CN102869799B - Aluminium die casting alloy - Google Patents
Aluminium die casting alloy Download PDFInfo
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- CN102869799B CN102869799B CN201180016277.8A CN201180016277A CN102869799B CN 102869799 B CN102869799 B CN 102869799B CN 201180016277 A CN201180016277 A CN 201180016277A CN 102869799 B CN102869799 B CN 102869799B
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Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/20—Accessories: Details
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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
Abstract
Aluminum die casting alloy comprising 2 to 6 % by weight nickel, 0.1 to 0.4 % by weight zirconium, 0.1 to 0.4 % by weight vanadium, optionally up to 5 % by weight manganese, optionally up to 2 % by weight iron, optionally up to 1 % by weight titanium, optionally total max. 5 % by weight transition elements including scandium, lanthanum, yttrium, hafnium, niobium, tantalum, chromium and/or molybdenum, and aluminum as the remainder with further elements and impurities due to production total max. 1 % by weight.
Description
Technical field
The present invention relates to aluminium alloy, it can be undertaken processing by conventional high-pressure die casting and be dispersion-strengthened, age-hardenable, and has useful mechanical property when temperatures as high at least 300 DEG C.
Background technology
Aluminium alloy is one of most important lightweight material adopted in the automotive industry, and this is mainly because they have high specific tenacity.The conventional ceralumin of major part is based on aluminium-silicon eutectic system, and this is because it has excellent casting characteristics.Unfortunately, the solidus curve in this individual system is no more than 550 DEG C, and therefore the maximum operating temperature of aluminum-silicon alloy is limited in about 200 DEG C.In addition, the main alloying element (i.e. zinc, magnesium and copper) in conventional aluminum base alloy has high diffustivity in aluminium sosoloid.Therefore, although these elements put forward heavy alloyed room temperature strength, they compromise the thermostability of alloy.Such as, the aluminium alloy based on Al-Zn-Mn, Al-Cu-Mg and Al-Li system can reach very high tensile strength (being up to about 700MPa); But their mechanical property declines rapidly when they at high temperature use.In numerous applications, the stability of the mechanical property under high temperature---instead of high strength---is primary.Therefore conventional aluminium alloy cannot be used in this type of application, and needs a kind of lightweight, heat-staple material.
Prior art
Attempt the ceralumin that the thermostability with enhancing is provided in the prior art.At these trial Notables is that those use aluminium-nickel systems and with the addition of the alloy of a small amount of zirconium.Following journal of writings is the representative during these are attempted:
N.A.Belov, " Structure and Strength of Cast Alloys of the System Aluminum-Nickel-Zirconium, " Metallov, No.10,19-22 page, 1993.
N.A.Belov, " Principles of Optimizing the Structure of Creep-Resisting Casting Aluminum Alloys using Transition Metals, " Journal of Advanced Materials, 1st volume, No.4,321-329 page, 1994.
N.A.Belov, V.S.Zolotorevsky, S.Goto, A.N.Alabin, V.V.Istomin-Kastrovsky, and V.I.Mishin, " Effect of Zirconium on Liquidus and Hardening of Al-6% Ni Casting Alloy, " Metals Forum, the 28th volume, 533-538 page, 2004.
Aforesaid journal of writings is pointed out, the optimum structure at high temperature demonstrating the aluminium alloy of stability can be prepared on a kind of basis of eutectic composition, described eutectic composition by with at least 0.6 % by weight aluminium sosoloid (alpha-aluminum) phase of zirconium alloy, with the second-phase with high creep strength, i.e. nickel three aluminium (nickel tri-aluminide, Al3Ni) composition.
