EP2255021B1 - Steel alloy for a low alloy steel for producing high-tensile seamless steel tubing - Google Patents

Steel alloy for a low alloy steel for producing high-tensile seamless steel tubing Download PDF

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Publication number
EP2255021B1
EP2255021B1 EP09712055A EP09712055A EP2255021B1 EP 2255021 B1 EP2255021 B1 EP 2255021B1 EP 09712055 A EP09712055 A EP 09712055A EP 09712055 A EP09712055 A EP 09712055A EP 2255021 B1 EP2255021 B1 EP 2255021B1
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Prior art keywords
steel
max
alloy
content
tensile
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French (fr)
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EP2255021A2 (en
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Christoph Kaucke
Guido Kubla
Heinz Sanders
Charles Stallybrass
André Schneider
Markus Schütz
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Vallourec Deutschland GmbH
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V&M Deutschland GmbH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten

Abstract

The invention relates to a steel alloy for a low alloy steel for producing high-tensile, weldable, hot-rolled seamless steel tubing, in particular construction tubing. The chemical composition (in % by mass) is: 0.15 - 0.18 % C; 0.20 - 0.40 % Si; 1.40 - 1.60 % Mn; max. 0.05 % P; max. 0.01 % S; >0.50 - 0.90 % Cr; > 0.50 - 0.80 % Mo; >0.10 - 0.15 % V; 0.60 - 1.00 % W; 0.0130 - 0.0220 % N; the remainder is made up of iron with production-related impurities; with the optional addition of one or more elements selected from Al, Ni, Nb, Ti, with the proviso that the relationship V/N has a value of between 4 and 12 and the Ni content of the steel is not more than 0.40 %.

Description

Die Erfindung betrifft eine Stahllegierung für einen niedrig legierten Stahl zur Herstellung hochfester schweißbarer nahtloser Stahlrohre gemäß Patentanspruch 1.The invention relates to a steel alloy for a low-alloy steel for producing high-strength weldable seamless steel pipes according to claim 1.

Insbesondere betrifft die Erfindung Rohre, die auch von der Kreisform abweichende Querschnitte aufweisen können und als Konstruktionsrohre für besonders hoch beanspruchte geschweißte Stahlbaukonstruktionen, beispielsweise im Kran-, Brücken-, Schiff-, Hebezeug- und Lastfahrzeugbau, vorgesehen sind.In particular, the invention relates to tubes which may also have deviating cross-sections and are provided as construction tubes for particularly highly stressed welded steel structures, for example in crane, bridge, ship, hoist and truck construction.

Solche Rohre können neben kreisförmigen Querschnitten je nach Anforderung und Einsatzbereich z. B. quadratische, rechteckige oder auch vieleckige Querschnitte aufweisen.Such tubes can in addition to circular cross sections depending on the requirements and application z. B. have square, rectangular or polygonal cross-sections.

Stahllegierungen für derartige Stahlrohre sind beispielsweise aus der DE 199 42 641 A1 bekannt. Diese bekannte Stahllegierung weist neben geringen Zusätzen an Chrom, Molybdän und Vanadin als Besonderheit für einen niedrig legierten Stahl unter Verzicht von Nickel einen Zusatz von Wolfram im Bereich von 0,30 - 1,00% auf.Steel alloys for such steel pipes are for example from DE 199 42 641 A1 known. This known steel alloy, in addition to minor additions of chromium, molybdenum and vanadium as a peculiarity for a low alloy steel waiving nickel addition of tungsten in the range of 0.30 - 1.00%.

Durch den Verzicht des ansonsten zwingend erforderlichen Nickels bzw. durch die Beschränkung des Ni-Gehaltes auf niedrige Werte soll Klebzunder vermieden werden und dadurch die Oberflächenbeschaffenheit, insbesondere beim Warmpilgem von Rohren aus diesen Stählen, verbessert werden, um die ansonsten erforderliche aufwändige zerspanende Nacharbeit der Oberfläche zu vermeiden.By dispensing with the otherwise absolutely necessary nickel or by restricting the Ni content to low values, adhesive scale should be avoided and the surface finish, in particular in the hot piled up of pipes made of these steels, be improved by the otherwise required complex machining finishing of the surface to avoid.

