EP1561833B1 - Steel for manufacturing of high strength elements with an excellent low temperature toughness and use thereof - Google Patents
Steel for manufacturing of high strength elements with an excellent low temperature toughness and use thereof Download PDFInfo
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- EP1561833B1 EP1561833B1 EP04002612A EP04002612A EP1561833B1 EP 1561833 B1 EP1561833 B1 EP 1561833B1 EP 04002612 A EP04002612 A EP 04002612A EP 04002612 A EP04002612 A EP 04002612A EP 1561833 B1 EP1561833 B1 EP 1561833B1
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 69
- 239000010959 steel Substances 0.000 title claims abstract description 69
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 230000000977 initiatory effect Effects 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 4
- 229910001566 austenite Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 2
- 239000010955 niobium Substances 0.000 abstract 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract 2
- 239000011574 phosphorus Substances 0.000 abstract 2
- 239000011593 sulfur Substances 0.000 abstract 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 239000011651 chromium Substances 0.000 abstract 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 abstract 1
- 239000011733 molybdenum Substances 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005098 hot rolling Methods 0.000 description 5
- 238000005496 tempering Methods 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Images
Classifications
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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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- 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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- 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
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
Definitions
- the invention relates to a steel for the production of high-strength components with outstanding low-temperature toughness.
- Such steels are used for example for the production of stop or lashing, as they are needed for the attachment and securing of loads.
- these steels are processed into hot-rolled bar steel, wire rod or bright steel, from which welded round steel chains are then made.
- the stainless steels 23 MnNiCrMo 5 3 and 23 MnNiCrMo 5 which are known for this purpose and are specified in DIN 17 115, each have (in% by weight) 0.20-0.26% C, ⁇ 0.25% Si, 1, 10-1.40% Mn, each 0.020% P and S, the sum of the contents of P and S not exceeding 0.035%, if necessary 0.020-0.050% Al, up to 0.014% N and 0.40-0.60% Cr.
- the steel 23 MnNiCrMo 5 2 is additionally supplemented with 0.20-0.30% Mo and 0.70-0.90% Ni, while the steel 23 MnNiCrMo 5 4 additionally has 0.50-0.60% Mo and 0.90 - contains 1.10% Ni.
- the object of the invention was therefore to provide a high-strength steel, which still has an excellent toughness even at low temperatures, so that the risk of breakage of each of the steel component produced is reduced to a minimum, even under unfavorable, harsh operating conditions.
- advantageous uses of this steel are to be specified.
- steel according to the invention for the production of high-strength components with outstanding low-temperature toughness has the following composition (in% by weight): C: 0.08 - 0.25%, Si: 0.10 - 0.30%, Mn: 0.80 - 1.60%, P: ⁇ 0.020%, S: ⁇ 0.015%, where the sum of P and S content is ⁇ 0.030%, Cr: 0.40 - 0.80%, Not a word: 0.30 - 0.50%, Ni: 0.70 - 1.20%, al: 0.020-0.060%, N: 0.007-0.018%, V: ⁇ 0.15%, Nb: ⁇ 0.07%, where the sum of V and Nb content is ⁇ 0.020%, Remaining iron and unavoidable impurities.
- the individual alloy components are selected such that a property profile which optimally meets the requirements is achieved.
- This is achieved by the inventively predetermined contents of Cr, Ni and N and the minimum sum of the contents of Nb and V.
- inventive Steel good cold forming and has high strength in the finished state.
- it is characterized by a high notched impact strength and such a low brittle fracture transition temperature that it comes only at temperatures for brittle fracture, which are substantially lower than the brittle fracture temperature of known from the prior art steels.
- the C contents lying in the range from 0.08 to 0.25% by weight ensure the good low-temperature resistance of steels according to the invention. Particularly positive results are obtained in this context if the C content is 0.16-0.23% by weight.
- the good through-hardenability and tempering resistance of the steel according to the invention is achieved .
- the safety with which this combined effect is achieved can be increased by increasing the Cr content to 0.40-0.65% by weight and the Mo contents to 0.35-0.50% by weight. % can be set.
- steel according to the invention in the sum contains at least 0.02 wt .-% Nb and V and at the same time the contents of V to max. 0.15 wt .-% and Nb to max. 0.07 wt .-% are limited, ensuring that the desired fine grain structure is still preserved even at higher temperatures.
- V is not present in the steel according to the invention or only as an unavoidable impurity.
- finished steel according to the invention regularly has an austenite grain size finer than ASTM 10.
- the fineness of the structure of the invention steel is thus substantially larger than that of known steels, for which according to DIN 17 115 an austenite grain size of ASTM 5 is required.
- the invention thus provides a steel which still has excellent toughness even at low temperatures. Due to the favorable combination of its properties, the risk of breakage of a component produced from inventive steel is reduced to a minimum even under unfavorable, harsh operating conditions.
- Steel according to the invention is preferably processed into rolled steel.
- the aim of the processing is to preserve the finest possible fine-grained structure of the steel according to the invention via each of the processing steps. This includes not only the process steps performed during heating and rolling, but also the annealing treatments that occur and performed after deformation to the component.
- the heating and rolling conditions are selected such that, despite onset of diffusion processes during heating, high rolling temperatures are avoided in order to suppress the formation of coarse grain.
- the temperatures during further forming are also selected by a controlled withdrawal of energy during hot forming so that the desired microstructure is obtained with its fine-grained structure.
- steel according to the invention is particularly suitable for the production of high-strength components by cold forming with subsequent tempering.
