CN102859019A - Cr-containing steel pipe for line pipe and having excellent intergranular stress corrosion cracking resistance at welding-heat-affected portion - Google Patents
Cr-containing steel pipe for line pipe and having excellent intergranular stress corrosion cracking resistance at welding-heat-affected portion Download PDFInfo
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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
- C22C38/40—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
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
- C21D1/25—Hardening, combined with annealing between 300 degrees Celsius and 600 degrees Celsius, i.e. heat refining ("Vergüten")
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
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- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/50—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for welded joints
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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
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- 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
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- 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
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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
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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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
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/005—Ferrite
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/008—Martensite
Abstract
Disclosed is a Cr-containing steel pipe that is for a line pipe, has high X65- to X80-grade strength, excellent toughness, corrosion resistance, and sulfide stress corrosion cracking resistance, and has excellent intergranular stress corrosion cracking resistance at a welding-heat-affected portion. Specifically, a composition is used containing, by mass%, 0.001-0.015% C, 0.05-0.50% Si, 0.10-2.0% Mn, 0.001-0.10% Al, 15.0-18.0% Cr, 2.0-6.0% Ni, 1.5-3.5% Mo, 0.001-0.20% V, and no more than 0.015% N in a manner so as to satisfy Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N being 11.5-13.3. As a result, the welding-heat-affected portion that, during welding, has been heated to the ferrite single-phase temperature region that is at least 1300 DEG C and then cooled becomes a configuration of which at least 50% of the former ferrite grain boundaries are occupied by a martensite phase and/or an austenite phase, and a steel pipe is formed of which the formation of a layer deficient in Cr carbide is suppressed, and the intergranular stress corrosion cracking resistance of the welding-heat-affected portion is markedly increased. The need to perform post-welding heat treatment is eliminated, and the result is achieved of greatly reducing construction time of welded-pipe structures.
Description
Technical field
The present invention relates suitable as well for conveying the (oil Well) or gas (gas Well) production of crude oil or natural gas pipeline (pipe Line) of line pipe steel (steel Pipe For Linepipe) containing Cr steel (Cr containing steel pipe), particularly in extremely harsh corrosive environments (corrosion environment) the corrosion resistance (corrosion resistance) and weld heat affected zone (welded heat affected zone) resistance intergranular stress corrosion cracking resistance (resistance to intergranular stress corrosion cracking or resistance to IGSCC) improvements.
Background technology
In recent years, from surging (the skyrocketing crude oil prices) of crude oil price and in the future petroleum resources (oil resources) may exhausted such viewpoint soon, the oil field that the corrodibility that the deep reservoir of the degree of depth of just in the past never paying close attention at active development (depth) (deep layer oil well) gas field or temporarily abandon is developed is strong, gas field etc.Such oil field, the common degree of depth in gas field are dark, and its atmosphere is high temperature, contain carbonic acid gas (carbon dioxide gas) CO
2, chlorion (chloride ion) Cl
-Deng harsh corrosive environment.In addition, the harsh oil field of drilling environment (drilling environment), the exploitation in gas field of seabed (bottom of the ocean) and so on are also gradually many.Require to use the steel pipe of high strength (high-strength), high tenacity (high-toughness) and excellent corrosion resistance as the pipeline of the crude oil of carrying in such oil field, the gas field produces, Sweet natural gas, and from reducing the such viewpoint of laying cost (laying cost) of pipeline, also require to use the steel pipe that possesses excellent weldability (weldability).
For such requirement, for example record a kind of martensitic stainless steel pipe (martensitic stainless steel pipe) that spool is used that is suitable as in the patent documentation 1, its unreal welding connects postheat treatment (post weld heat treatment) and just can prevent from producing intergranular stress corrosion cracking (intergranular stress corrosion cracking) (referred to as IGSCC) at welding heat affected zone, and the anti-intergranular stress corrosion cracking behavior of welding heat affected zone is excellent.The martensitic stainless steel pipe of record has following composition in the patent documentation 1: % contains C in quality: be lower than 0.0100%, N: be lower than 0.0100%, Cr:10～14%, Ni:3～8%, Si:0.05～1.0%, Mn:0.1～2.0%, below the P:0.03%, below the S:0.010%, Al:0.001～0.10%, also contain and be selected from below the Cu:4%, below the Co:4%, below the Mo:4%, W:4% is with lower one kind or two or more and be selected from below the Ti:0.15%, below the Nb:0.10%, below the V:0.10%, below the Zr:0.10%, below the Hf:0.20%, Ta:0.20% is with lower one kind or two or more, and satisfies Csol and be lower than 0.0050%.In the technology of patent documentation 1 record, effective solid solution C amount (the effective content of dissolved carbon:Csol) Csol that effectively plays a role by the formation that makes Cr carbide (carbide) is lower than 0.0050%, thereby prevent from forming the Cr carbide at original austenite crystal prevention (prior-austenite grain boundaries), prevent from belonging to the formation of Cr defect layer (Cr depleted zones) of the cause of welding heat affected zone intergranular stress corrosion cracking, can unreal welding connect postheat treatment and just be suppressed at welding heat affected zone and produce the intergranular stress corrosion cracking.
