US20120291925A1 - Aluminum magnesium lithium alloy with improved fracture toughness - Google Patents

Aluminum magnesium lithium alloy with improved fracture toughness Download PDF

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Publication number
US20120291925A1
US20120291925A1 US13/473,303 US201213473303A US2012291925A1 US 20120291925 A1 US20120291925 A1 US 20120291925A1 US 201213473303 A US201213473303 A US 201213473303A US 2012291925 A1 US2012291925 A1 US 2012291925A1
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Bernard Bes
Frank Eberl
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Constellium Issoire SAS
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Constellium France SAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • 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
    • C22F1/047—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 magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent

Definitions

  • the invention relates to aluminum-magnesium-lithium alloy products, and more particularly such products, their manufacturing processes and use, designed in particular for aircraft and aerospace construction.
  • Aluminum alloys containing lithium are of great interest in this respect, because lithium can reduce the density of aluminum by 3% and increase the modulus of elasticity by 6% for each percent of added lithium weight.
  • their performance as compared to the other usual properties must generally attain that of alloys in regular use, in particular in terms of the balance between static mechanical strength properties (tensile and compression yield stress, ultimate tensile strength) and damage tolerance properties (fracture toughness, resistance to fatigue crack propagation), these properties being in general in opposition to each other.
  • These alloys must also have sufficient corrosion resistance, allowing them to be formed according to the usual processes and to have low residual stresses in order to be able to be machined integrally.
  • GB patent 1,172,736 discloses an alloy containing 4 to 7% Mg by weight, 1.5-2.6% Li, 0.2-1% Mn and/or 0.05-0.3% Zr, the rest aluminum, useful for applications requiring high mechanical resistance, good corrosion resistance, low density and a high modulus of elasticity.
  • U.S. Pat. No. 5,431,876 discloses a ternary group of aluminum lithium and magnesium or copper alloys, including at least one additive such as zirconium, chromium and/or manganese.
  • U.S. Pat. No. 6,551,424 describes a manufacturing process for products made of aluminum-magnesium-lithium alloy of composition (as a percentage by weight) Mg: 3.0-6.0. Li: 0.4-3.0, Zn up to 2.0, Mn up to 1.0, Ag up to 0.5, Fe up to 0.3, Si up to 0.3, Cu up to 0.3, 0.02-0.5 of an element selected from the group made up of Sc, Hf, Ti, V, Nd, Zr, Cr, Y, Be, including straight and cross cold rolling.
  • U.S. Pat. No. 6,461,566 describes an alloy composed as follows (as a percentage by weight), Li: 1.5-1.9, Mg: 4.1-6.0, Zn 0.1-1.5, Zr 0.05-0.3, Mn 0.01-0.8 H, 0.9 10 ⁇ 5 -4.5 10-5 and at least one element selected from the group Be 0.001-0.2, Y 0.001-0.5 and Sc 0.01-0.3.
  • RU patent 2171308 describes an alloy composed as follows (as a percentage by weight), Li: 1.5-3.0, Mg: 4.5-7.0, Fe 0.01-0.15, Na: 0.001-0.0015, H, 1.7 10 ⁇ 5 -4.5 10 ⁇ 5 and at least one element selected from the group Zr 0.05-0.15, Be 0.005-0.1, and Sc 0.05-0.4 and at least one element selected from the group Mn 0.005-0.3, Cr 0.005-0.2, and Ti 0.005-0.2, the rest aluminum.
  • RU patent 2163938 describes an alloy containing (as a percentage by weight by weight) Mg: 2.0-5.8. Li: 1.3-2.3, Cu: 0.01-0.3, Mn: 0.03-0.5, Be: 0.0001-0.3, and at least one element from among Zr and Sc: 0.02-0.25 and at least one element from among Ca and Ba: 0.002-0.1, the rest aluminum.
  • Patent application DE 1 558 491 describes in particular an alloy containing (in weight %) Mg: 4-7, Li: 1.5-2.6, Mn: 0.2-1.0, Zr 0.05-0.3 et/ou Ti 0.05-0.15ou Cr 0.05-0.3.
