CN102639732A - Copper alloy sheet - Google Patents
Copper alloy sheet Download PDFInfo
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- CN102639732A CN102639732A CN201080051566.7A CN201080051566A CN102639732A CN 102639732 A CN102639732 A CN 102639732A CN 201080051566 A CN201080051566 A CN 201080051566A CN 102639732 A CN102639732 A CN 102639732A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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Abstract
Provided is a Corson copper alloy sheet which satisfies property requirements for terminals or connectors, such as strength and bendability. The copper alloy sheet is a copper alloy sheet for electric/electronic components which has a copper alloy composition containing, in terms of mass%, 0.8-5% Ni and/or Co and 0.2-1.5% Si, with the remainder comprising Cu and incidental impurities, wherein the areal proportion of crystal grains deflected at an angle less than 15 from the cube orientation has been regulated so as to be less than 10% and the areal proportion of crystal grains deflected at an angle of 15-30 from the cube orientation has been regulated to 15% or higher. The copper alloy sheet has excellent strength and bendability.
Description
Technical field
The present invention relates to excellent copper alloy plate, particularly be fit to automobile with the intensity of interconnecting piece purposes such as terminal, junctor and the copper alloy plate of excellent in bending workability.
Background technology
In recent years, the miniaturized of electronic machine and light-weighted requirement improve, and miniaturized and lightweight electric, electronic unit constantly develop.The low back of the bodyization of bonder terminal, thin spaceization are developed, consequently, the employed copper alloy plate of these bonder terminals are required to have the higher intensity and the bendability of excellence more.The widely-used at present beryllium copper of copper alloy plate that needs the bendability of HS and excellence, but beryllium copper is very expensive, and metallic beryllium has stronger toxicity.Therefore, the alloy of these materials instead, the usage quantity of corson alloy (Cu-Ni-Si) constantly increases.
Corson alloy is nickel silicide compound (Ni
2Si) alloy that the solid solution limit of copper is changed along with temperature is to separate out through timeliness to handle solidified and separate out the curing alloy, and its thermotolerance, electric conductivity, intensity are good.
But for this corson alloy, if improve the intensity of copper alloy plate, then electroconductibility or bendability reduce.That is, in high-intensity corson alloy, the problem of existence is that it is very difficult having favorable conductive rate and bendability.
To such problem, there is following technology:, improve bendability (for example, with reference to patent documentation 1) through the size of precipitate in the control corson alloy as the high strength copper alloy of excellent in bending workability.In addition, proposed to improve the technology (for example, with reference to patent documentation 2) of intensity, bendability through the crystal particle diameter of control corson alloy.But; For connector material; Particularly will be through carrying out the BW bending machining with the wiggle parallel with rolling direction with test film that plate width direction cuts out abreast, but these materials do not reach intensity, the bendability of market demands, require the further raising of these characteristics.
On the other hand, in recent years, carried out setting up jointly and knitted the trial that improves bendability through control sets.For example, existence is orientated the method (with reference to patent documentation 3) that makes bendability good through control Cube.In addition, also there is the technology (for example, with reference to patent documentation 4) of improving bendability through (200) diffraction intensity that improves X ray.But; According to the inventor's etc. discovery, (200) diffraction intensity that improves Cube orientation or X ray is effective to improving bendability really, but has following problems: if improve these performances; Then the processing during material deformation is solidified coefficient and is diminished, and tensile strength reduces.
The prior art document
Patent documentation
Patent documentation 1: japanese kokai publication hei 6-184680 communique
Patent documentation 2: TOHKEMY 2006-161148 communique
Patent documentation 3: TOHKEMY 2006-152392 communique
Patent documentation 4: TOHKEMY 2009-007666 communique
Summary of the invention
The problem that invention will solve
The inventor etc. study the mechanism in the bending machining of section's gloomy copper nisiloy series copper alloy, results verification the shear zone that the plate surface produces during bending machining be crack reason.In addition, confirmed that this shear zone can reduce through the Cube orientation is assembled, and still, also finds the problem that exists tensile strength to reduce simultaneously.As the reason that this intensity reduces, can think because: because that coefficient is solidified in the processing during distortion is little, so Cube is oriented in than under the low strength and deforms, and can not improve intensity fully, causes rupturing.
In view of the above problems; The objective of the invention is to; A kind of excellent in bending workability is provided; And have excellent intensity, be fit to electric, electronic machine with lead frame, junctor, terminal material etc., particularly electric, the electronic machine of the junctor of suitable automobile mounted purposes etc. and terminal material, rly., switch etc. are used copper alloy plate.
The method of dealing with problems
Discoveries such as the inventor can be defined in the bendability and the HS of coming to realize simultaneously excellence in the specified range through having 15 ~ 30 ° of area occupation ratios with the crystalline orientation grain of interior deviation angle with respect to the Cube orientation.The present invention is based on this discovery and accomplishes.
That is, the present invention provides following scheme.
(1) a kind of copper alloy plate material for electric and electronic components, it has excellent intensity and bendability, and this copper alloy plate comprises copper alloy compositions, and said copper alloy compositions comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities; Wherein, The area occupation ratio that will be lower than 15 ° crystal grain with respect to the deviation angle of Cube orientation is controlled at and is lower than 10%, and will be controlled at more than 15% with respect to the area occupation ratio of crystal grain that the Cube orientation has a deviation angle of 15 ~ 30 °.
(2) above-mentioned (1) described copper alloy plate material for electric and electronic components wherein, also contains 0.05 ~ 0.5% Cr.
(3) above-mentioned (1) or (2) described copper alloy plate material for electric and electronic components wherein, also contain among Zn, Sn, Mg, Ag, Mn and the Zr one or more, and its total amount is 0.01 ~ 1.0%.
(4) each described copper alloy plate material for electric and electronic components in above-mentioned (1) ~ (3), it has implemented different friction (different friction) cold-rolling treatment after the solution processing.
