Therefore, to allow the use of CO2 as a refrigerant, the pipes must withstand an operating pressure of 200 bar for high temperatures of 130-170 ° C which is high compared to current conditions, the order of 5 bars at 60 ° C.
  • Alloys have been proposed for the production of flat tubes for heat exchangers (gas coolers, evaporators) of air conditioning systems using CO2 as a refrigerant gas.
  • JP 2005-068557 discloses a composition alloy (% by weight) Mn: 0.8 - 2, Cu: 0.22 - 0.6, Ti: 0.01 - 0.2, Fe: 0.01 - 0.4, Zn ⁇ 0.2, Sn ⁇ 0.018, In ⁇ 0.02.
  • JP 2007-070699 discloses a composition alloy (% by weight) Si: 0.31 - 0.7, Fe: 0.3 - 0.6, Mn: 0.01 - 0.4, and optionally Ti 0.01 - 0.3, Zr 0.05 - 0.3, Cr 0.05 - 0.3.
  • the patent application WO 99/18250 of the same company relates to an alloy designated X3020 having a better formability than X3030 by adding Mg (up to 1%) and Zr (up to 0.30%). Cr is preferably maintained below 0.02%, or even 0.01%, Ti is preferably maintained above 0.12% and Zn above 0.1%.
  • the patent application WO 00/50656 of Norsk Hydro relates to an alloy of composition: Si: 0.05 - 0.15, Fe: 0.06 - 0.35, Cu ⁇ 0.10, Mn: 0.01 - 1.0, Mg: 0 , 02 - 0.60, Cr ⁇ 0.25, Zn: 0.05 - 0.70, Ti ⁇ 0.25, Zr ⁇ 0.20.
  • Cr is preferably maintained below 0.15% and is only allowed for reasons of recycling of manufacturing scrap other alloys.
  • Zn is preferably maintained above 0.1%.
  • the patent application WO 02/055750 of the Applicant relates to an alloy having an improved corrosion resistance of composition Si ⁇ 0.30, Fe: 0.20 - 0.50, Cu ⁇ 0.05, Mn: 0.5 - 1.2, Mg ⁇ 0 , 05, Zn ⁇ 0.50, Cr: 0.10 - 0.30, Ti ⁇ 0.05, Zr ⁇ 0.05.
  • the problem addressed by the present invention is to provide a 3XXX alloy spun product of improved mechanical strength, so as to be able to withstand high pressures, and in particular for operating temperatures of 130 to 170 ° C, and having identical or superior performance in terms of manufacturing, shaping, assembly and corrosion resistance to those of current products.
  • the preferred contents are (% by weight): Si 0.05 - 0.15, Fe: 0.05 - 0.25, Cu ⁇ 0.01, Mn: 0.9 - 1.1, Mg 0.6 - 0.9, Zn: ⁇ 0.05, Cr: 0.15 - 0.25, Ti ⁇ 0.04, Zr ⁇ 0.04, Ni ⁇ 0.01.
  • the subject of the invention is also a process for manufacturing spunbonded alloy tubes according to the invention comprising casting a billet, optionally homogenizing this billet, spinning a tube, stretching said tube one or more passes, and annealing continuously at a temperature between 350 and 500 ° C with a rise in temperature of less than 10 s.
  • Yet another object of the invention is the use of a spun product according to the invention in the manufacture of motor vehicles.
  • the alloy of the 3XXX series according to the invention has a relatively high magnesium content and a zinc content reduced to the level of impurity. Contrary to the teaching of the prior art which recommends the addition of zinc and titanium to the alloys of the 3XXX series to improve their resistance to corrosion, the alloy according to the invention has a good corrosion behavior with a content zinc and a titanium content reduced to the level of impurities.
  • the zinc content should be less than 0.20% by weight, more preferably less than 0.05% by weight and even more preferably less than 0.04% by weight.
  • the titanium content must be less than 0.05% by weight, preferably less than 0.04% by weight and even more preferably less than 0.03% by weight.
  • the low zinc and titanium contents are an advantage with regard to the recycling of the alloy products according to the invention.
  • the magnesium content is between 0.5 and 1.0% by weight and preferably between 0.6 and 0.9% by weight.
  • the addition of magnesium at a content of at least 0.5% by weight and preferably at least 0.6% by weight makes it possible to increase the mechanical strength very significantly.
  • the magnesium content must however be limited to a maximum of 1.0% by weight and preferably 0.9% by weight to ensure satisfactory brazeability of the products, as well as a good performance in terms of extrusionability.
  • the addition of chromium at a concentration of between 0.10 and 0.30% by weight and preferably at a concentration of between 0.15 and 0.25% by weight makes it possible to improve the corrosion resistance of the alloy.
