EP2061912B1 - ALUMINIUM ALLOY OF THE AlZnMg TYPE AND METHOD OF PRODUCING IT - Google Patents
ALUMINIUM ALLOY OF THE AlZnMg TYPE AND METHOD OF PRODUCING IT Download PDFInfo
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- EP2061912B1 EP2061912B1 EP07800163.3A EP07800163A EP2061912B1 EP 2061912 B1 EP2061912 B1 EP 2061912B1 EP 07800163 A EP07800163 A EP 07800163A EP 2061912 B1 EP2061912 B1 EP 2061912B1
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- weight
- aluminum
- heat treatment
- alloy
- aluminum alloy
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- 229910000838 Al alloy Inorganic materials 0.000 title claims description 21
- 238000000034 method Methods 0.000 title claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 32
- 229910052782 aluminium Inorganic materials 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000003754 machining Methods 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000000641 cold extrusion Methods 0.000 claims description 2
- 238000003483 aging Methods 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 32
- 239000000956 alloy Substances 0.000 description 32
- 230000035882 stress Effects 0.000 description 17
- 238000002474 experimental method Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 238000010791 quenching Methods 0.000 description 6
- 230000000171 quenching effect Effects 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000009749 continuous casting Methods 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910019018 Mg 2 Si Inorganic materials 0.000 description 1
- 229910017706 MgZn Inorganic materials 0.000 description 1
- -1 aluminum-zinc-magnesium Chemical compound 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910021338 magnesium silicide Inorganic materials 0.000 description 1
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/10—Alloys based on aluminium with zinc as the next major constituent
-
- 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
- C22F1/053—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 zinc as the next major constituent
Definitions
- the invention relates to aluminum alloys, in particular those aluminum alloys, which are suitable for the production of low-stress and high-strength aluminum pre-material.
- the invention further relates to a process for producing such aluminum pre-materials.
- Tools for plastic injection molding require low-tension and high-strength primary material.
- the cause of stresses in the starting material are the residual stresses from the continuous casting process, caused by temperature gradients during casting, as well as those from the heat treatment, which are stresses caused by the quenching process. Tensions in the starting material lead to an impairment of the dimensional stability during machining and thus to the distortion of the component. Usually straightening due to narrow tolerances is not possible, the workpieces must be imposed.
- the precipitation-hardenable aluminum alloy EN AW-6082 an AlMgSi1Mn alloy
- this material is cast in the continuous casting to rectangular formats and then subjected to the formation of the precipitated at the grain boundaries alloying elements and to compensate for casting (ds concentration differences of alloying elements) of a first heat treatment (the so-called homogenization).
- a second heat treatment to adjust the mechanical properties.
- a forming step eg rolling
- the state of the art here is to carry out a full cure, comprising a solution heat treatment, a subsequent quenching in cold water and a subsequent heat aging.
- solution annealing the hardness-forming agent magnesium silicide Mg 2 Si is dissolved by diffusion in the primary mixed crystal at temperatures around 550 ° C, depending on the format, for 6 to 10 hours.
- quenching in cold water which causes cooling to below 150 ° C in less than 20 seconds, there is a freezing of the equilibrium state set at the solution annealing temperature, which corresponds to an unbalance state at room temperature.
- the subsequent thermal aging at temperatures of 150 to 200 ° C for 8 to 15 hours represents a targeted elimination of hardness to adjust the strength.
- Aluminum ingots treated in this way have very good mechanical properties, but are unsuitable for use in mechanical processing because of the residual stresses created by quenching in cold water. Therefore, the aluminum billets are subjected to cold working to degrade most of the residual stresses from the quenching process. The aluminum ingots are subsequently stretched by 1 to 5% of the original length for heat treatment by means of hydraulic systems.
- Aluminum plates produced by this extensive process are characterized by good mechanical strength, but are only low tension, a delay in mechanical processing can still occur.
- thermomechanical load of such aluminum plates leads to a steady loss of strength and thus leads to continuously increasing wear of the tool.
- the aluminum alloy according to the invention comprises 5.3-5.5% by weight of zinc, 0.2-0.25% by weight of chromium, 0.2-0.3% by weight of manganese and 0, 3 - 0.4 wt .-% copper.
- the aluminum alloy according to the invention is suitable for the production of aluminum pre-material for subsequent mechanical processing or for use in cold extrusion presses.
- the aluminum pre-material is preferably an aluminum cast plate.
- a further object of the invention is a post-treatment of aluminum pre-fabricated from an aluminum alloy according to the invention with the aim to obtain a low-tension and high-strength aluminum pre-material, which for the subsequent mechanical processing and the workpieces produced from the starting material, eg base plates for plastic injection molds, advantageous mechanical properties ensures.
- This after-treatment according to the invention provides a first heat treatment at up to 480 ° C., a cooling to room temperature and a subsequent second heat treatment at up to 200 ° C.
- cold aging occurs at about room temperature for 2 to 5 days.
- a second heat treatment in two stages.
- a temperature of 80 to 120 ° C during a period of 6 to 12 hours is preferably provided while in the second stage a Temperature of 135 to 150 ° C for 10 to 16 hours is provided.
- AlZnMg alloys of different composition were cast in a series of continuous castings into rectangular formats of 1550 x 250 x 3000 mm and tested for their mechanical properties after complete cold curing.
