CN102959111A - Free-cutting stainless-steel cast product and process for producing same - Google Patents
Free-cutting stainless-steel cast product and process for producing same Download PDFInfo
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- CN102959111A CN102959111A CN2011800311626A CN201180031162A CN102959111A CN 102959111 A CN102959111 A CN 102959111A CN 2011800311626 A CN2011800311626 A CN 2011800311626A CN 201180031162 A CN201180031162 A CN 201180031162A CN 102959111 A CN102959111 A CN 102959111A
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- C—CHEMISTRY; METALLURGY
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- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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- C21D6/00—Heat treatment of ferrous alloys
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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Abstract
The present invention addresses the problem of providing a free-cutting stainless-steel cast product which can satisfy all of excellent cuttability, environmental preservation, and corrosion resistance and a process for producing the cast product. The stainless-steel cast product contains an agent for imparting free-cutting properties, and has a configuration characterized in that the agent for imparting free-cutting properties is h-BN particles and has been evenly and dispersedly precipitated in the steel. The process has a configuration characterized in that a stainless-steel cast product containing h-BN particles precipitated therein is heated and then quenched to cause the h-BN particles to disappear through formation of a solid solution and the cast product is thereafter tempered to thereby dispersedly reprecipitate h-BN particles.
Description
Technical field
The present invention relates to add soon cut and (easily cut free-cutting) stainless steel cast product and the production method thereof of additive.
Background technology
The vital stainless steel cast product of erosion resistance, for example, the tube stub (for example, elbow, pipe box and pipe connecting) that is used for pipework, vacuum apparatus and Analytical equipment, valve and flange connector is produced by casting.Complex-shaped goods such as forging and rolling, carry out machining (mechanical workout) but pass through to cast structure, such as pressing, punching and screw thread without plastic working.These goods need to have good erosion resistance, therefore usually use austenitic stainless steel, such as SUS 304 and SUS 316.But work hardening occurs in austenitic stainless steel easily.Therefore known austenitic stainless steel since the work hardening of contiguous cutting surface generation have poor machinability (machinability, machinability).
In routine techniques, provide and cut soon stainless steel, wherein add sulphur (S), plumbous (Pb) or selenium (Se) as cutting additive soon, purpose is to improve machinability.But the application of Pb brings environmental problem, and is connected connection with the drink mechanism in view of security consideration is unsuitable for food.Se is known to be the harmful element of environment, and its application is under an embargo.SUS 303, and---can cut soon stainless steel by the commercial sulphur that adds that obtains---comprises about 0.3% S.That trace also adversely affects the element of erosion resistance even S is known.Therefore, the application of SUS 303 is unsuitable for the important equipment of erosion resistance.
Adding sulphur cuts soon stainless steel and only can be used for the low-corrosiveness environment or need not in the goods of erosion resistance.Owing to these reasons, guarantee that the stainless steel cast product of cutting soon of good machinability and erosion resistance also is not provided at present.
PTL1 disclose guarantee simultaneously good machinability, erosion resistance and mechanical property cut soon stainless steel and production method thereof.For guaranteeing all machinabilities, erosion resistance and mechanical characteristics, the present invention cuts soon stainless machinability and improves about 25% with respect to the stainless material of routine by following making: the ingot casting after the casting is forged with rolling to eliminate cast structure, and separate out again (redeposition, re-precipitating) hexagonal boron nitride (h-BN) particle.
Although machinability by forge and rolling after heat-treat the stainless steel that has been improved and be developed, disclosed such as PTL1, unexposed machinability is improved and keeps the stainless steel cast product of cast structure.
Summary of the invention
Technical problem
Therefore, the object of the present invention is to provide and cut soon the stainless steel cast product---it can guarantee all good machinabilities, environment friendly and erosion resistance, as not needing very high mechanical characteristics, but needs machinability to obtain the cast steel goods of complicated shape; And provide its production method.
The solution of problem scheme
The present invention is based on such opinion and realize: the stainless steel cast product of machinability and excellent corrosion resistance and production method thereof can provide by following: utilize effectively that hexagonal boron nitride (h-BN) particle is good as the solid lubricant performance, stable chemical nature and not by the characteristic of acid or alkali infringement; And even the cast structure state by carry out specific heat treatment utilize the separating out of h-BN (precipitation, precipitation) or sosoloid/separate out again.