- These components may be, for example, means for carrying, pulling, lifting, conveying or securing loads associated with the highest strength class.
- Such summarized under the preamble stop and lashing items include, for example, attachment points, hooks, brackets, loops, chains, joints, swirl elements, rockers, struts, spindle and ratchet tensioner, load blocks and the like.
- inventive steel means for connecting components with excellent performance properties are, for example, bolts or other connection or force transmission elements, such as screws, clamps, rods or the like.
- Chains produced according to the invention can safely withstand high loads even in great cold, without the risk of breakage or comparable damage occurring.
- round steel chains, in particular welded round steel chains can be produced which are able to cope with the highest demands.
- the components made of steel according to the invention regularly have a strength of at least 1200 MPa, in particular more than 1550 MPa, 1600 MPa or 1650 MPa. It should be emphasized in this context that, with a strength of at least 1550 MPa, the brittle fracture transition temperature FATT of the components made from steel according to the invention is regularly at most - 60 ° C. This limit temperature is significantly lower than in known steels.
- the notch impact value is regularly more than 45 J and the respective component has a technical crack initiation toughness J IC of more than 170 N / mm at -60 ° C., in particular more than 185 N / mm.
- the crack initiation toughness J IC is one in the ASTM 1820 defined value, which allows an assessment of the ductile fracture tendency of a steel material.
- the high toughness of the steel according to the invention is also noticeable in that the components produced from such steel regularly have an elongation at break of more than 28%.
- the rolled steel After hot rolling and a long-term heat treatment, which was done to set a favorable for the subsequent cold working strength, the rolled steel has been formed into chain links, which have been closed after assembly of the chain by welding.
- the chains produced in this way had a fine grain structure of ASTM 11, a strength of 1270 N / mm 2 and a brittle fracture transition temperature FATT of -70 ° C determined at this strength. Its impact value was 557 J at -60 ° C test temperature and the elongation at break was 28%.
Abstract
Description
Die Erfindung betrifft einen Stahl zur Herstellung von hochfesten Bauteilen mit herausragender Tieftemperaturzähigkeit. Derartige Stähle werden beispielsweise für die Herstellung von Anschlag- oder Zurrmitteln verwendet, wie sie für die Befestigung und Sicherung von Lasten benötigt werden. Insbesondere werden diese Stähle zu warmgewalzten Stabstahl, Walzdraht oder Blankstahl verarbeitet, aus denen dann geschweißte Rundstahlketten gefertigt werden.The invention relates to a steel for the production of high-strength components with outstanding low-temperature toughness. Such steels are used for example for the production of stop or lashing, as they are needed for the attachment and securing of loads. In particular, these steels are processed into hot-rolled bar steel, wire rod or bright steel, from which welded round steel chains are then made.
Die an Stähle der voranstehend erläuterten Art gestellten Anforderungen sind in der DIN 17 115 formuliert. Neben einer guten Umformbarkeit und einer ebenso guten Eignung zum Verschweißen müssen die Stähle hervorragende Festigkeits- und Zähigkeitseigenschaften besitzen, um die sich aufgrund der in der Praxis auftretenden Belastungen stellenden Anforderungen zu erfüllen.The requirements imposed on steels of the type described above are formulated in DIN 17 115. In addition to good formability and equally good welding ability, the steels must have excellent strength and toughness properties to meet the requirements imposed by the stresses encountered in practice.
Die zu diesem Zweck bekannten, in der DIN 17 115 angegebenen Edelstähle 23 MnNiCrMo 5 3 und 23 MnNiCrMo 5 4 weisen (in Gew.-%) jeweils 0,20 - 0,26 % C, ≤ 0,25 % Si, 1,10 - 1,40 % Mn, jeweils 0,020 % P und S, wobei die Summe der Gehalte an P und S 0,035 % nicht überschreitet, erforderlichenfalls 0,020 - 0,050 % Al, bis zu 0,014 % N und 0,40 - 0,60 % Cr. Dem Stahl 23 MnNiCrMo 5 2 sind zusätzlich 0,20 - 0,30 % Mo und 0,70 - 0,90 % Ni zugegeben, während der Stahl 23 MnNiCrMo 5 4 zusätzlich 0,50 - 0,60 % Mo und 0,90 - 1,10 % Ni enthält.The stainless steels 23 MnNiCrMo 5 3 and 23 MnNiCrMo 5 4, which are known for this purpose and are specified in DIN 17 115, each have (in% by weight) 0.20-0.26% C, ≦ 0.25% Si, 1, 10-1.40% Mn, each 0.020% P and S, the sum of the contents of P and S not exceeding 0.035%, if necessary 0.020-0.050% Al, up to 0.014% N and 0.40-0.60% Cr. The steel 23 MnNiCrMo 5 2 is additionally supplemented with 0.20-0.30% Mo and 0.70-0.90% Ni, while the steel 23 MnNiCrMo 5 4 additionally has 0.50-0.60% Mo and 0.90 - contains 1.10% Ni.