- a tensile test according to EN 10002-5 was carried out; the values given are average values of 20 tensile specimens each.
- the AIZnMg alloys were further compared with the known reference alloy EN AW-6082, which was treated in the manner conventional in the art.
- the alloy was quenched in the condition T651, ie solution treated, stretched to 1-3% low tension, cured while hot, subjected to mechanical testing.
- the mechanical characteristics obtained are as follows: Tensile strength R M [MPa] 0.2% proof stress P P0.2 [MPa] Elongation at break A5 [%] Brinell Hardness HB 10 288 248 7.5 90
- the sample plates prepared from the alloys of Experiments 1 to 3 were stress relieved in a first heat treatment step at 400 to 450 ° C for 40 to 80 minutes, after cooling to room temperature at a rate of about 200 ° C / h a second heat treatment was carried out to shorten the cold curing at temperatures of 85 to 120 ° C for 24 to 26 hours.
- the alloys of tests 1 to 3 of the currently commonly used alloy A are superior in terms of mechanical strength, elongation at break and Brinell hardness.
- the alloy according to the invention exhibits a significantly higher tensile strength both with respect to the reference alloy and with respect to the alloys of Experiments 1 and 2 and is distinguished from the reference alloy by a significantly higher Brinell hardness value.
- An aluminum casting plate of an alloy having the composition of Experiment 3 was subjected to a post-treatment according to Experiment 3, except that the second heat treatment was carried out in two stages.
- the first stage included a heat treatment at about 90 ° C for 8 to 10 hours; the second stage included a heat treatment at about 145 ° C for 14 to 16 hours.
- temperatures of the heat treatments which are advantageous for achieving the desired mechanical characteristics and the duration of the respective heat treatments required for this purpose can vary within the ranges specified in the patent claims, depending on the composition of the particular aluminum alloy according to the invention.
- the optimum parameters for the particular alloy according to the invention can easily be determined by the person skilled in the art by means of experiments that are in his or her abilities.
- the higher hardness in comparison to the reference alloy increases the resistance to mechanical stress in use, the property of cold curing in the alloys according to the invention leads after thermal stress to a healing effect of the mechanical properties.
- the durability of e.g. Tools for plastic injection molding is thereby significantly increased.
- the high hardness of the alloys according to the invention in the cold-cured state and their compared to the reference alloy significantly reduced elongation also bring in the machining very short-breaking chips, the achievable surface quality, characterized by roughness and the visual impression is therefore improved compared to the reference alloy.
- the alloys according to the invention are also outstandingly suitable for decorative anodic oxidation.
- the chromium content minimizes the tendency of the stress corrosion cracking alloy of the present invention to have a negative influence on the anodic oxidation due to the maximum content of 0.3% by weight.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Forging (AREA)
- Powder Metallurgy (AREA)
- Shaping Metal By Deep-Drawing, Or The Like (AREA)
- Continuous Casting (AREA)
Description
Die Erfindung betrifft Aluminiumlegierungen, insbesondere solche Aluminiumlegierungen, welche zur Herstellung von spannungsarmem und hochfestem Aluminiumvormaterial geeignet sind. Die Erfindung betrifft ferner ein Verfahren zur Herstellung derartiger Aluminiumvormaterialien.The invention relates to aluminum alloys, in particular those aluminum alloys, which are suitable for the production of low-stress and high-strength aluminum pre-material. The invention further relates to a process for producing such aluminum pre-materials.
Zur Herstellung von komplexen Bauteilen aus Aluminiumplatten durch mechanische Bearbeitung z.B. von Werkzeugen für den Kunststoffspritzguss ist spannungsarmes und hochfestes Vormaterial erforderlich.For producing complex components from aluminum plates by mechanical processing e.g. Tools for plastic injection molding require low-tension and high-strength primary material.
Die Ursache für Spannungen im Vormaterial sind die Eigenspannungen vom Stranggießprozess, bedingt durch Temperaturgradienten beim Gießen, sowie jene von der Wärmebehandlung, das sind Spannungen bedingt durch den Abschreckvorgang. Spannungen im Vormaterial führen bei der mechanischen Bearbeitung zu einer Beeinträchtigung der Formstabilität und damit zum Verzug des Bauteils. Üblicherweise ist ein Richten auf Grund enger Toleranzen nicht möglich, die Werkstücke müssen ausgeschossen werden.The cause of stresses in the starting material are the residual stresses from the continuous casting process, caused by temperature gradients during casting, as well as those from the heat treatment, which are stresses caused by the quenching process. Tensions in the starting material lead to an impairment of the dimensional stability during machining and thus to the distortion of the component. Usually straightening due to narrow tolerances is not possible, the workpieces must be imposed.