Aforesaid journal of writings is also pointed out, is obtained through the solid alloy composition (aluminium, aluminium nickel master alloy and aluminium zirconium hardener) of carefully weighing by melting at about 900 DEG C by the object of these reasonable offer.This relatively high melt temperature is to be dissolved in by high zirconium content (zirconium of >=0.6 % by weight) in aluminium and to obtain homogeneous aluminium-nickel-zirconium melt necessary.In addition, aforesaid journal of writings is pointed out, aluminium-nickel-zirconium melt must cool under the speed of cooling faster than 10 DEG C/sec, solidifies and at room temperature keep the homogeneous supersaturated solid solution of zirconium in alpha-aluminum to make it.In addition, aforesaid journal of writings is pointed out, when material cools from melt temperature, it can by casting and being configured as required goods in a mold.Described mould must allow material to be cooled to room temperature more than the speed of 10 DEG C/sec from melt temperature.Finally, aforesaid journal of writings is pointed out, casting solid articles can between 350 DEG C and 450 DEG C of temperature ageing treatment, make alloy hardening meticulous zirconium three aluminium (Al to precipitate
3zr) particle.
After suitably being processed, the alloy that aforesaid journal of writings is set forth has better mechanical property at elevated temperatures compared with the ceralumin of routine.But, except the content of zirconium in non-alloyed is more than 0.4 % by weight, otherwise there will not be sclerosis in the alloy of setting forth at aforesaid journal of writings, and be at least 0.6 % by weight except the content of zirconium in non-alloyed, otherwise there will not be remarkable sclerosis.The Second Phase Particle that the zirconium of small amount can not produce the volume with the remarkable sclerosis of enough inducing alpha-aluminum sosoloid (is Al in the case
3zr).Fig. 1 describes the alloy for prior art, the solids content variation with temperature existed in melt.This figure demonstrates alloy and only just can melt completely when temperature is more than 850 DEG C.The alloy that so high temperature of fusion makes aforesaid journal of writings set forth cannot be processed as molded article by conventional high-pressure die casting, because the temperature that can be incorporated into the melt in the pressure chamber of conventional high-pressure pressure die-casting machine should more than 750 DEG C.
High rate of cooling---more than 10 DEG C/sec---is necessary at room temperature keeping the zirconium of 0.6 % by weight in alpha-aluminum in sosoloid.Except Hpdc, cannot reach in the goods that the casting technique that so fast rate of cooling passes through routine at great majority is cast.Therefore, except casting minimum goods in graphite or copper mould, the alloy that aforesaid journal of writings is set forth cannot be processed as molded article by conventional casting technique.
Summary of the invention
The present invention relates to a class aluminium alloy, it is (i) dispersion-strengthened, (ii) can carry out age hardening to improve mechanical property, and (iii) can by conventional high-pressure die-casting process to be created on the molded article up to having useful mechanical property at least 300 DEG C of temperature.
An object of the present invention is to provide lightweight, wear-resistant and corrosion-resistant material, it can be cast by conventional high-pressure pressure casting method and be heat-staple at up at least 300 DEG C of temperature.
Aforesaid object is reached by a kind of aluminum diecasting alloy according to the present invention, and it comprises
The nickel of 2 to 6 % by weight,
The zirconium of 0.1 to 0.4 % by weight,
The vanadium of 0.1 to 0.4 % by weight,
Optionally be up to the manganese of 5 % by weight,
Optionally be up to the iron of 2 % by weight,
Optionally be up to the titanium of 1 % by weight,
With the aluminium as residuum, and be altogether up to the impurity of 1 % by weight due to production.
A preferred nickel scope is 4 to 6 % by weight, and a preferred zirconium scope is 0.1 to 0.3 % by weight, and a preferred vanadium scope is 0.3 to 0.4 % by weight.
Alloy of the present invention has general chemical constitution: aluminium-nickel-zirconium-vanadium, and its chemical constitution optimum turns to and makes its liquidus temperature lower than 750 DEG C.
After melt solidification, nickel and aluminium define a kind of eutectic structure, by the sosoloid of nickel in aluminium (being called alpha-aluminum phase) with by nickel three aluminium (Al
3ni) the second-phase composition formed.With the alloy phase ratio not containing eutectic composition in microtexture, the alloy containing eutectic composition in microstructure has narrower solidification range, is therefore less inclined to generation hot tearing.Al
3ni phase exists with the form of thin rod, and the diameter of described thin rod is in 300 to 500nm scope.If be cooled to room temperature from melt temperature to carry out obtaining enough fast (such as, the speed with more than 10 DEG C/sec), then zirconium and vanadium also will be dissolved in alpha-aluminum phase.After the controlled thermal life process of solid alloy subsequently, zirconium and vanadium are combined with aluminium by solid state reaction, and formation chemical constitution is Al
3zr
xv
1-xreinforced deposition phase.The metastable Al of submicron-scale
3zr
xv
1-xparticle has L1
2cubic crystal structure, and be distributed in equably in alpha-aluminum sosoloid.