Ein anderer Stahl zur Herstellung von Ketten zum Festmachen bzw. Vertäuen von Schiffen oder Bohrplattformen bestimmten Ketten ist aus der chinesischen Patentveröffentlichung CN-1281906 bekannt. Aus dem in der Datenbank WPINDEX verfügbaren Abstract zu dieser Veröffentlichung geht hervor, dass der bekannte Stahl (in Gew.-%) 0,25 - 0,35 % C, 0,15 - 0,30 % Si, 1,45 % - 1,75 % Mn, 0,90 - 1,40 % Cr, 1,00 - 1,20 % Ni, 0,45 - 0,65 % Mo, 0,02 - 0,06 % Nb, 0,020 - 0,05 % Al, bis zu 0,020 % P, bis zu 0,15 % S, bis zu 0,20 % Cu, bis zu 0,03 % Sn, bis zu 0,01 % Sb, bis zu 0,04 % As, bis zu 0,005 % B, bis zu 0,009 % N, bis zu 0,0020 % O, bis zu 0,0002 % H, Rest Fe und unvermeidbare Verunreinigungen enthält, wobei zusätzlich ein Kohlenstoffäquivalent größer 1,4 sein muss.Another steel used to make chains for mooring ships or drilling platforms is known from Chinese Patent Publication CN-1281906. The abstract available in the WPINDEX database for this publication shows that the known steel (in% by weight) contains 0.25-0.35% C, 0.15-0.30% Si, 1.45% 1.75% Mn, 0.90-1.40% Cr, 1.00-1.20% Ni, 0.45-0.65% Mo, 0.02-0.06% Nb, 0.020-0, 05% Al, up to 0.020% P, up to 0.15% S, up to 0.20% Cu, up to 0.03% Sn, up to 0.01% Sb, up to 0.04% As, up to 0.005% B, up to 0.009% N, up to 0.0020% O, up to 0.0002% H, remainder containing Fe and unavoidable impurities, with an additional carbon equivalent greater than 1.4.
Praktische Erfahrungen zeigen, dass die bekannten Stähle bei Raumtemperatur zwar die hinsichtlich Festigkeit und Zähigkeit gestellten Anforderungen erfüllen, dass es jedoch bei tieferen Temperaturen insbesondere in Bezug auf die Zähigkeit zu Problemen kommt.Practical experience shows that the known steels at room temperature meet the requirements in terms of strength and toughness, but that problems occur at lower temperatures, in particular with regard to toughness.
Aufgabe der Erfindung war es daher, einen hochfesten Stahl zu schaffen, der auch bei tiefen Temperaturen noch eine hervorragende Zähigkeit besitzt, so dass die Gefahr eines Bruchs des aus dem Stahl jeweils erzeugten Bauteils auch unter ungünstigen, harten Betriebsbedingungen auf ein Minimum reduziert ist. Zudem sollen vorteilhafte Verwendungen dieses Stahls angegeben werden.The object of the invention was therefore to provide a high-strength steel, which still has an excellent toughness even at low temperatures, so that the risk of breakage of each of the steel component produced is reduced to a minimum, even under unfavorable, harsh operating conditions. In addition, advantageous uses of this steel are to be specified.
In Bezug auf den Stahl wird diese Aufgabe erfindungsgemäß dadurch gelöst, dass erfindungsgemäßer Stahl zur Herstellung von hochfesten Bauteilen mit herausragender Tieftemperaturzähigkeit, die folgende Zusammensetzung aufweist (in Gew.-%):
Rest Eisen und unvermeidbare Verunreinigungen.With regard to the steel, this object is achieved according to the invention in that steel according to the invention for the production of high-strength components with outstanding low-temperature toughness has the following composition (in% by weight):
Remaining iron and unavoidable impurities.
Bei erfindungsgemäßem Stahl sind die einzelnen Legierungskomponenten so gewählt, dass ein den sich stellenden Anforderungen optimal gerecht werdendes Eigenschaftsprofil erreicht ist. Dies wird durch die erfindungsgemäß vorgegebenen Gehalte an Cr, Ni und N sowie die Mindestsumme der Gehalte an Nb und V erreicht. Indem die erfindungsgemäß vorgegebenen Gehaltsbereiche für diese Legierungselemente eingehalten werden, werden eine besonders hohe Zähigkeit, eine gute Durchhärtbarkeit, eine verbesserte Anlassbeständigkeit und eine besonders feine Kornstruktur erreicht. Gleichzeitig ist erfindungsgemäßer Stahl gut kaltverformbar und besitzt im fertig verarbeiteten Zustand hohe Festigkeiten. Zudem zeichnet er sich durch eine hohe Kerbschlagzähigkeit sowie eine so niedrige Sprödbruchübergangstemperatur aus, dass es erst bei Temperaturen zum Sprödbruch kommt, die wesentlich niedriger liegen als die Sprödbruchtemperatur von aus dem Stand der Technik bekannten Stählen.In the case of steel according to the invention, the individual alloy components are selected such that a property profile which optimally meets the requirements is achieved. This is achieved by the inventively predetermined contents of Cr, Ni and N and the minimum sum of the contents of Nb and V. By observing the content ranges specified for these alloying elements according to the invention, a particularly high toughness, a good through hardenability, an improved tempering resistance and a particularly fine grain structure are achieved. At the same time is inventive Steel good cold forming and has high strength in the finished state. In addition, it is characterized by a high notched impact strength and such a low brittle fracture transition temperature that it comes only at temperatures for brittle fracture, which are substantially lower than the brittle fracture temperature of known from the prior art steels.
Die im Bereich von 0,08 - 0,25 Gew.-% liegenden C-Gehalte sorgen für die gute Tieftemperaturbeständigkeit erfindungsgemäßer Stähle. Besonders positive Ergebnisse ergeben sich in diesem Zusammenhang dann, wenn der C-Gehalte 0,16 - 0,23 Gew.-% beträgt.The C contents lying in the range from 0.08 to 0.25% by weight ensure the good low-temperature resistance of steels according to the invention. Particularly positive results are obtained in this context if the C content is 0.16-0.23% by weight.
