Classifications

• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
  • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
  • B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
  • B22D11/003—Aluminium alloys
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
  • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
  • B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
  • B22D11/041—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds for vertical casting
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
  • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
  • B22D21/002—Castings of light metals
  • B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
• • C—CHEMISTRY; METALLURGY
  • C21—METALLURGY OF IRON
  • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
  • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
  • C21D1/26—Methods of annealing
• • 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
  • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C21/00—Alloys based on aluminium
  • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
  • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
• • 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
• • 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
• • 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
  • C22F1/043—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 silicon as the next major constituent

Definitions

• the invention relates to the field of aluminum alloy sheets for the manufacture of bodywork parts or automotive structure also called "white box”.
• the invention relates to the use of such sheets having excellent formability in stamping, thus making it possible to produce pieces of complex geometry or requiring deep stampings such as for example a door liner or a load floor.
• the sheets used according to the invention are particularly suitable for the production of complex parts dimensioned in rigidity.
• the static mechanical characteristics in tension in other words the tensile strength R m , the conventional yield stress at 0.2% elongation Rp 0; 2 , and the elongation at break A% are determined by a tensile test according to standard NF EN ISO 6892-1.
• Aluminum alloys are increasingly used in the automotive industry to reduce the weight of vehicles and thus reduce fuel consumption and greenhouse gas emissions.
• the aluminum alloy sheets are used in particular for the manufacture of many parts of the "white box” among which are distinguished body skin parts (or outer body panels) such as the front wings, roofs or pavilions, skins hood, trunk or door, and lining parts or body structure components such as door linings, hood, or load floors (cockpit and trunk).
• body skin parts or outer body panels
• skins hood or pavilions
• skins hood or trunk or door
• lining parts or body structure components such as door linings, hood, or load floors (cockpit and trunk).
• alloys for application in body skin results from a compromise between sometimes conflicting requirements such as: formability, final mechanical strength after baking paints, yield strength during shaping, crimping ability, surface quality, ability to assemble, corrosion resistance, cost, recyclability, etc.
• alloys of the Al-Mg-Si type have been retained to date, that is to say alloys of the AA6xxx series.
• alloys AA6016, AA6016A, AA6005A, AA6014, as far as Europe is concerned, and alloys AA61 11 and AA6022 in the United States, are the most used for this type of applications, in thicknesses of the order of 1mm, mainly because of their relatively good formability in stamping and crimping in the "hardened” state T4, their high hardening during the baking of the paints and their excellent surface appearance after shaping.
• alloys of the AA5xxx (Al-Mg) series with a limited magnesium content (typically Mg ⁇ 5%) are, to date, the most used, mainly because they offer a good compromise between formability in the annealed state or state O, mechanical properties after shaping, thermal stability and resistance to corrosion in service.
• the most commonly used alloys are AA5182, AA5754, and AA5454.
• the elongation A 50 rupture of the AA3003 type alloy which is nevertheless known for its good ductility associated with a yield strength R p o, 2 of 40 MPa, has its elongation at 50 drop to substantially 25 % when magnesium is added to increase the yield strength R p0j2 up to 70 MPa, as appears for alloy AA3004.
• the aim of the invention is to obtain this compromise of ductility and of optimum yield strength, by proposing an aluminum alloy sheet for automotive structure components, also known as a "white box", having a significantly improved formability that is stable over time. and better than the state of the art, and allowing the realization by conventional embossing at room temperature of automotive parts of complex geometry unrealizable from the aluminum alloy sheets currently used in the field of automotive construction.
• This sheet must also have a minimum of mechanical strength, but also a very good resistance to corrosion and especially filiform corrosion.
• the subject of the invention is the use of an aluminum alloy sheet for the manufacture of a stamped part of a bodywork or bodywork structure, also called a "blank body", characterized in that said sheet has a limit of elasticity Rp 0; 2 greater than or equal to 60 MPa and an axial tensile elongation A 80 greater than or equal to 34%.
• said sheet has a hole expansion ratio, known to those skilled in the art under the name HER (Hole Expansion Ratio), greater than 50, or even greater than or equal to 55.
