CA2792432A1 - Process for producing die-cast parts - Google Patents
Process for producing die-cast parts Download PDFInfo
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- CA2792432A1 CA2792432A1 CA2792432A CA2792432A CA2792432A1 CA 2792432 A1 CA2792432 A1 CA 2792432A1 CA 2792432 A CA2792432 A CA 2792432A CA 2792432 A CA2792432 A CA 2792432A CA 2792432 A1 CA2792432 A1 CA 2792432A1
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- Prior art keywords
- aluminum alloy
- working space
- kneading
- nanoparticles
- die
- Prior art date
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- Abandoned
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- 238000000034 method Methods 0.000 title claims description 25
- 230000008569 process Effects 0.000 title claims description 25
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 55
- 239000007787 solid Substances 0.000 claims abstract description 51
- 238000004898 kneading Methods 0.000 claims abstract description 49
- 238000004512 die casting Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 238000010008 shearing Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- XUGISPSHIFXEHZ-GPJXBBLFSA-N [(3r,8s,9s,10r,13r,14s,17r)-10,13-dimethyl-17-[(2r)-6-methylheptan-2-yl]-2,3,4,7,8,9,11,12,14,15,16,17-dodecahydro-1h-cyclopenta[a]phenanthren-3-yl] acetate Chemical compound C1C=C2C[C@H](OC(C)=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 XUGISPSHIFXEHZ-GPJXBBLFSA-N 0.000 claims description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 2
- OVHDZBAFUMEXCX-UHFFFAOYSA-N benzyl 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OCC1=CC=CC=C1 OVHDZBAFUMEXCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000567 combustion gas Substances 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 2
- OLQSNYOQJMTVNH-UHFFFAOYSA-N germanium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Ge+4] OLQSNYOQJMTVNH-UHFFFAOYSA-N 0.000 claims description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010118 rheocasting Methods 0.000 description 1
- 238000010117 thixocasting Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B22D17/007—Semi-solid pressure die casting
-
- 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
- B22D17/08—Cold chamber machines, i.e. with unheated press chamber into which molten metal is ladled
- B22D17/10—Cold chamber machines, i.e. with unheated press chamber into which molten metal is ladled with horizontal press motion
-
- 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
- B22D17/30—Accessories for supplying molten metal, e.g. in rations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D25/00—Special casting characterised by the nature of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Molds, Cores, And Manufacturing Methods Thereof (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Continuous Casting (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
In a method for producing die-cast parts from an aluminum alloy, the aluminum alloy is exposed to high shear forces in a mixing and kneading machine (30) having a housing (31) having a working chamber (34) enclosed by an inner housing jacket (32) and a worm shaft (36), which rotates about a longitudinal axis (x) and moves back and forth in a translational manner along the longitudinal axis (x) in the inner housing jacket (32) and which is provided with kneading blades (38), and having kneading pins (38), which are fastened to the inner housing jacket (32) and which protrude into the working chamber (34), wherein liquid aluminum alloy is fed into the working chamber (34) at one end of the housing (31) and removed from the working chamber (34) as partially solidified aluminum alloy having a specified solid fraction at the other end of the housing (31), transferred into a filling chamber (12) of a die-casting machine (10), and pushed into a mold by means of a piston (20), wherein the solid fraction of the aluminum alloy is set to the specified solid fraction in the working chamber (34) by specific cooling and heating of the working chamber (34).
Description
Process for producing die-cast parts The invention relates to a process for producing die-cast parts made of an aluminum alloy.
Die-cast parts made of aluminum alloys are being used ever more frequently, inter alia, in the automotive industry for reasons of an increasing demand for weight reduction. For casting technology reasons, it is generally the case that a cast part wall thickness of about 2 mm cannot be undershot, for example in the case of nodes for space frame structures, with conventional die-casting processes. The filling of the die-casting mold with partially solid metal melts by using thixocasting or rheocasting leads to better filling of the mold and, as a result, to a possible further reduction in the cast part wall thickness to about 1 mm. As the wall thickness decreases, however, the reduced force-absorption capability increasingly becomes a limiting factor. This disadvantage by itself could be countered by the addition of nanoparticles to an aluminum alloy matrix. However, there is a lack of suitable processes for cost-effectively producing aluminum alloys reinforced with nanoscale particles and for the preparation thereof to form partially solid metal melts for die casting.
The invention is based on the object of providing a process of the type mentioned in the introduction, with which process a partially solid aluminum alloy melt can be provided continuously in a cost-effective manner and further processed to form die-cast parts. It is a further object of the invention to provide a process for producing die-cast parts which are reinforced with nanoparticles and are made of an aluminum alloy, with which process a partially solid aluminum alloy melt can be provided continuously in a cost-effective manner under the action of shearing forces typical of the process with a high fine dispersion of nanoparticles and further processed to form die-cast parts.