Für derartige Einsatzzwecke hat sich besonders die ausscheidungshärtbare Aluminiumknetlegierung EN AW-6082, eine Legierung vom Typ AlMgSi1Mn, etabliert. Zur Herstellung von Platten wird dieser Werkstoff im Stranggießverfahren zu Rechteckformaten vergossen und im Anschluss daran zur Einformung der an den Korngrenzen ausgeschiedenen Legierungselementen sowie zum Ausgleich von Gussseigerungen (ds Konzentrationsunterschiede von Legierungselementen) einer ersten Wärmebehandlung (der sogenannten Homogenisierung) unterzogen. Danach erfolgt eine zweite Wärmebehandlung zur Einstellung der mechanischen Eigenschaften. Zwischen der ersten und der zweiten Wärmebehandlung kann ein Umformschritt (z.B. ein Walzen) erfolgen.For such applications, in particular, the precipitation-hardenable aluminum alloy EN AW-6082, an AlMgSi1Mn alloy, has become established. For the production of plates, this material is cast in the continuous casting to rectangular formats and then subjected to the formation of the precipitated at the grain boundaries alloying elements and to compensate for casting (ds concentration differences of alloying elements) of a first heat treatment (the so-called homogenization). This is followed by a second heat treatment to adjust the mechanical properties. Between the first and the second heat treatment, a forming step (eg rolling) can take place.
Stand der Technik ist hier die Durchführung einer Vollaushärtung, umfassend ein Lösungsglühen, ein anschließendes Abschrecken in kaltem Wasser sowie eine danach erfolgende Warmauslagerung. Beim Lösungsglühen wird der Härtebildner Magnesiumsilicid Mg2Si durch Diffusion im Primärmischkristall bei Temperaturen um 550°C in Abhängigkeit vom Format während 6 bis 10 Stunden aufgelöst. Mit dem Abschrecken in kaltem Wasser, welches ein Abkühlen auf unter 150°C in weniger als 20 Sekunden bewirkt, kommt es zu einem Einfrieren des bei Lösungsglühtemperatur eingestellten Gleichgewichtszustandes, der einem Ungleichgewichtszustand bei Raumtemperatur entspricht. Die anschließende Warmauslagerung bei Temperaturen von 150 bis 200°C während 8 bis 15 Stunden stellt eine gezielte Ausscheidung des Härtebildners zur Einstellung der Festigkeit dar.The state of the art here is to carry out a full cure, comprising a solution heat treatment, a subsequent quenching in cold water and a subsequent heat aging. In solution annealing, the hardness-forming agent magnesium silicide Mg 2 Si is dissolved by diffusion in the primary mixed crystal at temperatures around 550 ° C, depending on the format, for 6 to 10 hours. With quenching in cold water, which causes cooling to below 150 ° C in less than 20 seconds, there is a freezing of the equilibrium state set at the solution annealing temperature, which corresponds to an unbalance state at room temperature. The subsequent thermal aging at temperatures of 150 to 200 ° C for 8 to 15 hours represents a targeted elimination of hardness to adjust the strength.
Derart behandelte Aluminiumbarren besitzen sehr gute mechanische Eigenschaften, sind jedoch für die Verwendung zur mechanischen Bearbeitung auf Grund der durch das Abschrecken in kaltem Wasser vorhandenen Eigenspannungen ungeeignet. Daher werden die Aluminiumbarren einer Kaltumformung zum Abbau des größten Teiles der Eigenspannungen vom Abschreckprozess unterzogen. Dabei werden die Aluminiumbarren im Anschluss zur Wärmebehandlung mittels hydraulischer Anlagen um 1 bis 5% der ursprünglichen Länge gereckt.Aluminum ingots treated in this way have very good mechanical properties, but are unsuitable for use in mechanical processing because of the residual stresses created by quenching in cold water. Therefore, the aluminum billets are subjected to cold working to degrade most of the residual stresses from the quenching process. The aluminum ingots are subsequently stretched by 1 to 5% of the original length for heat treatment by means of hydraulic systems.
Nach diesem umfangreichen Verfahren hergestellte Aluminiumplatten zeichnen sich durch gute mechanische Festigkeiten aus, liegen jedoch nur spannungsarm vor, ein Verzug bei der mechanischen Bearbeitung kann dennoch auftreten.Aluminum plates produced by this extensive process are characterized by good mechanical strength, but are only low tension, a delay in mechanical processing can still occur.
Die thermomechanische Belastung solcher Aluminiumplatten z.B. beim Kunststoffspritzgießen führt zu einem stetigen Verlust von Festigkeit und führt damit zu kontinuierlich steigendem Verschleiß des Werkzeuges.The thermomechanical load of such aluminum plates, for example in plastic injection molding leads to a steady loss of strength and thus leads to continuously increasing wear of the tool.
Es besteht daher weiterhin ein Bedarf an Aluminiumlegierungen, aus welchen spannungsarmes und hochfestes Aluminiumvormaterial, beispielsweise ein Form Gussplatten, hergestellt werden kann, welches Vormaterial zur mechanischen Weiterbearbeitung zB zur Herstellung von Grundplatten für Kunststoffspritzgusswerkzeuge geeignet ist.There is therefore still a need for aluminum alloys from which low-tension and high-strength aluminum pre-material, for example a cast plate mold, can be produced, which primary material is suitable for mechanical further processing, for example for the production of base plates for plastic injection molds.