• HER Hole Expansion Ratio
• its composition is as follows (% by weight): Si: 0.15 - 0.50; Fe: 0.3 - 0.7; Cu: 0.05 - 0.10; Mn: 1.0 - 1.5 or even 1.0 - 1.2 and better 1.1 - 1.2; other elements ⁇ 0.05 each and ⁇ 0.15 in total, remains aluminum.
• the Fe content is at least 0.3%.
• the preferred Si content is from 0.15 to 0.30%.
• the method of manufacturing said sheet comprises the following steps: Vertical continuous or semi-continuous casting of a plate and scalping said plate, Homogenization at a temperature of at least 600 ° C for at least 5 hours, preferably at least 6 hours, followed by controlled cooling to a temperature of 550 to 450 ° C, typically 490 ° C, at least 7 hours, preferably at least 9 hours, then cooling to room temperature in at least 24 hours with, advantageously, controlled slow cooling to substantially 150 ° C in at least 15 hours, preferably at least 15 hours. 16 hours.
• wetting typically by planing in tension or between rollers or by "skin pass", with a rate comprised between 1 and 10%,
• the degree of hardening mentioned above is between 1 and 5%.
• the chemical etching is carried out, after alkaline degreasing, in acid medium with a loss of mass of the sheet of at least 0.2 g / m and per face.
• the invention also encompasses a stamped part of bodywork or body structure manufactured by stamping from a sheet having at least one of the aforementioned characteristics. It is chosen, for example, in the group comprising interior panels or door liners, cabin floor, boot floor, spare wheel housing or cockpit side.
• Figure 1 shows a schematic section of the tooling used to measure the hole expansion ratio (HER) with A in the blank, B the punch and C the matrix.
• Figure 2 specifies the dimensions in mm of the tools used to determine the value of the parameter known to those skilled in the art under the name of LDH (Limit Dome Height) characteristic of the drawability of the material.
• LDH Limit Dome Height
• FIG 3 shows a motor vehicle door structure with, in the foreground, the inner panel typically achievable from a sheet according to the invention.
• the invention is based on the finding made by the applicant that it was entirely possible to use, for stamped body panels or bodywork structure also called "white box", sheets having excellent ductility, especially due to an elongation at break of 80 greater than or equal to typically 34%, and a sufficient mechanical strength, in particular because of a yield strength Rp 0.2 greater than or equal to typically 60 MPa, as well as very good resistance to filiform corrosion.
• Such use has the advantage of excellent formability, especially in stamping, allowing the realization of automotive parts of complex geometry not feasible with aluminum alloys commonly used in the automotive industry. It also allows the conversion of aluminum steel with very little modification of the shape of the tools designed for forming steels other than those related to taking into account the greater thickness of the sheet metal. aluminum alloy used.
• a typical alloy composition for the sheet used according to the invention is as follows (% by weight): Si: 0.15 - 0.50; Fe: 0.3 - 0.7 and better 0.5 - 0.7; Cu: 0.05 - 0.10; Mn: 1.0 - 1.5 and better 1, 0-1, 2 or 1.1-1.2; other elements ⁇ 0.05 each and ⁇ 0, 15 in total, remains aluminum.
• the most advantageous range of content is 0.15 to 0.30%.
• Fe a minimum content of 0.3%, and better still 0.5%, substantially reduces the solubility of manganese in solid solution, which makes it possible to obtain a sensitivity to the rate of positive deformation, delays the rupture during the deformation after necking, and thus improves ductility and formability. Iron is also necessary for the formation of a high density of intermetallic particles guaranteeing good "hardenability" during shaping.
• Mn a minimum content of 1.0% is necessary to obtain the required level of mechanical characteristics and to form sufficient precipitates providing a good "hardenability”.
• the range of the most advantageous content is 1.0 to 1.2 or even 1.1 to 1.2%.
• Mg its content is limited to that of an impurity (less than 0.05%).
• An addition of magnesium could increase the mechanical characteristics by solid solution but would very strongly decrease the sensitivity to the speed of deformation and therefore the ductility.