In addition, put down in writing the spool high-strength stainless steel steel pipe of excellent corrosion resistance in the patent documentation 2.The high-strength stainless steel steel pipe of record has following composition in the patent documentation 2: contain C:0.001～0.015% in quality %, N:0.001～0.015%, Cr:15～18%, Ni:0.5% is above and be lower than 5.5%, Mo:0.5～3.5%, V:0.02～0.2% and Si:0.01～0.5%, Mn:0.1～1.8%, below the P:0.03%, below the S:0.005%, N:0.001～0.015%, below the O:0.006%, and satisfy simultaneously Cr+0.65Ni+0.6Mo+0.55Cu-20C 〉=18.5, Cr+Mo+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N 〉=11.5 and C+N≤0.025.In the technology of patent documentation 2 records, contain an amount of ferritic phase, when keeping ferrite-martensite duplex structure (dual phase microstructure) Cr content is adjusted into higher 15～18% and contain, can form thus hot workability (hot workability) and low-temperature flexibility (low temperature toughness) even excellent have the abundant intensity used as spool containing the steel pipe that also has excellent erosion resistance under 200 ℃ the high-temperature corrosion environment of carbonic acid gas, chlorion.
Patent documentation 1: TOHKEMY 2005-336601 communique (WO2005/073419A1)
Patent documentation 2: TOHKEMY 2005-336599 communique
Summary of the invention
Yet, under harsh corrosive atmosphere, even according to the technology of record in the patent documentation 1, also exist to be suppressed at the problem that welding heat affected zone produces the intergranular stress corrosion cracking fully, present situation is to weld postheat treatment to prevent from producing the intergranular stress corrosion cracking at welding heat affected zone.In addition, steel pipe according to the technology manufacturing of patent documentation 2 record is not considered anti-intergranular stress corrosion cracking behavior fully, improve Cr content, from anti-this viewpoint of intergranular stress corrosion cracking behavior, compare further decline with the steel pipe of record in the low patent documentation 1 of Cr content, existence can't be suppressed at welding heat affected zone fully and produce intergranular stress corrosion this problem that ftractures.
The object of the invention is to solve the problem of above-mentioned prior art, provide the spool of anti-intergranular stress corrosion cracking behavior excellence of desirable high strength, toughness, erosion resistance and halophile stress corrosion crack (resistance to sulfide stress cracking) excellence and welding heat affected zone with containing the Cr steel pipe.The object of the invention steel pipe is X65～X80 level steel pipe (yield strength (YS) is the steel pipe of 448-651MPa)." tenacity excellent " refers to absorbed energy (absorbed energy) E under in Charpy impact test (Charpy impact test)-40 ℃ in addition, herein
-40(J) be the above situation of 50J.In addition, " excellent corrosion resistance " refers to that the corrosion speed (mm/year) (below, referred to as mm/y) in the saturated 150 ℃ of lower 200g/literNaCl aqueous solution of the carbonic acid gas that makes 3.0MPa is the following situation of 0.10mm/y.Should illustrate that " steel pipe " of indication also comprises weldless steel tube (seamless steel pipe), Welded Steel Pipe (welded steel pipe) here.
The inventor etc. conduct in-depth research the various factors of the anti-intergranular stress corrosion cracking behavior that affects welding heat affected zone under corrosive environment ferrite-martensitic stainless steel pipe, that contain carbonic acid gas, chlorion that contains 16～17% Cr in order to achieve the above object.
It found that, in such ferrite-martensitic stainless steel, the intergranular stress corrosion cracking is caused by following reason: form thick ferrite crystal grain at this heat affected zone in the heating cycle (heating cycle) when welding, in refrigeration cycle (cooling cycle) thereafter, separate out the Cr carbide at the crystal boundary of this thick ferrite crystal grain, follow it due to its crystal boundary formation Cr defect layer.And then, the inventor etc. expect in this steel, at the Cr carbide before the crystal boundary of thick ferrite crystal grain is separated out, at least from crystal boundary produce ferrite (ferrite) (α) → (γ) phase transformation of austenite (austenite), make most crystal boundaries can be occupied by austenite, then can stop the Cr carbide to be separated out to crystal boundary, can suppress the formation of Cr defect layer, prevent the generation of intergranular stress corrosion cracking.And further found that of research in order to produce α → γ phase transformation from crystal boundary at the Cr carbide before crystal boundary is separated out, needs to optimize compositing range so that compositing range satisfies following formula (1);
11.5≤Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N≤13.3…（1）。
Research according to inventor etc., new discovery makes { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } to become composition below 13.3 by making, can make carbide be difficult to separate out at crystal boundary (Cr carbide), therefore also be difficult to occur the formation of Cr defect layer, can prevent the intergranular stress corrosion cracking.This is because if { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } becomes below 13.3, then become the low composition of ratio of ferrite former, in this case, in the girth welding when pipeline laying (girth welding), although form thick ferritic phase single phase structure in the zone that is exposed to above under near 1200 ℃ of such high temperature the fusing point (melting point) during heating, but produce α → γ phase transformation during cooling, produce the γ phase from crystal boundary or intragranular.Under these circumstances, because γ compares with α, the solubility product of carbide (solubility product) is large, is difficult to carbide precipitate (Cr carbide) at crystal boundary, therefore also is difficult to occur the formation of Cr defect layer, can prevent the intergranular stress corrosion cracking.And, in cooling thereafter, γ phase most of or all will become mutually martensitic phase, this is needless to say more.
On the other hand, when becoming { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } for the high composition of the ratio that surpasses 13.3 such ferrite formers, because the thick ferritic phase single phase structure that forms is in cooling thereafter, do not produce α → γ phase transformation, directly reach room temperature, so separate out the Cr carbide at crystal boundary, form the Cr defect layer, become and easily produce the intergranular stress corrosion cracking.
