EP1867748A1 - Acier inoxydable duplex - Google Patents

Acier inoxydable duplex Download PDF

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Publication number
EP1867748A1
EP1867748A1 EP06290991A EP06290991A EP1867748A1 EP 1867748 A1 EP1867748 A1 EP 1867748A1 EP 06290991 A EP06290991 A EP 06290991A EP 06290991 A EP06290991 A EP 06290991A EP 1867748 A1 EP1867748 A1 EP 1867748A1
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EP
European Patent Office
Prior art keywords
steel
bar
hot
rolled
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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EP06290991A
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German (de)
English (en)
French (fr)
Inventor
Bernard Bonnefois
Jérôme Peultier
Mickael Serriere
Jean-Michel Hauser
Eric Chauveau
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ugitech SA
Industeel Creusot
Original Assignee
Ugitech SA
Industeel Creusot
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ugitech SA, Industeel Creusot filed Critical Ugitech SA
Priority to EP06290991A priority Critical patent/EP1867748A1/fr
Priority to AU2007259069A priority patent/AU2007259069B2/en
Priority to CA2656946A priority patent/CA2656946C/fr
Priority to TW096121708A priority patent/TWI463020B/zh
Priority to MX2008016172A priority patent/MX2008016172A/es
Priority to KR1020087030667A priority patent/KR101169627B1/ko
Priority to ES07803755T priority patent/ES2401601T3/es
Priority to CN2007800297393A priority patent/CN101501234B/zh
Priority to PL07803755T priority patent/PL2038445T3/pl
Priority to BRPI0713673-0B1A priority patent/BRPI0713673B1/pt
Priority to RU2009101139/02A priority patent/RU2406780C2/ru
Priority to DK07803755.3T priority patent/DK2038445T3/da
Priority to EP07803755A priority patent/EP2038445B1/fr
Priority to SI200731163T priority patent/SI2038445T1/sl
Priority to PCT/FR2007/000994 priority patent/WO2007144516A2/fr
Priority to US12/305,014 priority patent/US20100000636A1/en
Publication of EP1867748A1 publication Critical patent/EP1867748A1/fr
Priority to ZA200810587A priority patent/ZA200810587B/xx
Priority to US14/622,402 priority patent/US20150167135A1/en
Priority to US16/371,563 priority patent/US20190226068A1/en
Withdrawn legal-status Critical Current

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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
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    • B21B1/26—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by hot-rolling, e.g. Steckel hot mill
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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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Definitions

  • the present invention relates to a duplex stainless steel, more particularly intended for the manufacture of structural elements for production plants (chemical, petrochemical, paper, offshore) or energy production, without being there limited, and the method of manufacturing a sheet, strip, bars, son, or profiles of this steel.
  • This steel can more generally be used in substitution of a type 304L stainless steel in many applications, for example, in previous industries or in the food industry, including parts made from formed son (welded grids ..) profiles (strainers ..), axes ... One could also make molded parts and forged parts.
  • stainless steel grades 304 and 304L are known, the microstructure of which in the annealed state is essentially austenitic; when cold-worked, they may also contain a variable proportion of martensite. These steels, however, have high additions of nickel, the cost is generally prohibitive. In addition, these grades may pose a problem from a technical point of view for certain applications because they have low tensile characteristics in the annealed state, especially with regard to the yield strength, and a low resistance to stress corrosion.
  • austenitic-ferritic stainless steels which are composed mainly of a mixture of ferrite and austenite, such as 1.4362, 1.4655, 1.4477, 1.4462, 1.4507, 1.4410, 1.4501 and 1.4424 steels of the standard.
  • EP10088 all of which contain more than 3.5% nickel. These steels are particularly resistant to corrosion and stress corrosion.
  • ferritic or ferrito-martensitic stainless steel grades the microstructure of which, for a defined range of heat treatments, is composed of two constituents, ferrite and martensite, preferably in a ratio of 50/50, such as grade 1.4017 of EN10088.
  • These grades with a chromium content generally less than 20%, have high mechanical tensile properties, but do not exhibit satisfactory corrosion resistance.