• Zn in the same way, its content is limited to that of an impurity (less than 0.05% or even 0.01%) because, like magnesium, remaining in solid solution, it would also decrease the sensitivity to the speed of deformation and thus the formability.
• impurity less than 0.05% or even 0.01%
• the manufacture of the sheets for use according to the invention mainly comprises the casting, typically vertical semi-continuous plates followed by their scalping.
• the plates are then homogenized at a temperature of at least 600 ° C for at least 5 hours, preferably at least 6 hours, followed by controlled cooling to a temperature of 550 to 450 ° C, typically 490 ° C. C, in at least 7 hours, preferably at least 9 hours, then cooling to room temperature in at least 24 hours with, advantageously, controlled slow cooling to substantially 150 ° C in at least 15 hours preferably at least 16 hours.
• This type of homogenization of the bi-bearing type, with controlled cooling makes it possible to "expel" the manganese from the solid solution by precipitation with the effect of obtaining a good formability thanks to:
• the sheets or coils are then annealed at a temperature of at least 350 ° C.
• the strip or sheet for use according to the invention is then subjected to work hardening with a permanent deformation rate of between 1 and 10%, and preferably between 1 and 5%.
• This work-hardening can be obtained for example by rolling with a low reduction of the "skin pass" type, or by planing under tension in tension, or between rollers.
• This work hardening has the effect of significantly increasing the mechanical strength, including the elastic limit, without significant impact on the elongation at break or ductility.
• This disturbed layer depends on the rolling conditions and the reduction in thickness experienced by the sheet; the stripping must therefore be adapted according to these parameters.
• the sheet in question is at least 0.2 g / m and per side, better still 0.3 g / m or even 0.4 g / m 2 .
• the examples below show very good results obtained for a value of 0.5 g / m which can therefore be an optimal minimum.
• It can be made either from a coil on a continuous line of chemical surface treatments, by spraying or immersing the unwound strip, or on cut sheet blanks, by immersion in baths.
• the sheet or strip is subjected to a series of treatments comprising at least one etching step and a series of rinses.
• the purpose of the latter is to remove the chemical residues left at the outlet of the pickling bath or baths.
• Table 1 summarizes the chemical compositions in percentages by weight (% by weight) of the alloys used during the tests. They are identified by A, Al, A2, B under the abbreviated name "Compo. In Table 2.
• the plates of cases 1 to 6 were subjected to a homogenization treatment at 610 ° C consisting of a temperature rise in 16 hours up to 600 ° C, a hold of 8 hours between 600 and 610 ° C then controlled cooling to 490 ° C in 9 hours, and then to room temperature in about a day.
• the plates of cases 7 and 8 underwent a shorter homogenization treatment consisting of a rise at 610 ° C without holding followed by cooling at 530 ° C in 5 hours, followed directly by hot rolling.
• Comparative Examples 9 and 10 consisting of AA6016 and AA5182 type alloys, have undergone standard homogenizations for these types of alloys.
• the next hot rolling step is first carried out on a reversible rolling mill up to a thickness of about 40 mm and then on a hot tandem rolling mill with 4 stands up to a thickness of 3.2 mm.
• This hot-rolling step is preceded for the case 1 to 6 of a reheating which makes it possible to bring the temperature of the foundry plate from the ambient temperature to the rolling start temperature of 500 ° C. in 9 hours. .
• This hot rolling step is followed by a cold rolling step which makes it possible to obtain sheets 1.15 mm thick.
• a final annealing then allows a recrystallization of the alloys so as to obtain a state O.
• This annealing was carried out in passage furnace for the cases 1 to 4 and 6 to 8 and consisted bringing the metal to a temperature of 410 ° C in about 10 seconds and then cooling it.
• the recrystallization annealing was carried out in a static oven and consisted in bringing the metal to a temperature of 350 ° C. in 6 hours.
• the recrystallization annealing took place in a pass-through oven and consisted of bring the metal to a temperature of 365 ° C in about 30 seconds and then cool.