Next, the experimental result as basis of the present invention is described.From the various steel pipes that change each component content, take size to be the test film material of thickness 4mm * width 15mm * length 115mm, the material central part is given the Thermal Cycle of condition shown in Figure 1.And, take the structure observation test film the test film after giving Thermal Cycle, grind, corrode, the tissue after the Thermal Cycle is given in observation, be determined at phase transformation resultant (martensitic phase and/or austenite phase) in the former α crystal boundary have or not with by the length of the shared former α crystal boundary of phase transformation resultant (martensitic phase and/or austenite are mutually), calculate the rate that occupies with respect to former α crystal boundary total length.
And then, cut out the test film of thickness 2mm * width 15mm * length 75mm from the central part of the test film material of having given Thermal Cycle that obtains, implement the test of U stress in bending corrosion cracking.As shown in Figure 2, the test of U stress in bending corrosion cracking is that test film is bent to the U font with inside radius: 8.0mm, impregnated in the test in the corrosive fluid.The corrosive fluid that uses is liquid temperature: 100 ℃, CO
2The 50g/l NaCl solution of pressure: 0.1MPa, pH:2.0.Should illustrate that test period is 168h.
After the test, observation by light microscope test film cross section with 100 times, investigation has flawless, be designated as when crackle is arranged ▲, be designated as zero during flawless, the relation that former α crystal boundary is occupied rate and { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } is shown in 3.Among Fig. 3, { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } of formula (1) was above 13.3 o'clock, with respect to former ferrite crystal boundary total length by the ratio of the mutually occupied length of martensitic phase and/or austenite for being lower than 50%, expression has produced the intergranular stress corrosion cracking.
The present invention is based on above-mentioned opinion and further furthers investigate and finish.That is, purport of the present invention is as described below.
(1) a kind of spool of anti-intergranular stress corrosion cracking behavior excellence of welding heat affected zone is with containing the Cr steel pipe, it is characterized in that, has following composition: in quality %, contain C:0.001～0.015% in the mode that satisfies following formula (1), Si:0.05～0.50%, Mn:0.10～2.0%, below the P:0.020%, below the S:0.010%, Al:0.001～0.10%, Cr:15.0～18.0%, Ni:2.0～6.0%, Mo:1.5～3.5%, V:0.001～0.20%, below the N:0.015%, remainder is Fe and inevitable impurity
Formula (1)
11.5≤Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N ≤13.3…（1）
(wherein, Cr, Mo, W, Si, C, Mn, Ni, Cu, N: the content of each element (quality %)),
And, be heated to the single-phase temperature province of ferrite and the welding heat affected zone that is cooled becomes with undertissue in when welding: with the ratiometer with respect to former ferrite crystal boundary total length, being occupied mutually by martensitic phase and/or austenite more than 50% of former ferrite crystal boundary.
(2) it is characterized in that having following composition with containing the Cr steel pipe such as (1) described spool: on the basis of above-mentioned composition, also contain a kind or 2 kinds that is selected from Cu:0.01～3.5%, W:0.01～3.5% in quality %.
(3) such as (1) or (2) described spool with containing the Cr steel pipe, it is characterized in that having following composition: on the basis of above-mentioned composition, also contain in quality % and be selected from one kind or two or more in Ti:0.01～0.20%, Nb:0.01～0.20%, Zr:0.01～0.20%.
(4) such as each described spool in (1)～(3) with containing the Cr steel pipe, it is characterized in that having following composition: on the basis of above-mentioned composition, also contain a kind or 2 kinds that is selected from Ca:0.0005～0.0100%, REM:0.0005～0.0100% in quality %.
According to the present invention, can need not to weld postheat treatment, reach the spool of the anti-intergranular stress corrosion cracking behavior excellence of making welding heat affected zone with containing the Cr steel pipe inexpensively, industrially play significant effect.In addition, according to the present invention, following effect is arranged also: can the steel pipe structures such as pipeline not welded postheat treatment ground and construct, the engineering time etc. can be shortened, significantly reducing construction cost.
Description of drawings
Fig. 1 is the explanatory view of the model utility welding analog thermal cycling (simulated welding thermal cycle) that represents embodiment and use.
Fig. 2 is the explanatory view that model utility represents the bending status of the U stress in bending corrosion cracking test usefulness test film (test specimen for U-bend test) that embodiment uses.
Fig. 3 be expression with respect to former ferrite crystal boundary total length by the relation of the ratio of the mutually occupied length of martensitic phase and/or austenite and formula (1) and have or not and produce the ftracture figure of (referred to as IGSCC) of intergranular stress corrosion.
Embodiment
At first, the composition restriction reason of steel pipe of the present invention described.Below, unless otherwise specified, quality % only represents with %.
C：0.001～0.015%
C helps the element of gaining in strength, and needs in the present invention to contain more than 0.001%.
On the other hand, if contain in a large number above 0.015%, then make the toughness variation of welding heat affected zone.If contain in a large number, then particularly be difficult to prevent the intergranular stress corrosion cracking of welding heat affected zone.Therefore, C is defined as 0.001～0.015% scope.And, be preferably 0.002～0.010%.
Si：0.05～0.50%
Si be as de-acidying agent (deoxidizing agent) when playing a role solid solution and the element of gaining in strength need in the present invention to contain more than 0.05%.But, if contain in a large number above 0.50%, then make the toughness drop of mother metal, welding heat affected zone.Therefore, Si is limited to 0.05～0.50% scope.And, be preferably 0.10～0.40%.