Durch die Eingrenzung der Cr-Gehalte auf 0,40 - 0,80 Gew.-% in Kombination mit Mo-Gehalten, die 0,30 - 0,50 Gew.-% betragen, wird die gute Durchhärtbarkeit und Anlassbeständigkeit des erfindungsgemäßen Stahls erreicht. Die Sicherheit, mit der diese kombinierte Wirkung erzielt wird, kann dabei dadurch erhöht werden, dass die Cr-Gehalt auf 0,40 - 0,65 Gew.-% und die Mo-Gehalte auf 0,35 - 0,50 Gew.-% eingestellt werden.By limiting the Cr contents to 0.40-0.80% by weight in combination with Mo contents of 0.30-0.50% by weight, the good through-hardenability and tempering resistance of the steel according to the invention is achieved , The safety with which this combined effect is achieved can be increased by increasing the Cr content to 0.40-0.65% by weight and the Mo contents to 0.35-0.50% by weight. % can be set.
Ni-Gehalte von 0,70 - 1,20 Gew.-%, insbesondere 0,75 - 1,00 Gew.-%, bewirken in erfindungsgemäßem Stahl die besonders hervorzuhebende gute Tieftemperaturzähigkeit.Ni contents of from 0.70 to 1.20% by weight, in particular from 0.75 to 1.00% by weight, in the steel according to the invention bring about the particularly good low-temperature toughness.
Die Gehalte an Al von 0,020 - 0,060 Gew.-%, insbesondere 0,020 - 0,045 Gew.-%, und N von 0,007 - 0,018 Gew.-%, insbesondere 0,007 - 0,015 Gew.-%, führen in erfindungsgemäßen Stählen zu einer besonderes feinen Kornstruktur.The contents of Al of 0.020-0.060% by weight, in particular 0.020-0.045% by weight, and N of 0.007-0.018% by weight, in particular 0.007-0.015% by weight, lead to a particularly fine in steels according to the invention grain structure.
Schließlich ist dadurch, dass erfindungsgemäßer Stahl in der Summe mindestens 0,02 Gew.-% Nb und V enthält und gleichzeitig die Gehalte an V auf max. 0,15 Gew.-% und Nb auf max. 0,07 Gew.-% beschränkt sind, sichergestellt, dass das angestrebte Feinkorngefüge auch bei höheren Temperaturen noch erhalten bleibt. Überraschend hat sich in diesem Zusammenhang herausgestellt, dass dieser Effekt besonders sicher dann eintritt, wenn der erfindungsgemäße Stahl frei von Vanadium ist. Gemäß einer bevorzugten Ausgestaltung ist V daher in erfindungsgemäßem Stahl gar nicht bzw. nur als unvermeidbare Verunreinigung vorhanden.Finally, the fact that steel according to the invention in the sum contains at least 0.02 wt .-% Nb and V and at the same time the contents of V to max. 0.15 wt .-% and Nb to max. 0.07 wt .-% are limited, ensuring that the desired fine grain structure is still preserved even at higher temperatures. Surprisingly, it has been found in this context that this effect occurs particularly reliably when the steel according to the invention is free from vanadium. According to a preferred embodiment, therefore, V is not present in the steel according to the invention or only as an unavoidable impurity.
Das Feinkorn bleibt auch im Zuge der Vergütungsbehandlung stabil. So weist erfindungsgemäßer, fertig verarbeiteter Stahl regelmäßig eine Austenitkorngröße auf, die feiner als ASTM 10 ist. Die Feinheit des Gefüges erfindungsgemäßen Stahls ist damit wesentlich größer als die von bekannten Stählen, für die gemäß der DIN 17 115 eine Austenitkorngröße von ASTM 5 gefordert wird.The fine grain also remains stable in the course of the tempering treatment. Thus, finished steel according to the invention regularly has an austenite grain size finer than ASTM 10. The fineness of the structure of the invention steel is thus substantially larger than that of known steels, for which according to DIN 17 115 an austenite grain size of ASTM 5 is required.
Mit der Erfindung steht somit ein Stahl zur Verfügung, der auch bei tiefen Temperaturen noch eine hervorragende Zähigkeit besitzt. Aufgrund der günstigen Kombination seiner Eigenschaften ist die Gefahr eines Bruchs eines aus erfindungsgemäßem Stahl erzeugten Bauteils auch unter ungünstigen, harten Betriebsbedingungen auf ein Minimum reduziert.The invention thus provides a steel which still has excellent toughness even at low temperatures. Due to the favorable combination of its properties, the risk of breakage of a component produced from inventive steel is reduced to a minimum even under unfavorable, harsh operating conditions.