Invention 1 is the embodiment that comprises the stainless steel cast product of cutting soon additive, and this cuts additive soon is hexagonal boron nitride (h-BN) particle, and wherein the h-BN particle has 200nm to 10 μ m particle diameter, is spheroidal particle, and disperses equably in steel and separate out.
Invention 2 is embodiments of the stainless steel cast product production method of invention 1, this production method is included in the casting solidification process 1, control melting stainless speed of cooling in 250 ℃ to 850 ℃ the temperature range, thus disperse therein and separate out the h-BN particle.
Invention 3 is embodiments of the stainless steel cast product production method of invention 1, this production method comprises: the heating Cast Stainless Steel, the h-BN particle is separated out unevenly in the cast structure of this Cast Stainless Steel, then make Cast Stainless Steel quench to become solid solution state, eliminate thus the h-BN particle; And make the Cast Stainless Steel tempering again to disperse and to separate out the h-BN particle.
Invention 4 is embodiments of the stainless steel cast product production method of invention 1, and this production method comprises: the melting stainless steel is quenched in 1,250 ℃ to 850 ℃ temperature range, to obtain cast structure, wherein do not separate out the h-BN particle; And make Cast Stainless Steel 950 ℃ of tempering to the temperature of 1,100 ℃ of scope, to disperse therein and to separate out the h-BN particle.
Invention 5 is the embodiments according to invention 2 to 4 described stainless steel cast product production methods, and wherein the add-on of boron (B) is by mass 0.003% to by mass 0.5%, and the add-on of nitrogen (N) is that the N/B mol ratio becomes 1 or larger.
Invention 6 is the embodiments according to invention 5 described stainless cast product production methods, wherein B adds in the stainless steel of melting with the form of ferro-boron or metal boron, and N adds in the melting stainless steel as the stainless melting atmosphere of melting by gas mixture or the decompression nitrogen that argon and nitrogen (argon+nitrogen) are provided.
Invention 7 is the embodiments according to invention 5 described stainless steel cast product production methods, and wherein B adds in the melting stainless steel with the form of ferro-boron or metal boron, and N adds in the melting stainless steel with the form of nitrogenous compound or iron alloy.
The advantageous effects of invention
Can provide owing to disperse equably and separate out h-BN particle as good solid lubricant, machinability improves and stainless steel cast product that erosion resistance does not worsen, this solid lubricant stable chemical nature and not by acid or alkali infringement; And provide its production method.
Invention 1 not only can be guaranteed good machinability and environment friendly, and can guarantee erosion resistance.
These effects obtain by effectively using as the good h-BN particle of Cast Stainless Steel solid lubricant character.This using of h-BN particle makes the such stainless steel cast product of realization become possibility; this stainless steel cast product is not only guaranteed machinability; and because there is not the harmful element of environment for use, for example Pb and Se and guarantee environment friendly, and suppress the deterioration of erosion resistance.
Because machinability improves, and can reduce the power consumption of cutting machine.The minimizing of this power consumption causes the carbon dioxide discharging to reduce.Further, can expect the raising of productivity, so the stainless steel cast product can carry out high speed machine processing.
The accompanying drawing summary
Fig. 1 is the SEM microgram with dispersion state of separating out that shows precipitate on the fracture surface of exploitation material 1.
Fig. 2 is the SEM microgram with dispersion state of separating out that shows precipitate on the fracture surface of exploitation material 3.
Fig. 3 is the SEM microgram with dispersion state of separating out that shows precipitate on the fracture surface of comparative material 2.
Fig. 4 is that demonstration exploitation material 4 and comparative material 1 and 2 cutting speed in turning process are resisted the with joint efforts figure of (resultant tool force, combined cutting force) Relations Among with cutting.
Fig. 5 is that demonstration exploitation material 1 to 3 and comparative material 3 cutting speed in turning process are resisted the with joint efforts figure of Relations Among with cutting.
Fig. 6 is the figure that shows the corrosion test result of the exploitation material 4 that carries out according to stainless sulfuric acid testing method (JIS G 0591) and comparative material 1 and 2.
Embodiment is described
The present invention has above-mentioned feature, and its embodiment will be described below.