Mn：0.10～2.0%
Mn is solid solution and the intensity that helps to increase steel generates austenitic element simultaneously, suppresses ferrite to generate, and improves the toughness of mother metal, welding heat affected zone.Such effect need to contain more than 0.10%, if but above containing on 2.0% ground, then effect is saturated, can't expect the effect that conforms to content.Therefore, Mn is limited to 0.10～2.0% scope.And, be preferably 0.20～0.90%.
Below the P:0.020%
P makes carbon dioxide corrosion resistant (CO
2Corrosion resistance), the element of the erosion resistance variation such as halophile stress corrosion crack, preferably reduce as far as possible in the present invention, but extreme minimizing can cause the rising of manufacturing cost.Scope as implementing and not make in industrial low price the erosion resistance variation is defined as P below 0.020%.And, be preferably below 0.015%.
Below the S:0.010%
S is the element that makes the remarkable variation of hot workability in the steel pipe manufacturing processed, and is preferably the least possible, if be reduced to below 0.010%, then can carry out the steel pipe manufacturing of common operation, so S is defined as below 0.010%.And, be preferably below 0.004%.
Al：0.001～0.10%
Al is the element with powerful deacidification, in order to obtain such effect, need to contain more than 0.001%, if but above containing on 0.10% ground, then toughness is brought detrimentally affect.Therefore, Al is defined as below 0.10%.And, be preferably below 0.05%.
Cr：15.0～18.0%
Cr forms protection tunicle (protective surface film), improves the element of the erosion resistances such as carbon dioxide corrosion resistant, halophile stress corrosion crack.Particularly for the purpose that improves the erosion resistance under the harsh corrosive environment, need to contain more than 15.0% in the present invention.On the other hand, contain if surpass 18.0% ground, then hot workability reduces.Therefore, Cr is defined as 15.0～18.0% scope.
Ni：2.0～6.0%
Ni has firmly acts on the protection tunicle, is also to help the element of gaining in strength when improving the erosion resistance of carbon dioxide corrosion resistant, halophile stress corrosion crack etc.In order to obtain such effect, need to contain more than 2.0%, if but above containing on 6.0% ground, then reduce hot workability, and cause the reduction of intensity.Therefore, Ni is defined as 2.0～6.0% scope.And, be preferably 3.0～5.0%.
Mo：1.5～3.5%
Mo has and strengthens because of Cl
-The resistivity of the spot corrosion that (chlorion) causes (pitting corrosion) effect, be that erosion resistance is improved the element with useful effect.In order to obtain such effect, need to contain more than 1.5%.On the other hand, surpass 3.5% if contain, then hot workability reduces, and makes manufacturing cost surging.Therefore, Mo is defined as 1.5～3.5% scope.And, be preferably 1.8～3.0%.
V：0.001～0.20%
V has the element that improves the effect of anticorrosion stress-resistant cracking behavior when helping the increase of intensity.Contain 0.001% when above, such effect is remarkable, if but surpass 0.20% ground and contain, then reduce toughness.Therefore, V is defined as 0.001～0.20% scope.And, be preferably 0.010～0.10%.
Below the N:0.015%
N has the effect of raising pitting corrosion resistance (pitting corrosion resistance), but also is the element with the effect of remarkable reduction weldability, and is preferably the least possible in the present invention, but extreme minimizing will cause manufacturing cost to rise.As the scope that can implement and not make in industrial low price the erosion resistance variation, with 0.015% as the upper limit.
Mentioned component is basal component, can also be as required on the basis of essentially consist as a kind that selects element to select to contain to be selected from Cu:0.01～3.5%, W:0.01～3.5% or 2 kinds and/or be selected from one kind or two or more in Ti:0.01～0.20%, Nb:0.01～0.20%, Zr:0.01～0.20% and/or be selected from a kind or 2 kinds that selects in Ca:0.0005～0.0100%, REM:0.0005～0.0100%.
Be selected from a kind or 2 kinds in Cu:0.01～3.5%, W:0.01～3.5%
Cu, W all are the elements that improve carbon dioxide corrosion resistant, can select as required to contain.
Cu is the element that improves carbon dioxide corrosion resistant and help to gain in strength.In order to obtain such effect, preferably contain more than 0.01%, if but contain and surpass 3.5%, then effect is saturated, can't expect the effect that conforms to content, and is unfavorable economically.Therefore, contain sometimes, preferably Cu is defined as 0.01～3.5% scope.And, more preferably 0.30～2.0%.
W is the element that improves carbon dioxide corrosion resistant and improve anticorrosion stress-resistant cracking behavior, halophile stress corrosion crack and pitting corrosion resistance.In order to obtain such effect, preferably contain more than 0.01%, if but surpass 3.5% ground and contain, then effect is saturated, can't expect the effect that conforms to content, and is unfavorable economically.Therefore, in the situation about containing, preferably W is defined as 0.01～3.5% scope.And, more preferably 0.30～2.0%.
Be selected from one kind or two or more in Ti:0.01～0.20%, Nb:0.01～0.20%, Zr:0.01～0.20%
Compare with Cr, Ti, Nb, Zr form the strong element of carbide trend, have the effect of separating out the Cr carbide when suppressing cooling at crystal boundary, can select as required to contain one kind or two or more.In order to obtain such effect, contain respectively preferably that Ti:0.01% is above, Nb:0.01% above, more than the Zr:0.01%, if but surpass Ti:0.20%, Nb:0.20% respectively, Zr:0.20% ground contains, then weldability, toughness drop.Therefore, contain sometimes, preferably be defined as respectively the scope of Ti:0.01～0.20%, Nb:0.01～0.20%, Zr:0.01～0.20%.And, more preferably Ti:0.02～0.10%, Nb:0.02～0.10%, Zr:0.02～0.10%.