The first object is achieved according to the invention in that the aluminum alloy is exposed to high shearing forces in a mixing and kneading machine, having a housing with a working space, which is surrounded by an inner housing sleeve, and a worm shaft, which rotates about a longitudinal axis and moves to and fro translationally in the longitudinal axis in the inner housing sleeve and is provided with kneading blades, and with kneading bolts, which are fastened to the inner housing sleeve and protrude into the working space, wherein liquid aluminum alloy is fed to the working space at one end of the housing and, at the other end of the housing, is removed from the working space as partially solid aluminum alloy with a predefined solids content, is transferred into a filling chamber of a die-casting machine and is introduced into a casting mold by means of a piston, wherein the solids content of the aluminum alloy in the working space is set to the predefined solids content by cooling and heating the working space in a targeted manner. Here, the high shearing forces present in the kneading process in the partially solidified phase state continuously comminute dendritic branches which form, and this leads to an increased ductility of the die-cast parts. The high compression forces additionally lead to a greater transfer of heat, which ultimately makes it possible to set the solids content in the aluminum alloy more precisely.
The second object is achieved according to the invention in that nanoparticles are mixed with the aluminum alloy and finely dispersed in the aluminum alloy by high shearing forces in a mixing and kneading machine, having a housing with a working space, which is surrounded by an inner housing sleeve, and a worm shaft, which rotates about a longitudinal axis and moves to and fro translationally in the longitudinal axis in the inner housing sleeve and is provided with kneading blades, and with kneading bolts, which are fastened to the inner housing sleeve and protrude into the working space, wherein liquid aluminum alloy and nanoparticles are fed to the working space at one end of the housing and, at the other end of the housing, are removed from the working space as partially solid aluminum alloy with a predefined solids content and with nanoparticles finely dispersed in the aluminum alloy, are transferred into a filling chamber of a die-casting machine and are introduced into a casting mold by means of a piston, wherein the solids content of the aluminum alloy in the working space is set to the predefined solids content by cooling and heating the working space in a targeted manner. Here, in addition to the comminution of dendritic branches which form and the resultant higher ductility, the high shearing forces present in the kneading process in the partially solidified phase state finely disperse the nanoparticles, which is required for the strength-increasing effect thereof.
It is expedient that the inner housing sleeve is surrounded by an outer housing sleeve such that an intermediate space preferably in the form of a hollow cylinder is formed, and cold and/or hot gases are conducted through the intermediate space for cooling and heating the working space. Air, preferably compressed air, is preferably conducted through the intermediate space for cooling, and hot gases, preferably combustion gases, are preferably conducted through the intermediate space for heating.
The gases are preferably conducted through the intermediate space in countercurrent to the direction in which the aluminum alloy is transported.
Die-cast parts made of aluminum alloys are being used ever more frequently, inter alia, in the automotive industry for reasons of an increasing demand for weight reduction. For casting technology reasons, it is generally the case that a cast part wall thickness of about 2 mm cannot be undershot, for example in the case of nodes for space frame structures, with conventional die-casting processes. The filling of the die-casting mold with partially solid metal melts by using thixocasting or rheocasting leads to better filling of the mold and, as a result, to a possible further reduction in the cast part wall thickness to about 1 mm. As the wall thickness decreases, however, the reduced force-absorption capability increasingly becomes a limiting factor. This disadvantage by itself could be countered by the addition of nanoparticles to an aluminum alloy matrix. However, there is a lack of suitable processes for cost-effectively producing aluminum alloys reinforced with nanoscale particles and for the preparation thereof to form partially solid metal melts for die casting.
The invention is based on the object of providing a process of the type mentioned in the introduction, with which process a partially solid aluminum alloy melt can be provided continuously in a cost-effective manner and further processed to form die-cast parts. It is a further object of the invention to provide a process for producing die-cast parts which are reinforced with nanoparticles and are made of an aluminum alloy, with which process a partially solid aluminum alloy melt can be provided continuously in a cost-effective manner under the action of shearing forces typical of the process with a high fine dispersion of nanoparticles and further processed to form die-cast parts.
The first object is achieved according to the invention in that the aluminum alloy is exposed to high shearing forces in a mixing and kneading machine, having a housing with a working space, which is surrounded by an inner housing sleeve, and a worm shaft, which rotates about a longitudinal axis and moves to and fro translationally in the longitudinal axis in the inner housing sleeve and is provided with kneading blades, and with kneading bolts, which are fastened to the inner housing sleeve and protrude into the working space, wherein liquid aluminum alloy is fed to the working space at one end of the housing and, at the other end of the housing, is removed from the working space as partially solid aluminum alloy with a predefined solids content, is transferred into a filling chamber of a die-casting machine and is introduced into a casting mold by means of a piston, wherein the solids content of the aluminum alloy in the working space is set to the predefined solids content by cooling and heating the working space in a targeted manner. Here, the high shearing forces present in the kneading process in the partially solidified phase state continuously comminute dendritic branches which form, and this leads to an increased ductility of the die-cast parts. The high compression forces additionally lead to a greater transfer of heat, which ultimately makes it possible to set the solids content in the aluminum alloy more precisely.