Alloy of the present invention also can comprise the manganese being up to 5 % by weight and the iron being up to 2 % by weight.Except forming metal aluminide (its can further reinforced alloys), iron and manganese are also useful compositions in Hpdc alloy, because they tend to alleviate the welding of alloy to stamping die parts.
Alloy of the present invention also can comprise the magnesium being up to 2 % by weight, the hafnium being up to 2 % by weight, be up to 1 % by weight titanium, be up to 1 % by weight molybdenum, be up to 1 % by weight chromium, be up to 0.5 % by weight silicon, be up to the copper of 0.5 % by weight and be up to the zinc of 0.5 % by weight.
Alloy of the present invention preferably includes the Al of substantially homogeneous dispersion
3zr
xv
1-xparticle, wherein x is a part of one, and it depends on the ratio of Zr:V in alloy, and described particle has and is less than about 50nm and the equivalent diameter being preferably less than about 30nm.
Alloy of the present invention preferably includes to have and is less than about 500nm, is preferably less than about 300nm and is less than the Al of equivalent diameter of about 100nm especially
3ni particle.
Alloy of the present invention can comprise the calorize manganese particle of substantially homogeneous dispersion, and it has the equivalent diameter being less than about 50nm, being preferably less than about 30nm.
Alloy of the present invention can comprise the iron aluminide particle of substantially homogeneous dispersion, and it has the equivalent diameter being less than about 50nm, being preferably less than about 30nm.
Itself and prior art are comprised nickel and zirconium by one of alloy of the present invention, but the feature that the aluminium alloy (being described in the journal of writings of N.A.Belov) not comprising vanadium makes a distinction is alloy of the present invention has much lower liquidus temperature (be usually less than 750 DEG C, relative to prior art alloy higher than 850 DEG C).Lower liquidus temperature makes alloy of the present invention be processed as molded article by conventional high-pressure die casting, and the alloy of prior art is not processed as molded article by conventional high-pressure die casting, and is therefore restricted to casts little goods in graphite jig.
Itself and prior art are comprised nickel and zirconium by another of alloy of the present invention, but the feature that the aluminium alloy not comprising vanadium makes a distinction is precipitation hardening particle in alloy of the present invention is Al
3zr
xv
1-xparticle is (with the Al in prior art alloy
3zr Particle Phase ratio).Due to compared with the size (0.159nm) of zirconium atom, the size (0.132nm) of vanadium atom is less, so Al
3zr
xv
1-xthe lattice parameter of lattice is less than Al
3the lattice parameter of Zr lattice, and it more mates the lattice parameter of alpha-aluminum matrix.Due to this reason, use Al
3zr
xv
1-xthe aluminum-nickel alloy ratio Al of precipitation hardening
3the aluminum-nickel alloy of Zr precipitation hardening is more thermally-stabilised.
Foregoing and other feature of the present invention and advantage will become clearer from the following detailed description and accompanying drawing.
Accompanying drawing explanation
Fig. 1 is the solidification path of aluminium-6 % by weight nickel-0.6 % by weight zirconium alloy of a Practical computer teaching;
Fig. 2 is the solidification path of aluminium-6 % by weight nickel-0.1 % by weight zirconium-0.4 % by weight vanadium alloy of a Practical computer teaching.