Konstruktionsrohre für die oben genannten Anwendungsbereiche unterliegen höchsten Beanspruchungen hinsichtlich Festigkeit und Zähigkeit bei tiefen Temperaturen bis zu -40°C.Construction tubes for the above applications are subject to the highest demands in terms of strength and toughness at low temperatures down to -40 ° C.

Um die geforderten Eigenschaften zu erreichen müssen die Rohre nach dem Warmwalzen einer Vergütungsbehandlung unterzogen werden.In order to achieve the required properties, the tubes must be subjected to a tempering treatment after hot rolling.

Mit dem aus der DE 199 42 641 A1 als FGS 70 bekannten Stahl, wurden alle geforderten Mindestwerte für Streckgrenze, Zugfestigkeit, Bruchdehnung und Kerbschlagarbeit sicher erreicht.With the from the DE 199 42 641 A1 Steel known as FGS 70, all required minimum values for yield strength, tensile strength, elongation at break and impact energy were achieved safely.

Die Anforderungen an Konstruktionsrohre für die vorgenannten Anwendungsbereiche sind allerdings in den letzten Jahren immer weiter gewachsen, so dass heute zunehmend Bedarf an Konstruktionsrohren mit folgenden Anforderungen besteht:

  • Streckgrenze Rp0,2 min.:    960 MPa
  • Zugfestigkeit Rm:    980 -1150 MPa
  • Kerbschlagarbeit Av (längs):    27 J bei -40°C
  • Gewährleistung der allgemeinen Schweißbarkeit
  • niedriger, bzw. eingeschränkter Ni-Gehalt
However, the requirements for construction tubes for the aforementioned application areas have grown steadily in recent years, so that today there is an increasing demand for construction tubes with the following requirements:
  • Yield strength R p0.2 min .: 960 MPa
  • Tensile strength Rm: 980-1150 MPa
  • Notched impact Av (longitudinal): 27 J at -40 ° C
  • Ensuring general weldability
  • low or limited Ni content

Die geforderte Steigerung der Festigkeit bei ausreichender Zähigkeit von warmgefertigten nahtlosen Rohren für die beschriebenen Anwendungsbereiche erfordert die Entwicklung neuer Legierungskonzepte. Speziell im Streckgrenzenbereich um 1000 MPa erreichen konventionelle Legierungskonzepte keine ausreichende Zähigkeit bei tiefen Temperaturen.The required increase in strength with sufficient toughness of hot-finished seamless tubes for the applications described requires the development of new alloy concepts. Especially in the yield strength range around 1000 MPa, conventional alloy concepts do not achieve sufficient toughness at low temperatures.

Der die Festigkeit steigernde Mechanismus, der gleichzeitig zu einer Steigerung der Zähigkeit führt, ist bekanntermaßen die Verringerung der Korngröße. Sie kann z. B. durch die Zulegierung von Nickel oder Molybdän und der damit verbundenen Verringerung der Umwandlungstemperatur, erzielt werden.The strength-increasing mechanism, which at the same time leads to an increase in toughness, is known to reduce the grain size. You can z. Example by the addition of nickel or molybdenum and the associated reduction in the transformation temperature can be achieved.

Diese Legierungskonzepte führen jedoch zu einer Steigerung des Kohlenstoffäquivalentes und damit verbunden zu einer schlechteren Schweißbarkeit. Zudem erhöhen Nickel und Molybdän die Legierungskosten signifikant und außerdem verschlechtert Nickel zusätzlich die Oberflächenqualität der warmgewalzten Rohre.However, these alloy concepts lead to an increase in the carbon equivalent and, associated therewith, to a poorer weldability. In addition, nickel and molybdenum significantly increase the alloying costs, and in addition, nickel additionally deteriorates the surface quality of the hot-rolled tubes.

Die naheliegende Möglichkeit der Erhöhung des Kohlenstoffgehaltes zur Festigkeitssteigerung würde jedoch zu einer Verschlechterung der Zähigkeit und einer starken Erhöhung des Kohlenstoffäquivalentes führen.The obvious possibility of increasing the carbon content to increase the strength, however, would lead to a deterioration of the toughness and a large increase in the carbon equivalent.

Vanadium wird ebenfalls zur Steigerung der Festigkeit genutzt. Dieses Konzept basiert auf der Mischkristallhärtung des Vanadium und der Ausscheidung feinster Vanadium-Karbide während der Anlassbehandlung.Vanadium is also used to increase strength. This concept is based on the solid-solution hardening of vanadium and the precipitation of finest vanadium carbides during annealing.