  • a first subject of the present invention is a wrought product made of aluminum alloy composed as follows, as a percentage by weight,
  • Another subject of the present invention is a manufacturing process for a wrought product according to the invention including, optionally successively,
  • Still another subject of the present invention is the use of a product of the invention to produce, for example, aircraft structural elements.
  • FIG. 1 R Curve in direction L-T (test-specimen CCT760).
  • FIG. 2 R Curve in direction T-L (test-specimen CCT760).
  • FIG. 3 Fracture toughness K app (L-T) according to the tensile yield stress R p0.2 (L) for alloys A, C and D.
  • All the indications concerning the chemical composition of the alloys are expressed as a percentage by weight based on the total weight of the alloy.
  • the expression 1.4 Cu means that the copper content expressed as a percentage by weight is multiplied by 1.4.
  • Alloys are designated in conformity with the rules of The Aluminium Association, known to those skilled in the art. The density depends on the composition and is determined by calculation rather than by a method of weight measurement. The values are calculated in compliance with the procedure of The Aluminium Association, which is described on pages 2-12 and 2-13 of “Aluminum Standards and Data”. The definitions of the metallurgical tempers are indicated in European standard EN 515.
  • the tensile static mechanical properties in other words the ultimate tensile strength R m , the conventional yield stress at 0.2% of elongation Rp 0.2 and elongation at break A %, are determined by a tensile test according to standard EN ISO 6892-1, sampling and test direction being defined by standard EN 485-1.
  • a curve giving the effective stress intensity factor as a function of the effective crack extension, known as R curve, is given according to standard ASTM E 561.
  • the critical stress intensity factor K C in other words the intensity factor which makes the crack unstable, is calculated from R curve.
  • the stress intensity factor K CO is also calculated by allotting the initial crack length at the beginning of the monotonic load, at critical load. These two values are calculated for a test-specimen of the required shape.
  • K app represents factor K CO corresponding to the test-specimen which was used to carry out the test of R curve.
  • K Ceff represents factor K C corresponding to the test-specimen which was used to carry out the test of R curve.
  • ⁇ a eff(max) represents the crack extension of the last valid point of R curve.
  • the length of R curve—namely the maximum crack extension of the curve— is a parameter that is in itself important, in particular for fuselage design.
  • “Structural element” of a mechanical construction here refers to a mechanical part for which the static and/or dynamic mechanical properties are particularly important for the performance of the structure, and for which a structural analysis is usually prescribed or performed. These are typically elements the failure of which is likely to endanger the safety of said construction, its users or others.
  • these structural elements include the parts which make up the fuselage (such as the fuselage top skin, stringers, bulkheads, circumferential frames), the wings (such as the top or bottom wing skin, stringers or stiffeners, ribs and spars) and the tail unit, made up of horizontal and vertical stabilizers, as well as floor beams, seat tracks and doors.
  • a selected grade of aluminum alloys which contain specific and critical amounts of magnesium, lithium, zirconium, titanium, iron and silicon makes it possible to manufacture wrought products having an improved compromise of properties, in particular between mechanical resistance and damage tolerance, while having good performance in terms of corrosion.
  • the magnesium content of the products according to the invention preferably lies from 4.0 to 5.0% by weight.
  • the magnesium content is at least 4.3% by weight and preferentially 4.4% by weight.
  • a maximum content of 4.7% by weight or advantageously 4.6% by weight of magnesium is preferred.
  • the lithium content of the products according to the invention preferably lies from 1.0 to 1.6% by weight.
  • the present inventors noted that a limited lithium content, in the presence of certain additional elements, makes it possible in some embodiments to very significantly improve fracture toughness and fatigue crack propagation speed, which largely compensates for the slight increase in density and the reduction in static mechanical properties.
  • the maximum lithium content is 1.5% by weight and preferably 1.45% by weight or preferentially 1.4% by weight.
  • a minimum lithium content of 1.1% by weight and preferably of 1.2% of weight is advantageous, in particular in order to improve resistance to intergranular corrosion.