Embodiment
The dispersion-strengthened of aluminium alloy depends on the generation of dispersed granules in alloy substrate.This strengthening mechanism with the alloy based on aluminium-nickel system for typical case.The aluminum-nickel alloy of hypoeutectic and eutectic is at a kind of nickel three aluminium (Al containing fine dispersion
3solidify in the structure of Ni) particle, described particle is in the matrix be made up of the sosoloid of nickel in aluminium (alpha-aluminum).Because nickel three aluminium is insoluble to aluminium substantially when being up to about 855 DEG C, aluminum-nickel alloy is more stable than aluminum-silicon alloy at elevated temperatures.But aluminium-nickel binary alloy does not possess enough mechanical propertys, because their room temperature tensile yield strength is no more than 80MPa concerning most of automobile application; And therefore these alloys need extra strengthening.
Precipitation strength is that well-known strengthening is with the mechanism being typical aluminium alloy based on the alloy of Solder for Al-Cu Joint Welding system.In these alloys, in alpha-aluminum matrix, the precipitation of calorize copper particle is by thermal control, to produce the efficient hardening of alloy substrate.
The present invention, in conjunction with the characteristic of the sclerosis mechanism of previously described two types, obtains the aluminium alloy most of automobile application to enough raising thermomechanical intensity.Alloy of the present invention contains creep resistance nickel three aluminum particulate of fine dispersion and the reinforced deposition based on zirconium and vanadium, i.e. Al
3zr
xv
1-x.
Comprise nickel and zirconium in prior art, but do not comprise in the alloy (being described in the journal of writings of N.A.Belov) of vanadium, form one and there is chemical constitution Al
3the strengthening phase of Zr.In alloy of the present invention, strengthening phase is also based on Al
3zr structure, but vanadium atom instead of part zirconium atom.The Precise Representation of the strengthening phase in alloy of the present invention is Al
3zr
xv
1-x, wherein x is a part of one, and its size depends on zirconium: vanadium ratio.The effect that vanadium plays in alloy of the present invention is very important for making alloy be processed as goods by Hpdc.Relevant with the size of the volume fraction of precipitation and deposit seeds by the degree of strengthening of precipitation induction.The small sized particles of large volume fraction is very important for strengthening.Prior art alloy is in order to produce the Al of about 0.83 volume %
3zr strengthening phase adopts the minimum zirconium of 0.6 % by weight.Demonstrate, this content is enough for the remarkable strengthening of alloy.But demonstrate the investigation of Fig. 1, the liquidus temperature of the alloy containing 0.6% zirconium is more than 850 DEG C.This relatively high melt temperature does not allow to use conventional Hpdc, and therefore the alloy of prior art is not produced in a large number by Hpdc operation.A preferred form of alloy of the present invention adopts the only zirconium of 0.1 % by weight and the vanadium of 0.4 % by weight.This mixture produces the Al of about 0.84 volume %
3zr
xv
1-xstrengthening phase.In alloy of the present invention, adopt the main advantage of vanadium to be that the liquidus temperature of alloy of the present invention is only about 730 DEG C---see Fig. 2, it allows using conventional high-pressure die casting by during alloy production molded article of the present invention.
The wide in range description of material of the present invention after optimal processing is, it is a kind of alpha-aluminum (the pole dilution sosoloid of nickel in aluminium) matrix, its containing the 0.8-1.0 volume % that has an appointment based on zirconium and vanadium and have by chemical formula Al
3zr
xv
1-xthe homogeneous distribution strengthening phase of the structure represented, and homogeneous nickel three aluminum particulate be dispersed in alloy substrate of about 1-10 volume %.Have in the material of maximum strength of the present invention being processed as, Al
3zr
xv
1-xreinforcing particle is metastable, has L1
2cubic structure, links together with alpha-aluminum matrix, and has the mean diameter being less than about 25nm.
The generation of this structure needs: (1) cools fast from melt temperature, and the controlled thermal life process of (2) cured article.