  • Manganese is the main alloying element, its addition is carried out at a concentration of between 0.5 and 1.2% by weight and preferably at a concentration of between 0.9 and 1.1% by weight.
  • the content of iron and silicon must be less than 0.30% by weight.
  • the iron content is at most 0.25% by weight and the silicon content is at most 0.15% by weight. Too high a content of these elements contributes to the degradation of the corrosion resistance. It is preferable, mainly for economic reasons of recycling, that the silicon and iron contents are at least 0.05% by weight.
  • the addition of other elements may have a detrimental effect on the alloy and must therefore have a content of less than 0.05% by weight and less than 0.15% in total.
  • the presence of zirconium, nickel or copper can degrade the corrosion resistance properties and the content of these elements should be less than 0.05% by weight.
  • the nickel and copper content is less than 0.01% by weight and the zirconium content is less than 0.04% by weight.
  • the method of manufacturing the spun products comprises casting billets of the indicated alloy, optionally homogenizing the billets, heating them and spinning to obtain a tube in straight length or crown, and optionally one or several stretching passes to bring the product to the desired dimensions.
  • the tube can, if it is stretched, then advantageously continuously annealed by high velocity scrolling through a passage oven, preferably an induction furnace. Heating the spun product is very fast, less than 10 seconds, and preferably 2 seconds, and the product scrolls at a speed between 20 and 200 m / min. The oven temperature is maintained between 350 and 500 ° C.
  • the product can after the annealing undergo a new stretching to increase the mechanical strength (state H).
  • This continuous annealing leads to a fine-grain equiaxed microstructure, of a mean grain size, measured by the intercepts method, of less than 40 ⁇ m, and typically of the order of 25 ⁇ m.
  • the fine-grained microstructure is particularly advantageous with respect to the mechanical properties and corrosion resistance of the tubes.
  • the products according to the invention have a high mechanical strength.
  • the breaking strength at room temperature is increased by at least 40% compared to a product according to the demand.
  • WO 02/055750 having a comparable manganese content.
  • the advantage is even more marked for the tests carried out at high temperature.
  • the breaking strength at 170 ° C is increased by almost 60% compared to a product according to demand.
  • WO 02/055750 having a comparable manganese content.
  • the spun products according to the invention have, in the H12 state, a breaking strength Rm greater than 150 MPa at room temperature and greater than 140 MPa at 170 ° C.
  • the products spun according to the preferred composition of the invention exhibit, in the H12 state, a breaking strength Rm greater than 160 MPa at room temperature and greater than 150 MPa at 170 ° C.
  • the products according to the invention have, in the H12 state, a plastic gap at room temperature slightly lower than that of the products according to the demand. WO 02/055750 but surprisingly an improved relative plastic gap for test temperatures greater than or equal to 130 ° C.
  • the relative plastic difference obtained with the products according to the invention is greater than 5% for a test temperature of 140 ° C. Moreover, even after aging at 130 ° C., the relative plastic difference at the H 12 state remains greater than 5%.
  • the products according to the invention also have good corrosion performance. In particular, the products according to the invention do not exhibit deep pits during a salt spray test of SWAAT type according to the ASTM G85A3 standard. It is possible that this favorable result results, at least in part, from the absence of MgZn 2 precipitates which may form in the event of the simultaneous presence of Mg and Zn and which may have a detrimental effect, in particular on the corrosion resistance.
  • a preferred form of the spun product according to the invention is a cylindrical tube having only one cavity.
  • the spun products according to the invention can be used especially as tubes in the manufacture of motor vehicles.