The second object is achieved according to the invention in that nanoparticles are mixed with the aluminum alloy and finely dispersed in the aluminum alloy by high shearing forces in a mixing and kneading machine, having a housing with a working space, which is surrounded by an inner housing sleeve, and a worm shaft, which rotates about a longitudinal axis and moves to and fro translationally in the longitudinal axis in the inner housing sleeve and is provided with kneading blades, and with kneading bolts, which are fastened to the inner housing sleeve and protrude into the working space, wherein liquid aluminum alloy and nanoparticles are fed to the working space at one end of the housing and, at the other end of the housing, are removed from the working space as partially solid aluminum alloy with a predefined solids content and with nanoparticles finely dispersed in the aluminum alloy, are transferred into a filling chamber of a die-casting machine and are introduced into a casting mold by means of a piston, wherein the solids content of the aluminum alloy in the working space is set to the predefined solids content by cooling and heating the working space in a targeted manner. Here, in addition to the comminution of dendritic branches which form and the resultant higher ductility, the high shearing forces present in the kneading process in the partially solidified phase state finely disperse the nanoparticles, which is required for the strength-increasing effect thereof.
It is expedient that the inner housing sleeve is surrounded by an outer housing sleeve such that an intermediate space preferably in the form of a hollow cylinder is formed, and cold and/or hot gases are conducted through the intermediate space for cooling and heating the working space. Air, preferably compressed air, is preferably conducted through the intermediate space for cooling, and hot gases, preferably combustion gases, are preferably conducted through the intermediate space for heating.
The gases are preferably conducted through the intermediate space in countercurrent to the direction in which the aluminum alloy is transported.
The solids content of the aluminum alloy is preferably set to 40 to 80%, in particular to more than 50%.
In a preferred embodiment of the process according to the invention, the partially solid aluminum alloy is removed from the working space as a partially solid metal strand. The continuously emerging, partially solid metal strand is split into partially solid metal portions and the partially solid metal portions are transferred into the filling chamber of the die-casting machine.
The content of the nanoparticles in the alloy is preferably between about 0.1 and 10% by weight.
Suitable, cost-effective nanoparticles consist preferably of fumed silica, such as e.g. Aerosil .
However, it is also possible to use other nanoparticles, such as e.g. the known carbon nanotubes (CNT) and also further, nanoscale particles which are produced, for example, by the known Aerosil process and are made of metal and semimetal oxides, such as e.g. aluminum oxide (A1203), titanium dioxide (TiO2), zirconium oxide (Zr02) , antimony(III) oxide, chromium(III) oxide, iron(III) oxide, germanium(IV) oxide, vanadium(V) oxide or tungsten(VI) oxide.
Further advantages, features and details of the invention will become apparent from the following description of preferred exemplary embodiments and with reference to the drawing, which serves merely for elucidation and is not to be interpreted as having a limiting effect. Schematically, in the drawing, figure 1 shows a longitudinal section through a die-casting machine with an upstream mixing and kneading machine;
-figure 2 shows a longitudinal section through part of a mixing and kneading machine;
figure 3 shows a cross section through the mixing and 5 kneading machine shown in figure 1;
figure 4 shows characteristic shearing and stretching flow fields in a product mass, triggered by a kneading blade moving past a kneading bolt;
figure 5 shows the continuous production of partially solid starting material for die casting with an arrangement according to figure 1.
A plant, shown in figure 1, for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy has a die-casting machine 10 and a mixing and kneading machine 30 upstream of the die-casting machine 10.
The die-casting machine 10, which is shown only in part in the drawing, is a commercially available machine for conventionally die casting aluminum alloys and has, inter alia, a filling chamber 12, which is connected to a stationary side 18 of a casting mold, with an opening 16 for receiving the metal which is to be ejected from the filling chamber 12 and introduced into a mold cavity 14 of the casting mold by means of a piston 20.
The mixing and kneading machine 30 is shown in detail in figures 2 and 3. The basic design of such a mixing and kneading machine is known, for example, from CH-A-278 575. The mixing and kneading machine 30 has a housing 31 with a working space 34, which is surrounded by an inner housing sleeve 32 and in which there is arranged a worm shaft 36, which rotates about a longitudinal axis x and moves to and fro translationally in the longitudinal axis x in the inner housing sleeve 32. The worm shaft 36 is interrupted in the circumferential direction such that individual kneading blades 38 are formed. Axial through openings 40 are thereby formed between the individual kneading blades 38. Kneading bolts 42 protrude from the inner side of the inner housing sleeve 32 into the working space 34. The kneading bolts 42 on the housing side engage into the axial through openings 40 of the kneading blades 38 arranged on the main or worm shaft 36. A drive shaft 44 arranged concentrically to the worm shaft 36 is guided out of the inner housing sleeve 32 at the end and is connected to a drive unit (not shown in the drawing) for executing a rotational movement of the worm shaft 36. A device interacting with the worm shaft 36 for executing the translational movement of the worm shaft 36 is likewise not shown in the drawing.