  • the zirconium content of the products according to the invention preferably lies from 0.05 to 0.15% by weight and the titanium content lies from 0.01 to 0.15% by weight.
  • the presence of these elements in conjunction with the working conditions used advantageously makes it possible in some embodiments to maintain a substantially unrecrystallized granular structure.
  • the present inventors noted that it is in some cases not necessary to add scandium to these alloys to obtain the desired substantially unrecrystallized granular structure and that the addition of scandium could even prove to be detrimental by making the alloy particularly fragile and difficult to cold roll down to thicknesses less than 3 mm,
  • the scandium content is thus advantageously less than 0.01% by weight.
  • the titanium content is from 0.01 to 0.05% by weight.
  • Manganese and/or chromium may also be added to contribute in particular to control the granular structure, their content advantageously remaining at a maximum of 0.5% by weight.
  • the alloy contains at least one element from among Mn and Cr with, as a percentage by weight Mn: 0.05-0.5 or 0.05-0.3 and Cr: 0.05-0.3, and an element not chosen from among Mn and Cr having a content lower than 0.05% by weight. Improvement of hot ductility helps, in particular hot working, which enables reducing the rejection rate during transformation.
  • the alloy contains at least one element from among Ag and Cu with, as a percentage by weight Cu: 0.05-0.3 and Ag: 0.05-0.3, and an element not chosen from among Ag and Cu having a content lower than 0.05% by weight.
  • these elements can contribute, in particular, to the static mechanical properties.
  • Ag and/or Cu content are advantageously less than 0.05% by weight.
  • the wrought products according to the invention preferably contain a small quantity of iron and silicon, the content of these elements ranging from 0.02 to 0.2% by weight.
  • the present inventors think that the presence of these elements may contribute, by forming intermetallic phases and/or by contributing to forming dispersoids in particular when manganese is present, to improving damage tolerance properties by avoiding the localization of bending.
  • the Fe content and/or the Si content are as a percentage by weight, Fe: 0.04-0.15, Si: 0.04-0.15.
  • the Fe content and/or the Si content is less than 0.15% by weight and preferably less than 0.1% by weight.
  • the Zn content is preferably a maximum of 0.5% by weight. In an advantageous embodiment of the invention, the Zn content is less than 0.2% by weight and preferably lower than 0.05% by weight. Deliberate Zn addition is typically not desirable because this element can contribute to deteriorate hot ductility without providing any advantageous effect on resistance to intergranular corrosion. Moreover Zn addition contributes to increase the alloy density, which is often not desirable.
  • the products according to the invention have a maximum Be content of 5 ppm and preferably 2 ppm of Be and/or a maximum Na content of l Oppm and/or a maximum Ca content of 20 ppm.
  • the wrought products according to the invention are preferentially extruded products such as sections, rolled products such as sheets or plates and/or forged products
  • a suitable manufacturing process of the products according to the invention includes the successive steps of preparing a molten metal bath in order to obtain an aluminum alloy composed according to the invention, casting said alloy in rough shape, optionally homogenizing the product so cast, hot and optionally cold working, solution heat-treating the product so worked, and quenching, optionally cold working the product that has undergone solution heat-treatment and has been quenched, and artificial aging at a temperature of less than 150° C.
  • a molten metal bath is produced in order to obtain an aluminum alloy composed according to the invention.
  • the molten metal bath is then cast typically in rough shape, typically a rolling slab, extrusion billet, or forging stock.
  • the rough shape is then optionally homogenized in order to reach a temperature ranging from 450° C. to 550° and preferably from 480° C. to 520° C. for a length of time ranging from 5 to 60 hours.
  • the homogenization treatment can be carried out in one or more steps. However the present inventors did not note any significant advantage provided by homogenization and in a preferred embodiment of the invention, one proceeds directly to hot working following simple reheating without carrying out any homogenization.
  • Hot working typically by extrusion, rolling and/or forging, is carried out preferably with an input temperature greater than 400° C. and advantageously greater than 430° C. or even 450° C.