In production method of the present invention, the melting of Cast Stainless Steel is undertaken by melting furnace, and this melting furnace can be regulated melting atmosphere, and generally is used for stainless melting.In melting, ferro-boron or metal boron is as the source of B, but the low melting point ferro-boron be applied in the technical advantage that has, and be economical, because the cost of per unit weight B is low.
For general standard, B content is confirmed as the final B content in the stainless steel cast product, and it is preferably by mass 0.003% to by mass 0.5%, and more preferably by mass 0.01% to by mass 0.2%.
For the method for adding N, there is the method for the N in the stainless steel absorption melting atmosphere that makes melting and will forms the nitride of stainless alloying element such as chromium nitride and nitrided ferro-chromium join the stainless method of melting.
For general standard, the N content in the stainless steel cast product can be that the mol ratio of N/B becomes 1 or larger amount.When the mol ratio of N/B in the Cast Stainless Steel less than 1 the time, the amount of solute B increases, this reduces the h-BN grain amount of separating out that can be used for machinability.Therefore, the mol ratio of expectation N/B is large as far as possible.N content depends on the chemical constitution of Cast Stainless Steel and changes, but along with B increases, the balance N concentration in the steel reduces, because B increases the activity of N.In SUS 304 stainless chemical constitutions, N content is by mass 0.25% or lower---be not included in the melting under the pressurized nitrogen atmosphere.
In the above described manner the preparation the melting stainless steel that contains B and N by in casting mold solidificating period in the Precipitation Temperature scope of h-BN, namely its speed of cooling of control particle diameter of can separating out in cast structure and distribute is the h-BN spheroidal particle of 200nm to 10 μ m in 1,250 ℃ to 850 ℃.
In the stainless steel cast product, the h-BN of girth growth (coarsely grown) to about 20 μ m to about 30 μ m sizes can distribute in the part goods and separate out unevenly, and this depends on the speed of cooling in the rear process of cooling of casting.For the uneven distribution of avoiding thick h-BN particle with separate out:
(1) speed of cooling after the control casting;
(2) use metallic mould; With
(3) design of consideration casting mold is such as casting position and feed head shape.
By remaining on the relatively short time of 1,200 ℃ or higher temperature (for example, at 1,250 ℃, 0.5 hour to 1 hour), the h-BN that separates out in the stainless steel cast product is decomposed into B and N, and changes sosoloid in the matrix of Cast Stainless Steel.Notice that this processing can not be carried out when the melting of stainless steel cast product, therefore must under the temperature that is lower than the steel fusing point, process.
By quenching from this state, obtain containing the stainless steel cast product of B and N, it is in oversaturated solid solution state.Hardening step can be water quenching, and it generally carries out for stainless steel, but the speed of cooling in the temperature range of separating out h-BN of mentioning hereinafter need to be adjusted to the speed of cooling that does not occur to separate out.
Supersaturation B and N separate out as h-BN in the drawing process of 800 ℃ to 1,150 ℃ temperature again.When carrying out under the temperature of tempering about 800 ℃, the h-BN nucleation has precedence over growth, and this is that namely the equilibrium solubility of B and N and supersaturation solubleness difference under this temperature is large owing to following two factors; And the diffusion length of B and N is little, because B and N velocity of diffusion under this temperature is low.Therefore, h-BN extremely trickle and that evenly separate out appears in the whole material.When tempering when carrying out under the temperature about 1,150 ℃, form contrast with tempering under the temperature about 800 ℃, the h-BN precipitate of girth growth occurs, this is because the h-BN growth has precedence over nucleation.
Therefore, be suitable for obtaining the h-BN of good machinability for separating out particle diameter and distributing, the selection of tempering temperature is extremely important.As the result of tentative experiment, particle diameter and distribution are suitable for obtaining the tempering temperature of good machinability preferably in 950 ℃ to 1,100 ℃ scope.
Can direct quenching during to tempering temperature when cast product, h-BN does not separate out in castingprocesses.Under this casting condition that obtains B and N sosoloid, obviously do not need to carry out thermal treatment under 1,200 ℃ or the higher temperature to decompose the h-BN particle.
For the time of tempering, the higher then time of tempering temperature is shorter because temperature when high the velocity of diffusion of B and N fast.Therefore, the time in 0.5 hour to 3 hours scope, preferred 1 hour to 2 hours.For restriction h-BN further growth, after tempering, quench.