The cylindrical inner housing sleeve 32 of the mixing and kneading machine 30, which delimits the working space 34, is surrounded by a cylindrical outer housing sleeve 46. The inner housing sleeve 32 and the outer housing sleeve 46 form a dual sleeve and thereby enclose an intermediate space 48 in the form of a hollow cylinder.
An introduction opening 50 for feeding liquid aluminum alloy and optionally nanoparticles into the working space 34 is provided at that end of the housing 31 which is close to the drive side of the worm shaft 36.
Although only one introduction opening 50 is shown in the drawing, two separate introduction openings for the aluminum alloy and for the nanoparticles can be provided. In principle, it is also possible to admix the nanoparticles with the liquid aluminum alloy even before the metal is introduced into the kneading and mixing machine 30. An outlet opening 52 for removing partially solid aluminum alloy optionally with nanoparticles dispersed therein is provided at that end of the inner housing sleeve 32 which is remote from the drive side of the worm shaft 36.
Inlet openings 54, 56 for introducing cold or hot gases into the intermediate space 48 are provided in the outer housing sleeve 46 at that end of the housing 31 which is remote from the drive side of the worm shaft 36. Correspondingly, outlet openings 58, 60 for the discharge of the gases from the intermediate space 48 are provided at that end of the housing 31 which is close to the drive side of the worm shaft 36. In order to ensure a maximum throughflow of gas, which is distributed uniformly over the circumference of the inner housing sleeve 32, from the inlet openings 54, 56 to the outlet openings 58, 60, and thus a uniform discharge of heat from the working space 34 or a uniform introduction of heat into the working space 34, the inlet and outlet openings 54, 56 and 58, 60, respectively, are according to figure 3 arranged distributed uniformly about the circumference of the outer housing sleeve 46.
Figure 4 shows, in a schematic illustration, characteristic shearing and stretching flow fields in a product mass P, as triggered by a kneading blade 38 moving past a kneading bolt 42 in the case of a mixing and kneading machine 30 formed according to the prior art. The direction in which the kneading blade 38 rotates is indicated schematically by a curved arrow A, whereas the translational movement of the kneading blade 38 is indicated by a double-headed arrow B. The rotational movement of the kneading blade 38 means that its tip splits the product mass P, as indicated by arrows C, D. There is a gap 41, the width of which varies depending on the rotation and translational movement of the worm shaft 36, between the kneading bolt 42 and the main face 39 of the kneading blade 38, which faces toward the kneading bolt 42, and the kneading blade 38 moving past the latter. A shearing process is brought about in the product mass P in this gap 41, as indicated by arrow E. The product mass P
expands and reorientates itself both upstream and downstream of the kneading bolt 42, as indicated by rotation arrows F, G. As already mentioned in the introduction, there is a maximum convergence of the kneading blade 38 and the kneading bolt 42 and thus a maximum shearing rate in the product mass P per shearing cycle owing to the sinusoidal axial movement of the respective kneading blade 38 on a line.
In the text which follows, the mode of operation of the plant for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy is explained in more detail, by way of example, with reference to figures 1 and 2.
An aluminum alloy melt kept just above the liquidus temperature of the alloy is fed to the working space 34 in metered form alone or together with nanoparticles via the introduction opening 50. The pinching of the partially solidified aluminum alloy with nanoparticles between the kneading blades 38 and the kneading bolts 42 results in the application of high shearing forces, which both lead to the comminution of dendritic branches and finely disperse the nanoparticles present in the form of agglomerates. Efficient, homogenizing mixing results from the combination of a radial and longitudinal mixing effect. By controlling the flow of cold and hot gases through the intermediate space 48 between the inner housing sleeve 32 and the outer housing sleeve 46, the solids content of the aluminum alloy in the working space 34 is set such that it is in the desired range when the metal is removed through the outlet opening 52.
In a preferred embodiment of the process according to the invention, the partially solid aluminum alloy is removed from the working space as a partially solid metal strand. The continuously emerging, partially solid metal strand is split into partially solid metal portions and the partially solid metal portions are transferred into the filling chamber of the die-casting machine.
The content of the nanoparticles in the alloy is preferably between about 0.1 and 10% by weight.
Suitable, cost-effective nanoparticles consist preferably of fumed silica, such as e.g. Aerosil .
However, it is also possible to use other nanoparticles, such as e.g. the known carbon nanotubes (CNT) and also further, nanoscale particles which are produced, for example, by the known Aerosil process and are made of metal and semimetal oxides, such as e.g. aluminum oxide (A1203), titanium dioxide (TiO2), zirconium oxide (Zr02) , antimony(III) oxide, chromium(III) oxide, iron(III) oxide, germanium(IV) oxide, vanadium(V) oxide or tungsten(VI) oxide.