  • the object of the present invention is to overcome the disadvantages of the steels and manufacturing processes of the prior art by providing a stainless steel having good mechanical characteristics and in particular a tensile yield strength greater than 400 or 450MPa to the annealed or dissolved state, a high resistance to corrosion and in particular greater than or equal to that of 304L, good microstructural stability and good resilience of the welded zones, without the addition of expensive additive elements, as well as a process for producing sheets, strips, bars, wires, or profiles made of this steel that is simplified to use.
  • said ingot or hot slab is rolled at a temperature of between 1150 and 1280 ° C. to obtain a so-called quarto sheet, and then a heat treatment is carried out at a temperature of between 900 and 1100 ° C. and said sheet is cooled by quenching in air.
  • the invention also covers a method of manufacturing a steel section, according to which a cold forming of a hot-rolled bar obtained according to the invention is carried out, as well as a method of manufacturing a forged part made of steel. steel, according to which a hot-rolled bar obtained according to the invention is fed in pieces, and then forging said billet between 1100 ° C. and 1280 ° C.
  • the duplex stainless steel according to the invention comprises the contents defined below.
  • the carbon content of the grade is less than or equal to 0.05% and preferably less than 0.03% by weight.
  • the chromium content of the grade is between 21 and 25% by weight, preferably between 22 and 24% by weight in order to obtain a good resistance to corrosion, which is at least equivalent to that obtained with the shades of the type 304 or 304L.
  • the nickel content of the grade is between 1 and 2.95% by weight.
  • This austenite forming element is voluntarily maintained at a low level because of its cost. It is added in order to obtain good properties of resistance to the formation of corrosion cavities and to obtain a good compromise resilience / ductility. It has indeed the advantage of translating the transition curve of the resilience to low temperatures, which is particularly advantageous for the manufacture of thick quarto plates for which the properties of resilience are important.
  • the nickel content is limited, in the steel according to the invention, it has been found that, in order to obtain a suitable austenite content after heat treatment between 900 ° C. and 1100 ° C., other elements must be added. austenite formers in unusually high amounts and to limit the contents of ferrite-forming elements.
  • the nitrogen content of the grade is between 0.16 and 0.28%, which generally implies that nitrogen is added to the steel during processing.
  • This austenite forming element first makes it possible to obtain a two-phase ferrite + austenite duplex steel containing a proportion of austenite suitable for good resistance to stress corrosion, and also to obtain high mechanical characteristics for the metal. It still allows to have a good microstructural stability in the heat-affected zone of the welded zones. Its maximum content is limited because, beyond 0.28%, solubility problems can be observed: formation of blowholes during the solidification of slabs, blooms, ingots, moldings or welds.
  • the manganese content also austenite-forming element below 1150 ° C, is maintained below 2.0% by weight, and preferably below 1.5% by weight, because of the adverse effects of this element on many points.
  • the ferro-manganese additions normally used to make up the grade also contain significant levels of phosphorus, and also selenium, which are not desired to be introduced into the steel and which are difficult to remove when refining the shade. Manganese disrupts this refining by limiting the possibility of decarburization.
  • Molybdenum a ferrite-forming element
  • Molybdenum a ferrite-forming element
  • the contents of these two elements are such that the sum Mo + W / 2 is less than 0.50% by weight, preferably less than 0.4% by weight and particularly preferably less than 0.3%. in weight.
  • the present inventors have found that by keeping these two elements, as well as their sums, below the values indicated, there was no observing intermetallic precipitation embrittlement, which allows in particular to de-constrain the manufacturing process steel sheets or strips in allowing air cooling of the sheets and strips after heat treatment or hot work. In addition, they observed that by controlling these elements within the limits claimed, the weldability of the grade was improved.
  • Copper an austenite forming element
  • This element improves the resistance to corrosion in a reducing acid medium.
  • its content is limited to 0.50% by weight to avoid the formation of epsilon phases that it is desired to avoid, because they cause hardening of the ferritic phase and embrittlement of the duplex alloy.
  • the oxygen content is preferably limited to 0.010% by weight in order to improve its forging ability.
  • Boron is an optional element that can be added to the grade according to the invention to the extent of 0.003% by weight, in order to improve its transformation when hot. In another embodiment, however, it is preferred to limit the boron content to less than 0.0005% by weight to limit the risks of cracking on welding and continuous casting.
  • Silicon a ferrite-forming element
  • Silicon is present in a content of less than 1.4% by weight.