Embodiment
(embodiment 1)
Commercially available austenitic stainless steel (SUS 304) pole (weight: 18kg) be used as fused raw material, and carry out melting by the vacuum induction melting furnace.The chemical constitution of fused raw material (by mass %) comprises 0.04% C, 0.30% Si, 1.00% Mn, 0.030% P, 0.024% S, 8.09% Ni and 18.05% Cr.When melting, the N gas of dividing potential drop 0.07MPa is introduced the vacuum induction melting furnace, with the N concentration in the steel of regulating melting.After the melting, the commercially available ferro-boron (by mass 19.2% B) of predetermined amount is added in the steel of melting, to regulate B concentration.Gains are remained in the decompression nitrogen atmosphere 20 minutes, and under 1,600 ℃, be cast as casting cast iron casting type, thereby generate ingot casting.The target value of B content is respectively by mass 0.02%, by mass 0.05% and by mass 0.1% in the exploitation material 1 to 3, and the target value of its N content is respectively by mass 0.2%.
Comparision of production material 1(is corresponding to SUS 304 Cast Stainless Steels without h-BN under same melt and casting condition), generate ingot casting in the mode identical with exploitation material 1 to 3, condition is fused raw material melting under Ar atmosphere.Material 2 as a comparison, generate the material (corresponding to the SUS303 Cast Stainless Steel, add sulphur and cut soon Cast Stainless Steel) that 0.3% S by mass adds comparative material 1.Material 3 as a comparison, generate to be similar to exploitation material 1 to 3, and 0.2% N adds the material of comparative material 1 by mass.
For making N consistent on the impact of machinability and erosion resistance, the N dividing potential drop in the melting atmosphere is adjusted to 0.005MPa, thereby generates the ingot casting that has the exploitation material 4 of identical N level with comparative material 1 and 2.As fused raw material, use the same material used with exploitation material 1 to 3, and the target value of B content is by mass 0.05%, this is identical with target value of developing material 2.The analytical value of B, N and S in the material that generates after the casting (exploitation material 1 to 4, comparative material 1 to 3) (unit: by mass %) is presented in the table 1.
Table 1
The analytical value of B, N and S in each sample (unit: by mass %) ("-" expression is analyzed)
| Sample | B% | N% | S% |
| Exploitation material 1 | 0.021 | 0.22 - | |
| Exploitation material 2 | 0.049 | 0.20 - | |
| Exploitation material 3 | 0.096 | 0.20 - | |
| Exploitation material 4 | 0.047 | 0.065 - | |
| Comparative material 1- | 0.057 - | ||
| Comparative material 2- | 0.063 | 0.29 | |
| Comparative material 3 | <0.001 | 0.21 - |
Carry out the h-BN solution-treated for ingot casting, namely under 1,250 ℃, in air, thermal treatment is 0.5 hour in resistance heading furnace, then carries out water quenching outside stove.Carry out h-BN for the ingot casting of water quenching and separate out processing, namely under 1,050 ℃, in air, thermal treatment is 1 hour in resistance heading furnace, then carries out water quenching outside stove.For the condition that makes cast structure is identical, this thermal treatment of exploitation material and comparative material is carried out under the same conditions.
Fig. 1 to 3 is respectively the SEM(scanning electronic microscope with dispersion state separated out that shows precipitate in exploitation material 1, exploitation material 3 and the comparative material 2) microgram.The pole that with diameter is 3.6mm cuts off from heat treated sample, at the circumference upper cut, and crooked in the incision site place, and observes the fracture surface of curved rod by SEM.SEM is equipped with energy dispersion X-ray spectrum (EDS), by EDS the non-metallic inclusions of observing at fracture surface is carried out ultimate analysis, thereby determines non-metallic inclusions.
In Fig. 1, in the visual field of * 200 magnifications, observe the concave bottom that some h-BN particles (being represented by solid arrow) with 10 μ m or smaller szie are dispersed in whole fracture surface.Equally, observe some spherical MnS particles (being represented by dotted arrow), the size that it has about 10 μ m is derived from the Determination of Trace Sulfur and the manganese that comprise in the fused raw material.