It is necessary for cooling fast from melt temperature, to guarantee that zirconium and vanadium are at room temperature retained in alpha-aluminum matrix with solution; That is, at room temperature containing Al
3the alloy of Ni eutectic phase and second-phase (zirconium and vanadium supersaturated solid solution in alpha-aluminum).For alloy of the present invention, the rate of cooling more than 10 DEG C/sec is necessary, to obtain a kind of zirconium and the supersaturated solid solution of vanadium in alpha-aluminum.One of the advantage of alloy of the present invention alloy is compared to existing technology that it designed to be able to by conventional high-pressure die casting and is processed as molded article, and the molten alloy wherein at about 750 DEG C of temperature is introduced directly in the pressure chamber of pressure die-casting machine.It is under high pressure injected in a steel die subsequently; Pressure on maintenance alloy, until completion of cure, then discharges cured article.Known in conventional high-pressure die casting operation rate of cooling usually more than 10 DEG C/sec.Therefore, make the castmethod of article formation also be provided as and obtain strengthening element (zirconium and vanadium) the necessary quenching of homogeneous supersaturated solid solution in alpha-aluminum.
Necessary with the controlled thermal life process of the solidification cast product of reasonable offer of the present invention, with by metastable L1
2cube Al
3zr
xv
1-xreinforcing particle is deposited in alpha-aluminum sosoloid.This can have been come by a kind of thermal life handling procedure of optimization.This program comprises solidification cast product is remained on 2-6 hour between 250 DEG C and the temperature of 350 DEG C, holds it in 2-6 hour between 350 DEG C and the temperature of 450 DEG C subsequently.A kind of preferred thermal life handling procedure comprise solidification cast product remained on 350 DEG C 3 hours, subsequently it is kept 3 hours again at 450 DEG C.With by Al
3zr
xv
1-xthe while that reinforcing particle being deposited in alpha-aluminum sosoloid, the thermal life handling procedure of specifying is smashed and changes Al
3the shape of Ni eutectic rod and become the particle of submicron-scale.Al
3cracked and the nodularization of Ni eutectic rod improves the overall ductility of cast product.
Although the present invention has shown with regard to its detailed embodiment and described, it will be appreciated by persons skilled in the art that not departing from the spirit and scope of the present invention for required protection, the various changes in form and details can have been made.
Claims (13)
1. aluminum diecasting alloy, it comprises
The nickel of 4 to 6 % by weight,
The zirconium of 0.1 to 0.3 % by weight,
The vanadium of 0.3 to 0.4 % by weight,
Optionally be up to the manganese of 5 % by weight,
Optionally be up to the iron of 2 % by weight,
Optionally be up to the titanium of 1 % by weight,
With the aluminium as residuum, and due to produce total be up to 1 % by weight impurity.
2. the aluminum diecasting alloy of claim 1, it also comprises
Be up to the hafnium of 2 % by weight,
Be up to the magnesium of 2 % by weight,
Be up to the chromium of 1 % by weight,
Be up to the molybdenum of 1 % by weight,
Be up to the silicon of 0.5 % by weight,
Be up to the copper of 0.5 % by weight,
Be up to the zinc of 0.5 % by weight.
3. the aluminum diecasting alloy any one of claim 1 to 2, it comprises the Al of substantially homogeneous dispersion
3zr
xv
1-xparticle, wherein x is a part of one, and it depends on the ratio of Zr:V in alloy, and described particle has the equivalent diameter being less than 50nm.
4. the aluminum diecasting alloy of claim 3, wherein Al
3zr
xv
1-xparticle has the equivalent diameter being less than 30nm.
5. the aluminum diecasting alloy any one of claim 1 to 2, it comprises the Al with the equivalent diameter being less than 500nm
3ni particle.
6. the aluminum diecasting alloy of claim 5, it comprises the Al of the equivalent diameter being less than 300nm
3ni particle.
7. the aluminum diecasting alloy of claim 5, it comprises the Al of the equivalent diameter being less than 100nm
3ni particle.
8. the aluminum diecasting alloy any one of claim 1 to 2, it comprises the calorize manganese particle of substantially homogeneous dispersion, and described particle has the equivalent diameter being less than 50nm.
9. the aluminum diecasting alloy of claim 8, wherein calorize manganese particle has the equivalent diameter being less than 30nm.
10. the aluminum diecasting alloy any one of claim 1 to 2, it comprises the iron aluminide particle of substantially homogeneous dispersion, and described particle has the equivalent diameter being less than 50nm.