  • Aluminum, a ferrite-forming element is present at a content of less than 0.05% by weight and preferably of between 0.005% and 0.040% by weight in order to obtain inclusions of calcium aluminates with a low melting point .
  • the maximum aluminum content is also limited in order to avoid excessive formation of aluminum nitrides. The action of these two elements silicon and aluminum is essentially to ensure good deoxidation of the steel bath during the preparation.
  • Cobalt an austenite forming element
  • Cobalt is maintained at a content of less than 0.5% by weight, and preferably less than 0.3% by weight. This element is a residual brought by the raw materials. It is limited particularly because of the handling problems it can pose after irradiation of parts in nuclear facilities.
  • the rare earths may be added to the composition in an amount of 0.1% by weight and preferably less than 0.06% by weight. These include cerium and lanthanum. We limit the contents in these elements as they are likely to form unwanted intermetallics.
  • Vanadium a ferrite-forming element
  • Vanadium may be added in the grade of up to 0.5% by weight and preferably less than 0.2% by weight in order to improve the cavernous corrosion resistance of the steel.
  • Niobium a ferrite-forming element
  • Niobium may be added in the grade of 0.3% by weight and preferably less than 0.050% by weight. It improves the tensile strength of the grade, thanks to the formation of fine niobium nitrides. Its content is limited to limit the formation of coarse niobium nitrides.
  • Titanium a ferrite-forming element
  • Titanium may be added in the grade of 0.1% by weight and preferably less than 0.02% by weight to limit the formation of titanium nitrides formed in the liquid steel in particular.
  • Calcium may also be added to the grade according to the invention to obtain a calcium content of less than 0.03% by weight, and preferably greater than 0.0005% by weight, in order to control the nature of the inclusions of calcium. oxides and improve machinability.
  • the content of this element is limited because it is likely to form with sulfur calcium sulphides which degrade the properties of corrosion resistance.
  • the sulfur is maintained at a content of less than 0.010% by weight and preferably less than 0.003% by weight.
  • this element forms sulphides with manganese or calcium, sulphides whose presence is detrimental to the resistance to corrosion. It is considered an impurity.
  • Magnesium addition up to a final content of 0.1% can be made to modify the nature of the sulfides and oxides.
  • the selenium is preferably maintained at less than 0.005% by weight because of its detrimental effect on the corrosion resistance.
  • This element is generally added to the grade as impurities in ferro-manganese ingots.
  • Phosphorus is maintained at less than 0.040% by weight and is considered an impurity.
  • the rest of the composition consists of iron and impurities.
  • zirconium, tin, arsenic, lead or bismuth may be present in a content of less than 0.100% by weight and preferably less than 0.030% by weight to avoid welding problems.
  • the arsenic may be present in a content of less than 0.030% by weight and preferably less than 0.020% by weight.
  • the lead may be present in a content of less than 0.002% by weight and preferably less than 0.0010% by weight.
  • the bismuth may be present in a content of less than 0.0002% by weight and preferably less than 0.00005% by weight.
  • Zirconium may be present at 0.02%.
  • the microstructure of the steel according to the invention in the annealed state, is composed of austenite and ferrite, which are preferably, after treatment of 1 hour at 1000 ° C., in a proportion of 35 to 65% by weight. ferrite volume and more preferably from 35 to 55% by volume of ferrite.
  • the IF number must be between 40 and 70.
  • the microstructure does not contain other phases which would be harmful for its mechanical properties in particular, such as the sigma phase and other intermetallic phases.
  • the cold worked state a part of the austenite may have been converted to martensite, depending on the effective deformation temperature and the amount of cold deformation applied.
  • the steel according to the invention can be prepared and manufactured in the form of hot-rolled sheets, also called quarto plates, but also in the form of hot-rolled strips, from slabs or ingots and also under Cold rolled strip form from hot rolled strip. It can also be hot rolled into bars or wire-machines or into profiles or forged; these products can then be hot-formed by forging or cold-formed into drawn bars or profiles or into drawn wires.
  • the steel according to the invention can also be used by molding followed or not by heat treatment.
  • This ingot, this slab or this bloom are generally obtained by melting the raw materials in an electric furnace, followed by a vacuum reflow of the AOD or VOD type with decarburization.