Further advantages, features and details of the invention will become apparent from the following description of preferred exemplary embodiments and with reference to the drawing, which serves merely for elucidation and is not to be interpreted as having a limiting effect. Schematically, in the drawing, figure 1 shows a longitudinal section through a die-casting machine with an upstream mixing and kneading machine;
-figure 2 shows a longitudinal section through part of a mixing and kneading machine;
figure 3 shows a cross section through the mixing and 5 kneading machine shown in figure 1;
figure 4 shows characteristic shearing and stretching flow fields in a product mass, triggered by a kneading blade moving past a kneading bolt;
figure 5 shows the continuous production of partially solid starting material for die casting with an arrangement according to figure 1.
A plant, shown in figure 1, for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy has a die-casting machine 10 and a mixing and kneading machine 30 upstream of the die-casting machine 10.
The die-casting machine 10, which is shown only in part in the drawing, is a commercially available machine for conventionally die casting aluminum alloys and has, inter alia, a filling chamber 12, which is connected to a stationary side 18 of a casting mold, with an opening 16 for receiving the metal which is to be ejected from the filling chamber 12 and introduced into a mold cavity 14 of the casting mold by means of a piston 20.
The mixing and kneading machine 30 is shown in detail in figures 2 and 3. The basic design of such a mixing and kneading machine is known, for example, from CH-A-278 575. The mixing and kneading machine 30 has a housing 31 with a working space 34, which is surrounded by an inner housing sleeve 32 and in which there is arranged a worm shaft 36, which rotates about a longitudinal axis x and moves to and fro translationally in the longitudinal axis x in the inner housing sleeve 32. The worm shaft 36 is interrupted in the circumferential direction such that individual kneading blades 38 are formed. Axial through openings 40 are thereby formed between the individual kneading blades 38. Kneading bolts 42 protrude from the inner side of the inner housing sleeve 32 into the working space 34. The kneading bolts 42 on the housing side engage into the axial through openings 40 of the kneading blades 38 arranged on the main or worm shaft 36. A drive shaft 44 arranged concentrically to the worm shaft 36 is guided out of the inner housing sleeve 32 at the end and is connected to a drive unit (not shown in the drawing) for executing a rotational movement of the worm shaft 36. A device interacting with the worm shaft 36 for executing the translational movement of the worm shaft 36 is likewise not shown in the drawing.
The cylindrical inner housing sleeve 32 of the mixing and kneading machine 30, which delimits the working space 34, is surrounded by a cylindrical outer housing sleeve 46. The inner housing sleeve 32 and the outer housing sleeve 46 form a dual sleeve and thereby enclose an intermediate space 48 in the form of a hollow cylinder.
An introduction opening 50 for feeding liquid aluminum alloy and optionally nanoparticles into the working space 34 is provided at that end of the housing 31 which is close to the drive side of the worm shaft 36.
Although only one introduction opening 50 is shown in the drawing, two separate introduction openings for the aluminum alloy and for the nanoparticles can be provided. In principle, it is also possible to admix the nanoparticles with the liquid aluminum alloy even before the metal is introduced into the kneading and mixing machine 30. An outlet opening 52 for removing partially solid aluminum alloy optionally with nanoparticles dispersed therein is provided at that end of the inner housing sleeve 32 which is remote from the drive side of the worm shaft 36.
Inlet openings 54, 56 for introducing cold or hot gases into the intermediate space 48 are provided in the outer housing sleeve 46 at that end of the housing 31 which is remote from the drive side of the worm shaft 36. Correspondingly, outlet openings 58, 60 for the discharge of the gases from the intermediate space 48 are provided at that end of the housing 31 which is close to the drive side of the worm shaft 36. In order to ensure a maximum throughflow of gas, which is distributed uniformly over the circumference of the inner housing sleeve 32, from the inlet openings 54, 56 to the outlet openings 58, 60, and thus a uniform discharge of heat from the working space 34 or a uniform introduction of heat into the working space 34, the inlet and outlet openings 54, 56 and 58, 60, respectively, are according to figure 3 arranged distributed uniformly about the circumference of the outer housing sleeve 46.
Figure 4 shows, in a schematic illustration, characteristic shearing and stretching flow fields in a product mass P, as triggered by a kneading blade 38 moving past a kneading bolt 42 in the case of a mixing and kneading machine 30 formed according to the prior art. The direction in which the kneading blade 38 rotates is indicated schematically by a curved arrow A, whereas the translational movement of the kneading blade 38 is indicated by a double-headed arrow B. The rotational movement of the kneading blade 38 means that its tip splits the product mass P, as indicated by arrows C, D. There is a gap 41, the width of which varies depending on the rotation and translational movement of the worm shaft 36, between the kneading bolt 42 and the main face 39 of the kneading blade 38, which faces toward the kneading bolt 42, and the kneading blade 38 moving past the latter. A shearing process is brought about in the product mass P in this gap 41, as indicated by arrow E. The product mass P
expands and reorientates itself both upstream and downstream of the kneading bolt 42, as indicated by rotation arrows F, G. As already mentioned in the introduction, there is a maximum convergence of the kneading blade 38 and the kneading bolt 42 and thus a maximum shearing rate in the product mass P per shearing cycle owing to the sinusoidal axial movement of the respective kneading blade 38 on a line.