(5) a kind of method of manufacture of copper alloy plate material for electric and electronic components, this method comprises: the operation that molten alloyed copper is cast; Heat or the heat treated operation of homogenizing; Implement different friction hot rolling treatment procedures; Implement the operation of cold-rolling treatment; Implement the operation of process annealing; Implement the solution treatment procedures; Implement different friction cold-rolling treatment operation; And implement the operation of ageing treatment, and said copper alloy metal liquation comprises copper alloy compositions, and said copper alloy compositions comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities.
(6) method of manufacture of above-mentioned (5) described copper alloy plate material for electric and electronic components, wherein, the up-down rollers that the cold rolling use surfaceness of said different friction is different is carried out.
The effect of invention
Copper alloy plate intensity of the present invention is high and have excellent in vending workability, and demonstrates high conductivity.In addition, add element, can also further improve the above-mentioned rerum natura of copper alloy plate through adding other.Processibility when the heat-resisting separability in the time of in addition, can also realizing welding, the raising of resistance to migration, hot rolling and the raising of stress relaxation characteristics.
Embodiment
Down in the face of HS of the present invention and have excellent in vending workability, and the preferred metal structure of the high copper alloy plate material for electric and electronic components of the present invention of electric conductivity is elaborated.At this, " Cu alloy material " is meant the copper alloy raw material is processed into the material to shaped (for example, plate, bar, paper tinsel, rod, line etc.).Wherein, sheet material is meant to have specific thicknesses, dimensionally stable, on the face direction, have the material of width, broadly comprises web.At this, in sheet material, " material surface " is meant " plate top layer ", and " depth location of material " is meant " position of thickness of slab direction ".The thickness of sheet material is not special to be limited, and still, considers more remarkable effect of the present invention, also is fit to practical application, is preferably 8 ~ 800 μ m, more preferably 50 ~ 70 μ m.
In addition; Copper alloy plate of the present invention is stipulated its characteristic with the integrated rate (aggregation rate) of the atomic plane of milled sheet on assigned direction; But; In the present invention; As long as have above-mentioned characteristic as copper alloy plate; The shape of copper alloy plate is not limited to sheet material or web, and tubing also can be used as the sheet material explanation and treats as sheet material.
(median size)
The average crystalline particle diameter of copper alloy plate of the present invention is preferably below the 50 μ m.The average crystalline particle diameter under the situation of any bending machining of Good Way (GW) bending machining, Bad Way (BW) bending machining, all is difficult for becoming the shear zone of crackle reason when above-mentioned higher limit is following, therefore preferred.Here, Good Way is meant rolling parallel direction, and Bad Way is meant rolling vertical direction.In addition, crystal particle diameter is obtained through JIS H0501 (patterning method).
(regulation in the EBSD mensuration)
For the set tissue of copper alloy plate of the present invention; Particularly in order to realize intensity and bendability simultaneously; Need have following set tissue: according to the mensuration result of SEM-EBSD method (following); The area occupation ratio of crystal grain that is lower than 15 ° with respect to the deviation angle (misorientation) of Cube orientation is for being lower than 10%, and is that the area occupation ratio of 15 ~ 30 ° crystal grain is more than 15% with respect to the deviation angle that Cube is orientated, and is preferably more than 20% and is lower than 50%.
Under the situation of copper alloy plate, mainly form the set tissue that is called as Cube orientation, Goss orientation, Brass orientation, Copper orientation, S orientation etc. as follows, and have crystal face corresponding to above-mentioned set tissue.
Even the formation of these set tissues also can be different because of the difference of processing, heat treating method under the situation of the phase isomorphous system.Under the situation by the set tissue of the rolling materials such as sheet material that form, with face and direction indication, face is with { ABC} representes, direction usefulness＜DEF＞expression.The method for expressing of the crystalline orientation in this specification sheets adopts the rolling direction (RD) of material as X axle, plate width direction (TD) as Y axle, rolling normal direction (ND) rectangular coordinate system as the Z axle; Use and the vertical crystal indices of Z axle (hkl) and the indices of crystallographic direction [uvw] parallel with the X axle in each zone in the material, representes with the form of (hkl) [uvw].Be accompanied by above-mentioned notation, the following expression of each orientation.
As stated, the set tissue of common copper alloy plate is made up of considerable orientation factor, and still, if the composition of these crystal faces changes, then the plastic behavior of material such as sheet material changes, and processibilities such as bending also change.
The set of the gloomy copper nisiloy series high strength copper alloy plate of section in the past is organized in situation about making through usual method; As after to state embodiment said; { { { 011} < 211>becomes main body to 001} < 100>S orientation in addition to the Cube orientation, and the ratio of Cube orientation reduces for 123} < 634>and Brass orientation.Therefore, particularly in the BW bending machining, be easy to generate shear zone, the bendability variation.On the other hand, improve under the situation of toughness improving the gathering that deviation angle with respect to the Cube orientation is lower than 15 ° crystal grain, can produce intensity and reduce such problem.
Relative therewith, the set tissue of copper alloy plate of the present invention { deviation angle of 001} < 100>is that the area occupation ratio of 15～30% crystal grain is more than 15%, is the excellent set tissue of intensity and toughness with respect to Cube orientation.Need to prove, in the present invention,, allow other orientation to be orientated existence as secondary as long as be that the area occupation ratio of 15～30 ° crystal grain is 15% or more with respect to the deviation angle of Cube orientation.
The set tissue of copper alloy plate { deviation angle of 001} < 100>is that the concentration class of 15～30 ° orientation grain is measured and obtained through following method: adopt EBSD that the electron microscope tissue based on SEM is measured, and be orientated analysis based on the data that obtain, use crystalline orientation distribution function (ODF) with respect to Cube orientation.At this, to the square sample area of the 1200 μ m that comprise 400 above crystal grain, scan, and orientation is analyzed with 0.5 μ m step-length.Need to prove,, therefore,, and get its MV and obtain preferably through on thickness direction, some distribution of orientations arbitrarily being analyzed because these distribution of orientations change on the thickness direction of material.
This SEM-EBSD method is the abbreviation of Scanning Electron Microscopy-Electron Back Scattered Diffraction Pattern (ESEM-EBSD) method.That is, be each crystal grain irradiating electron beam that manifests on scanning electron microscope (SEM) image, and identify the method for each crystalline orientation by its diffraction electronics.