• alloy AA6016 type the cold rolling was also followed by a heat treatment at the end of the range but it is different and consists of a solution and quenching performed in a passage oven by raising the metal temperature up to 540 ° C in about 30 seconds and quenching.
• a chemical etching of the mechanically disturbed layer resulting from the rolling was also carried out in a reel on a continuous line.
• the sheet has undergone a series of surface treatments including, after an alkaline degreasing and rinsing, a stripping step with sulfuric and hydrofluoric acids.
• the attack rate measured by loss of mass on a sample immersed in the pickling bath, was 1.2 g / m 2 per face in 1 minute.
• the pickling was carried out by spraying on the strip followed by triple rinsing.
• the loss of mass at the end of the treatment was 0.5 g / m 2 per face for cases 2 to 5.
• the stripping was less extensive and the mass loss was 0.10 g / m2.
• the sheet is passed through a tensioning machine, so as to slightly plastically deform the material between 1 and 5%.
• specimens have in particular a width of 20 mm and a calibrated length of 120 mm.
• cases 2 to 5 are the only ones to combine elongation at break values A 80 greater than or equal to 34% combined with conventional yield strength values.
• Rp 0 , 2 greater than or equal to 60 MPa.
• Case 1 corresponding to a sheet that has not undergone the planing step, has a lower value of Rp 0> 2 equal to 49 MPa.
• Case 7 corresponding to a sheet having not undergone a homogenization of the type of that described in this invention, has an elongation value at break A 8 o lower and lower than 34% although the value of Rp 0 , 2 only 55 MPa.
• Case 8 corresponding to a sheet of composition outside the invention, has a much smaller elongation A 80 .
• the test consists of stamping with a flat-bottomed punch of diameter 202 mm (see Figure 1) a blank having at its center a circular hole of diameter 100 mm. Stamping is done on blanked side. Blocking of the blank between the die and the blank holder is ensured by means of a retaining ring and a pressure of 13 MPa exerted by the blank clamp.
• the circular hole of 100 mm diameter is made in the center of a circular blank of 350 mm diameter by water jet cutting.
• the speed of movement of the punch is 40 mm / min. The movement of the punch stops when the force on the punch falls by 100 daN / 0.2 s, which corresponds to the beginning of a crack from the edge of the hole. The test is finished.
• HER (Df-Di) / Di where Di is the initial diameter of the hole in the blank (here 100 mm) and Df is the final diameter of the hole after stopping the test.
• cases 2 to 5 are the only ones to combine HER hole expansion ratio values greater than 50 or even 55 with conventional yield strength values Rp. 0, 2 greater than or equal to 60 MPa.
• Case 1 corresponding to a sheet that did not undergo the planing step, has a HER value greater than 50 but associated with a low Rp 0.2 value of 49 MPa.
• the other comparative cases (7 to 10) have HER values significantly lower than those of the plates according to the invention. Measurement of LDH (Limit Dome Height).
• the LDH parameter is widely used for the evaluation of the drawability of sheets with a thickness of 0.5 to 2 mm. It has been the subject of many publications, including that of R. Thompson, "The LDH test to evaluate sheet metal formability - Final Report of the LDH Committee of the North American Deep Drawing Research Group," SAE conference, Detroit, 1993, SAE Paper No. 930815. This is a trial of stamping a blank blocked at the periphery by a ring. The blanking pressure is controlled to prevent slippage in the rod. The blank, dimensions 120 x 160 mm, is biased in a mode close to the plane strain. The punch used is hemispherical.
• Figure 2 shows the dimensions of the tools used to perform this test.
• Table 2 shows the LDH parameter values obtained on specimens of
• case 1 also has an LDH value greater than 32 mm, but associated with a value of Rp 0> 2 quite low equal to 49 MPa.
• case 6 has a value of Rp 0, 2 high, equal to 94 MPa, but associated with an LDH value of less than 32 mm.
• Comparative Examples 7 to 9 corresponding to sheets that have not undergone the homogenization treatment or whose chemical composition is outside the invention, have LDH values that are significantly lower than those of the sheets according to the invention.