In Fig. 2, be similar to Fig. 1, in the visual field of * 200 magnifications, observe the h-BN particle with 10 μ m or smaller szie and be dispersed in the whole fracture surface.In Fig. 2, the h-BN amounts of particles approximately is 10 times of h-BN amounts of particles of exploitation material 1, and itself and B concentration are proportional.By the h-BN particle shape of observing among Fig. 1 and 2 as can be known, in the process of setting of molten steel, oversaturated B and N separate out as the h-BN particle in the molten steel.
In the situation of the comparative material 2 of Fig. 3, in the visual field of * 200 magnifications, observe in the concave bottom of whole fracture surface and be of a size of in a large number about 10 μ m to the MnS spheroidal particle of about 30 μ m.These MnS particles also are observed in Fig. 1, and by its particle diameter and as can be known steel crystallization when being in molten state of shape.
About the evaluation test of machinability, the pole sample that cuts off from the cast steel sample is carried out lathe turning test, this cast steel sample is the comparative material 1 and 2 and exploitation material 4 after the thermal treatment.The result is presented among Fig. 4.As shown in table 1, these three kinds of materials have substantially the same N contents level, are by mass about 0.06%.The h-BN particle that disperses in Fig. 4 display material or MnS particle are on the impact of machinability.The turning test condition comprises that depth of cut 1.0mm, input speed 0.1mm/rev and tool material M30(are without chip-breaking), do not use machining oil, and turning cutting speed is 12m/min to 200m/min.Under these conditions, obtain observed value.
With comparative material 1(corresponding to SUS 304 Cast Stainless Steels) compare, exploitation material 4 reduces the cutting opposing and makes a concerted effort 20% in middle cutting speed district, reduce the cutting opposing in high cutting speed district and make a concerted effort 11%, and its machinability significantly improves.
Comparative material 2 is to add sulphur to cut soon Cast Stainless Steel, and the machinability of exploitation material is lower than comparative material 2.But, in the important situation of cast steel goods erosion resistance, can not use comparative material 2.Only developing material and can guarantee good machinability and erosion resistance, can not negate that the exploitation material is with respect to the superiority of comparative material.
Fig. 5 has shown that exploitation material 1 to 3 and comparative material 3(do not add B in the turning process) cutting speed and the cutting opposing of the sample relation between making a concerted effort, in exploitation material 1 to 3, the addition difference of B.As shown in table 1, these four kinds of materials have substantially the same N contents level, are approximately by mass 0.2%.Fig. 5 has shown that the interpolation of B is on the impact of machinability.Compare for 0% comparative material 3 by mass with B concentration, observe the exploitation material that adds B and reduce cutting resistance in nearly all cutting speed district, determine that therefore the interpolation of B has improved machinability.
As the evaluation test of stainless steel erosion resistance, the cast steel sample of having heat-treated is carried out corrosion test.The result is presented among Fig. 6.Because N helps stainless erosion resistance, and the material with identical N concentration level is compared.Fig. 6 has shown the corrosion test result who carries out according to stainless steel sulfuric acid testing method (JIS G 0591).The condition of test is as follows.Each sample continuous dip is entered the 5%H of boiling
2SO
46 hours.The value that corrosion weight loss is obtained divided by the sample initial surface area is defined as etching extent.More resulting etching extent.
After erosion resistance based on the material of the fact of whether adding h-BN compared, between exploitation material 4 and comparative material 1, almost do not observe any difference, and determine the erosion resistance deterioration.On the other hand, the etching extent of comparative material 2 is compared remarkable increase with exploitation material 4 with comparative material 1, and this shows can not usage comparison material 2 when the needs erosion resistance.
The present invention obviously is not limited to above-described embodiment, and detail of the present invention comprises numerous embodiments.
Industrial applicability
Such as above detailed description, the present invention can easily provide environmental friendliness, machinability raising and erosion resistance not to have the stainless steel cast product that worsens, so the present invention can provide the good applicability of stainless steel cast product in a plurality of manufacture fields.
Reference listing
Patent documentation
PTL 1 international application published WO2008/016158
Claims (7)
1. stainless steel cast product comprises:
Cut soon additive, it is hexagonal boron nitride (h-BN) particle;
Wherein said h-BN particle has the particle diameter of 200nm to 10 μ m, is spheroidal particle, and disperses equably in described stainless steel cast product and separate out.