  • the grade can then be cast in the form of ingots, or in the form of slabs or blooms by continuous casting in a bottomless mold. It could also be envisaged to cast the shade directly in the form of thin slabs, in particular by continuous casting between counter-rotating rolls.
  • the ingot or slab or bloom After supplying the ingot or slab or bloom, it is optionally heated to reach a temperature between 1150 and 1280 ° C, but it is also possible to work directly on the slab that has just been continuously cast, in the hot casting.
  • the slab or the slab is then hot-rolled to obtain a so-called quarto sheet which generally has a thickness of between 5 and 100 mm.
  • the reduction rates generally used at this stage vary between 3 and 30%.
  • This sheet is then subjected to a heat treatment of resuspension of precipitates formed at this stage by reheating at a temperature between 900 and 1100 ° C, and then cooled.
  • the method according to the invention provides an air quenching cooling which is easier to implement than the cooling conventionally used for this type of shade, which is a faster cooling, using water. However, it remains possible to cool with water if desired.
  • the quarto plate can be glued, cut and stripped, if it is desired to deliver it in this state.
  • This bare steel can also be rolled on a band train at thicknesses between 3 and 10 mm.
  • wire of diameter less than or equal to 13 mm When wire of diameter less than or equal to 13 mm has been manufactured, it can be cooled by quenching with water in turns spread on a conveyor after passing them on the conveyor in 2 to 5 minutes through a furnace. solution at a temperature between 850 ° C and 1100 ° C.
  • Subsequent heat treatment in the oven can be performed optionally on these bars or rings already treated in the hot rolling, if it is desired to complete the recrystallization of the structure and slightly lower the mechanical characteristics in traction.
  • An industrial casting according to the invention of 150 tons referenced 8768 was performed. This grade was developed by melting in the electric oven, then refined under vacuum with decarburization to reach the target carbon level. It was then continuously cast into slabs of section 220 x 1700 mm, then hot rolled after heating to 1200 ° C in so-called quarto plates of thickness 7, 12 and 20mm. The sheets thus obtained are then subjected to a heat treatment at about 1000 ° C. in order to put in solution the different precipitates present at this stage. At the end of the heat treatment, the sheets are cooled with water and then planed, cut and stripped.
  • compositions in percentages by weight of the various grades developed in the laboratory or in an industrial way are collated in Table 1, as well as those of various industrial products or semi-finished products elaborated in electric furnace, refining with the AOD, casting in ingot or in continuous, mentioned for comparison.
  • the casting according to the invention No. 14441, has, below 1300 ° C., a ferrite content suitable for the hot conversion into a duplex structure.
  • a ferrite content suitable for resistance to stress corrosion after treatment in the range of 950 ° C to 1100 ° C, it has a ferrite content suitable for resistance to stress corrosion.
  • the ferrite content was also measured by the grid method (according to ASTM E 562) on forged bars after heat treatment at 1030 ° C and on thermally affected areas of electrode deposited weld seams with constant energy. leading to cooling rates of 20 ° C / sec at 700 ° C.
  • the results (ferrite contents of base metal and heat-affected zone) are given in Table 3. It can be seen that the flows 14441 and 14604 according to the invention have a ferrite content in the base metal and in the affected zone. thermally favoring resistance to localized and stressed corrosion, as well as resilience (see Table 5).
  • the 14439 ingot has blistered and is unusable. To avoid this phenomenon during airflows at atmospheric pressure, it is therefore necessary to limit the nitrogen content of the castings according to the invention to less than 0.28% by weight.
  • the hot deformation capacity was evaluated using hot tensile tests carried out on specimens whose calibrated portion, 8 mm in diameter and 5 mm in length, is heated by Joule effect for 80 seconds at 1280. ° C, then cooled to 2 ° C per second until the test temperature varies between 900 and 1280 ° C. When this temperature is reached, the rapid pull is immediately triggered at a speed of 73 mm / s; after breaking, the necking diameter is measured at the fracture.
  • the resilience values determined at 20 ° C. for laboratory flows 14441 and 14604 and industrial casting 8768, all three according to the invention, are all greater than 200 J, which is satisfactory. given the level of the elastic limit of these grades.
  • the resilience values at 20 ° C are less than 100 J. This confirms the need for a sufficient nitrogen addition for to obtain a satisfactory level of tenacity.
  • Corrosion resistance tests were carried out both on the bars forged from laboratory laps and on coupons taken from hot-rolled sheets from industrial castings.