Mit den vorgenannten Legierungskonzepten können die geforderten Eigenschaften jedoch nicht erreicht werden.With the aforementioned alloy concepts, however, the required properties can not be achieved.

Eine Verringerung der Korngröße zur Verbesserung der mechanischen Eigenschaften kann grundsätzlich auch durch thermomechanische Behandlung erfolgen.A reduction of the grain size to improve the mechanical properties can in principle be carried out by thermomechanical treatment.

Die spezifische Temperaturführung bei der Warmfertigung nahtloser Rohren erlaubt jedoch nicht die erforderliche Absenkung der Umformtemperatur für die Anwendung bekannter Konzepte für eine thermomechanische Behandlung.However, the specific temperature control in hot seamless tube manufacturing does not allow for the required reduction in forming temperature for the application of known thermo-mechanical treatment concepts.

Bislang können die geforderten hohen Anforderungen nur mit hoch legierten Stählen erreicht werden, die aufgrund ihrer hohen Kosten keine oder nur geringe Marktakzeptanz gefunden haben.So far, the required high requirements can only be achieved with highly alloyed steels, which have found little or no market acceptance due to their high costs.

Aufgabe der Erfindung ist es, eine kostengünstige Stahllegierung für einen niedrig legierten Stahl zur Herstellung hochfester schweißbarer nahtloser Stahlrohre, insbesondere Konstruktionsrohre, anzugeben, der die genannten Mindestanforderungen hinsichtlich Streckgrenze, Zugfestigkeit und Kerbschlagarbeit sicher erfüllt und darüber hinaus eine gute allgemeine Schweißbarkeit gewährleistet und beim Warmwalzen zu optisch einwandfreien Oberflächen führt.The object of the invention is to provide a low-cost steel alloy for a low-alloy steel for producing high-strength weldable seamless steel pipes, in particular construction pipes, which meets the minimum requirements for yield strength, tensile strength and impact energy safely and beyond ensures good overall weldability and during hot rolling leads to optically flawless surfaces.

Diese Aufgabe wird ausgehend vom Oberbegriff in Verbindung mit den kennzeichnenden Merkmalen des Anspruches 1 gelöst. Vorteilhafte Weiterbildungen sind Gegenstand von Unteransprüchen.This object is achieved starting from the preamble in conjunction with the characterizing features of claim 1. Advantageous developments are the subject of dependent claims.

Nach der Lehre der Erfindung wird für einen niedrig legierten Stahl zur Herstellung hochfester schweißbarer warmgewalzter nahtloser Stahlrohre, insbesondere Konstruktionsrohre, eine Stahllegierung mit folgender chemischer Zusammensetzung vorgeschlagen:

  • 0,15- 0,18 % C
  • 0,20 - 0,40 % Si
  • 1,40 - 1,60 % Mn
  • max. 0,05 % P
  • max. 0,01 % S
  • >0,50 - 0,90 % Cr
  • >0,50 - 0,80 % Mo
  • >0,10 - 0,15 % V
  • 0,60- 1,00 % W
  • 0,0130 - 0,0220 % N
Rest Eisen mit erschmelzungsbedingten Verunreinigungen, mit optionaler Zugabe eines oder mehrerer Elemente von Al, Ni, Nb und Ti, mit der Maßgabe, dass das Verhältnis V/N einen Wert von 4 bis 12 aufweist und der Ni- Gehalt des Stahls nicht mehr als 0,40 % beträgt.According to the teachings of the invention, for a low alloy steel for producing high strength weldable hot rolled seamless steel tubes, in particular construction tubes, a steel alloy having the following chemical composition is proposed:
  • 0.15-0.18% C
  • 0.20-0.40% Si
  • 1.40 - 1.60% Mn
  • Max. 0.05% P
  • Max. 0.01% S
  • > 0.50-0.90% Cr
  • > 0.50 - 0.80% Mo
  • > 0.10 - 0.15% V
  • 0.60-1.00% W
  • 0.0130 - 0.0220% N
The remainder is iron with impurities due to fusion, with optional addition of one or more elements of Al, Ni, Nb and Ti, provided that the ratio V / N has a value of 4 to 12 and the Ni content of the steel is not more than 0 , 40%.