  • the present inventors noted that even by carrying out these intermediate heat treatment operations, they had not been able to industrially cold roll reference alloy sheets down to a thickness of 2 mm, whereas this step proved to be possible with alloy sheets according to the invention.
  • the sheets according to the invention have a preferred thickness of at least 0.5 mm and preferably of at least 0.8 mm or 1 mm.
  • the product After hot and optionally cold working, the product undergoes solution heat-treatment and is quenched. Before undergoing solution heat-treatment, it may be advantageous to carry out heat treatment at a temperature ranging from 300 to 420° C. in one or more steps, in order to improve control of the substantially unrecrystallized granular structure.
  • Solution heat-treatment is preferably carried out, according to the composition of the product, at a temperature ranging from 370 to 500° C. Quenching can be carried out, for example, in water and/or in air. It is advantageous to carry out air quenching because the intergranular corrosion properties are improved.
  • the product that undergoes solution heat-treatment and is then quenched can optionally be cold worked once more. Flattening or straightening operations are typically performed at this step but it is also possible to carry out more thorough working so as to still further improve the mechanical properties.
  • the metallurgical temper obtained for the rolled products is advantageously a T6 or T6X or T8 or T8X temper and for extruded products advantageously a T5 or T5X temper in the case of press quenching or a T6 or T6X or T8 or T8Xtemper.
  • the product finally undergoes artificial aging at a temperature of less than 150° C.
  • artificial aging is carried out in three steps: a first step at a temperature ranging from 70 to 100° C., a second step at a temperature ranging from 100 to 140° C. and a third step at a temperature ranging from 90 to 110° C., the duration of these steps being typically from 5 to 50 h.
  • substantially unrecrystallized granular structure is taken to mean an unrecrystallized granular structure content at mid-thickness greater than 70% and preferably greater than 85%.
  • the rolled products according to the invention have particularly advantageous characteristics.
  • the rolled products preferably have a thickness ranging from 0.5 mm to 15 mm, but products of thickness greater than 15 mm, up to 50 mm or even 100 mm or more may have advantageous properties.
  • the rolled products obtained by the process according to the invention have, for a thickness ranging from 0.5 to 15 mm, at mid-thickness at least one static mechanical strength property among properties (i) to (iii) and at least one damage tolerance property among properties (iv) to (vi)
  • the rolled products according to the invention typically have an improved isotropy of mechanical properties, in particular fracture toughness.
  • rolled products according to the invention such as those that have been air-quenched have a weight loss less than 20 mg/cm 2 and preferably less than 15 mg/cm 2 after the intergranular corrosion test NAMLT (“Nitric Acid Mass Loss Test” ASTM-G67).
  • the wrought products according to the invention are advantageously used to produce structural elements for aircraft, in particular airplanes.
  • Preferred aircraft structural elements are in particular a fuselage skin obtained advantageously with sheets of thickness 0.5 to 12 mm according to the invention, a fuselage framework a stringer obtained advantageously with sections according to the invention or a rib.
  • alloys A to C are reference alloys.
  • the plates were heated and hot-rolled to a thickness of approximately 4 mm. Cold-rolling tests to thickness 2 mm were carried out after heat treatment made up of two successive steps of one hour at 340° C. followed by 1 hour at 400° C. Only the alloy sheets according to the invention could be cold-rolled successfully to the final thickness, reference alloy sheets having broken at thickness 2.6 mm
  • the sheets underwent solution heat-treatment at 480° C. for 20 min, this treatment being preceded by heat treatment made up of two successive steps of one hour at 340° C. followed by 1 hour at 400° C. After solution heat-treatment, the sheets were air-quenched and flattened. Artificial aging was carried out for 10 hours at 85° C. followed by 16 hours at 120° C. followed by 10 hours at 100° C.
  • the granular structure of all the samples was substantially unrecrystallized, the rate of recrystallization at mid-thickness being less than 10%.
  • FIG. 3 shows the improvement in the compromise between yield stress and fracture toughness.
  • the improvement in K app (L-T) is greater than 25% whereas the reduction in yield stress is less than 15% compared to alloy C sheet.
  • the length of the R-curve is also significantly improved, and so ⁇ a eff(max) (T-L) is improved by more than 30%.