Be selected from a kind or 2 kinds in Ca:0.0005～0.0100%, REM:0.0005～0.0100%
Ca, REM are situated between to be improved the element of hot workability, the manufacturing stability when casting continuously by the morphology Control (morphologycontrol) of inclusion (inclusion), can select as required to contain.In order to obtain such effect, preferably contain respectively more than the Ca:0.0005%, more than the REM:0.0005%, if but contain above Ca:0.0100%, REM:0.0100% ground respectively, then cause the increase of inclusion amount, reduce the degree of cleaning (cleanness) of steel.Therefore, when containing, preferably be defined as respectively the scope of Ca:0.0005～0.0100%, REM:0.0005～0.0100%.And, more preferably Ca:0.0010%～0.0030%, REM:0.0010～0.0050%.
In the present invention, with the scope of mentioned component and satisfy the content of adjusting each composition in the mode of following formula (1).
11.5≤Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N≤13.3 ... (1) (wherein, Cr, Mo, W, Si, C, Mn, Ni, Cu, N: the content of each element (quality %))
The intermediate value { Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N } of formula (1) is to estimate the index of hot workability and anti-intergranular stress corrosion cracking behavior, in the present invention, in above-mentioned scope, adjust the content of each element in the mode of 11.5～13.3 the scope that satisfies formula (1).If the intermediate value of formula (1) is lower than 11.5, then hot workability is not enough, can't guarantee the needed sufficient hot workability of manufacturing of weldless steel tube, is difficult to carry out the manufacturing of weldless steel tube.On the other hand, if the intermediate value of formula (1) significantly surpasses 13.3, then as mentioned above, anti-intergranular stress corrosion cracking behavior reduces.Because such situation, with the content of each element with in above-mentioned scope and the mode that satisfies formula (1) adjust.
Remainder beyond the mentioned component is made of Fe and inevitable impurity.As inevitable impurity, can allow below the O:0.010%.
Steel pipe of the present invention has above-mentioned composition, and has martensitic phase as matrix phase (basephase), counts the tissue that the austenite below 30% consists of mutually in ferritic phase and the volume fraction of volume fraction 10～50%.Should illustrate, also comprise tempered martensite phase (tempered martensite phase) in the martensitic phase.In order to ensure desirable intensity, preferably contain martensitic phase more than 25% in volume fraction.In addition, ferritic phase is the tissue of soft raising processibility (workability), from improving this viewpoint of processibility, preferably contains more than 10% in volume fraction.On the other hand, contain if surpass 50% ground, then become and to guarantee desirable high strength (X65 is more than the YS:448MPa).In addition, austenite is mutually for improving the tissue of toughness, if but surpass 30% then be difficult to guarantee intensity.
Should illustrate, austenite has following situation mutually: all do not become mutually martensitic phase when quench treatment, the situation that a part is residual, and, a part of reverse transformation of martensitic phase, ferritic phase (reverse transformation) when temper and stabilization, after the cooling as the mutually residual situation of austenite.
Should illustrate, in having the steel pipe of the present invention of above-mentioned composition and above-mentioned tissue, when being formed with weld part, because in the compositing range of the present application steel, become the single-phase temperature province of ferrite in time more than 1300 ℃, so the welding heat affected zone that is heated to the single-phase temperature province of ferrite more than 1300 ℃ during preferred weld and is cooled becomes such as undertissue: with the ratiometer with respect to former ferrite crystal boundary (prior-ferrite grain boundaries) total length, being occupied mutually by martensitic phase and/or austenite more than 50% of former ferrite crystal boundary.Thus, can avoid the Cr carbide to separate out at the crystal boundary of thick former ferrite grain, suppress the generation of intergranular stress corrosion cracking, improve the anti-intergranular stress corrosion cracking behavior of welding heat affected zone.
Then, as an example the preferred manufacture method of steel pipe of the present invention is described with weldless steel tube.
At first, preferably use the melting method commonly used such as converter (converter), electric furnace (electric furnace), vacuum melting furnace (vacuum melting furnace) that the molten steel (molten steel) with above-mentioned composition is carried out melting, make the steel materials such as steel billet (billet) with the method that Continuous casting process (continuous casting method), ingot casting-split rolling method method (slabing mill method for rolling an ingot) etc. are commonly used.Then, heat these steel materials, use commonly completely to be this graceful axle tube rolling mode (Mannesmann-plug mill method) or completely to be that the manufacturing process of this graceful axle tube rolling mode (Mannesmann-mandrel mill method) carries out the weldless steel tube that hot rolling (hot rolling), tubing form desirable size.Preferably the weldless steel tube behind the tubing is implemented with more than the air cooling (air-cooling rate), (accelerated cooling) cooled off in the acceleration that preferably is cooled to room temperature in the speed of cooling of 800～500 ℃ average 0.5 ℃/s more than.Thus, so long as have the steel pipe of the composition in the compositing range of the present invention, just can become the tissue of martensitic phase as described above as substrate.If speed of cooling is lower than 0.5 ℃/s, then can't become the tissue of martensitic phase as described above as substrate.Martensitic phase is referred to that as the tissue of substrate meaning martensitic phase is the tissue of volume fraction maximum or has volume fraction volume fraction about equally with other tissue of volume fraction maximum herein.