Die erfindungsgemäße Stahllegierung setzt auf der Entwicklung des aus der DE 199 42 641 A1 bekannten wolframlegierten Feinkornbaustahls auf.The steel alloy according to the invention is based on the development of the DE 199 42 641 A1 known tungsten-alloyed fine grain structural steel.

Aus bisherigen Erfahrungen ist nicht bekannt, dass Wolfram einen negativen Einfluss auf die Schweißbarkeit hat. Die maximal erreichbare Streckgrenzensteigerung durch die Legierung mit Wolfram ist nach Untersuchungen allerdings nur bis ca. 900 MPa gegeben. Eine weitere Steigerung ist ausschließlich durch eine Erhöhung des Wolframgehaltes nicht möglich. Als günstig hat sich deshalb ein W-Gehalt von 0,60 -1,0 %, vorzugsweise von 0,7 - 0,9 % herausgestellt.From previous experience it is not known that tungsten has a negative influence on the weldability. The maximum achievable yield strength increase by the alloy with tungsten is, however, only given up to about 900 MPa. A further increase is not possible exclusively by increasing the tungsten content. Therefore, a W content of 0.60-1.0%, preferably 0.7-0.9%, has proven favorable.

Die im Zuge der vorliegenden Erfindung durchgeführten Versuche haben überraschend gezeigt, dass bei einer im Vergleich zur bekannten Stahllegierung nur geringfügig höheren Zugabe an Legierungselementen wie Cr und Mo, die Einhaltung bestimmter V/N-Verhältnisse zu einem deutlichen Festigkeitssprung unter Einhaltung der geforderten Mindestkerbschlagarbeit von 27 J bei -40°C führt.The experiments carried out in the course of the present invention have surprisingly shown that in a comparison to the known steel alloy only slightly higher addition of alloying elements such as Cr and Mo, the compliance of certain V / N ratios to a significant jump in strength while maintaining the required minimum notch impact of 27 J at -40 ° C leads.

Für das Erreichen einer gewissen "Basisfestigkeit" hat sich herausgestellt, dass die Summe der Zugaben an Cr, Mo und W jedoch mindestens 1,5 Gew. % betragen sollten.However, to achieve a certain "basic strength", it has been found that the sum of the additions of Cr, Mo and W should be at least 1.5% by weight.

Die Erfindung beinhaltet das innovative Konzept der Anhebung der Rekristallisationsstopptemperatur deutlich über die Endwälztemperatur durch gezielte Mikrolegierung mit Vanadium und Stickstoff. Basierend auf umfangreichen thermodynamischen Berechnungen muss das Verhältnis der Gehalte von V und N zwischen 4 und 12 liegen, um den gewünschten Effekt zu erreichen.The invention includes the innovative concept of raising the recrystallization stop temperature significantly above the final rolling temperature through targeted micro-alloying with vanadium and nitrogen. Based on extensive thermodynamic calculations, the ratio of the contents of V and N must be between 4 and 12 in order to achieve the desired effect.

Generell sind hohe Gehalte an gelöstem Stickstoff als nachteilig für die Zähigkeit zu betrachten. Durch die geeignete Wahl des V/N-Verhältnisses im Bereich von 4 -12 kann der Gehalt an gelöstem Stickstoff allerdings auf ein Minimum reduziert werden, während gleichzeitig die gebildeten Vanadium-Karbonitride den beschriebenen Effekt der Kornfeinung durch thermomechanische Behandlung bewirken.In general, high levels of dissolved nitrogen are considered detrimental to toughness. However, by properly choosing the V / N ratio in the range of 4 -12, the content of dissolved nitrogen can be minimized while at the same time the vanadium carbonitrides formed cause the described effect of grain refining by thermomechanical treatment.

Der somit ungewöhnlich hohe aber durch die Bildung von Vanadium-Karbonitriden unschädliche bzw. sogar zur Kornfeinung eingesetzte Stickstoffgehalt der Legierung ermöglicht zudem vorteilhaft den Verzicht auf kostenintensive Entgasungsbehandlungen im Rahmen der Sekundärmetallurgie.The thus unusually high but not harmful by the formation of vanadium carbonitrides or even used for grain refining nitrogen content of the alloy also advantageously allows the waiver of costly degassing treatments in the context of secondary metallurgy.