About deviation angle, be the center calculation rotation angle with the common axis of rotation, as deviation angle with respect to ideal orientation by above-mentioned exponential representation.For example, with respect to S orientation (231) [6-43], (121) [1-11] as turning axle, is the relation of rotating 19.4 ° with (201017) direction, with this angle as deviation angle.The turning axle that common axis of rotation adopts the enough minimum angle of deviation kilsyth basalts of ability to reach.All measuring point is calculated this deviation angle, remain into behind the radix point first, use to have to be lower than 15 °, 15 ~ 30 ° areas with each crystal grain of interior orientation divided by whole mensuration area, as area occupation ratio with respect to the Cube orientation as significant figure.
When carrying out EBSD mensuration, in order to obtain distinct Kikuchi lines diffraction image, after mechanical mill, the abrasive particle of use colloid silica carries out matrix surface measuring after the mirror ultrafinish again.
At this, describe through the characteristic that comparison EBSD is measured with X-ray diffraction mensuration.At first; First that enumerates is: these five kinds in ND//(111), (200), (220), (311), (420) face that having only of can utilizing that the method for X-ray diffraction measures satisfied the Bragg diffraction condition and can be accessed sufficient diffraction intensity, the crystalline orientation of for example being expressed by ND//(511) face, ND//high index such as (951) face that is equivalent to 15 ~ 30 ° with respect to the deviation angle of Cube orientation can not be measured.That is, measure, at first obtain information about their orientation through adopting EBSD, thus, the clear and definite specific alloy structure and the relation of effect.Second is: what X-ray diffraction was measured is ND//{ part of the crystalline orientation that hkl} ± 0.5 ° degree is included; Relative therewith; Because measuring, EBSD utilized the Kikuchi pattern; Therefore can access and enlist the services of the special relevant information of alloy structure widely that is not limited to particular crystal plane, as whole alloy material, it is difficult can clearly adopting X-ray diffraction to stipulate.As stated, measure the content and the different in kind of the information that obtains through EBSD mensuration and X-ray diffraction.In addition, in this manual, short of special instruction, the result of EBSD are that the ND direction of copper alloy plate is carried out.
(alloy composition etc.)
Then, the qualification reason of the chemical ingredients in the copper alloy plate of the present invention being formed (the content % of record is all in quality %) describes.
·Ni、Co、Si
The content of Ni is 0.5 ~ 5.0%.Ni together contains with following Si, is when ageing treatment, to form the Ni that separates out
2The Si phase, thus help to improve the element of copper alloy plate intensity.When the content of Ni is very few, above-mentioned Ni
2Si is not enough mutually, can not improve the tensile strength of copper alloy plate.On the other hand, if the content of Ni is too much, then electric conductivity reduces, in addition, and hot rolling processibility variation.Therefore, the content of Ni is 0.5 ~ 5.0%, is preferably 1.5 ~ 4.0% scope.
The content of Co is 0.5 ~ 5.0%.Co and Si together contain, and are when ageing treatment and Ni likewise forms the Co that separates out
2The Si phase, thus help to improve the element of copper alloy plate intensity.When the content of Co is very few, above-mentioned Co
2Si is not enough mutually, can not improve the tensile strength of copper alloy plate.On the other hand, if the content of Co is too much, then electric conductivity reduces.In addition, hot rolling processibility variation.Therefore, the content of Co is 0.5 ~ 5.0%, is preferably 0.8 ~ 3.0% scope.
Above-mentioned Ni and Co can contain 0.5 ~ 5.0% for two kinds altogether.If contain Ni and Co, then when carrying out ageing treatment, separate out Ni
2Si and Co
2Si both, thereby can improve timeliness intensity.When the total amount of the content of Ni and Co is very few, can not improve tensile strength, if too much, then electric conductivity, hot rolling processibility reduce.Therefore, the total amount of the content of Ni and Co is 0.5 ~ 5.0%, is preferably 0.8 ~ 4.0% scope.Particularly needing under the situation of high conductivity, preferably making the addition of the addition of Co more than Ni.
Si and above-mentioned Ni, Co together contain, and when ageing treatment, form the Ni that separates out
2Si or Co
2The Si phase, thus help to improve the intensity of copper alloy plate.The content of Si is being counted with stoichiometric ratio under the situation of Ni/Si=4.2, Co/Si=4.2, and electric conductivity and intensity balance are best.Therefore, the content of Si is that to make Ni/Si, Co/Si, (Ni+Co)/Si be 3.2 ~ 5.2, is preferably the amount of 3.5 ~ 4.5 scope.
Departing from this scope, excessively contain under the situation of Si respectively, though can improve the tensile strength of copper alloy plate, the Si of excess electron excess fraction solid solution in the matrix of copper, the electric conductivity of copper alloy plate reduces.In addition, under the situation that Si excessively contains, the castibility during casting, hot rolling and the rolling processibility when cold rolling also reduce, and are easy to generate casting crack and rolling crack.On the other hand, departing from this scope, under the very few situation of the content of Si, Ni
2Si and Co
2The precipitated phase of Si is not enough, can not improve the tensile strength of plate.
Other element
Except above-mentioned composition, copper alloy can also contain 0.01 ~ 0.5% Cr.Cr has the effect of the crystal grain miniaturization that makes in the alloy, helps to improve the intensity and the bendability of copper alloy plate.If Cr content is very few, then this effect not if Cr content is too much, forms crystallisate when then casting, and timeliness intensity reduces.Preferred content is 0.05 ~ 0.3%.
For high strength copper alloy sheet material of the present invention; Except above-mentioned essentially consist; As adding element,, can also contain a kind of in following or more than two kinds in quality %; That is, Sn:0.05 ~ 1.0%, Zn:0.01 ~ 1.0%, Ag:0.01 ~ 1.0%, Mn:0.01 ~ 1.0%, Zr:0.1 ~ 1.0%, Mg:0.01 ~ 1.0%.Wherein, contain under the situation more than two kinds, its total amount is 0.01 ~ 1.0%.These elements all are the elements that have as the acting in conjunction effect of any character in the further raising intensity of the main purpose of copper alloy of the present invention and electric conductivity or the bendability.Below, the distinctive action effect of putting down in writing each element and the meaning that contains scope.