  • the crack propagation speed was determined as per standard E647 on CCT test-specimens of width 160 mm.
  • Air-quenched alloy sheets according to the invention have low sensitivity to intergranular corrosion for a thickness of 4 mm and are not sensitive to intergranular corrosion for a thickness of 2 mm.
  • small ingots were cast to evaluate hot ductility and intergranular corrosion properties of different alloys.
  • the size of the ingot after machining was in mm 255 ⁇ 180 ⁇ 28.
  • composition of the alloys is provided in Table 7.
  • Hot ductility was evaluated on tests samples machined from the small ingots after homogenization of 12 h at 505° C.
  • the hot ductility test was carried out with a servo hydraulic instrument provided by Servotest Testing Systems Ltd on specific test samples having a thickness of 20 mm and at a deformation rate of 1 s ⁇ 1 .
  • the test consists in the compression of a sample containing two holes. Due to the compression,
  • Alloys E and F which contain Mn and Cr have an advantageous hot ductility whereas hot ductility of reference alloy I which contains 0.6 wt. % Zn is the lowest among tested alloys.
  • the small ingots were hot rolled to a thickness of 4 mm.
  • the sheets so obtained were solution heat treated at 480° C., this treatment being preceded by a heat treatment made up of two successive steps of one hour at 345° C. followed by 1 hour at 400° C. After solution heat treatment, the sheets were air quenched and flattened by controlled stretching with a 2% permanent set. Artificial aging was carried out for 10 hours at 85° C. followed by 16 hours at 120° C. followed by 10 hours at 100° C.
  • Alloy G which in particular is different from alloy D through a lower copper content, exhibits a very low weight loss.
  • Alloy I which contains Zn is not different from alloy G for resistance to intergranular corrosion.
  • Alloy H which has a lithium content lower than that of the other tested alloys, exhibits a higher weight loss.

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US13/473,303 2011-05-20 2012-05-16 Aluminum magnesium lithium alloy with improved fracture toughness Abandoned US20120291925A1 (en)

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US201161488196P 2011-05-20 2011-05-20
FR11/01555 2011-05-20
FR1101555A FR2975403B1 (fr) 2011-05-20 2011-05-20 Alliage aluminium magnesium lithium a tenacite amelioree
US13/473,303 US20120291925A1 (en) 2011-05-20 2012-05-16 Aluminum magnesium lithium alloy with improved fracture toughness

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EP (1) EP2710163B1 (fr)
CN (1) CN103687971B (fr)
BR (1) BR112013029789B1 (fr)
CA (1) CA2836531C (fr)
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CN104533228A (zh) * 2014-12-25 2015-04-22 常熟市古里镇鑫良铝合金门窗厂 一种耐腐蚀铝合金用门框
CN105483576A (zh) * 2015-12-18 2016-04-13 西南铝业（集团）有限责任公司 一种铝锂合金型材生产时表面黑白斑点控制方法
US20160160320A1 (en) * 2013-07-11 2016-06-09 Aleris Rolled Products Germany Gmbh Method of producing aluminium alloys containing lithium
US9365917B1 (en) * 2014-03-24 2016-06-14 The United States Of America As Represented By The Administrator Of The National Aeronatics And Space Administration Method of heat treating aluminum—lithium alloy to improve formability
WO2017064407A1 (fr) * 2015-10-15 2017-04-20 Constellium Issoire Toles minces en alliage aluminium-magnesium-zirconium pour applications aerospatiales
CN106834828A (zh) * 2017-02-27 2017-06-13 广东兴发铝业有限公司 一种海工装备用铝合金及其制备方法
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US20170218493A1 (en) * 2014-09-29 2017-08-03 Constellium Issoire Method for manufacturing products made of magnesium-lithium-aluminum alloy