Erfindungsgemäßer Stahl wird bevorzugt zu Walzstahl verarbeitet. Ziel der Verarbeitung ist es, über jeden der Verarbeitungsschritte das möglichst feinkörnige Gefüge des erfindungsgemäßen Stahls zu bewahren. Dies umfasst nicht nur die während des Erwärmens und Walzens durchgeführten Prozessschritte, sondern auch die Glühbehandlungen, die vor und nach der Verformung zum Bauteil durchgeführt werden. So werden erfindungsgemäß die Wärm- und Abwalzbedingungen so gewählt, dass trotz einsetzender Diffusionsvorgänge beim Wärmen hohe Walztemperaturen vermieden werden, um die Entstehung von grobem Korn zu unterdrücken. Die Temperaturen bei der weiteren Umformung werden durch einen geregelten Entzug von Energie bei der Warmumformung zudem so gewählt, dass das angestrebte Gefüge mit seiner feinkörnigen Struktur erhalten wird. Ein beschleunigter Wärmeentzug direkt nach der letzten Umformarbeit verhindert dabei im Sinne eines "Einfrierens" des zuletzt erreichten Gefügezustands unerwünschte Ausscheidungsvorgänge, die andernfalls eine Abnahme der Härte und Zähigkeit zur Folge hätten. Stattdessen werden durch eine Langzeitwärmebehandlung gezielte Ausscheidungszustände der Carbonitride hinsichtlich ihrer Größe und Verteilung hergestellt, um die für eine Kaltverformung des Stahls zum jeweiligen Bauteil gewünschten relativ niedrigen Werkstofffestigkeiten des Stahls im warmgewalzten Zustand zu erhalten.Steel according to the invention is preferably processed into rolled steel. The aim of the processing is to preserve the finest possible fine-grained structure of the steel according to the invention via each of the processing steps. This includes not only the process steps performed during heating and rolling, but also the annealing treatments that occur and performed after deformation to the component. Thus, according to the invention, the heating and rolling conditions are selected such that, despite onset of diffusion processes during heating, high rolling temperatures are avoided in order to suppress the formation of coarse grain. The temperatures during further forming are also selected by a controlled withdrawal of energy during hot forming so that the desired microstructure is obtained with its fine-grained structure. An accelerated removal of heat directly after the last forming work prevents unwanted precipitation processes in the sense of a "freezing" of the last microstructure state that would otherwise result in a decrease in hardness and toughness. Instead, by means of a long-term heat treatment, specific precipitation states of the carbonitrides are produced with regard to their size and distribution in order to obtain the relatively low material strengths of the steel in the hot-rolled state which are required for cold deformation of the steel to the respective component.
Aufgrund seines besonderen Eigenschaftsspektrums eignet sich erfindungsgemäßer Stahl insbesondere zur Herstellung von hochfesten Bauteilen durch Kaltverformen mit nachfolgendem Vergüten. Bei diesen Bauteilen kann es sich beispielsweise um Mittel zum Tragen, Ziehen, Heben, Fördern oder Sichern von Lasten handeln, die der höchsten Festigkeitsklasse zugeordnet sind. Derartige unter dem Oberbegriff Anschlag- und Zurrmittel zusammengefasste Gegenstände umfassen beispielsweise Anschlagpunkte, Haken, Bügel, Ösen, Ketten, Gelenke, Wirbelelemente, Wippen, Streben, Spindel- und Ratschenspanner, Lastböcke und Vergleichbares.Due to its special property spectrum, steel according to the invention is particularly suitable for the production of high-strength components by cold forming with subsequent tempering. These components may be, for example, means for carrying, pulling, lifting, conveying or securing loads associated with the highest strength class. Such summarized under the preamble stop and lashing items include, for example, attachment points, hooks, brackets, loops, chains, joints, swirl elements, rockers, struts, spindle and ratchet tensioner, load blocks and the like.
Auch lassen sich aus erfindungsgemäßem Stahl Mittel zum Verbinden von Bauelementen mit hervorragenden Gebrauchseigenschaften fertigen. Bei diesen Bauelementen handelt es sich beispielsweise um Bolzen oder andere Verbindungs- oder Kraftübertragungselemente, wie Schrauben, Klemmen, Stangen oder Vergleichbares.Also can be made of inventive steel means for connecting components with excellent performance properties. These components are, for example, bolts or other connection or force transmission elements, such as screws, clamps, rods or the like.
Ein Anwendungsgebiet, für das sich erfindungsgemäßer Stahl besonders gut verwenden lässt, ist die Herstellung von Ketten. Aus erfindungsgemäß beschaffenem Stahl erzeugte Ketten ertragen auch in großer Kälte sicher hohe Belastungen, ohne dass die Gefahr eines Bruchs oder vergleichbare Beschädigungen auftreten. So lassen sich aus erfindungsgemäßem Stahl Rundstahlketten, insbesondere geschweißte Rundstahlketten, herstellen, die höchsten Anforderungen sicher gewachsen sind.One field of application for which steel according to the invention can be used particularly well is the production of chains. Chains produced according to the invention can safely withstand high loads even in great cold, without the risk of breakage or comparable damage occurring. Thus, from steel according to the invention, round steel chains, in particular welded round steel chains, can be produced which are able to cope with the highest demands.
Die aus erfindungsgemäßem Stahl gefertigten Bauteile besitzen regelmäßig eine Festigkeit von mindestens 1200 MPa, insbesondere mehr als 1550 MPa, 1600 MPa oder 1650 MPa. Hervorzuheben ist in diesem Zusammenhang, dass bei einer Festigkeit von mindestens 1550 MPa die Sprödbruchübergangstemperatur FATT der aus erfindungsgemäßem Stahl gefertigten Bauteile regelmäßig bei höchstens - 60 °C liegt. Diese Grenztemperatur ist deutlich niedriger als bei bekannten Stählen.The components made of steel according to the invention regularly have a strength of at least 1200 MPa, in particular more than 1550 MPa, 1600 MPa or 1650 MPa. It should be emphasized in this context that, with a strength of at least 1550 MPa, the brittle fracture transition temperature FATT of the components made from steel according to the invention is regularly at most - 60 ° C. This limit temperature is significantly lower than in known steels.