The aluminum diecasting alloy of 11. claims 10, wherein iron aluminide particle has the equivalent diameter being less than 30nm.
The die-cast part that 12. aluminum alloy any one of claim 1 to 6 are standby.
The method of the die-cast part that the aluminum alloy of 13. 1 kinds of productions any one of claim 1 to 6 is standby, its interalloy, by keeping 2-6 hour by the temperature of solidification die-cast part between 250 DEG C and 350 DEG C, to keep at the temperature subsequently between 350 DEG C and 450 DEG C 2-6 hour and by age hardening.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP10159192 | 2010-04-07 | ||
| EP10159192.3 | 2010-04-07 | ||
| PCT/EP2011/055318 WO2011124590A1 (en) | 2010-04-07 | 2011-04-06 | Aluminium die casting alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102869799A CN102869799A (en) | 2013-01-09 |
| CN102869799B true CN102869799B (en) | 2015-06-03 |
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ID=42978206
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201180016277.8A Expired - Fee Related CN102869799B (en) | 2010-04-07 | 2011-04-06 | Aluminium die casting alloy |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US20130199680A1 (en) |
| EP (2) | EP2396436B1 (en) |
| JP (1) | JP2013528699A (en) |
| KR (1) | KR20130067242A (en) |
| CN (1) | CN102869799B (en) |
| AU (1) | AU2011237946A1 (en) |
| BR (1) | BR112012025191A2 (en) |
| CA (1) | CA2793148A1 (en) |
| ES (1) | ES2529473T3 (en) |
| MX (1) | MX2012011575A (en) |
| PL (1) | PL2653578T3 (en) |
| RU (1) | RU2570264C2 (en) |
| WO (1) | WO2011124590A1 (en) |
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- 2011-04-06 US US13/634,358 patent/US20130199680A1/en not_active Abandoned
- 2011-04-06 PL PL13176662T patent/PL2653578T3/en unknown
- 2011-04-06 MX MX2012011575A patent/MX2012011575A/en not_active Application Discontinuation
- 2011-04-06 JP JP2013503092A patent/JP2013528699A/en active Pending
- 2011-04-06 EP EP11712263.0A patent/EP2396436B1/en not_active Not-in-force
- 2011-04-06 WO PCT/EP2011/055318 patent/WO2011124590A1/en active Application Filing
- 2011-04-06 KR KR1020127024129A patent/KR20130067242A/en not_active Application Discontinuation
- 2011-04-06 CN CN201180016277.8A patent/CN102869799B/en not_active Expired - Fee Related
- 2011-04-06 ES ES13176662.8T patent/ES2529473T3/en active Active
- 2011-04-06 RU RU2012145233/02A patent/RU2570264C2/en not_active IP Right Cessation
- 2011-04-06 BR BR112012025191A patent/BR112012025191A2/en not_active IP Right Cessation
- 2011-04-06 AU AU2011237946A patent/AU2011237946A1/en not_active Abandoned
- 2011-04-06 EP EP13176662.8A patent/EP2653578B1/en not_active Not-in-force
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Also Published As
| Publication number | Publication date |
|---|---|
| CN102869799A (en) | 2013-01-09 |
| EP2396436A1 (en) | 2011-12-21 |
| EP2396436B1 (en) | 2013-07-24 |
| WO2011124590A1 (en) | 2011-10-13 |
| AU2011237946A1 (en) | 2012-09-27 |
| CA2793148A1 (en) | 2011-10-13 |
| EP2653578A1 (en) | 2013-10-23 |
| RU2570264C2 (en) | 2015-12-10 |
| EP2653578B1 (en) | 2014-09-17 |
| BR112012025191A2 (en) | 2016-06-21 |
| RU2012145233A (en) | 2014-05-20 |
| PL2653578T3 (en) | 2015-03-31 |
| ES2529473T3 (en) | 2015-02-20 |
| JP2013528699A (en) | 2013-07-11 |
| MX2012011575A (en) | 2012-12-05 |
| KR20130067242A (en) | 2013-06-21 |
| US20130199680A1 (en) | 2013-08-08 |
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