Sn is mainly used in the element that improves copper alloy plate intensity, when in the purposes of paying attention to these characteristics, using, optionally contains.If the content of Sn is very few, then its effect that improves intensity is insufficient.On the other hand, if contain Sn, then there is the trend of the electric conductivity reduction of copper alloy plate.If particularly Sn is too much, then being difficult to make the electric conductivity of copper alloy plate is more than the 20%IACS.Therefore, containing under the situation of Sn, the content that preferably makes Sn is 0.01 ~ 1.0% scope.
Through adding Zn, heat-resisting separability and resistance to migration in the time of can improving welding.If the content of Zn is very few, then its effect is insufficient.On the other hand, have the trend of the electric conductivity reduction of copper alloy plate when containing Zn, if Zn is too much, then being difficult to make the electric conductivity of copper alloy plate is more than the 20%IACS.Therefore, preferably making the content of Zn is 0.01 ~ 1.0% scope.
Ag helps to improve the intensity of copper alloy plate.If the content of Ag is very few, then its effect is insufficient.On the other hand, when excessively containing Ag, its effect reaches capacity, and is therefore not preferred.Therefore, containing under the situation of Ag, the content that preferably makes Ag is 0.01 ~ 1.0% scope.
Mn is used to improve the processibility of alloy when hot rolling.If the content of Mn is very few, then its effect is insufficient.On the other hand, if Mn is too much, the mobile variation of the liquation when then copper alloy is cast, qualified casting reduces.Therefore, containing under the situation of Mn, the content that makes Mn is 0.01 ~ 1.0% scope.
Zr mainly makes the crystal grain miniaturization, thereby improves the intensity and the bendability of copper alloy plate.If the content of Zr is very few, then its effect is insufficient.On the other hand, if Zr is too much, then form compound, the processibility of the rolling grade of copper alloy plate reduces.Therefore, containing under the situation of Zr, the content that makes Zr is 0.01 ~ 1.0% scope.
Mg is used to improve stress relaxation characteristics.Therefore, needing under the situation of stress relaxation characteristics, the scope 0.01 ~ 1.0% optionally contains.If Mg is very few, then insufficient as the effect of target, when Mg is too much, can cause the drawback that electric conductivity reduces, therefore not preferred.
(method of manufacture etc.)
Then, below the preferable production process (preferred implementation) of copper alloy plate of the present invention is described.
Corson alloy sheet material of the present invention through casting, hot rolling, cold rolling 1, process annealing, cold rolling 2, the solution heat-transmission is handled, cold rolling 3, timeliness thermal treatment, pinch pass, stress relief annealed each operation are made.The method of manufacture of copper alloy plate of the present invention itself can through with the identical method manufacturing of situation of in the past corson alloy.For set tissue, need to limit creating conditions of each operation, particularly in order to make copper alloy plate of the present invention, preferred stringent regulations process annealing and cold rolling 3 condition.
In this embodiment, casting is that the copper alloy metal liquation that composition is adjusted to behind the above-mentioned compositing range is cast.Then, ingot bar carried out face cutting after, under 800 ~ 1000 ℃, heat or homogenizing thermal treatment, carry out hot rolling then, and the plate after the hot rolling carried out water-cooled.
After the hot rolling, the face cutting is carried out on the surface, carried out cold rolling 1 then.If this rolling rate of cold rolling 1 is fully high, then thereafter up to producing the finished product, Brass orientation and S orientation wait and also can too not develop, and can fully improve the deviation angle that is orientated with respect to Cube and be 15 ~ 30 ° area occupation ratio.Therefore, cold rolling 1 rolling rate is preferably more than 70%.
Cu alloy material of the present invention is characterised in that, cold rolling 1 with between the solution heat-transmission handles, under 300 ~ 800 ℃, carries out after the process annealing of 5 second ~ 2 hour, apply rolling rate and be 3 ~ 80% cold rolling 2.Process annealing does not make material perfect recrystallization through to heat-treat than the low temperature of solution heat-transmission treatment temp, thereby can access the inferior annealed structure that the part recrystallize has taken place.In cold rolling 2,, can in material, import uneven strain on the microcosmic through hanging down the rolling of working modulus.Through the effect of above-mentioned two operations, in the recrystallize set tissue after the solution heat-transmission is handled, can access the crystalline orientation of expectation.The preferred scope of process annealing is for carrying out 10 second ~ 1 minute under 400 ~ 700 ℃, special preferred range is for carrying out for 15 second ~ 45 seconds under 500 ~ 650 ℃.The preferred scope of cold rolling 2 working modulus is 5 ~ 55%, and further preferred range is 7 ~ 45%.
In the past, the such thermal treatment of above-mentioned process annealing was in order to make the material recrystallize, to reduce intensity and carry out, and reduced the load in subsequent handling rolling thus.In addition, rolling purpose is to reduce thickness of slab, if be the ability of common rolls, then adopts usually to surpass 80% working modulus.Process annealing among the present invention and cold worked purpose are different with these common contents, are used to make the crystalline orientation behind the recrystallize to have property according to qualifications.
In this embodiment, the solution processing carried out for 5 second ~ 300 seconds under 600 ~ 1000 ℃.Concentration according to Ni and Co is different, and necessary temperature condition changes, and therefore need select suitable temperature condition according to Ni, Co concentration.If the solution temperature is more than the above-mentioned lower value, then in ageing treatment process, can fully keep intensity, if the solution temperature is below the above-mentioned higher limit, then material can not soften to more than the necessary degree, can suitably realize shape control, and is therefore preferred.At this moment, preferably making deviation angle with respect to Cube orientation is that the area occupation ratio of 15 ~ 30 ° crystal grain is 15 ~ 50%.