Es ist daher ein Ziel der vorliegenden Erfindung, Aluminiumlegierungen bereitzustellen, aus welchen spannungsarmes und hochfestes Aluminiumvormaterial hergestellt werden kann. Es ist ein weiteres Ziel der vorliegenden Erfindung eine Aluminiumlegierung herzustellen, welche bereits aufgrund ihrer chemischen Zusammensetzung spannungsarme und hochfeste Vormaterialien liefern kann. Ein weiteres Ziel der Erfindung besteht darin, eine Nachbehandlung für ein aus einer erfindungsgemäßen Legierung hergestelltes Vormaterial bereitzustellen, welche gegenüber der aus dem Stand der Technik bekannten Vollaushärtung Vorteile liefert, ua wesentlich wirtschaftlicher und umweltschonender ist, und eine weitere Verbesserung der Festigkeitswerte der erfindungsgemäßen Legierungen ermöglicht.It is therefore an object of the present invention to provide aluminum alloys from which low stress and high strength aluminum precursor material can be made. It is a further object of the present invention to produce an aluminum alloy which, by virtue of its chemical composition, can already provide low-stress and high-strength starting materials. A further object of the invention is to provide a post-treatment for a starting material made from an alloy according to the invention, which offers advantages over the full cure known from the prior art, inter alia much more economical and environmentally friendly, and enables a further improvement in the strength values of the alloys according to the invention ,
Diese Ziele werden erfindungsgemäß durch eine Legierung mit der nachstehenden Zusammensetzung erreicht:
- 5,0 - 5,8 Gew.-% Zink
- 1,1 - 1,2 Gew.-% Magnesium
- 0,2 - 0,3 Gew.-% Chrom
- 0,1 - 0,3 Gew.-% Mangan
- 0,1 - 0,4 Gew.-% Kupfer
- 0,05 - 0,15 Gew.-% Titan
- 0,005 - 0,05 Gew.-% Cer
- 0,005 - 0,05 Gew.-% Samarium
- max. 0,2 Gew.-% Silizium
- max. 0,3 Gew.-% Eisen
- max. 0,005 Gew.-% Zirkonium
- und als Rest Aluminium.
- 5.0-5.8% by weight of zinc
- 1.1-1.2% by weight of magnesium
- 0.2-0.3% by weight chromium
- 0.1-0.3% by weight of manganese
- 0.1-0.4% by weight of copper
- 0.05-0.15% by weight of titanium
- 0.005-0.05% by weight cerium
- 0.005-0.05% by weight of samarium
- Max. 0.2% by weight of silicon
- Max. 0.3% by weight of iron
- Max. 0.005 wt% zirconium
- and as the rest aluminum.
In einer bevorzugten Ausführungsform umfasst die erfin dungsgemäße Aluminiumlegierung 5,3 - 5,5 Gew.-% Zink, 0,2 - 0,25 Gew.-% Chrom, 0,2 - 0,3 Gew.-% Mangan und 0,3 - 0,4 Gew.-% Kupfer.In a preferred embodiment, the aluminum alloy according to the invention comprises 5.3-5.5% by weight of zinc, 0.2-0.25% by weight of chromium, 0.2-0.3% by weight of manganese and 0, 3 - 0.4 wt .-% copper.
Die erfindungsgemäße Aluminiumlegierung eignet sich zur Herstellung von Aluminiumvormaterial zur nachfolgenden mechanischen Bearbeitung oder zum Einsatz für Kaltfließpressen. Bevorzugt handelt es sich bei dem Aluminiumvormaterial um eine Aluminiumgussplatte.The aluminum alloy according to the invention is suitable for the production of aluminum pre-material for subsequent mechanical processing or for use in cold extrusion presses. The aluminum pre-material is preferably an aluminum cast plate.
Ein weiteres Ziel der Erfindung besteht in einer Nachbehandlung von aus einer erfindungsgemäßen Aluminiumlegierung hergestelltem Aluminiumvormaterial mit dem Ziel, ein spannungsarmes und hochfestes Aluminiumvormaterial zu erhalten, welches für die nachfolgende mechanische Bearbeitung und den aus dem Vormaterial hergestellten Werkstücken, zB Grundplatten für Kunststoffspritzgusswerkzeuge, vorteilhafte mechanische Eigenschaften sicherstellt.A further object of the invention is a post-treatment of aluminum pre-fabricated from an aluminum alloy according to the invention with the aim to obtain a low-tension and high-strength aluminum pre-material, which for the subsequent mechanical processing and the workpieces produced from the starting material, eg base plates for plastic injection molds, advantageous mechanical properties ensures.
Diese erfindungsgemäße Nachbehandlung sieht eine erste Wärmebehandlung bei bis zu 480°C, eine Abkühlung auf Raumtemperatur und eine daran anschließende zweite Wärmebehandlung bei bis zu 200°C vor. In bevorzugter Weise erfolgt vor der zweiten Wärmebehandlung eine Kaltauslagerung bei etwa Raumtemperatur während 2 bis 5 Tagen.This after-treatment according to the invention provides a first heat treatment at up to 480 ° C., a cooling to room temperature and a subsequent second heat treatment at up to 200 ° C. Preferably, prior to the second heat treatment, cold aging occurs at about room temperature for 2 to 5 days.
Als für die Verbesserung der mechanischen Kennwerte weiters besonders vorteilhaft hat sich eine zweite Wärmebehandlung in zwei Stufen gezeigt. In der ersten Stufe wird dabei bevorzugt eine Temperatur von 80 bis 120° C während einer Dauer von 6 bis 12 Stunden vorgesehen, während in der zweiten Stufe eine Temperatur von 135 bis 150°C während 10 bis 16 Stunden vorgesehen wird.Further particularly advantageous for the improvement of the mechanical characteristics is a second heat treatment in two stages. In the first stage, a temperature of 80 to 120 ° C during a period of 6 to 12 hours is preferably provided while in the second stage a Temperature of 135 to 150 ° C for 10 to 16 hours is provided.