Ebenso bemerkenswert ist, dass bei aus erfindungsgemäßem Stahl erzeugten Bauteilen der Kerbschlagarbeitswert regelmäßig mehr als 45 J beträgt und das jeweilige Bauteil eine technische Rissinitiierungszähigkeit JIC von mehr als 170 N/mm bei -60 °C, insbesondere mehr als 185 N/mm aufweist. Der Rissinitiierungszähigkeit JIC ist ein in der ASTM 1820 definierter Wert, der eine Bewertung der Zähbruchneigung eines Stahlwerkstoffs ermöglicht.It is also noteworthy that, in the case of components produced from steel according to the invention, the notch impact value is regularly more than 45 J and the respective component has a technical crack initiation toughness J IC of more than 170 N / mm at -60 ° C., in particular more than 185 N / mm. The crack initiation toughness J IC is one in the ASTM 1820 defined value, which allows an assessment of the ductile fracture tendency of a steel material.
Die hohe Zähigkeit des erfindungsgemäßen Stahls macht sich auch darin bemerkbar, dass die aus solchem Stahl erzeugten Bauteile regelmäßig eine Bruchdehnung von mehr als 28 % aufweisen.The high toughness of the steel according to the invention is also noticeable in that the components produced from such steel regularly have an elongation at break of more than 28%.
Nachfolgend wird die Erfindung anhand eines Ausführungsbeispiels näher erläutert.The invention will be explained in more detail with reference to an embodiment.
Ein Stahl mit (in Gew.-%)
- 0,19 %C,
- 0,20 % Si,
- 1,31 % Mn,
- 0,005 % P,
- 0,010 % S,
- P-Gehalt + S-Gehalt = 0,015 %,
- 0,45 % Cr,
- 0,37 % Mo,
- 0,88 % Ni,
- 0,400 % Al,
- 0,008 % N,
- 0,01 % V,
- 0,06 % Nb,
- (V-Gehalt + Nb-Gehalt = 0,07 %),
- Rest Fe und unvermeidbare Verunreinigungen
- 0.19% C,
- 0.20% Si,
- 1.31% Mn,
- 0.005% P,
- 0.010% S,
- P content + S content = 0.015%,
- 0.45% Cr,
- 0.37% Mo,
- 0.88% Ni,
- 0.400% Al,
- 0.008% N,
- 0.01% V,
- 0.06% Nb,
- (V content + Nb content = 0.07%),
- Residual Fe and unavoidable impurities
Nach dem Warmwalzen und einer Langzeitwärmebehandlung, die für die Einstellung einer für die anschließende Kaltverformung günstige Festigkeit erfolgte, ist der Walzstahl zu Kettengliedern geformt worden, die nach dem Zusammensetzen der Kette durch Schweißen geschlossen worden sind.After hot rolling and a long-term heat treatment, which was done to set a favorable for the subsequent cold working strength, the rolled steel has been formed into chain links, which have been closed after assembly of the chain by welding.
Die auf diese Weise erzeugten Ketten wiesen eine feine Kornstruktur von ASTM 11, eine Festigkeit von 1270 N/mm2 und eine bei dieser Festigkeit ermittelte Sprödbruchübergangstemperatur FATT von -70 °C auf. Ihr Kerbschlagarbeitswert lag bei 557 J bei -60 °C Prüftemperatur und die Bruchdehnung betrug 28 %.The chains produced in this way had a fine grain structure of ASTM 11, a strength of 1270 N / mm 2 and a brittle fracture transition temperature FATT of -70 ° C determined at this strength. Its impact value was 557 J at -60 ° C test temperature and the elongation at break was 28%.
Im beigefügten Diagramm ist für erfindungsgemäßen Stahl der Verlauf des Zähbruchwertes J-Integral über die Risserweiterung REW bei einer Temperatur von - 60 °C für eine normalisierte Anfangsrisslänge a/w von 0,4 aufgetragen. Es zeigt sich, dass bei dem technisch relevanten Beginn der stabilen Risserweiterung eine Rissinitiierungszähigkeit JIC.von 185 N/mm2 vorliegt.In the attached diagram, the course of the tensile fracture value J-integral over the crack extension REW at a temperature of -60 ° C. for a normalized initial crack length a / w of 0.4 is plotted for steel according to the invention. It turns out that at the technically relevant beginning of the stable crack extension, a crack initiation toughness J IC of 185 N / mm 2 is present.
Claims (23)
- Steel for the production of high-strength components with excellent low-temperature toughness, having the following composition (in % by weight):
C: 0.08 to 0.25 %, Si: 0.10 to 0.30 %, Mn: 0.80 to 1.60 %, P: ≤ 0.020 %, S: ≤ 0.015 %, Cr: 0.40 to 0.80 %, Mo: 0.30 to 0.50 %, Ni: 0.70 to 1.20 %, Al: 0.020 to 0.060 %, N: 0.007 to 0.018 %, V: ≤ 0.15 %, Nb: ≤ 0.07 %, - Steel according to Claim 1, characterised in that its C content is from 0.16 % by weight to 0.23 % by weight.
- Steel according to any one of the preceding claims, characterised in that its Mn content is from 1.00 % by weight to 1.35 % by weight.
- Steel according to any one of the preceding claims, characterised in that its Cr content is from 0.40 % by weight to 0.65 % by weight.
- Steel according to any one of the preceding claims, characterised in that its Mo content is from 0.35 % by weight to 0.50 % by weight.
- Steel according to any one of the preceding claims, characterised in that its Ni content is from 0.75 % by weight to 1.00 % by weight.