Should illustrate, can replace the acceleration cooling behind the rolling, reheat, quench treatment (quenching) and temper (tempering).As quench treatment, preferably reheat more than 800 ℃, after this temperature keeps more than the 10min with air cooling more than or be cooled to processing below 100 ℃ in the speed of cooling of 800～500 ℃ average 0.5 ℃/more than the s.Be lower than 800 ℃ if reheat temperature, then can't guarantee to become desirable with the tissue of martensitic phase as substrate.
As temper, preferably quench treatment post-heating to 500 ℃～700 ℃, more preferably 580 ℃～680 ℃ temperature keeps laggard line space deepfreeze of specified time.The erosion resistance that can have both thus, desirable high strength, desirable high tenacity and desirable excellence.
So far, be illustrated as an example of weldless steel tube example, but the present invention is not limited thereto.Also can use the steel pipe material (steel plate) with above-mentioned composition, make electricresistance welded steel pipe, UOE steel pipe with common operation, form the spool steel pipe.Should illustrate, for electricresistance welded steel pipe, UOE steel pipe, also preferably steel pipe material (steel plate) or steel pipe be implemented above-mentioned quenching-temper, make the steel pipe with above-mentioned tissue.
In addition, can form welding structure thing (steel pipe structure) by welded joint the invention described above steel pipe.Should illustrate that the welded joint of steel pipe of the present invention also comprises the situation that steel pipe of the present invention is engaged with other kind steel-pipe welding.In these welding structure things that welded joint steel pipe of the present invention forms, be heated to the single-phase temperature province of ferrite more than 1300 ℃ during preferred weld and the welding heat affected zone that is cooled has with the welding heat affected zone with respect to the tissue that is occupied mutually by martensitic phase and/or austenite more than 50% of the former ferrite crystal boundary of ratiometer of former ferrite crystal boundary total length.Thus, suppress the intergranular stress corrosion cracking, do not weld the anti-intergranular stress corrosion cracking behavior that postheat treatment just improves welding heat affected zone.
Below, further specify the present invention based on embodiment.
Embodiment
With the molten steel of the composition shown in the table 1 with vacuum melting furnace (vacuum melting furnace) melting, degassed after, be cast as the 100kgf bloom, utilize forge hot (hot forging) to make the steel pipe material of specified dimension.Heat these steel pipe elements, carry out tubing by the hot-work of the seamless milling train that uses a model (model seamless mill) (the seamless milling train of small test), make weldless steel tube (external diameter 65mm φ * wall thickness 5.5mm).
Under the former state state that cools off behind the tubing, whether the weldless steel tube that visual investigation obtains the cracking of surfaces externally and internally has occured, and estimates hot workability.Should illustrate, when length of tube direction end face can be seen crackle more than the length 5mm, be evaluated as " crackle is arranged ", be designated as *, in addition be evaluated as " flawless ", be designated as zero.
Then, from the weldless steel tube that obtains, take test specimen (steel pipe), with the condition shown in the table 2 this test specimen (steel pipe) is implemented quench treatment, temper.
From the test specimen (steel pipe) of having implemented quench treatment and temper, take test film, implement structure observation (microstructure observation), tension test (tensile test), shock test (impact test), corrosion test (corrosion test), sulfide-stress cracking test and the test of U stress in bending corrosion cracking.Test method is as described below.
(1) structure observation
From the test specimen (steel pipe) that obtains, take the structure observation test film.With structure observation with test film grind, after the corrosion, use that opticmicroscope (optical microscope) (multiplying power (magnification ratio): 1000 times) is observed, shooting, appraisement organization, utilize image analysis apparatus (image analyzer) to try to achieve the tissue minute rate of each phase in the mother metal (base metal).Should illustrate that the γ amount uses X-ray diffraction method (X-ray diffraction method) to measure.
(2) tension test
The mode that becomes draw direction with tube axial direction is taked API arcuation tension test sheet (Arc-shaped pieces for a tensile test specified in the API standards) from the test specimen (steel pipe) that obtains, implement tension test, try to achieve tensile properties (yield strength YS, tensile strength TS), estimate strength of parent.
(3) shock test
According to the regulation of JIS Z 2242, from the test specimen (steel pipe) that obtains, take V notched specimen (5.0mm is thick), implement Charpy impact test (Charpy impact test), try to achieve the absorbed energy vE under-40 ℃
-40(J), estimate base metal tenacity.
(4) corrosion test
Utilize mechanical workout, from the test specimen (steel pipe) that obtains, take the corrosion test sheet of thickness 3mm * width 25mm * length 50mm, implement corrosion test, estimate erosion resistance (carbon dioxide corrosion resistant, pitting corrosion resistance).Corrosion test is that the 200g/liter NaCl aqueous solution that the carbonic acid gas that makes 3.0MPa is satisfied 150 ℃ remains in the autoclave (autoclave), and the corrosion test sheet be impregnated in this aqueous solution, keeps 30 days.The weight of determination test sheet after corrosion test finishes is come Calculation of corrosion speed by the changes in weight (weight subtracts) before and after the corrosion test.In addition, after corrosion test, utilize 10 times magnifying glass (laupe) viewing test sheet surface to have or not spot corrosion to produce to the corrosion test sheet.Be evaluated as when producing spot corrosion *, be evaluated as zero when not producing.