After the solution processing, carry out 5 ~ 40% cold rolling 3.Carrying out this when cold rolling, if implement the cold rolling of this working modulus, then set is organized within the scope of the invention, and is therefore preferred.Discovery according to inventor etc.; If it is rolling to implement different friction through the different roller of the roughness of cold roll; Then be lower than 15 ° crystal grain with respect to the deviation angle of Cube orientation and carry out small orientation rotation, can make orientation concentrate on deviation angle with respect to the Cube orientation is on 15 ~ 30 ° the orientation.Can think this be because, in different friction was rolling, rolling stock was different with following its plasticity constraint in the above, because the difference that this plasticity retrains can import small shearing strain.At this, the difference of the center line average roughness Ra of preferred top roll and lower roll is 0.05 ~ 3.0 μ m, more preferably 2.4 ~ 2.8 μ m.The roughness of roller can regulate the roller roughening through utilizing pouncing paper.Cold rolling 3 have the effect that increases the timeliness amount of separating out, and also help to improve intensity.
Ageing treatment is carried out 8 hours scope of 0.5 h ~ under 400 ~ 600 ℃.Concentration according to Ni and Co is different, and necessary temperature condition changes, and therefore, is necessary to select suitable temperature condition according to Ni, Co concentration.The temperature of ageing treatment is above-mentioned lower value when above, and the timeliness amount of separating out can not reduce, and can fully keep intensity.In addition, the temperature of ageing treatment is above-mentioned higher limit when following, and precipitate can not thickization, can keep intensity.
Preferably making the working modulus of the pinch pass after the solution processing is below 0 ~ 20%.If working modulus is too high, then Cube orientation grain is orientated rotation to Brass, S and Copper orientation etc., and set is organized in outside the scope of the present invention.
The characteristic of the copper alloy plate of manufacturing of the present invention is approved with whether organizing in specialized range, utilize EBSD to analyze the checking of carrying out to carry out through copper alloy plate really.
Embodiment
Below, based on embodiment further explain the present invention, but the present invention is not limited to these embodiment.
Below, embodiments of the invention are described.Each copper alloy of forming shown in the below table 1 is cast, the manufactured copper alloy sheets, and each characteristic such as its intensity, electric conductivity, toughness estimated.
At first, cast, obtain the ingot bar of thick 30mm, wide 100mm, long 150mm through DC (Direct Chill, directly cold shock) method.Then, these ingot bars are heated to 900 ℃, after this temperature keeps 1 hour, are rolled into thickness 14mm, and cooling rapidly.Then, the face cutting of 1mm has been carried out on the two sides respectively, remove the deoxidation overlay film after, implement rolling rate and be 90 ~ 98% cold rolling 1.Then, under 600 ~ 700 ℃, carry out 1 hour thermal treatment, implement cold rolling 2 with 5 ~ 20% cold rolling rate.Then, under 700 ~ 950 ℃ various conditions, carry out the solution processing, cool off with the speed of cooling more than 15 ℃/second immediately.Then, implement rolling rate be 5 ~ 40% cold rolling 3.At this moment, using the difference of the surface roughness Ra of up-down rollers is the roller of 0.05 ~ 3.0 μ m.Then, in the non-active gas environment, 400 ~ 600 ℃ of ageing treatment of implementing 2 hours down, the rate that is rolled then is the finish rolling below 20%, makes the regular 0.15mm of being of final thickness of slab.After the finish rolling, the material to after handling in the low-temperature annealing of implementing for 30 seconds under 400 ℃ carries out the various characteristics evaluation.
For the copper alloy plate of such manufacturing, each example all Use Limitation is handled the back by the test portion that copper alloy plate cuts out, and has implemented test as follows and evaluation.
Is that 15 ~ 30 ° of area occupation ratios with interior crystalline orientation grain are measured through aforesaid method to the tissue of copper alloy plate test portion, the area occupation ratio and the deviation angle that are lower than 15 ° crystalline orientation grain with respect to the deviation angle of Cube orientation.It is as shown in the table for these results.
Need to prove,, used the OIM5.0HIKARI of TSL manufactured as the EBSD determinator.
In addition, area occupation ratio, (2) tensile strength, (3) electric conductivity, (4) toughness of (1) each crystalline orientation grain of above-mentioned copper alloy plate test portion are estimated.
(1) for the area occupation ratio of crystalline orientation grain, shows that deviation angle with respect to Cube orientation is lower than 15 ° area occupation ratio and be 15 ~ 30 ° area occupation ratio with respect to the deviation angle of Cube orientation.
(2) tensile strength is used No. 5 test films of record among the JIS Z 2201, obtains based on JIS Z 2241 standards.Tensile strength is rounding to the integral multiple of 5MPa, representes.
(3) electric conductivity is obtained based on JIS H 0505 standard.
(4) for bendability, be that 90 ° of bendings are carried out in 5mm, curvature R=0 ~ 0.6 with pliability test sheet width w, the ratio of minimum profile curvature radius that does not crack (R) and thickness of slab (t) is defined as R/t.
Embodiments of the invention shown in the embodiment 1 ~ 31 of table 1.The set of embodiment 1 ~ 31 is organized within the scope of the invention, its intensity, excellent in bending workability.
Shown in the table 2 is with respect to comparative example of the present invention.The Ni of comparative example 1,2,5 or the content of Co lack than the scope of the present invention's regulation, so tensile strength is obviously lower.The Ni of comparative example 3,4,6,7 or the content of Co are too much, so have produced crackle during hot rolling, so ended manufacturing.
Table 3 is to use the ingot bar identical with the embodiment of table 1, the example that the influence that the difference pair set tissue of the average roughness Ra of the top and bottom rolls to cold rolling 3 brings is studied.The set of the embodiment 10-2 of table 3,10-3,22-2,22-3,29-2,29-3 is organized in the scope of the present invention's example, its intensity and excellent in bending workability.On the other hand, the difference of the Ra of comparative example 10-2,22-2,29-2 is little, therefore is lower than 15 ° area occupation ratio height with respect to the deviation angle of Cube orientation, and intensity reduces.In addition, the difference of the Ra of comparative example 10-3,22-3,29-3 is big, and therefore 15 ° ~ 30 ° of deviation angles with respect to the Cube orientation are lower with interior area occupation ratio, and bendability reduces.