• the filiform corrosion resistance was evaluated and compared to that of AA6016-T4 alloy sheets usually used in the field of automobile bodywork.
• specimens coated with a cataphoresis layer are used. These painted specimens are then scratched, placed in a corrosive atmosphere to initiate corrosion, then exposed to controlled conditions of temperature and humidity favoring filiform corrosion according to standard NF EN 3665. After an exposure time of 1000 hours in climatic chamber at 40 ⁇ 2 ° C and 82 ⁇ 3% humidity, the degree of filiform corrosion is assessed according to standard NF EN 3665 method 3.
• the degreasing is carried out by immersing for 10 minutes in a "Almeco" bath with a concentration of 18 to 40 g / l and 65 ° C. During this degreasing attack the "metal" is about 0.3 g / m 2 or about 1 10 nm.
• the phosphating treatment is carried out by immersion according to the Chemetall instruction manual "Die Phosphatierung als Vor anger vor der Lacktechnik"("Phosphating as pretreatment for painting"). During this step the etching of the metal is about 0.9 g / m 2 or about 330 nm.
• the phosphate-free conversion treatment, by hydrolysis and condensation of polysiloxanes, or Oxsilan®, is carried out by dipping in a bath of Oxsilan® MM0705A at 25 g / l with a withdrawal rate of 25 cm / min, which corresponds to a deposit of about 4 mg Si / m 2 . During this step the metal is not attacked.
• the cataphoresis product used is CathoGuard® 800 from BASF, an epoxy-based lacquer.
• the thickness of the targeted cataphoresis layer is 23 microns; it is obtained by a deposit of 2 minutes in a bath at 30 ° C with a voltage of 260 V, followed by baking for 15 minutes at 175 ° C.
• the filiform corrosion resistance is considered good (index O) if there is no attack or if a beginning of filiform corrosion takes place in the form of few filaments and a length of less than 2 mm.
• the resistance to filiform corrosion is considered insufficient in the opposite case (index X).
• case 8 all the cases tested, with the exception of case 8, have good resistance to filiform corrosion if the cataphoresis is preceded by a degreasing and phosphating (surface treatment 2).

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Mechanical Engineering (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Thermal Sciences (AREA)
• Crystallography & Structural Chemistry (AREA)
• Physics & Mathematics (AREA)
• Shaping Metal By Deep-Drawing, Or The Like (AREA)
• Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
• Other Surface Treatments For Metallic Materials (AREA)
• Metal Rolling (AREA)
• Heat Treatment Of Sheet Steel (AREA)
• Manufacturing & Machinery (AREA)
• Combustion & Propulsion (AREA)
• Transportation (AREA)
• ing And Chemical Polishing (AREA)
• Automobile Manufacture Line, Endless Track Vehicle, Trailer (AREA)
• Body Structure For Vehicles (AREA)

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• 2013
  • 2013-07-11 FR FR1301644A patent/FR3008427B1/fr active Active
• 2014
  • 2014-07-09 EP EP17162984.3A patent/EP3199655A3/de not_active Withdrawn
  • 2014-07-09 DE DE17162984.3T patent/DE17162984T1/de active Pending
  • 2014-07-09 JP JP2016524857A patent/JP6625530B2/ja not_active Expired - Fee Related
  • 2014-07-09 CN CN201480039612.XA patent/CN105378125B/zh active Active
  • 2014-07-09 RU RU2016104405A patent/RU2690253C2/ru active
  • 2014-07-09 DE DE14758586.3T patent/DE14758586T1/de active Pending
  • 2014-07-09 EP EP14758586.3A patent/EP3019637B1/de active Active
  • 2014-07-09 WO PCT/FR2014/000160 patent/WO2015004340A1/fr not_active Ceased
  • 2014-07-09 BR BR112016000278A patent/BR112016000278B1/pt not_active IP Right Cessation
  • 2014-07-09 KR KR1020167003517A patent/KR20160030563A/ko not_active Abandoned
  • 2014-07-09 US US14/903,729 patent/US10253402B2/en active Active

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