US10465263B2 (en) 2013-07-11 2019-11-05 Aleris Rolled Products Germany Gmbh System and method for adding molten lithium to a molten aluminium melt
US10835942B2 (en) 2016-08-26 2020-11-17 Shape Corp. Warm forming process and apparatus for transverse bending of an extruded aluminum beam to warm form a vehicle structural component
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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FR3026410B1 (fr) * 2014-09-29 2019-07-26 Constellium Issoire Produit corroye en alliage aluminium magnesium lithium
CN105369170A (zh) * 2015-12-18 2016-03-02 西南铝业（集团）有限责任公司 一种铝锂合金型材黑白斑点控制方法
FR3057476B1 (fr) * 2016-10-17 2018-10-12 Constellium Issoire Toles minces en alliage aluminium-magnesium-scandium pour applications aerospatiales
CN106769305A (zh) * 2016-12-16 2017-05-31 西南铝业（集团）有限责任公司 2a97铝锂合金标准样品制备方法
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FR3077524B1 (fr) * 2018-02-08 2021-01-15 C Tec Constellium Tech Center Procede de fabrication d'une piece en alliage d'aluminium et de chrome
CN113661262B (zh) * 2019-04-05 2023-10-03 奥科宁克技术有限责任公司 冷成型铝锂合金的方法
CN110952003B (zh) * 2019-12-23 2021-05-11 江西理工大学 一种高强耐蚀Al-Mg-Sc-Zr合金及其制备方法

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US10465263B2 (en) 2013-07-11 2019-11-05 Aleris Rolled Products Germany Gmbh System and method for adding molten lithium to a molten aluminium melt
US9783871B2 (en) * 2013-07-11 2017-10-10 Aleris Rolled Products Germany Gmbh Method of producing aluminium alloys containing lithium
US20160160320A1 (en) * 2013-07-11 2016-06-09 Aleris Rolled Products Germany Gmbh Method of producing aluminium alloys containing lithium
US9365917B1 (en) * 2014-03-24 2016-06-14 The United States Of America As Represented By The Administrator Of The National Aeronatics And Space Administration Method of heat treating aluminum—lithium alloy to improve formability
US20170292180A1 (en) * 2014-09-29 2017-10-12 Constellium Issoire Wrought product made of a magnesium-lithium-aluminum alloy
US20170218493A1 (en) * 2014-09-29 2017-08-03 Constellium Issoire Method for manufacturing products made of magnesium-lithium-aluminum alloy
CN104453552A (zh) * 2014-12-25 2015-03-25 常熟市古里镇鑫良铝合金门窗厂 一种安全防摔铝合金门框
CN104533228A (zh) * 2014-12-25 2015-04-22 常熟市古里镇鑫良铝合金门窗厂 一种耐腐蚀铝合金用门框
WO2017064407A1 (fr) * 2015-10-15 2017-04-20 Constellium Issoire Toles minces en alliage aluminium-magnesium-zirconium pour applications aerospatiales
FR3042508A1 (fr) * 2015-10-15 2017-04-21 Constellium Issoire Toles minces en alliage aluminium-magnesium-zirconium pour applications aerospatiales
CN105483576A (zh) * 2015-12-18 2016-04-13 西南铝业（集团）有限责任公司 一种铝锂合金型材生产时表面黑白斑点控制方法
US10835942B2 (en) 2016-08-26 2020-11-17 Shape Corp. Warm forming process and apparatus for transverse bending of an extruded aluminum beam to warm form a vehicle structural component
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
CN106834828A (zh) * 2017-02-27 2017-06-13 广东兴发铝业有限公司 一种海工装备用铝合金及其制备方法
CN106868363A (zh) * 2017-02-27 2017-06-20 广东兴发铝业有限公司 一种铝合金钻杆材料及其制备方法
CN106939385A (zh) * 2017-02-27 2017-07-11 广东兴发铝业有限公司 一种全铝挂车用铝合金及其制备方法

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CA2836531A1 (fr) 2012-11-29
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FR2975403B1 (fr) 2018-11-02
CN103687971B (zh) 2018-01-05
BR112013029789B1 (pt) 2019-10-22
FR2975403A1 (fr) 2012-11-23
CN103687971A (zh) 2014-03-26
BR112013029789A2 (pt) 2017-01-17
CA2836531C (fr) 2019-07-23

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