In addition, the surface roughness Ra of roller is measured based on JIS B 0601 standard.
[table 1]
| No. | Ni | Co | Si | Cr | Other | Area occupation ratio 1 ※ 1 | Area occupation ratio 2 ※ 2 | Electric conductivity | Tensile strength (MPa) | R/t | |
| Embodiment | 1 | 1.5 | 0.4 | Mg：0.1 | 5 | 18 | 44 | ?740 | 0.33 | ||
| Embodiment | 2 | 2.3 | 0.5 | 7 | 15 | 42 | ?850 | 0.67 | |||
| Embodiment | 3 | 2.3 | 0.5 | 0.3 | 8 | 20 | 41 | ?870 | 0.67 | ||
| Embodiment | 4 | 2.3 | 0.5 | 0.1 | 6 | 19 | 42 | ?865 | 0.67 | ||
| Embodiment | 5 | 2.3 | 0.5 | 0.1 | Mg：0.1.Sn：0.1.Zn：0.5 | 9 | 31 | 39 | ?875 | 0.67 | |
| Embodiment | 6 | 2.3 | 0.5 | Mg：0.1.Sn：0.1 | 8 | 28 | 42 | ?860 | 0.67 | ||
| Embodiment | 7 | 2.3 | 0.5 | Ag：0.1 | 6 | 22 | 43 | ?855 | 0.67 | ||
| Embodiment | 8 | 2.3 | 0.5 | Mn：0.1 | 7 | 23 | 40 | ?860 | 0.67 | ||
| Embodiment | 9 | 2.3 | 0.5 | Zr：0.1 | 7 | 22 | 40 | ?860 | 0.67 | ||
| Embodiment | 10 | 3.8 | 0.9 | 0.1 | 7 | 23 | 38 | ?900 | 1 | ||
| Embodiment | 11 | 3.8 | 0.9 | 0.1 | Mg：0.1.Sn：0.1.Zn：0.5 | 5 | 24 | 36 | ?910 | 1 | |
| Embodiment | 12 | 3.8 | 0.9 | Sn：0.1 | 4 | 19 | 37 | ?900 | 1 | ||
| Embodiment | 13 | 3.8 | 0.9 | 0.2 | 8 | 27 | 37 | ?920 | 1 | ||
| Embodiment | 14 | 4.9 | 1.2 | Mg：0.1 | 8 | 17 | 33 | ?935 | 1.5 | ||
| Embodiment | 15 | 4.9 | 1.2 | 8 | 25 | 34 | ?930 | 1.5 | |||
| Embodiment | 16 | 4.9 | 1.2 | Mg：0.1.Sn：0.1.Zn：0.5 | 7 | 19 | 31 | ?940 | 1.5 | ||
| Embodiment | 17 | 1.2 | 1.2 | 0.6 | Mg：0.1 | 6 | 17 | 50 | ?870 | 0.67 | |
| Embodiment | 18 | 1.3 | 0.8 | 0.5 | Mg：0.1.Sn：0.1.Zn：0.5 | 8 | 16 | 51 | ?860 | 0.67 | |
| Embodiment | 19 | 1.3 | 0.8 | 0.5 | Ag：0.1 | 8 | 22 | 52 | ?860 | 0.67 | |
| Embodiment | 20 | 1.3 | 0.8 | 0.5 | Mn：0.1 | 6 | 24 | 49 | ?865 | 0.67 | |
| Embodiment | 21 | 1.3 | 0.8 | 0.5 | Zr：0.1 | 9 | 25 | 49 | ?865 | 0.67 | |
| Embodiment | 22 | 1.3 | 0.8 | 0.5 | 5 | 21 | 50 | ?840 | 0.67 | ||
| Embodiment | 23 | 2.1 | 0.7 | 0.7 | 0.1 | 7 | 27 | 47 | ?880 | 1 | |
| Embodiment | 24 | 2.4 | 1.2 | 0.9 | 8 | 40 | 42 | ?900 | 1 | ||
| Embodiment | 25 | 0.8 | 2.6 | 0.8 | 7 | 19 | 41 | ?880 | 1 | ||
| Embodiment | 26 | 0.6 | 2.8 | 0.8 | 8 | 26 | 62 | ?890 | 1 | ||
| Embodiment | 27 | 0.8 | 0.2 | Mg：0.1 | 7 | 18 | 60 | ?680 | 0 | ||
| Embodiment | 28 | 1.4 | 0.3 | Mg：0.1 | 4 | 20 | 55 | ?780 | 0.5 | ||
| Embodiment | 29 | 2.3 | 0.5 | 8 | 16 | 55 | ?860 | 0.67 | |||
| Embodiment | 30 | 3.1 | 0.7 | Mg：0.1.Sn：0.1.Zn：0.5 | 9 | 19 | 45 | ?870 | 1 | ||
| Embodiment | 31 | 3.6 | 0.9 | Ag0.1 | 6 | 20 | 55 | ?890 | 1 |
※ 2: the deviation angle with respect to the Cube orientation is lower than 15 ° area occupation ratio
※ 3: the area occupation ratio that with respect to the deviation angle of Cube orientation is 15～30 °
[table 2]
[table 3]
Then, for the copper alloy plate of creating conditions and making through in the past, the copper alloy plate of inventing for clear and definite and the application different are made copper alloy plate under its condition, and have carried out the evaluation with above-mentioned same characteristic project.In addition, the short of special instruction of the thickness of each sheet material is adjusted working modulus with the mode of thickness same as the previously described embodiments.The condition of following example all is creating conditions usually when considering that the application files an application, and does not adopt different friction rolling in cold rolling after solutionization.
(comparative example 101) ... The condition of TOHKEMY 2009-007666 communique
Adopt high-frequency melting furnace to fuse, cast this alloy, obtain ingot bar with 0.1 ~ 100 ℃/second speed of cooling to being combined with the alloy of forming by Cu and unavoidable impurities with same metallic element of the invention described above example 1-1 and surplus.It after keeping 3 minutes to 10 hours under 900 ~ 1020 ℃, is carried out hot-work, carry out shrend then, carry out surfacing again to remove the deoxidation rust deposite.Thereafter operation is to have made copper alloy c01 through the processing of implementing following operation A-3, B-3.