- Steel according to any one of the preceding claims, characterised in that its Al content is from 0.020 % by weight to 0.045 % by weight.
- Steel according to any one of the preceding claims, characterised in that its N content is from 0.007 % by weight to 0.015 % by weight.
- Steel according to any one of the preceding claims, characterised in that it has an austenite grain size that is finer than ASTM 10.
- Use of a steel composed according to any one of the preceding claims for the production of high-strength components by cold forming with subsequent temper-hardening.
- Use according to Claim 10, characterised in that the components are means for the carrying, pulling, lifting, conveying or securing of loads.
- Use according to Claim 10, characterised in that the components are means for the connection of structural elements.
- Use according to any one of Claims 10 to 12, characterised in that the components are chains.
- Use according to Claim 13, characterised in that the chains are round steel chains.
- Use according to either Claim 13 or Claim 14, characterised in that the chains are welded.
- Use according to any one of Claims 10 to 15, characterised in that the components have a strength of at least 1,200 MPa.
- Use according to Claim 16, characterised in that the strength is at least 1,550 MPa.
- Use according to either Claim 16 or Claim 17, characterised in that the strength is at least 1,600 MPa, in particular at least 1,650 MPa.
- Use according to any one of Claims 10 to 18, characterised in that at a strength of at least 1,550 MPa, the fracture appearance transition temperature FATT of the components is at most -60 °C.
- Use according to any one of Claims 10 to 19, characterised in that the notch impact working value is more than 45 J.
- Use according to any one of Claims 10 to 20, characterised in that the material of the component has a technical crack initiation toughness JIC of more than 170 N/mm2.
- Use according to Claim 21, characterised in that the technical crack initiation toughness JIC is more than 185 N/mm2.
- Use according to any one of Claims 10 to 22, characterised in that the components exhibit an elongation at break of more than 28 %.
Priority Applications (12)
Application Number | Priority Date | Filing Date | Title |
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AT04002612T ATE359382T1 (en) | 2004-02-05 | 2004-02-05 | STEEL FOR PRODUCING HIGH-STRENGTH COMPONENTS WITH OUTSTANDING LOW-TEMPERATURE TOUGHNESS AND USES OF SUCH A STEEL |
DK04002612T DK1561833T3 (en) | 2004-02-05 | 2004-02-05 | Steel for the production of high strength components with excellent low temperature toughness and applications of such steel |
ES04002612T ES2286518T3 (en) | 2004-02-05 | 2004-02-05 | STEEL FOR THE MANUFACTURE OF HIGHLY RESISTANT COMPONENTS WITH OVERHEAT STAY AT LOW TEMPERATURES AND USES OF A STEEL OF THIS TYPE. |
EP04002612A EP1561833B1 (en) | 2004-02-05 | 2004-02-05 | Steel for manufacturing of high strength elements with an excellent low temperature toughness and use thereof |
DE200420021326 DE202004021326U1 (en) | 2004-02-05 | 2004-02-05 | High strength steel alloy for fabrication of high-tensile components e.g. chain or hawser cable |
DE502004003457T DE502004003457D1 (en) | 2004-02-05 | 2004-02-05 | Steel for the manufacture of high strength components with outstanding low temperature toughness and uses of such a steel |
PCT/EP2005/001163 WO2005075693A1 (en) | 2004-02-05 | 2005-02-04 | Steel for producing high tensile structural components with excellent toughness at low temperatures and uses of such a steel |
US10/551,506 US20070107808A1 (en) | 2004-02-05 | 2005-02-04 | Steel for production of high-strength components with excellent low-temperature toughness and uses of a steel of this type |
BRPI0503588-0B1A BRPI0503588B1 (en) | 2004-02-05 | 2005-02-04 | steel for production of high strength components with excellent low temperature toughness and steel components |
JP2006551811A JP2007520633A (en) | 2004-02-05 | 2005-02-04 | Use of steel and the above types of steel to produce high strength parts with excellent low temperature toughness |
CN200580000079.7A CN1764734B (en) | 2004-02-05 | 2005-02-04 | Steel for producing high tensile structural components with excellent toughness at low temperatures and uses of such a steel |
ZA200507292A ZA200507292B (en) | 2004-02-05 | 2005-09-09 | Steel for producing high tensile structural components with excellent toughness at low temperatures and uses of such a steel |
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EP04002612A EP1561833B1 (en) | 2004-02-05 | 2004-02-05 | Steel for manufacturing of high strength elements with an excellent low temperature toughness and use thereof |
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EP1561833A1 EP1561833A1 (en) | 2005-08-10 |
EP1561833B1 true EP1561833B1 (en) | 2007-04-11 |
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US (1) | US20070107808A1 (en) |
EP (1) | EP1561833B1 (en) |
JP (1) | JP2007520633A (en) |
CN (1) | CN1764734B (en) |
AT (1) | ATE359382T1 (en) |
BR (1) | BRPI0503588B1 (en) |
DE (1) | DE502004003457D1 (en) |
DK (1) | DK1561833T3 (en) |