In the text which follows, the mode of operation of the plant for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy is explained in more detail, by way of example, with reference to figures 1 and 2.
An aluminum alloy melt kept just above the liquidus temperature of the alloy is fed to the working space 34 in metered form alone or together with nanoparticles via the introduction opening 50. The pinching of the partially solidified aluminum alloy with nanoparticles between the kneading blades 38 and the kneading bolts 42 results in the application of high shearing forces, which both lead to the comminution of dendritic branches and finely disperse the nanoparticles present in the form of agglomerates. Efficient, homogenizing mixing results from the combination of a radial and longitudinal mixing effect. By controlling the flow of cold and hot gases through the intermediate space 48 between the inner housing sleeve 32 and the outer housing sleeve 46, the solids content of the aluminum alloy in the working space 34 is set such that it is in the desired range when the metal is removed through the outlet opening 52.
The desired solids content of the aluminum alloy is set by measuring the change in viscosity of the metal melt in the kneading and mixing machine 30. The viscosity, which rises as the solids content of the partially solid aluminum alloy increases, can be determined, for example, by measuring the rotational resistance at the drive shaft 44 of the worm shaft 36. By determining the rotational resistance for defined solids contents, it is possible to specify appropriate setpoint values, to which measured actual values are regulated by controlling the flow of cold and hot gases through the intermediate space 48 between the inner housing sleeve 32 and the outer housing sleeve 46.
The aluminum alloy having the desired solids content and optionally comprising finely dispersed nanoparticles is introduced via the introduction opening 16 into the filling chamber 12 of the die-casting machine 10, and is injected intermittently from the latter into the mold cavity 14 of the casting mold from the filling chamber 12 in a known manner by means of the piston 20.
With reference to figure 5, the text which follows provides a more detailed explanation, by way of example, of the continuous production of partially solid, bar-shaped starting material for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy. The mode of operation explained above with reference to figures 1 and 2 is retained.
The aluminum alloy having the desired solids content and optionally comprising finely dispersed nanoparticles is continuously ejected via the outlet opening 52 in the form of a partially solid metal strand 70. Partially solid metal portions 72 are cut to -length from the partially solid metal strand 70, for example using a rotating blade. The partially solid metal portions 72 usually each correspond to the quantity of metal required for producing an individual 5 die-cast part and, for each shot, are transferred individually into the filling chamber 12 of the die-casting machine 10 and injected intermittently from the latter into the mold cavity 14 of the casting mold from the filling chamber 12 in a known manner by means of 10 the piston 20.
The partially solid metal strand 70 usually leaves the mixing and kneading machine 30 in the direction of the longitudinal axis x of the worm shaft 36 in a horizontal direction, although another, e.g. vertical, outlet direction is also conceivable. The cross section of the metal strand 70 is determined by the cross section of the outlet opening 52, and is usually circular. The partially solid metal portions 72 can be grasped by tongs, for example, and transferred into the filling chamber 12 of the die-casting machine 10.
The aluminum alloy having the desired solids content and optionally comprising finely dispersed nanoparticles is introduced via the introduction opening 16 into the filling chamber 12 of the die-casting machine 10, and is injected intermittently from the latter into the mold cavity 14 of the casting mold from the filling chamber 12 in a known manner by means of the piston 20.
With reference to figure 5, the text which follows provides a more detailed explanation, by way of example, of the continuous production of partially solid, bar-shaped starting material for die casting die-cast parts which are optionally reinforced with nanoparticles and are made of an aluminum alloy. The mode of operation explained above with reference to figures 1 and 2 is retained.
The aluminum alloy having the desired solids content and optionally comprising finely dispersed nanoparticles is continuously ejected via the outlet opening 52 in the form of a partially solid metal strand 70. Partially solid metal portions 72 are cut to -length from the partially solid metal strand 70, for example using a rotating blade. The partially solid metal portions 72 usually each correspond to the quantity of metal required for producing an individual 5 die-cast part and, for each shot, are transferred individually into the filling chamber 12 of the die-casting machine 10 and injected intermittently from the latter into the mold cavity 14 of the casting mold from the filling chamber 12 in a known manner by means of 10 the piston 20.
The partially solid metal strand 70 usually leaves the mixing and kneading machine 30 in the direction of the longitudinal axis x of the worm shaft 36 in a horizontal direction, although another, e.g. vertical, outlet direction is also conceivable. The cross section of the metal strand 70 is determined by the cross section of the outlet opening 52, and is usually circular. The partially solid metal portions 72 can be grasped by tongs, for example, and transferred into the filling chamber 12 of the die-casting machine 10.