  • the spun products according to the invention can be used as tubes for fuel lines, oil, brake fluid or refrigerant for automobiles and as tubes for heat exchangers for engine cooling and / or air conditioning systems.
  • passenger compartment especially if they use CO2 as a refrigerant gas.
  • the tubes, in particular the drawn tubes, according to the invention are more particularly adapted to be used in the form of cylindrical tubes preferably comprising only one cavity for the fluid transfer lines used in the cabin air-conditioning systems. of motor vehicles using CO2 as a refrigerant gas.
  • Bindings were cast and homogenized in 3 alloys listed A to C.
  • the alloys A and B respectively correspond to alloy compositions AA3103 and according to the demand.
  • Alloy C is in accordance with the invention.
  • the compositions of the alloys (% by weight) are shown in Table 1.
  • the billets were spun into tube crowns and then stretched to obtain tubes 12 mm in diameter and 1.25 mm thick. No significant differences were recorded for the three alloys with respect to their spinning and drawing properties. These crowns were continuously annealed in an induction furnace at a temperature set at 470 ° C, with a rate of passage between 60 and 120 m / min. The crowns were then subjected to a new stretching pass to bring them to H12 according to EN 515.
  • alloy C according to the invention leads to a greatly improved mechanical strength compared to that of alloy B for a test carried out at room temperature and even more widely improved for a test carried out at 170 ° C.
  • the breaking strength is improved by about 40% at room temperature and about 60% at 170 ° C.
  • the plastic gap for tests performed at at least 140 ° C is also greatly improved from 0% for alloy B to over 5% for alloy C for temperatures of 140 ° C and 170 ° C.
  • alloy C The properties of tensile strength and the yield strength of alloy C were also measured at 130 ° C. after aging for 72 hours at 130 ° C. and from 1000 hours at 130 ° C., and measured at 165 ° C. after aging. from 72h to 165 ° C and from 1000h to 165 ° C.
  • alloy B has been characterized only under the most severe conditions, that is to say measured at 165 ° C after aging from 1000h to 165 ° C.
  • Table 3 Mechanical characteristics obtained after aging at high temperature.
  • the alloy C according to the invention retains after aging the mechanical properties of resistance to fracture and yield strength significantly improved since increased by 40% relative to the alloy B.
  • the average grain size was measured by the intercepts method on samples from the 3 tubes. The results are shown in Table 4. The tubes obtained with the 3 alloys have equiaxized fine grains of the order of 20 microns. Table 4. Average grain size measured by the intercepts method. Alloy Direction L ( ⁇ m) T direction ( ⁇ m) Average ( ⁇ m) AT 22 18 20 B 20 16 18 VS 21 18 20
  • Corrosion resistance was measured using the Sea Water Acetic Acid Test (SWAAT) according to ASTM G85 A3. The measurements were made for periods of 500 cycles at the temperature of 49 ° C., on three tubes of length 200 mm of each alloy A, B and C. At the end of the test, the tubes were taken out of the tube. pregnant and stripped in a solution of nitric acid concentrated to 68% in order to dissolve the products of corrosion. On each tube, the depth of the pits is then measured optically on the surface by defocusing and the average depth of the deepest pits is calculated. The average Pmoy of the values obtained for the 3 tubes is then calculated. The corrosion resistance is even better than Pmoy is weak. The results of 5 successive SWAAT test campaigns are shown in Table 5.
  • alloy C according to the invention has a corrosion resistance equivalent to that of alloy B of the prior art and significantly improved compared to that of alloy A.
  • alloy C does not present no deep sting, it being understood that in the context of the present invention the term deep sting means a Pmoy value greater than 0.5 mm.
  • composition according to the invention and in particular the addition of Mg, the absence of Zn thus makes it possible to dramatically improve the mechanical strength, in particular for temperatures between 130 ° C. and 170 ° C., without compromising corrosion resistance, compared to alloy B.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Rigid Pipes And Flexible Pipes (AREA)
  • Extrusion Of Metal (AREA)