  • the critical pitting temperature in medium ferric chloride (FeCl 3 6%) was also determined according to ASTM G48-00 method C.
  • the pitting resistance was determined in deaerated neutral medium at 0.86 Moles / liter NaCl, corresponding to 5% by weight NaCl, at 35 ° C.
  • a measurement of the abandonment potential for 900 seconds is carried out.
  • a potentiodynamic curve is plotted at a speed of 100 mV / min from the abandonment to the pitting potential.
  • IRCL index of resistance to localized corrosion
  • SWIR Cr + 3 , 3 ⁇ MB + 16 ⁇ NOT + 2 , 6 ⁇ Or - 0 , 7 ⁇ mn (Cr, Mo, N, Ni and Mn contents in% by weight) gives a good account of the classification of the set of compositions containing less than 6% nickel in localized corrosion resistance (see FIGS. 3, 4 and 5).
  • Castings 14383 and 14660 outside the invention IRCL indices equal to 28.7 and 29.8, behave less well in corrosion than a steel type AISI 304L.
  • the steels according to the invention should preferably have an IRCL greater than 30.5 and preferably greater than 32.
  • Uniform corrosion was characterized by evaluating the loss of mass corrosion rate after immersion for 72 hours in a 2% sulfuric acid solution heated to 40 ° C.
  • E 3 pitting potential in neutral and chlorinated medium (NaCl 5%) at 35 ° C.
  • CPT critical temperature of puncture in ferric chloride medium
  • V uniform corrosion rate in sulfuric acid medium 2% at 40 ° C

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EP06290991A 2006-06-16 2006-06-16 Acier inoxydable duplex Withdrawn EP1867748A1 (fr)

Priority Applications (19)

Application Number Priority Date Filing Date Title
EP06290991A EP1867748A1 (fr) 2006-06-16 2006-06-16 Acier inoxydable duplex
BRPI0713673-0B1A BRPI0713673B1 (pt) 2006-06-16 2007-06-15 "aço inoxidável dúplex, processo para a fabricação de uma chapa, de uma tira, ou de uma bobina laminada a quente em aço ou de uma barra ou de um fio laminado(a) a quente em aço e peça moldada".
RU2009101139/02A RU2406780C2 (ru) 2006-06-16 2007-06-15 Нержавеющая сталь, полученная дуплекс-процессом
TW096121708A TWI463020B (zh) 2006-06-16 2007-06-15 雙重不銹鋼
MX2008016172A MX2008016172A (es) 2006-06-16 2007-06-15 Acero inoxidable duplex.
KR1020087030667A KR101169627B1 (ko) 2006-06-16 2007-06-15 듀플렉스 스테인리스강
ES07803755T ES2401601T3 (es) 2006-06-16 2007-06-15 Acero inoxidable dúplex
CN2007800297393A CN101501234B (zh) 2006-06-16 2007-06-15 双联不锈钢
PL07803755T PL2038445T3 (pl) 2006-06-16 2007-06-15 Stal nierdzewna dupleks
AU2007259069A AU2007259069B2 (en) 2006-06-16 2007-06-15 Duplex stainless steel
CA2656946A CA2656946C (fr) 2006-06-16 2007-06-15 Acier inoxydable duplex
DK07803755.3T DK2038445T3 (da) 2006-06-16 2007-06-15 Rustfrit duplex stål
EP07803755A EP2038445B1 (fr) 2006-06-16 2007-06-15 Acier inoxydable duplex
SI200731163T SI2038445T1 (sl) 2006-06-16 2007-06-15 Dupleks nerjavno jeklo
PCT/FR2007/000994 WO2007144516A2 (fr) 2006-06-16 2007-06-15 Acier inoxydable duplex
US12/305,014 US20100000636A1 (en) 2006-06-16 2007-06-15 Duplex stainless steel
ZA200810587A ZA200810587B (en) 2006-06-16 2008-12-15 Duplex stainless steel