Claims (10)
1. A process for producing die-cast parts made of an aluminum alloy, characterized in that the aluminum alloy is exposed to high shearing forces in a mixing and kneading machine (30), having a housing (31) with a working space (34), which is surrounded by an inner housing sleeve (32), and a worm shaft (36), which rotates about a longitudinal axis (x) and moves to and fro translationally in the longitudinal axis (x) in the inner housing sleeve (32) and is provided with kneading blades (38), and with kneading bolts (42), which are fastened to the inner housing sleeve (32) and protrude into the working space (34), wherein liquid aluminum alloy is fed to the working space (34) at one end of the housing (31) and, at the other end of the housing (31), is removed from the working space (34) as partially solid aluminum alloy with a predefined solids content, is transferred into a filling chamber (12) of a die-casting machine (10) and is introduced into a casting mold by means of a piston (20), wherein the solids content of the aluminum alloy in the working space (34) is set to the predefined solids content by cooling and heating the working space (34) in a targeted manner.
2. The process as claimed in claim 1, characterized in that the inner housing sleeve (32) is surrounded by an outer housing sleeve (46) such that an intermediate space (48) preferably in the form of a hollow cylinder is formed, and cold and/or hot gases are conducted through the intermediate space (48) for cooling and heating the working space (34).
3. The process as claimed in claim 2, characterized in that air, preferably compressed air, is conducted through the intermediate space (48) for cooling, and hot gases, preferably combustion gases, are conducted through the intermediate space (48) for heating.
4. The process as claimed in claim 2 or 3, characterized in that the gases are conducted through the intermediate space (48) in countercurrent to the direction in which the aluminum alloy is transported.
5. The process as claimed in one of claims 1 to 4, characterized in that, in order to set a desired solids content, the viscosity of the aluminum alloy in the working space (34) is measured and set to a predefined value by cooling and heating the working space (34) in a targeted manner.
6. The process as claimed in one of claims 1 to 5, characterized in that the solids content of the aluminum alloy is set to 40 to 80%, preferably to more than 50%.
7. The process as claimed in one of claims 1 to 6, characterized in that the partially solid aluminum alloy is removed from the working space (34) as a partially solid metal strand (70), the partially solid metal strand (70) is split into partially solid metal portions (72) and the partially solid metal portions (72) are transferred into the filling chamber (12) of the die-casting machine (10).
8. The process as claimed in one of claims 1 to 7, characterized in that, in order to produce die-cast parts reinforced with nanoparticles, nanoparticles are mixed with the aluminum alloy and finely dispersed in the aluminum alloy by high shearing forces in the mixing and kneading machine (30), wherein liquid aluminum alloy and nanoparticles are fed to the working space (34) at one end of the housing (31) and, at the other end of the housing (31), are removed from the working space (34) as partially solid aluminum alloy with a predefined solids content and with nanoparticles finely dispersed in the aluminum alloy.
9. The process as claimed in claim 8, characterized in that the content of the nanoparticles in the alloy is 0.1 to 10% by volume.
10. The process as claimed in claim 9, characterized in that the nanoparticles used are fumed silica, carbon nanotubes (CNT) and also further, nanoscale particles of metal and semimetal oxides, such as e.g. aluminum oxide (A1203), titanium dioxide (Ti02), zirconium oxide (Zr02), antimony(III) oxide, chromium(III) oxide, iron(III) oxide, germanium(IV) oxide, vanadium(V) oxide or tungsten(VI) oxide.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| EP10157519.9 | 2010-03-24 | ||
| EP10157519 | 2010-03-24 | ||
| PCT/EP2010/062089 WO2011116838A1 (en) | 2010-03-24 | 2010-08-19 | Method for producing die-cast parts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2792432A1 true CA2792432A1 (en) | 2011-09-29 |
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| CA2792432A Abandoned CA2792432A1 (en) | 2010-03-24 | 2010-08-19 | Process for producing die-cast parts |
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| EP (1) | EP2393619B1 (en) |
| KR (1) | KR20130055563A (en) |
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| AU (1) | AU2010349399A1 (en) |
| BR (1) | BR112012023916A2 (en) |