(5) sulfide-stress cracking (SSC) test
From the test specimen (steel pipe) that obtains, take 4 pliability test sheets (four-point bending test) (size: thickness 4mm * width 15mm * length 115mm), enforcement is according to EFC(European Federation of Corrosion) 4 pliability tests of No.17, estimate the halophile stress corrosion crack.The experimental liquid that uses is 50g/liter NaCl+NaHCO
3Liquid (pH:4.5), limit circulation 10vol%H
2S+90vol%CO
2Test on the mixed gas limit, and investigation has non-cracking.Should illustrate, additional stress is made as the YS(yield strength of mother metal), test period is made as 720 hours (below, referred to as h).With the fracture test film be evaluated as *, not the fracture test film be evaluated as zero.
(6) U stress in bending corrosion cracking test
From the test specimen (steel pipe) that obtains, take size: the test film material of thickness 4mm * width 15mm * length 115mm, give the Thermal Cycle of condition shown in Figure 1 at the material central part.And, from the test film after the Thermal Cycle of having given condition shown in Figure 1, take the structure observation test film, to grind, corrode, the tissue after the Thermal Cycle is given in observation.Investigation has the phase transformation resultant (martensitic phase and/or austenite phase) of the former α crystal boundary of having no way of, and measures the length of the former α crystal boundary that former α crystal boundary occupied by phase transformation resultant (martensitic phase and/or austenite phase), calculates the rate that occupies with respect to former α crystal boundary total length.
And then, cut out the test film of thickness 2mm * width 15mm * length 75mm from the central part of having given the test film material after the Thermal Cycle that obtains, implement the test of U stress in bending corrosion cracking.U stress in bending corrosion cracking test bends to the U font with test film with inside radius: 8.0mm and is immersed in the corrosive fluid and tests.
The corrosive fluid that uses is liquid temperature: 100 ℃, CO
2Press: the 50g/literNaCl liquid of 0.1MPa, pH:2.0.Should illustrate that test period is 168h.
After the test, with 100 times observation by light microscope test film cross section, investigation has or not cracking, estimates anti-intergranular stress corrosion cracking behavior.Have cracking the time be designated as *, be designated as zero when not ftractureing.
The obtained results are shown in table 3.
The inventive example all becomes following steel pipe: have superior hot workability, have YS:448MPa(65ksi) above high strength, above high tenacity and the corrosion speed of vE-40:50J: the high corrosion resistance that 0.12mm/y is following, also do not produce sulfide-stress cracking, in the welding heat affected zone that is heated to more than 1300 ℃, also do not produce the intergranular stress corrosion cracking, the anti-intergranular stress corrosion cracking behavior of welding heat affected zone is excellent.In the comparative example beyond the scope of the present invention, hot workability reduction or toughness drop or erosion resistance reduce or the reduction of halophile stress cracking, and perhaps the anti-intergranular stress corrosion cracking behavior of welding heat affected zone reduces.
In addition, use the disclosed invention steel of the embodiment No.F of TOHKEMY 2005-336599 communique (patent documentation 2), G, M, N and O(steel No.U, V, W, X and Y) steel pipe (steel pipe No.27～31) made, as shown in table 1, the compositing range of each element satisfies the scope of the present application, but the formula of stipulating in the present application (1) is all above 13.3, so as shown in table 3, with respect to former ferrite crystal boundary total length, the ratio (rate that occupies (%) of former α crystal boundary) of the length that is occupied mutually by martensitic phase and/or austenite all is lower than 50%, and the intergranular stress corrosion cracking has all occured.
The effect of the anti-intergranular stress corrosion cracking behavior of this welding heat affected zone can't expect fully from TOHKEMY 2005-336599 communique (patent documentation 2).
Table 2
*) example of JP 2005-336599 communique
Claims (4)
1. a spool is characterized in that with containing the Cr steel pipe,
Has following composition:, contain in the mode that satisfies following formula (1) in quality %
C：0.001～0.015%、 Si：0.05～0.50%、
Below Mn:0.10～2.0%, the P:0.020%,
S:0.010% is following, Al:0.001～0.10%,
Cr：15.0～18.0%、 Ni：2.0～6.0%、
Mo：1.5～3.5%、 V：0.001～0.20%、
N: below 0.015%,
Remainder is Fe and inevitable impurity,
11.5≤Cr+Mo+0.4W+0.3Si-43.5C-0.4Mn-Ni-0.3Cu-9N≤13.3…（1）
In the formula (1), Cr, Mo, W, Si, C, Mn, Ni, Cu, N represent the content of each element, and unit is quality %;
And, be heated to the single-phase temperature province of ferrite during welding and the welding heat affected zone that is cooled becomes with undertissue: with the ratiometer with respect to former ferrite crystal boundary total length, being occupied mutually by martensitic phase and/or austenite more than 50% of former ferrite crystal boundary.
2. spool according to claim 1 wherein, has following composition with containing the Cr steel pipe: also contain a kind or 2 kinds that is selected from Cu:0.01～3.5%, W:0.01～3.5% in quality % on the basis of described composition.
3. spool according to claim 1 and 2 is with containing the Cr steel pipe, wherein, has following composition: on the basis of described composition, also contain in quality % and be selected from one kind or two or more in Ti:0.01～0.20%, Nb:0.01～0.20%, Zr:0.01～0.20%.