Im Rahmen des erfindungsgemäßen Legierungskonzeptes ist je nach Anforderungen eine optionale Zulegierung eines oder mehrerer Legierungselemente von Al, Ni, Nb und Ti vorgesehen. Diese Anforderungen können sich z. B. aus unterschiedlich zu walzenden Wanddicken der Rohre ergeben, die im Bereich von unter 10 mm bis über 80 mm liegen können und insbesondere bei größeren Wanddicken eine Zulegierung der genannten Elemente erforderlich machen, um die geforderten Eigenschaften durch Kornfeinung zu erreichen.As part of the alloying concept according to the invention, an optional alloying of one or more alloying elements of Al, Ni, Nb and Ti is provided, depending on the requirements. These requirements can be z. B. from different to be rolled wall thicknesses of the tubes, which may be in the range of less than 10 mm to about 80 mm and in particular for larger wall thicknesses require a Zulegierung said elements in order to achieve the required properties by grain refining.

Im Hinblick auf eine optimale Kosten-/Nutzenrelation des Legierungskonzeptes haben sich als günstig Gehalte von max. 0,03 % Al, max. 0,40 % Ni, max. 0,04 % Nb und max. 0,04 % Ti erwiesen.With regard to an optimal cost / benefit ratio of the alloy concept, favorable contents of max. 0.03% Al, max. 0.40% Ni, max. 0.04% Nb and max. 0.04% Ti proved.

Der Ni- Gehalt ist mit max. 0,40 % ausreichend niedrig, um bei dem für diese Stahlgüte hauptsächlich angewandten Rohrkontiverfahren eine ausreichend gute Obertlächenqualität zu erzeugen.The Ni content is with max. 0.40% low enough to produce a sufficiently good surface quality for the tube contour method mainly used for this steel grade.

Beim Einsatz des Warmpilgerverfahrens zur Herstellung nahtloser Rohre, ist zum Erreichen einer ausreichenden Oberflächenqualität der Ni- Gehalt auf 0,20 %, vorzugsweise 0,15%, insbesondere maximal 0,10 % beschränkt.When using the hot pilger method for producing seamless pipes, the Ni content is limited to 0.20%, preferably 0.15%, in particular not more than 0.10% to achieve a sufficient surface quality.

Die aus einer Betriebsschmelze mit der nachfolgend aufgeführten erfindungsgemäßen Stahllegierung erzeugten nahtlosen Stahlrohre weisen ausgezeichnete Werte hinsichtlich ihrer Festigkeits- und Zähigkeitseigenschaften auf.

  • 0,17%C
  • 0,32%Si
  • 1,54 % Mn
  • 0, 013 % P
  • 0,003 % S
  • 0,74 %Cr
  • 0,54 % Mo
  • 0,11 % V
  • 0,75 % W
  • 0,0142 % N
  • 0,023 % Al
  • 0,16 % Ni
  • 0,001 % Ti
  • 0,164 %Ni
  • mit V/N = 8,03
The seamless steel tubes produced from an operating melt with the steel alloy of the invention listed below have excellent strength and toughness properties.
  • 0.17% C
  • 0.32% Si
  • 1.54% Mn
  • 0, 013% P
  • 0.003% S
  • 0.74% Cr
  • 0.54% Mo
  • 0.11% V
  • 0.75% W
  • 0.0142% N
  • 0.023% Al
  • 0.16% Ni
  • 0.001% Ti
  • 0.164% Ni
  • with V / N = 8.03

Hieran wurden die in der nachfolgenden Tabelle aufgeführten Werte ermittelt. Die Werte sind die Mittelwerte aus jeweils vier Zugproben bzw. vier Kerbschlagbiegeproben. Die Proben wurden als Längsproben aus betrieblich erzeugten wärmebehandelten Rohren entnommen. Geometrie
(AD x WD) Rp0,2 Rm Rp0,2/Rm A5 Av (bei -40°C) 88,9 x 5,8 mm 1070 MPa 1128 MPa 0,95 14,1% 40 J 88,9 x 5,8 mm 1047 MPa 1107 MPa 0,95 13,0 % 41 J 177,8 x 12,6 mm 1067 MPa 1092 MPa 0,98 15,5% 42 J 177,8 x 12,6 mm 1076 MPa 1103 MPa 0,98 17,0 % 37 J Anforderungen > 960 MPa 980 -1150 MPa >10% > 27 J AD: Außendurchmesser, WD: Wanddicke This was used to determine the values listed in the table below. The values are the mean values of four tensile specimens or four notched-bar impact specimens. The samples were taken as longitudinal samples from heat-treated tubes made in-house. geometry
(AD x WD) R p0 , 2 R m R p0.2 / Rm A 5 Av (at -40 ° C) 88.9 x 5.8 mm 1070 MPa 1128 MPa 0.95 14.1% 40 y 88.9 x 5.8 mm 1047 MPa 1107 MPa 0.95 13.0% 41 y 177.8 x 12.6 mm 1067 MPa 1092 MPa 0.98 15.5% 42 y 177.8 x 12.6 mm 1076 MPa 1103 MPa 0.98 17.0% 37 y conditions > 960 MPa 980-1150 MPa > 10% > 27 y OD: outer diameter, WD: wall thickness