ES (1) | ES2286518T3 (en) |
WO (1) | WO2005075693A1 (en) |
ZA (1) | ZA200507292B (en) |
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DE102005034140A1 (en) * | 2005-07-19 | 2007-01-25 | Rud-Kettenfabrik Rieger & Dietz Gmbh U. Co. | High strength steel chain for the low temperature range |
CN101407893B (en) * | 2008-11-25 | 2011-04-06 | 武汉钢铁(集团)公司 | High strength, high heat input welding property, fire resistant and earthquake resistant steel for construction and production method thereof |
DE102011054840A1 (en) * | 2011-10-26 | 2013-05-02 | Rud Ketten Rieger & Dietz Gmbh U. Co. Kg | Hardening steel for grade 8 and higher hoisting, lifting, tensioning and / or lashing equipment, lifting, lifting, tensioning and / or lashing equipment, and method of making such a component |
CN103451529B (en) * | 2013-08-23 | 2015-09-16 | 苏州长盛机电有限公司 | A kind of Aluminum-titanium-iralloy alloy material |
CN104532143B (en) * | 2014-12-22 | 2016-11-16 | 江阴兴澄特种钢铁有限公司 | A kind of mining big specification, high-test chain steel and preparation method thereof |
US20200165711A1 (en) * | 2016-02-19 | 2020-05-28 | Nippon Steel & Sumitomo Metal Corporation | Steel |
EP3418411B1 (en) * | 2016-02-19 | 2020-11-04 | Nippon Steel Corporation | Steel useful as a material for chains |
US10947610B2 (en) | 2018-08-21 | 2021-03-16 | Exxonmobil Upstream Research Company | Mooring chains comprising high manganese steels and associated methods |
CN109058278A (en) * | 2018-09-26 | 2018-12-21 | 安徽博耐克摩擦材料有限公司 | A kind of braking automobile line |
CN109026974A (en) * | 2018-09-26 | 2018-12-18 | 安徽博耐克摩擦材料有限公司 | A kind of automobile brake cable |
CN109266975B (en) * | 2018-10-25 | 2021-08-31 | 青岛天赢智能工业股份有限公司 | High-strength high-low-temperature impact toughness alloy and preparation and heat treatment process thereof |
KR102065276B1 (en) * | 2018-10-26 | 2020-02-17 | 주식회사 포스코 | Steel Plate For Pressure Vessel With Excellent Toughness and Elongation Resistance And Manufacturing Method Thereof |
CN110484818B (en) * | 2019-09-03 | 2020-08-14 | 山东钢铁股份有限公司 | Steel for rubber core support of oil blowout preventer and production method thereof |
CN116623103A (en) * | 2023-05-16 | 2023-08-22 | 南京钢铁股份有限公司 | Breaking force 120 kN-level high-strength chain and preparation method thereof |
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US3432368A (en) * | 1965-02-25 | 1969-03-11 | Ishikawajima Harima Heavy Ind | Method for manufacturing nitride-containing low-carbon structural steels |
US4138278A (en) * | 1976-08-27 | 1979-02-06 | Nippon Steel Corporation | Method for producing a steel sheet having remarkably excellent toughness at low temperatures |
US4605449A (en) * | 1981-05-19 | 1986-08-12 | Arbed S.A. | Process for producing a rolled steel product having high weldability, a high yield strength and a good notch impact toughness at very low temperatures |
JPH04141546A (en) * | 1990-09-28 | 1992-05-15 | Aichi Steel Works Ltd | Non-heat treated steel for hot forging |
US5282906A (en) * | 1992-01-16 | 1994-02-01 | Inland Steel Company | Steel bar and method for producing same |
US5352304A (en) * | 1992-11-16 | 1994-10-04 | Allegheny Ludlum Corporation | High strength low alloy steel |
AU663023B2 (en) * | 1993-02-26 | 1995-09-21 | Nippon Steel Corporation | Process for manufacturing high-strength bainitic steel rails with excellent rolling-contact fatigue resistance |
JPH10168542A (en) * | 1996-12-12 | 1998-06-23 | Nippon Steel Corp | High strength steel excellent in low temperature toughness and fatigue strength and its production |
JP4132545B2 (en) * | 2000-02-23 | 2008-08-13 | 新日本製鐵株式会社 | Steel bars for high strength and toughness seismic isolation dampers with excellent low cycle fatigue characteristics |
CN1108397C (en) * | 2000-06-02 | 2003-05-14 | 江阴兴澄钢铁有限公司 | High-strength, high-toughness and corrosion resistant mooring chain steel and its production process |
GB2392919B (en) * | 2002-09-12 | 2005-01-19 | Corus Uk Ltd | Corrosion resistant steels |
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- 2004-02-05 ES ES04002612T patent/ES2286518T3/en not_active Expired - Lifetime
- 2004-02-05 EP EP04002612A patent/EP1561833B1/en not_active Expired - Lifetime
- 2004-02-05 DE DE502004003457T patent/DE502004003457D1/en not_active Expired - Lifetime
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- 2005-02-04 CN CN200580000079.7A patent/CN1764734B/en active Active
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- 2005-02-04 JP JP2006551811A patent/JP2007520633A/en active Pending
- 2005-02-04 WO PCT/EP2005/001163 patent/WO2005075693A1/en active Application Filing
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US20070107808A1 (en) | 2007-05-17 |
DE502004003457D1 (en) | 2007-05-24 |
WO2005075693A1 (en) | 2005-08-18 |
ES2286518T3 (en) | 2007-12-01 |
ZA200507292B (en) | 2007-04-25 |
JP2007520633A (en) | 2007-07-26 |
ATE359382T1 (en) | 2007-05-15 |
CN1764734B (en) | 2010-12-08 |
DK1561833T3 (en) | 2007-08-20 |
BRPI0503588B1 (en) | 2013-09-10 |
EP1561833A1 (en) | 2005-08-10 |
BRPI0503588A (en) | 2006-03-07 |
CN1764734A (en) | 2006-04-26 |
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