Claims (15)

  1. Strangpressprodukt, insbesondere ein gezogenes Rohr, aus einer Legierung mit einer Zusammensetzung bestehend aus (Gew.-%):
    0 < Si < 0,30 ; 0 < Fe < 0,30 ; Cu < 0,05 ; Mn: 0,5 -1,2 ; Mg: 0,5 -1,0 ; 0 < Zn < 0,20 ; Cr: 0,10 - 0,30 ; 0 < Ti < 0,05 ; Zr < 0,05 ; Ni < 0,05, weitere Elemente jeweils < 0,05 und insgesamt < 0,15, Rest Aluminium.
  2. Produkt nach Anspruch 1, dadurch gekennzeichnet, dass Zn < 0,05 Gew.-%.
  3. Produkt nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass Ti < 0,04 Gew.-% und vorzugsweise Ti < 0,03 Gew.-%.
  4. Produkt nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass Mg: 0,6 - 0,9 Gew.-%.
  5. Produkt nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass Fe: 0,05 - 0,25 Gew.-%.
  6. Produkt nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass (Gew.-%) Cu < 0,01, Ni < 0,01.
  7. Strangpressprodukt nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass seine Korngröße kleiner als 40 µm ist.
  8. Strangpressprodukt nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass seine Bruchfestigkeit Rm im Zustand H12 mehr als 150 MPa bei Raumtemperatur und mehr als 140 MPa bei 170 °C beträgt.
  9. Strangpressprodukt nach Anspruch 8 mit einer Zusammensetzung bestehend aus (Gew.-%):
    Si: 0,05 - 0,15 ; Fe: 0,05 - 0,25 ; Cu < 0,01 ; Mn: 0,9 - 1,1 ; Mg: 0,6 - 0,9 ; 0 < Zn < 0,05 ; Cr: 0,15 - 0,25 ; 0 < Ti < 0,04 ; Zr < 0,04 ; Ni < 0,01, dadurch gekennzeichnet, dass seine Bruchfestigkeit Rm im Zustand H12 mehr als 160 MPa bei Raumtemperatur und mehr als 150 MPa bei 170 °C beträgt.
  10. Strangpressprodukt nach einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, dass es sich um ein zylindrisches Rohr mit einem einzigen Hohlraum handelt.
  11. Verfahren zur Herstellung von stranggepressten Rohren nach einem der Ansprüche 1 bis 10, umfassend das Gießen eines Pressbarrens, das eventuelle Homogenisieren dieses Barrens, das Strangpressen eines Rohrs, das Ziehen dieses Rohrs in einem oder mehreren Durchgängen sowie das kontinuierliche Glühen bei einer Temperatur zwischen 350 und 500 °C mit einem Temperaturanstieg von weniger als 10 s.
  12. Verwendung eines Strangpressprodukts nach einem der Ansprüche 1 bis 11 in der Herstellung von Kraftfahrzeugen.
  13. Verwendung nach Anspruch 12 als Leitungsrohr für Kraftstoff, Öl, Bremsflüssigkeit oder Kältemittel.
  14. Verwendung nach Anspruch 12 als Wärmetauscherrohr für eine Kühlanlage eines Motors und/oder eine Klimaanlage eines Fahrzeuginnenraums, bei der CO2 als Kältegas verwendet wird.
  15. Verwendung nach Anspruch 12, bei der das Strangpressprodukt in Form eines zylindrischen Rohrs mit einem einzigen Hohlraum vorliegt, als Fluidübertragungsleitung in einer Klimaanlage eines Fahrzeuginnenraums, die CO2 als Kältegas verwendet.
EP08835982.3A 2007-07-27 2008-07-21 Extrudierte produkte in der aluminiumlegierung al-mn mit erhöhter mechanischer festigkeit Active EP2171114B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0705510A FR2919306B1 (fr) 2007-07-27 2007-07-27 Produits files en alliage d'aluminium al-mn a resistance mecanique amelioree
PCT/FR2008/001074 WO2009043993A1 (fr) 2007-07-27 2008-07-21 Produits filés en alliage d'aluminium al-mn à résistance mécanique améliorée