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| WO (1) | WO2011116838A1 (en) |
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| DE102010061959A1 (en) * | 2010-11-25 | 2012-05-31 | Rolls-Royce Deutschland Ltd & Co Kg | Method of making high temperature engine components |
| EP2522885A1 (en) | 2011-05-11 | 2012-11-14 | Rheinfelden Alloys GmbH & Co. KG | Seal arrangement |
| EP2564953A1 (en) * | 2011-09-05 | 2013-03-06 | Rheinfelden Alloys GmbH & Co. KG | Process for producing formed parts |
| CN103008610B (en) * | 2012-12-18 | 2015-05-27 | 华南理工大学 | Squeeze casting method of zinc alloy worm gear |
| AT518824A1 (en) * | 2016-05-31 | 2018-01-15 | Lkr Leichtmetallkompetenzzentrum Ranshofen Gmbh | Method for producing a profile from a metal alloy |
| AT518825A1 (en) * | 2016-05-31 | 2018-01-15 | Lkr Leichtmetallkompetenzzentrum Ranshofen Gmbh | Method for producing a profile from a metal alloy |
| DE102021203642B3 (en) | 2021-04-13 | 2022-09-08 | Volkswagen Aktiengesellschaft | Bearing core for a rubber-metal bearing, rubber-metal bearing and motor vehicle with such |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CH278575A (en) | 1949-11-04 | 1951-10-31 | List Heinz | Mixing and kneading machine. |
| US2892224A (en) * | 1957-05-09 | 1959-06-30 | Nat Lead Co | Heating of dies by internal combustion |
| DE2401654C2 (en) * | 1974-01-15 | 1975-11-20 | Matthias 4150 Krefeld Welsch | Method and device for the production of aluminum |
| IT1257114B (en) * | 1992-09-29 | 1996-01-05 | Weber Srl | PROCEDURE FOR OBTAINING REOCOLATED SOLID WOODS, IN PARTICULAR SUITABLE FOR USE FOR THE PRODUCTION OF HIGH MECHANICAL PERFORMANCE DIE CASTINGS. |
| IT1260684B (en) * | 1993-09-29 | 1996-04-22 | Weber Srl | METHOD AND PLANT FOR THE DIE-CASTING OF SEMI-LIQUID COMPONENTS WITH HIGH MECHANICAL PERFORMANCE STARTING FROM REOCOLATED SOLID. |
| JP3817786B2 (en) * | 1995-09-01 | 2006-09-06 | Ｔｋｊ株式会社 | Alloy product manufacturing method and apparatus |
| US5881796A (en) * | 1996-10-04 | 1999-03-16 | Semi-Solid Technologies Inc. | Apparatus and method for integrated semi-solid material production and casting |
| KR100607218B1 (en) * | 1998-03-31 | 2006-08-01 | 다카다 가부시키가이샤 | Method and apparatus for manufacturing metallic parts by injection molding from the semi-solid state |
| US6470955B1 (en) * | 1998-07-24 | 2002-10-29 | Gibbs Die Casting Aluminum Co. | Semi-solid casting apparatus and method |
| DE19907118C1 (en) * | 1999-02-19 | 2000-05-25 | Krauss Maffei Kunststofftech | Injection molding apparatus for producing molded metal parts with dendritic properties comprises an extruder with screw system |
| GB2354471A (en) * | 1999-09-24 | 2001-03-28 | Univ Brunel | Producung semisolid metal slurries and shaped components therefrom |
| US7264037B2 (en) * | 2003-07-02 | 2007-09-04 | Honda Motor Co., Ltd. | Molding of slurry-form semi-solidified metal |
| US7509993B1 (en) * | 2005-08-13 | 2009-03-31 | Wisconsin Alumni Research Foundation | Semi-solid forming of metal-matrix nanocomposites |
| DK1815958T3 (en) * | 2006-02-06 | 2009-02-09 | Buss Ag | Mixing and kneading machine |
| US7837811B2 (en) * | 2006-05-12 | 2010-11-23 | Nissei Plastic Industrial Co., Ltd. | Method for manufacturing a composite of carbon nanomaterial and metallic material |
| JP4224083B2 (en) * | 2006-06-15 | 2009-02-12 | 日精樹脂工業株式会社 | Method for producing composite metal material and method for producing composite metal molded product |
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- 2010-08-19 BR BR112012023916A patent/BR112012023916A2/en not_active IP Right Cessation
- 2010-08-19 MX MX2012010807A patent/MX2012010807A/en not_active Application Discontinuation
- 2010-08-19 KR KR1020127024127A patent/KR20130055563A/en not_active Application Discontinuation
- 2010-08-19 RU RU2012143377/02A patent/RU2012143377A/en not_active Application Discontinuation
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- 2010-08-19 EP EP10743166A patent/EP2393619B1/en not_active Not-in-force
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- 2010-08-19 CN CN201080065674XA patent/CN102834203A/en active Pending
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| RU2012143377A (en) | 2014-05-10 |
| WO2011116838A1 (en) | 2011-09-29 |
| AU2010349399A1 (en) | 2012-09-27 |
| CN102834203A (en) | 2012-12-19 |
| MX2012010807A (en) | 2013-01-22 |
| DK2393619T3 (en) | 2013-07-08 |
| PL2393619T3 (en) | 2013-09-30 |
| KR20130055563A (en) | 2013-05-28 |
| SI2393619T1 (en) | 2013-08-30 |
| ES2423326T3 (en) | 2013-09-19 |
| PT2393619E (en) | 2013-07-09 |
| EP2393619B1 (en) | 2013-04-03 |
| EP2393619A1 (en) | 2011-12-14 |
| HRP20130605T1 (en) | 2013-08-31 |
| US20130220568A1 (en) | 2013-08-29 |
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