4. each described spool wherein, has following composition with containing the Cr steel pipe according to claim 1～3: also contain a kind or 2 kinds that is selected from Ca:0.0005～0.0100%, REM:0.0005～0.0100% in quality % on the basis of described composition.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010095860 | 2010-04-19 | ||
| JP2010-095860 | 2010-04-19 | ||
| PCT/JP2011/059891 WO2011132765A1 (en) | 2010-04-19 | 2011-04-15 | Cr-CONTAINING STEEL PIPE FOR LINE PIPE AND HAVING EXCELLENT INTERGRANULAR STRESS CORROSION CRACKING RESISTANCE AT WELDING-HEAT-AFFECTED PORTION |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102859019A true CN102859019A (en) | 2013-01-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011800195748A Pending CN102859019A (en) | 2010-04-19 | 2011-04-15 | Cr-containing steel pipe for line pipe and having excellent intergranular stress corrosion cracking resistance at welding-heat-affected portion |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP2562284B1 (en) |
| JP (1) | JP5765036B2 (en) |
| CN (1) | CN102859019A (en) |
| BR (1) | BR112012026595A2 (en) |
| WO (1) | WO2011132765A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103233180A (en) * | 2013-05-17 | 2013-08-07 | 宝山钢铁股份有限公司 | High-strength dual-phase stainless steel tube and preparation method thereof |
| CN105177255A (en) * | 2015-10-15 | 2015-12-23 | 东北大学 | Heat treatment technological method for ferrite-austenite duplex stainless steel |
| CN106661683A (en) * | 2014-02-28 | 2017-05-10 | 搲陆瑞客巴西钢管股份公司 | Martensitic-ferritic stainless steel, manufactured product and processes using the same |
| CN110763612A (en) * | 2018-07-25 | 2020-02-07 | 中国石油化工股份有限公司 | Method for researching influence of martensite on stress corrosion cracking performance of austenitic steel |
| CN115807190A (en) * | 2022-11-28 | 2023-03-17 | 攀钢集团攀枝花钢铁研究院有限公司 | High-strength corrosion-resistant stainless steel seamless pipe for oil transportation and manufacturing method thereof |
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| BR112014025818B1 (en) | 2012-04-26 | 2019-06-11 | Jfe Steel Corporation | STEEL TUBE CONTAINING CR FOR PIPING. |
| JP5924256B2 (en) | 2012-06-21 | 2016-05-25 | Ｊｆｅスチール株式会社 | High strength stainless steel seamless pipe for oil well with excellent corrosion resistance and manufacturing method thereof |
| JP5967066B2 (en) * | 2012-12-21 | 2016-08-10 | Ｊｆｅスチール株式会社 | High strength stainless steel seamless steel pipe for oil well with excellent corrosion resistance and method for producing the same |
| JP6171834B2 (en) * | 2013-10-21 | 2017-08-02 | Ｊｆｅスチール株式会社 | Equipment column for manufacturing thick steel |
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| JP6137082B2 (en) * | 2014-07-31 | 2017-05-31 | Ｊｆｅスチール株式会社 | High strength stainless steel seamless steel pipe excellent in low temperature toughness and method for producing the same |
| JP6229794B2 (en) * | 2015-01-15 | 2017-11-15 | Ｊｆｅスチール株式会社 | Seamless stainless steel pipe for oil well and manufacturing method thereof |
| JP6206423B2 (en) * | 2015-01-22 | 2017-10-04 | Ｊｆｅスチール株式会社 | High strength stainless steel plate excellent in low temperature toughness and method for producing the same |
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- 2011-04-15 CN CN2011800195748A patent/CN102859019A/en active Pending
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- 2011-04-15 BR BR112012026595A patent/BR112012026595A2/en not_active Application Discontinuation
- 2011-04-15 WO PCT/JP2011/059891 patent/WO2011132765A1/en active Application Filing
- 2011-04-19 JP JP2011092571A patent/JP5765036B2/en active Active
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| JPS558404A (en) * | 1978-06-30 | 1980-01-22 | Nippon Steel Corp | Manufacture of austenitic stainless steel used in atmosphere of high-temperature and high-pressure water |
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| CN103233180A (en) * | 2013-05-17 | 2013-08-07 | 宝山钢铁股份有限公司 | High-strength dual-phase stainless steel tube and preparation method thereof |
| CN106661683A (en) * | 2014-02-28 | 2017-05-10 | 搲陆瑞客巴西钢管股份公司 | Martensitic-ferritic stainless steel, manufactured product and processes using the same |
| CN105177255A (en) * | 2015-10-15 | 2015-12-23 | 东北大学 | Heat treatment technological method for ferrite-austenite duplex stainless steel |
| CN110763612A (en) * | 2018-07-25 | 2020-02-07 | 中国石油化工股份有限公司 | Method for researching influence of martensite on stress corrosion cracking performance of austenitic steel |
| CN115807190A (en) * | 2022-11-28 | 2023-03-17 | 攀钢集团攀枝花钢铁研究院有限公司 | High-strength corrosion-resistant stainless steel seamless pipe for oil transportation and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2562284B1 (en) | 2020-06-03 |
| EP2562284A1 (en) | 2013-02-27 |
| JP2011241477A (en) | 2011-12-01 |
| JP5765036B2 (en) | 2015-08-19 |
| EP2562284A4 (en) | 2017-07-12 |
| BR112012026595A2 (en) | 2016-07-12 |
| WO2011132765A1 (en) | 2011-10-27 |
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Application publication date: 20130102 |