Publications (2)

Publication Number Publication Date
EP2171114A1 EP2171114A1 (de) 2010-04-07
EP2171114B1 true EP2171114B1 (de) 2017-03-22

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EP08835982.3A Active EP2171114B1 (de) 2007-07-27 2008-07-21 Extrudierte produkte in der aluminiumlegierung al-mn mit erhöhter mechanischer festigkeit

Country Status (9)

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US (1) US20100190027A1 (de)
EP (1) EP2171114B1 (de)
JP (1) JP2010534766A (de)
KR (1) KR20100065289A (de)
CN (1) CN101765674A (de)
BR (1) BRPI0814138A2 (de)
FR (1) FR2919306B1 (de)
MX (1) MX2010000785A (de)
WO (1) WO2009043993A1 (de)

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JP2011080121A (ja) * 2009-10-08 2011-04-21 Mitsubishi Alum Co Ltd フィンチューブ型エアコン熱交換器用押出チューブ及び熱交換サイクル用冷媒配管
CN102146543A (zh) * 2010-02-05 2011-08-10 古河Sky株式会社 挤压性质和牺牲阳极性质优异的连接件用铝合金挤压材料
CN105568087A (zh) * 2016-01-25 2016-05-11 吕五有 一种热交换用铝合金及其生产方法
CN105838948A (zh) * 2016-04-08 2016-08-10 董超超 新型高强度抗腐蚀电动汽车外壳
CN105886864A (zh) * 2016-04-08 2016-08-24 董超超 新型高强度抗腐蚀铝合金高压真空配电柜
CN105803279A (zh) * 2016-04-08 2016-07-27 董超超 新型高强度抗腐蚀太阳能电池边框
CN105714167A (zh) * 2016-04-08 2016-06-29 董超超 新型高强度抗腐蚀外墙保温装饰板
CN105734371A (zh) * 2016-04-08 2016-07-06 董超超 新型高强度抗腐蚀铝合金管道
CN105803278A (zh) * 2016-04-08 2016-07-27 董超超 新型高强度抗腐蚀铝合金门窗
CN105838949A (zh) * 2016-04-08 2016-08-10 董超超 新型高强度抗腐蚀电连接器元件
CN105734370A (zh) * 2016-04-08 2016-07-06 董超超 新型高强度抗腐蚀数据记录仪
CN105861895A (zh) * 2016-04-08 2016-08-17 董超超 新型高强度抗腐蚀建筑幕墙框架
CN106929717A (zh) * 2017-03-24 2017-07-07 淮北津奥铝业有限公司 汽车零部件用铝合金
CN112254563A (zh) * 2019-07-22 2021-01-22 海德鲁铝业(苏州)有限公司 具有高耐腐蚀性的长寿命铝合金和由该合金生产的螺旋槽管
KR102382428B1 (ko) * 2020-02-04 2022-04-04 (주)휘일 고내식성 알루미늄 합금을 이용한 자동차용 리시버드라이어 및 이의 제조 방법
CN111235437A (zh) * 2020-03-18 2020-06-05 河南誉金技术服务有限公司 一种家用空调换热器Al-Mn管材合金及其制备方法
CN112658053A (zh) * 2020-12-02 2021-04-16 中南大学 一种挤拉成形制造灭火器瓶身的方法

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Publication number Publication date
CN101765674A (zh) 2010-06-30
KR20100065289A (ko) 2010-06-16
EP2171114A1 (de) 2010-04-07
JP2010534766A (ja) 2010-11-11
FR2919306B1 (fr) 2009-10-02
BRPI0814138A2 (pt) 2015-02-03
MX2010000785A (es) 2010-03-30
US20100190027A1 (en) 2010-07-29
FR2919306A1 (fr) 2009-01-30
WO2009043993A1 (fr) 2009-04-09

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