US14/622,402 US20150167135A1 (en) 2006-06-16 2015-02-13 Duplex stainless steel
US16/371,563 US20190226068A1 (en) 2006-06-16 2019-04-01 Process for manufacturing hot-rolled plate, strip or coil made of duplex stainless steel

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AU (1) AU2007259069B2 (zh)
BR (1) BRPI0713673B1 (zh)
CA (1) CA2656946C (zh)
DK (1) DK2038445T3 (zh)
ES (1) ES2401601T3 (zh)
MX (1) MX2008016172A (zh)
PL (1) PL2038445T3 (zh)
RU (1) RU2406780C2 (zh)
SI (1) SI2038445T1 (zh)
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EP2199421A4 (en) * 2007-10-10 2016-07-20 Nippon Steel & Sumikin Sst MATERIAL FOR DUPLEX STAINLESS STEEL WIRE, STEEL WIRE, BOLT AND METHOD FOR PRODUCING THE BOLT
US11286546B2 (en) 2010-04-29 2022-03-29 Outokumpu Oyj Method for manufacturing and utilizing ferritic-austenitic stainless steel with high formability
WO2011135170A1 (en) 2010-04-29 2011-11-03 Outokumpu Oyj Method for manufacturing and utilizing ferritic-austenitic stainless steel with high formability
US9862168B2 (en) 2011-01-27 2018-01-09 Nippon Steel & Sumikin Stainless Steel Corporation Alloying element-saving hot rolled duplex stainless steel material, clad steel plate having duplex stainless steel as cladding material therefor, and production method for same
WO2012143610A1 (en) 2011-04-18 2012-10-26 Outokumpu Oyj Method for manufacturing and utilizing ferritic-austenitic stainless steel
EP2770076A4 (en) * 2011-10-21 2016-03-09 Nippon Steel & Sumikin Sst DUPLEX STAINLESS STEEL, DUPLEX STAINLESS STEEL BRACKET AND DUPLEX STAINLESS STEEL MATERIAL
DE102012100908A1 (de) 2012-02-03 2013-08-08 Klaus Kuhn Edelstahlgiesserei Gmbh Duplexstahl mit verbesserter Kerbschlagzähigkeit und Zerspanbarkeit
WO2013113718A1 (de) 2012-02-03 2013-08-08 Klaus Kuhn Edelstahlgiesserei Gmbh Duplexstahl mit verbesserter kerbschlagzähigkeit und zerspanbarkeit
CN102649222B (zh) * 2012-05-31 2014-01-29 浙江振兴石化机械有限公司 一种利用17-4ph不锈钢加工细长轴的方法
CN102649222A (zh) * 2012-05-31 2012-08-29 浙江振兴石化机械有限公司 一种利用17-4ph不锈钢加工细长轴的方法
CN110234778A (zh) * 2017-01-23 2019-09-13 杰富意钢铁株式会社 铁素体-奥氏体系双相不锈钢板
EP3556879A4 (en) * 2017-01-23 2020-01-15 JFE Steel Corporation FERRITIC / AUSTENITIC DUPLEX STAINLESS STEEL PLATE
US11142814B2 (en) 2017-01-23 2021-10-12 Jfe Steel Corporation Ferritic-austenitic duplex stainless steel sheet
CN110234778B (zh) * 2017-01-23 2022-05-17 杰富意钢铁株式会社 铁素体-奥氏体系双相不锈钢板

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RU2009101139A (ru) 2010-07-27
WO2007144516A2 (fr) 2007-12-21
ES2401601T3 (es) 2013-04-23
EP2038445A2 (fr) 2009-03-25
BRPI0713673A2 (pt) 2012-10-23
CA2656946A1 (fr) 2007-12-21
US20150167135A1 (en) 2015-06-18
KR20090031864A (ko) 2009-03-30
TW200815613A (en) 2008-04-01
KR101169627B1 (ko) 2012-07-30
RU2406780C2 (ru) 2010-12-20
DK2038445T3 (da) 2013-04-08
ZA200810587B (en) 2009-11-25
EP2038445B1 (fr) 2012-12-26
SI2038445T1 (sl) 2013-06-28
PL2038445T3 (pl) 2013-09-30
AU2007259069B2 (en) 2011-04-28
CN101501234B (zh) 2012-01-04
US20100000636A1 (en) 2010-01-07
BRPI0713673B1 (pt) 2014-11-25
AU2007259069A1 (en) 2007-12-21
US20190226068A1 (en) 2019-07-25
CA2656946C (fr) 2012-01-24
WO2007144516A3 (fr) 2008-04-10

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