Diese Ziele und weitere Aspekte der vorliegenden Erfindung werden nachstehend anhand von Beispielen, welche die Erfindung näher erläutern, aber nicht einschränken, weiter veranschaulicht.These objects and further aspects of the present invention are further illustrated below by way of examples which illustrate, but not limit, the invention in more detail.
In der Literatur ist der Effekt der Selbstaushärtung (Kaltaushärtung) von bestimmten Aluminiumlegierungen beschrieben. Besonders die Legierungsgruppe Aluminium-Zink-Magnesium neigt auf Grund der bei Raumtemperatur geringen Löslichkeit von Zink im Primärmischkristall zu diesem Effekt.In the literature, the effect of self-curing (cold curing) of certain aluminum alloys is described. In particular, the alloying group aluminum-zinc-magnesium tends due to the low room temperature solubility of zinc in primary quartz crystal to this effect.
Es wurden daher in einer Versuchsserie AlZnMg-Legierungen unterschiedlicher Zusammensetzung im Stranggießverfahren zu Rechteckformaten von 1550 x 250 x 3000 mm vergossen und nach vollständiger Kaltaushärtung auf ihre mechanische Eigenschaften geprüft. Dazu wurde ein Zugversuch nach EN 10002-5 durchgeführt; die angeführten Werte sind Mittelwerte aus je 20 Zugproben. Die AIZnMg-Legierungen wurden ferner mit der bekannten Referenzlegierung EN AW-6082, welche in der im Stand der Technik üblichen Weise behandelt wurde, verglichen.For this reason, AlZnMg alloys of different composition were cast in a series of continuous castings into rectangular formats of 1550 x 250 x 3000 mm and tested for their mechanical properties after complete cold curing. For this purpose, a tensile test according to EN 10002-5 was carried out; the values given are average values of 20 tensile specimens each. The AIZnMg alloys were further compared with the known reference alloy EN AW-6082, which was treated in the manner conventional in the art.
Es wurde eine Referenzlegierung mit der Zusammensetzung EN 573-3, Werkstoff EN AW-6082, verwendet. Diese Legierung besitzt normgemäß die folgende Zusammensetzung:
- 0,7 bis 1,3 Gew.-% Silizium
- 0,5 Gew.-% Eisen
- 0,1 Gew.-% Kupfer
- 0,4 bis 1,0 Gew.-% Mangan
- 0,6 bis 1,2 Gew.-% Magnesium
- 0,25 Chrom
- 0,2 Gew.-% Zink
- 0,1 Gew.-% Titan
- sonstige Legierungsbestandteile:
- einzeln 0,05 Gew.-%, gesamt 0,15 Gew.-%
- Rest: Aluminium
- 0.7 to 1.3 wt .-% silicon
- 0.5% by weight of iron
- 0.1% by weight of copper
- 0.4 to 1.0% by weight of manganese
- 0.6 to 1.2 wt .-% magnesium
- 0.25 chrome
- 0.2% by weight of zinc
- 0.1% by weight of titanium
- other alloy components:
- individually 0.05% by weight, total 0.15% by weight
- Rest: aluminum
Die Legierung wurde im Zustand T651, dh lösungsgeglüht, abgeschreckt, 1-3% spannungsarm gereckt, warm ausgehärtet, der mechanischen Prüfung unterzogen. Die dabei erhaltenen mechanischen Kennwerte sind wie folgt:
Aluminiumlegierung mit der Zusammensetzung von
4,86 Gew.-% Zink
0,92 Gew.-% Magnesium
0,18 Gew.-% Chrom
0,22 Gew.-% Mangan
0,09 Gew.-% Titan
0,21 Gew.-% Silizium
0,28 Gew.-% Eisen
0,01 Gew.-% Kupfer
Rest: AluminiumAluminum alloy with the composition of
4.86% by weight of zinc
0.92% by weight of magnesium
0.18 wt .-% chromium
0.22 wt .-% manganese
0.09% by weight of titanium
0.21 wt .-% silicon
0.28% by weight of iron
0.01% by weight of copper
Rest: aluminum
Die mit dieser Legierung erreichbaren mechanischen Kennwerte sind wie folgt:
Aluminiumlegierung mit der Zusammensetzung von
5,18 Gew.-% Zink
0,94 Gew.-% Magnesium
0,17 Gew.-% Chrom
0,21 Gew.-% Mangan
0,12 Gew.-% Titan
0,16 Gew.-% Silizium
0,28 Gew.-% Eisen
0,01 Gew.-% Kupfer
Rest: AluminiumAluminum alloy with the composition of
5.18% by weight of zinc
0.94% by weight of magnesium
0.17 wt .-% chromium
0.21 wt .-% manganese
0.12% by weight of titanium
0.16 wt .-% silicon
0.28% by weight of iron
0.01% by weight of copper
Rest: aluminum
Die mit dieser Legierung erreichbaren mechanischen Kennwerte sind wie folgt:
Eine Aluminiumlegierung mit der Zusammensetzung von
5,61 Gew.-% Zink
1,18 Gew.-% Magnesium
0,24 Gew.-% Chrom
0,24 Gew.-% Mangan
0,29 Gew.-% Kupfer
0,06 Gew.-% Titan
0,02 Gew.-% Cer
0,01 Gew.-% Samarium
0,12 Gew.-% Silizium
0,26 Gew.-% Eisen
0,001 Gew.-% Zirkonium
Rest: AluminiumAn aluminum alloy with the composition of
5.61% by weight of zinc
1.18 wt .-% magnesium
0.24 wt .-% chromium
0.24 wt .-% manganese