Comprise above once or twice solution heat-transmission processing in the manufacturing process; At this; Operation is classified in front and back so that last solution heat-transmission is wherein handled, will arrive middle solution and turn to operation only as the A-3 operation, and the operation that middle solutionization is later is as the B-3 operation.
Operation A-3: implementing the cross section decrement is the cold working 20% or more, 350 ~ 750 ℃ of thermal treatments of implementing 5 minutes ~ 10 hours down, implements the cross section decrement and be 5 ~ 50% cold working, 800 ~ 1000 ℃ of solution heat-transmission processing of implementing 5 second ~ 30 minute down.
Process B-3: implementing the cross section decrement is the cold working (being as good as friction) below 50%; 400 ~ 700 ℃ of thermal treatments of implementing 5 minutes ~ 10 hours down; Implementing the cross section decrement is the cold working 30% below, 200 ~ 550 ℃ of modified annealing of enforcement 5 second ~ 10 hour down.
The test body c01 that obtains and the foregoing description being as good as on the rolling this point of friction in creating conditions is different, is the do not meet the demands result of characteristic of tensile strength.
(comparative example 102) ... The condition of TOHKEMY 2006-283059 communique
Adopt electric furnace with the copper alloy of the composition of the invention described above example 1-1 in atmosphere, under charcoal coats, fuse, judgement could be cast.Ingot bar after the hot rolling melting, finish rolling become thickness 15mm.Then, implement cold rolling and thermal treatment (cold rolling 1 → solution continuous annealing → cold rolling 2 (being as good as friction) → ageing treatment → cold rolling 3 → short period of time annealing) to this hot-finished material, manufacturing has the copper alloy thin plate (c02) of given thickness.
The test body c02 that obtains and the foregoing description 1 have or not process annealing and cold rolling 2 and be as good as in rolling these 2 of the friction differently in creating conditions, be the result who does not satisfy bendability.
(comparative example 103) ... The condition of TOHKEMY 2006-152392 communique
In cryptol furnace, will have alloy that the invention described above example 1-1 forms in atmosphere, charcoal fuses under coating, and is cast as the cast iron book mold, obtains the ingot bar of thick 50mm, wide 75mm, long 180mm.And, surfacing is carried out on the surface of ingot bar, under 950 ℃ temperature, be rolled into thickness 15mm then, from the quenching water of the temperature more than 750 ℃.Then, remove the deoxidation rust deposite after, carry out cold rollingly, obtain the plate of given thickness.
Then, the use molten salt furnace after the quenching, through latter half of pinch pass (being as good as friction), is processed the cold-reduced sheet of each thickness after having carried out under temperature, heating the solution processing in 20 seconds in water.At this moment, as follows, these cold rolling working moduluses (%) are carried out various changes, process cold-reduced sheet (c03).As followsly to the temperature of these cold-reduced sheets (℃) and the time (hr) carry out various changes, carried out ageing treatment.
The test body c03 that obtains and the foregoing description 1 have or not process annealing and cold rolling 2 and be as good as in rolling these 2 of the friction differently in creating conditions, be the result who does not satisfy bendability.
(comparative example 104) ... The condition of TOHKEMY 2008-223136 communique
Copper alloy to shown in the embodiment 1 carries out melting, and uses vertical continuous casting machine to cast.Cut out the test portion of thickness 50mm by the casting sheet that obtains (thickness 180mm), take out after being heated 950 ℃, begin to carry out hot rolling.At this moment, be to set the passage programsheet more than 60% and being lower than the mode that also is rolled under 700 ℃ the temperature province with the rolling rate under 950 ℃ ~ 700 ℃ the temperature province.The final passage temperature of hot rolled is between 600 ℃ ~ 400 ℃.Total hot rolling rate of casting sheet is about 90%.After the hot rolling, remove the zone of oxidation on (surfacing) top layer through mechanical mill.
Then, carry out cold rollingly, offer the solution processing then.Temperature variation when keeping watch on the solution processing through the thermopair that is installed on specimen surface is obtained in the temperature-rise period TRT from 100 ℃ to 700 ℃.In 700 ~ 850 ℃ scope, adjust the arrival temperature according to alloy composition; Make that the average crystalline particle diameter (twin boundary not being regarded as crystal boundary) after the solution processing is 10 ~ 60 μ m, be adjusted at the hold-time under 700 ~ 850 ℃ the temperature province in the scope of 10 second ~ 10 minute.Then, the sheet material after the above-mentioned solution processing is implemented middle cold rolling (being as good as friction) with rolling rate, implement ageing treatment then.Aging temperature is 450 ℃ of material temperature, for aging time, is adjusted into according to alloy composition that hardness is the time of peak value under 450 ℃ the timeliness.According to such alloy composition, hold best solution treatment condition and timeliness treatment time through preliminary experiment.Then, carry out pinch pass with rolling rate.Then for the test portion that carries out after the pinch pass, 5 minutes low-temperature annealing in 400 ℃ the stove of further implementing again to pack into.Obtain supplying examination material c04 thus.Need to prove, as required, carry out surfacing halfway, make to supply the thickness of slab of examination material neat, be 0.2mm.Main creating conditions is described below.
[condition of TOHKEMY 2008-223136 embodiment 1]
Be lower than the hot rolling rate under 700 ℃ ~ 400 ℃: 56% (a time)
Cold rolling rate before the solution processing: 92%
Middle cold rolling rate: 20%
The cold rolling rate of pinch pass: 30%
From 100 ℃ to 700 ℃ TRT: 10 seconds
The test body c04 that obtains and the foregoing description 1 have or not process annealing and cold rolling 2 and be as good as on rolling this aspect of friction differently in creating conditions, be the result who does not satisfy bendability.