Claims (6)

  1. A steel alloy for a low-alloy steel for producing high-tensile, weldable, hot-rolled seamless steel tubes, particularly construction tubes, with the following chemical composition (in wt.%):
    0.15 - 0.18% C
    0.20 - 0.40% Si
    1.40-1.60%Mn
    max. 0.05% P
    max. 0.01% S
    >0.50 - 0.90% Cr
    >0.50 - 0.80% Mo
    >0.10-0.15%V
    0.60- 1.00% W
    0.0130-0.0220% N
    balance: iron with impurities resulting from steelmaking, with optional addition of one or more elements from Al, Ni, Nb and Ti, so that the optionally added elements have the following contents:
    max. 0.03% Al
    max. 0.40% Ni
    max. 0.04% Nb
    max. 0.04% Ti
    with the proviso that the ratio of V/N has a value of 4 to 12 and the Ni content of the steel is no more than 0.40%.
  2. The steel alloy according to claim 1,
    characterised in that
    the W content is 0.7 - 0.9%.
  3. The steel alloy according to one of claims 1 - 2,
    characterised in that
    the addition of Cr, Mo and W is at least 1.5 wt.%
  4. A high-tensile, weldable seamless steel tube, particularly a construction tube, produced by hot rolling with subsequent hardening and tempering, consisting of a steel with the following alloying composition: 0.15-0.18% C
    0.20 - 0.40% Si
    1.40-1.60%Mn
    max. 0.05% P
    max. 0.01% S
    >0.50 - 0.90% Cr
    >0.50 - 0.80% Mo
    >0.10-0.15%V
    0.60-1.00% W
    0.013-0.0220% N with
    4≤V/N≤12
    balance: iron with impurities resulting from steelmaking, containing one or more elements from Al, Ni, Nb and Ti, so that the elements optionally added to the steel alloy have the following contents:
    max. 0.03% Al
    max. 0.40% Ni
    max. 0.04% Nb
    max. 0.04% Ti
    and a Ni content of no more than 0.40%.
  5. The construction tube according to claim 4,
    characterised in that
    the W content of the steel alloy is 0.7 - 0.9%.
  6. The construction tube according to claim 5 ,
    characterised in that
    the addition of Cr, Mo and W is at least 1.5 wt.%.
EP09712055A 2008-02-20 2009-01-23 Steel alloy for a low alloy steel for producing high-tensile seamless steel tubing Active EP2255021B1 (en)

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DE102008010749A DE102008010749A1 (en) 2008-02-20 2008-02-20 Steel alloy for a low-alloyed steel for the production of high-strength seamless steel tubes
PCT/DE2009/000088 WO2009103259A2 (en) 2008-02-20 2009-01-23 Steel alloy for a low alloy steel for producing high-tensile seamless steel tubing

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KR20100122083A (en) 2010-11-19
PL2255021T3 (en) 2012-01-31
RU2010138609A (en) 2012-03-27
CN101952472A (en) 2011-01-19
CN101952472B (en) 2013-03-06
JP2011514932A (en) 2011-05-12
UA100548C2 (en) 2013-01-10
DE102008010749A1 (en) 2009-09-24
EP2255021A2 (en) 2010-12-01
AR070612A1 (en) 2010-04-21
US8865061B2 (en) 2014-10-21
US20110315277A1 (en) 2011-12-29
ATE522634T1 (en) 2011-09-15
JP5486515B2 (en) 2014-05-07
RU2482211C2 (en) 2013-05-20
ES2372801T3 (en) 2012-01-26
KR101563604B1 (en) 2015-10-27

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