0.29 wt .-% copper
0.06 wt.% Titanium
0.02 wt.% Cerium
0.01% by weight of samarium
0.12 wt .-% silicon
0.26 wt .-% iron
0.001 wt% zirconium
Rest: aluminum
Die mit dieser Legierung erreichbaren mechanischen Kennwerte sind wie folgt:
Zur Einstellung der mechanischen Eigenschaften wurden die aus den Legierungen der Versuche 1 bis 3 hergestellten Probenplatten in einem ersten Wärmebehandlungsschritt bei 400 bis 450°C während 40 bis 80 min spannungsarm geglüht, nach einem Abkühlen auf Raumtemperatur mit einer Geschwindigkeit von etwa 200°C/h wurde eine zweite Wärmebehandlung zur Verkürzung der Kaltaushärtung bei Temperaturen von 85 bis 120°C während 24 bis 26 Stunden durchgeführt.To adjust the mechanical properties, the sample plates prepared from the alloys of Experiments 1 to 3 were stress relieved in a first heat treatment step at 400 to 450 ° C for 40 to 80 minutes, after cooling to room temperature at a rate of about 200 ° C / h a second heat treatment was carried out to shorten the cold curing at temperatures of 85 to 120 ° C for 24 to 26 hours.
Während der ersten Wärmebehandlung (der Spannungsarmglühung) und der zweiten Wärmebehandlung zur Verkürzung der Kaltaushärtung wurde eine Kaltauslagerung bei etwa Raumtemperatur während 2 bis 5 Tagen durchgeführt, welche eine höhere 0,2%-Dehngrenze im Vormaterial zur Folge hat. Diese Verbesserung in der Dehngrenze wird auf eine vermehrte Ausscheidung der inkohärenten Phase MgZn2 während der Kaltauslagerung zurückgeführt.During the first heat treatment (the stress relief annealing) and the second heat treatment to shorten the cold cure, cold aging was carried out at about room temperature for 2 to 5 days, resulting in a higher 0.2% proof stress in the starting material. This improvement in yield strength is attributed to increased precipitation of the incoherent phase MgZn 2 during cold aging.
Die gegenüber dem üblichen Lösungsglühen wesentlich verkürzte erste Wärmebehandlung, sowie das nicht erforderliche Abschrecken in kaltem Wasser ermöglicht die Herstellung von sehr spannungsarmem Material. Restspannungen, welche bei einer mechanischen Bearbeitung zu Verzug führen würden, traten bei den Musterplatten nicht auf. Ein Recken ist daher nicht erforderlich.The compared to the usual solution annealing significantly shortened first heat treatment, and the unnecessary quenching in cold water allows the production of very low-stress material. Residual stresses, which at a mechanical processing would lead to distortion, did not occur in the sample plates. Stretching is therefore not required.
Aus einem Vergleich der Versuche A und 1 bis 3 zeigt sich, dass die Legierungen der Versuche 1 bis 3 der derzeit üblicherweise verwendeten Legierung A hinsichtlich der mechanischen Kennwerte Zugfestigkeit, Bruchdehnung und Brinellhärte überlegen sind. Dabei zeigt die erfindungsgemäße Legierung sowohl gegenüber der Referenzlegierung als auch gegenüber den Legierungen der Versuche 1 und 2 eine signifikant höhere Zugfestigkeit und zeichnet sich gegenüber der Referenzlegierung durch einen signifikant höheren Wert der Brinellhärte aus.It can be seen from a comparison of tests A and 1 to 3 that the alloys of tests 1 to 3 of the currently commonly used alloy A are superior in terms of mechanical strength, elongation at break and Brinell hardness. In this case, the alloy according to the invention exhibits a significantly higher tensile strength both with respect to the reference alloy and with respect to the alloys of Experiments 1 and 2 and is distinguished from the reference alloy by a significantly higher Brinell hardness value.
Eine Aluminiumgussplatte aus einer Legierung mit der Zusammensetzung des Versuchs 3 wurde einer Nachbehandlung entsprechend Versuch 3 unterzogen, mit dem Unterschied, dass die zweite Wärmebehandlung in zwei Stufen ausgeführt wurde. Die erste Stufe umfasste dabei eine Wärmebehandlung bei etwa 90° C während 8 bis 10 Stunden; die zweite Stufe umfasste eine Wärmebehandlung bei etwa 145°C während 14 bis 16 Stunden.An aluminum casting plate of an alloy having the composition of Experiment 3 was subjected to a post-treatment according to Experiment 3, except that the second heat treatment was carried out in two stages. The first stage included a heat treatment at about 90 ° C for 8 to 10 hours; the second stage included a heat treatment at about 145 ° C for 14 to 16 hours.