2. the production method of the described stainless steel cast product of claim 1 comprises:
In the casting solidification process in 1,250 ℃ to 850 ℃ temperature range control melting stainless speed of cooling, thereby disperse therein and separate out described h-BN particle.
3. the production method of the described stainless steel cast product of claim 1 comprises:
The heating Cast Stainless Steel is to the temperature that is equal to or higher than 1,200 ℃, described Cast Stainless Steel cast structure in the h-BN particle separate out unevenly, described Cast Stainless Steel is quenched, to become solid solution state, eliminate thus described h-BN particle; With
Make tempering under the temperature of described Cast Stainless Steel in 950 ℃ to 1, the 100 ℃ scopes, again to disperse and to separate out the h-BN particle.
4. the production method of the described stainless steel cast product of claim 1 comprises:
The melting stainless steel is quenched, with the cast structure that obtains separating out without the h-BN particle in 1,250 ℃ to 850 ℃ temperature range; With
Make tempering under the temperature of described Cast Stainless Steel in 950 ℃ to 1, the 100 ℃ scopes, to disperse therein and to separate out the h-BN particle.
5. the production method of each described stainless steel cast product in 4 according to claim 2, wherein the add-on of boron (B) is by mass 0.003% to 0.5%, the add-on of nitrogen (N) is so that the mol ratio of N/B becomes 1 or larger.
6. the production method of stainless steel cast product according to claim 5, wherein said B joins the melting stainless steel with the form of ferro-boron or metal boron, and described N joins described melting stainless steel by gas mixture or the decompression nitrogen that argon and nitrogen (argon+nitrogen) are provided as the stainless melting atmosphere of melting.
7. the production method of stainless steel cast product according to claim 5, wherein said B joins the melting stainless steel with the form of ferro-boron or metal boron, and described N joins the melting stainless steel with the form of nitrogenous compound or iron alloy.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010-167872 | 2010-07-27 | ||
| JP2010167872 | 2010-07-27 | ||
| PCT/JP2011/059910 WO2012014541A1 (en) | 2010-07-27 | 2011-04-22 | Free-cutting stainless-steel cast product and process for producing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
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| EP (1) | EP2537952B1 (en) |
| JP (1) | JP5713299B2 (en) |
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| JP6103746B2 (en) * | 2012-08-23 | 2017-03-29 | 国立研究開発法人物質・材料研究機構 | Free-cutting iron shape memory alloy |
| CN104513143A (en) | 2013-09-26 | 2015-04-15 | 陶氏技术投资有限责任公司 | Hydroformylation process |
| CN105331779A (en) * | 2015-11-20 | 2016-02-17 | 沈阳黎明航空发动机(集团)有限责任公司 | Technological method for reducing possibility of nitridation foaming of 1Cr13 steel part |
| CA3213539A1 (en) | 2021-03-31 | 2022-10-06 | Jason F. GILES | Hydroformylation processes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003129191A (en) * | 2001-10-24 | 2003-05-08 | Nisshin Steel Co Ltd | Boron nitride-containing stainless steel material with free-machinability, and manufacturing method therefor |
| EP2048257A1 (en) * | 2006-07-31 | 2009-04-15 | National Institute for Materials Science | Free-cutting stainless steel and process for producing the same |
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| JP6044037B2 (en) * | 2010-04-30 | 2016-12-14 | 国立研究開発法人物質・材料研究機構 | Free-cutting stainless steel material for precision machining and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003129191A (en) * | 2001-10-24 | 2003-05-08 | Nisshin Steel Co Ltd | Boron nitride-containing stainless steel material with free-machinability, and manufacturing method therefor |
| EP2048257A1 (en) * | 2006-07-31 | 2009-04-15 | National Institute for Materials Science | Free-cutting stainless steel and process for producing the same |
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| Publication number | Publication date |
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| EP2537952B1 (en) | 2016-12-28 |
| JP5713299B2 (en) | 2015-05-07 |
| WO2012014541A1 (en) | 2012-02-02 |
| EP2537952A4 (en) | 2014-05-07 |
| CN102959111B (en) | 2017-07-04 |
| JPWO2012014541A1 (en) | 2013-09-12 |
| EP2537952A1 (en) | 2012-12-26 |
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