Claims (according to the modification of the 19th of treaty)
1. copper alloy plate material for electric and electronic components, it has excellent intensity and bendability, and this copper alloy plate comprises the copper alloy composition, and said copper alloy composition comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities; Wherein, The area occupation ratio that will be lower than 15 ° crystal grain with respect to the deviation angle of Cube orientation is controlled at and is lower than 10%, and will be controlled at more than 15% with respect to the area occupation ratio of crystal grain that the Cube orientation has a deviation angle of 15 ~ 30 °.
2. copper alloy plate material for electric and electronic components according to claim 1 wherein, also contains 0.05 ~ 0.5% Cr.
3. copper alloy plate material for electric and electronic components according to claim 1 and 2 wherein, also contains among Zn, Sn, Mg, Ag, Mn and the Zr one or more, and its total amount is 0.01 ~ 1.0%.
4. according to each described copper alloy plate material for electric and electronic components in the claim 1 ~ 3, it has implemented different friction cold-rolling treatment after the solution processing.
5. junctor, it is processed by each sheet alloy in the claim 1 ~ 4.
6. the method for manufacture of a copper alloy plate material for electric and electronic components, it is a method of making following copper alloy plate, and said copper alloy plate comprises the copper alloy composition, and said copper alloy composition comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities, in the method, carries out following operation successively:
Composition is adjusted into the operation that the molten alloyed copper of above-mentioned compositing range is cast;
After ingot bar carried out face cutting, heat or homogenizing thermal treatment, carry out hot rolling then, and the plate after the hot rolling is carried out the operation of water-cooled at 800 ~ 1000 ℃;
After the hot rolling, the face cutting is carried out on the surface, and carried out cold rolling 1 operation more than 70% with rolling rate;
Cold rolling 1 and the solution processing between, 300 ~ 800 ℃ of process annealings of carrying out 5 second ~ 2 hour, be rolled cold rolling 2 operation of rate 3 ~ 80% then;
600 ~ 1000 ℃ of solution treatment procedures of carrying out for 5 second ~ 300 seconds; And
After the solution processing, it is rolling that the difference of utilizing the center line average roughness Ra of top roll and lower roll is that the roller of 0.05 ~ 3.0 μ m carries out different friction, as the cold rolling operation of working modulus 5 ~ 40%.
Explain or state (according to the modification of the 19th of treaty)
Below appended content be content according to the 19th modification of PCT treaty, international office is accepted the modification of this claim on May 6th, 2011.
The 1st ~ 6 of claims so that portion is new are replaced the 1st ~ 7 of original right requirement book.
Specification sheets based on treaty the 19th (1)
1. claim 5
Corrected the misdescription of pointing out in the opinion book of international survey mechanism.
2. claim 6
The content that adds claim 7, in addition, clear and definite each manufacturing process that points out in the opinion book of international survey mechanism.
Claims (7)
1. copper alloy plate material for electric and electronic components, it has excellent intensity and bendability, and this copper alloy plate comprises copper alloy compositions, and said copper alloy compositions comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities; Wherein, The area occupation ratio that will be lower than 15 ° crystal grain with respect to the deviation angle of Cube orientation is controlled at and is lower than 10%, and will be controlled at more than 15% with respect to the area occupation ratio of crystal grain that the Cube orientation has a deviation angle of 15 ~ 30 °.
2. copper alloy plate material for electric and electronic components according to claim 1 wherein, also contains 0.05 ~ 0.5% Cr.
3. copper alloy plate material for electric and electronic components according to claim 1 and 2 wherein, also contains among Zn, Sn, Mg, Ag, Mn and the Zr one or more, and its total amount is 0.01 ~ 1.0%.
4. according to each described copper alloy plate material for electric and electronic components in the claim 1 ~ 3, it has implemented different friction cold-rolling treatment after the solution processing.
5. junctor, its sheet alloy by claim 1 ~ 4 is processed.
6. the method for manufacture of a copper alloy plate material for electric and electronic components, this method comprises: the operation that molten alloyed copper is cast; Heat or the heat treated operation of homogenizing; Implement different friction hot rolling treatment procedures; Implement the operation of cold-rolling treatment; Implement the operation of process annealing; Implement the solution treatment procedures; Implement different friction cold-rolling treatment operation; And implement the operation of ageing treatment, and said copper alloy metal liquation comprises copper alloy compositions, and said copper alloy compositions comprises in quality %: any or two kinds among 0.8 ~ 5% Ni or the Co; 0.2 ~ 1.5% Si; Surplus is Cu and unavoidable impurities.
7. the method for manufacture of copper alloy plate material for electric and electronic components according to claim 5, wherein, the up-down rollers that the cold rolling use surfaceness of said different friction is different is carried out.
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| CN108149062A (en) * | 2018-02-10 | 2018-06-12 | 中南大学 | A kind of strong high conductive copper alloy of superelevation and preparation method thereof |
| CN108149062B (en) * | 2018-02-10 | 2019-09-20 | 中南大学 | A kind of strong high conductive copper alloy of superelevation and preparation method thereof |
| CN111500893A (en) * | 2020-06-10 | 2020-08-07 | 铜陵高铜科技有限公司 | Ultrahigh-strength copper alloy plate strip and manufacturing method thereof |
| CN111647768A (en) * | 2020-06-10 | 2020-09-11 | 铜陵高铜科技有限公司 | High-strength copper alloy sheet and method for producing same |
| CN114855026A (en) * | 2022-03-25 | 2022-08-05 | 宁波博威合金材料股份有限公司 | High-performance precipitation strengthening type copper alloy and preparation method thereof |
| CN114855026B (en) * | 2022-03-25 | 2023-02-14 | 宁波博威合金材料股份有限公司 | High-performance precipitation strengthening type copper alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20120104548A (en) | 2012-09-21 |
| EP2508632A4 (en) | 2013-12-18 |
| WO2011068124A1 (en) | 2011-06-09 |
| CN102639732B (en) | 2017-08-04 |
| EP2508632A1 (en) | 2012-10-10 |
| KR101419149B1 (en) | 2014-07-11 |
| JPWO2011068124A1 (en) | 2013-04-18 |
| JP4934759B2 (en) | 2012-05-16 |
| EP2508632B1 (en) | 2015-05-20 |
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