Die mit dieser Legierung erreichbaren mechanischen Kennwerte sind wie folgt:
Aus Versuch 4 ist ersichtlich, dass bei der erfindungsgemäßen Legierung durch eine zweite Wärmebehandlung, welche in zwei Stufen erfolgt, eine weitere signifikante Verbesserung der im Zusammenhang mit der vorliegenden Erfindung interessanten mechanischen Kennwerte erzielt werden kann.From experiment 4 it can be seen that in the alloy according to the invention by a second heat treatment, which takes place in two stages, a further significant improvement in the Can be achieved in connection with the present invention interesting mechanical characteristics.
Längere Behandlungszeiten führen zu keiner nennenswerten Verbesserung der mechanischen Kennwerte. Ein Anheben der Temperatur in der zweiten Stufe auf beispielsweise 160°C brachte ebenfalls keine Verbesserung und führte im Gegenteil zu einem Verlust an Festigkeit.Longer treatment times lead to no appreciable improvement in the mechanical characteristics. Raising the temperature in the second stage to, for example, 160 ° C also brought no improvement and on the contrary led to a loss of strength.
Die zur Erzielung der gewünschten mechanischen Kennwerte vorteilhaften Temperaturen der Wärmebehandlungen sowie die dazu erforderliche Dauer der jeweiligen Wärmebehandlungen können innerhalb der in den Patentansprüchen angeführten Bereiche in Abhängigkeit von der Zusammensetzung der jeweiligen erfindungsgemäßen Aluminiumlegierung variieren. Die für die jeweilige erfindungsgemäße Legierung optimalen parameter können vom Fachmann durch in seinem Können liegende Versuche jedoch einfach ermittelt werden.The temperatures of the heat treatments which are advantageous for achieving the desired mechanical characteristics and the duration of the respective heat treatments required for this purpose can vary within the ranges specified in the patent claims, depending on the composition of the particular aluminum alloy according to the invention. However, the optimum parameters for the particular alloy according to the invention can easily be determined by the person skilled in the art by means of experiments that are in his or her abilities.
Die im Vergleich zur Referenzlegierung höhere Härte erhöht die Widerstandsfähigkeit gegenüber mechanischer Belastung im Einsatz, die Eigenschaft der Kaltaushärtung bei den erfindungsgemäßen Legierungen führt nach thermischer Belastung zu einem Ausheileffekt der mechanischen Eigenschaften. Die Haltbarkeit von z.B. Werkzeugen für das Kunststoffspritzgießen wird dadurch wesentlich erhöht.The higher hardness in comparison to the reference alloy increases the resistance to mechanical stress in use, the property of cold curing in the alloys according to the invention leads after thermal stress to a healing effect of the mechanical properties. The durability of e.g. Tools for plastic injection molding is thereby significantly increased.
Die hohe Härte der erfindungsgemäßen Legierungen im kaltausgehärteten Zustand sowie deren gegenüber der Referenzlegierung signifikant verringerte Bruchdehnung bringen ferner bei der spanenden Bearbeitung sehr kurz brechende Späne, die erreichbare Oberflächenqualität, charakterisiert durch Rautiefe und den optischen Eindruck, ist daher im Vergleich zur Referenzlegierung verbessert.The high hardness of the alloys according to the invention in the cold-cured state and their compared to the reference alloy significantly reduced elongation also bring in the machining very short-breaking chips, the achievable surface quality, characterized by roughness and the visual impression is therefore improved compared to the reference alloy.
Die erfindungsgemäßen Legierungen eignen sich ferner auf Grund der tiefen Gehalte von Silizium und Mangan hervorragend zur dekorativen anodischen Oxidation. Der Chromgehalt reduziert die Neigung der erfindungsgemäßen Legierung zur Spannungsrisskorrosion auf ein Minimum, hat jedoch aufgrund des Maximalgehalts von 0,3 Gew.-% keinen negativen Einfluss auf die anodische Oxidation.Due to the low contents of silicon and manganese, the alloys according to the invention are also outstandingly suitable for decorative anodic oxidation. The chromium content minimizes the tendency of the stress corrosion cracking alloy of the present invention to have a negative influence on the anodic oxidation due to the maximum content of 0.3% by weight.
Claims (11)
- An aluminum alloy, characterized in that it comprises5.0 - 5.8 % by weight of zinc1.1 - 1.2 % by weight of magnesium0.2 - 0.3 % by weight of chromium0.1 - 0.3 % by weight of manganese0.1 - 0.4 % by weight of copper0.05 - 0.15 % by weight of titanium0.005 - 0.05 % by weight of cerium0.005 - 0.05 % by weight of samariuma maximum of 0.2 % by weight of silicona maximum of 0.3 % by weight of irona maximum of 0.005 % by weight of zirconiumand as the remainder, aluminum.
- The aluminum alloy as defined by claim 1, characterized in that it comprises5.3 - 5.5 % by weight of zinc0.2 - 0.25 % by weight of chromium0.2 - 0.3 % by weight of manganese0.3 - 0.4 % by weight of copper.
- The use of an aluminum alloy as defined by claims 1 and 2 for producing aluminum input material for subsequent mechanical machining.
- The use of an aluminum alloy as defined by claims 1 and 2 for producing aluminum input material for cold extrusion.
- The use as defined by claim 3 or 4, characterized in that the aluminum input material is a cast aluminum plate.
- An aluminum input material comprising an aluminum alloy as defined by claim 1 or 2.
- The aluminum input material in the form of a cast aluminum plate.
- A method for producing aluminum input material from an aluminum alloy as defined by claim 1 or 2, characterized in that a posttreatment includes first heat treatment at up to 480°C, cooling down to room temperature, and an ensuing second heat treatment at up to 200°C.
- The method as defined by claim 8, characterized in that before the second heat treatment, a natural age hardening at approximately room temperature is effected for from 2 to 5 days.
- The method as defined by claim 8 or 9, characterized in that the second heat treatment is effected in two stages.
- The method as defined by claim 10, characterized in that in the first stage, a temperature of from 80 to 120°C for a duration of 6 to 12 hours is provided, and in the second stage, a temperature of from 135 to 150° for 10 to 16 hours is provided.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT0147206A AT504089B1 (en) | 2006-09-04 | 2006-09-04 | ALUMINUM ALLOYING AND METHOD FOR THE PRODUCTION THEREOF |
| PCT/AT2007/000418 WO2008028208A1 (en) | 2006-09-04 | 2007-09-03 | ALUMINIUM ALLOY OF THE AlZnMg TYPE AND METHOD OF PRODUCING IT |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP2061912A1 EP2061912A1 (en) | 2009-05-27 |
| EP2061912B1 true EP2061912B1 (en) | 2013-05-01 |
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ID=38626916
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP07800163.3A Not-in-force EP2061912B1 (en) | 2006-09-04 | 2007-09-03 | ALUMINIUM ALLOY OF THE AlZnMg TYPE AND METHOD OF PRODUCING IT |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US8491733B2 (en) |
| EP (1) | EP2061912B1 (en) |
| AR (1) | AR062642A1 (en) |
| AT (1) | AT504089B1 (en) |
| CA (1) | CA2697691A1 (en) |
| MX (1) | MX2009002390A (en) |
| RU (1) | RU2484169C2 (en) |
| TW (1) | TWI434939B (en) |
| WO (1) | WO2008028208A1 (en) |
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| TWI467026B (en) * | 2013-06-27 | 2015-01-01 | China Steel Corp | Aluminum alloy sheet for anode and method of making the same |
| WO2015041867A1 (en) * | 2013-09-19 | 2015-03-26 | United Technologies Corporation | Age hardenable dispersion strengthened aluminum alloys |
| JP7244195B2 (en) * | 2019-07-11 | 2023-03-22 | 株式会社神戸製鋼所 | Method for manufacturing 7000 series aluminum alloy member |
| CN111304502A (en) * | 2020-04-07 | 2020-06-19 | 台山市金桥铝型材厂有限公司 | High-strength 7000 series aluminum alloy section for automobile body and manufacturing method |
| CN111270115A (en) * | 2020-04-07 | 2020-06-12 | 台山市金桥铝型材厂有限公司 | Method for manufacturing high-strength 7000 series aluminum alloy section for automobile body |
| US11859268B2 (en) | 2021-09-13 | 2024-01-02 | Ypf Tecnologia S.A. | Dissolvable magnesium alloy |
| CN114033591A (en) * | 2021-11-16 | 2022-02-11 | 苏州星波动力科技有限公司 | Aluminum alloy oil rail, forming method and manufacturing method thereof, engine and automobile |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB598192A (en) * | 1945-05-10 | 1948-02-12 | Richard Chadwick | Improvements in or relating to aluminium base alloys |
| CH266151A (en) * | 1946-06-28 | 1950-01-15 | Ici Ltd | Aluminum alloy. |
| CH268244A (en) * | 1947-02-19 | 1950-05-15 | Ici Ltd | Process for improving the corrosion resistance of aluminum alloys. |
| JPS6434548A (en) * | 1987-07-30 | 1989-02-06 | Furukawa Aluminium | Production of high strength aluminum foil |
| FR2744136B1 (en) * | 1996-01-25 | 1998-03-06 | Pechiney Rhenalu | THICK ALZNMGCU ALLOY PRODUCTS WITH IMPROVED PROPERTIES |
| RU2165995C1 (en) * | 1999-10-05 | 2001-04-27 | Государственное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" | Highly string aluminium-based alloy and product made of said alloy |
| RU2165996C1 (en) * | 1999-10-05 | 2001-04-27 | Государственное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" | Highly strong aluminium-based alloy and product thereof |
| RU2215807C2 (en) * | 2001-12-21 | 2003-11-10 | Региональный общественный фонд содействия защите интеллектуальной собственности | Aluminum-base alloy, article made of thereof and method for making article |
| US7048815B2 (en) * | 2002-11-08 | 2006-05-23 | Ues, Inc. | Method of making a high strength aluminum alloy composition |
-
2006
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| Publication number | Publication date |
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| AR062642A1 (en) | 2008-11-19 |
| EP2061912A1 (en) | 2009-05-27 |
| TW200831681A (en) | 2008-08-01 |
| AT504089B1 (en) | 2008-08-15 |
| US8491733B2 (en) | 2013-07-23 |
| RU2484169C2 (en) | 2013-06-10 |
| RU2009112403A (en) | 2010-10-20 |
| AT504089A1 (en) | 2008-03-15 |
| MX2009002390A (en) | 2009-06-08 |
| WO2008028208A1 (en) | 2008-03-13 |
| US20100089506A1 (en) | 2010-04-15 |
| CA2697691A1 (en) | 2008-03-13 |
| TWI434939B (en) | 2014-04-21 |
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