WO2011068124A1 - 銅合金板材 - Google Patents
銅合金板材 Download PDFInfo
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- WO2011068124A1 WO2011068124A1 PCT/JP2010/071494 JP2010071494W WO2011068124A1 WO 2011068124 A1 WO2011068124 A1 WO 2011068124A1 JP 2010071494 W JP2010071494 W JP 2010071494W WO 2011068124 A1 WO2011068124 A1 WO 2011068124A1
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- WIPO (PCT)
- Prior art keywords
- copper alloy
- alloy sheet
- rolling
- cold rolling
- treatment
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Classifications
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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
- 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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- 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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- 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
Definitions
- the present invention relates to an excellent copper alloy sheet material, and more particularly to a copper alloy sheet material having excellent strength and bending workability, which is suitable for connection parts such as terminals and connectors for automobiles.
- Corson alloy is an alloy in which the solid solution limit of nickel silicide (Ni 2 Si) to copper changes with temperature, and is a precipitation-hardening alloy that hardens by aging precipitation treatment, and has good heat resistance, conductivity, and strength. .
- Ni 2 Si nickel silicide
- this Corson alloy if the strength of the copper alloy sheet is improved, the conductivity and the bending workability decrease. That is, in a high strength Corson alloy, it is a very difficult problem to have good conductivity and bendability.
- the present inventors confirmed that the shear band generated on the surface of the plate during bending is the cause of the crack. Moreover, although it confirmed that this shear zone could be reduced by accumulating Cube orientation, the problem that tensile strength fell simultaneously was also discovered. The reason for the decrease in strength is considered to be that because the Cube orientation has a small work-hardening coefficient at the time of deformation, deformation occurs at a relatively low strength, and the strength is not sufficiently improved to cause breakage.
- the object of the present invention is to provide a lead frame, connector, terminal material and the like for electric and electronic devices, which is excellent in bending workability and excellent in strength, particularly for automotive vehicles and the like.
- the object of the present invention is to provide a copper alloy sheet material for electric and electronic devices suitable for a connector, a terminal material, a relay, a switch and the like.
- the present inventors have found that by defining the area ratio of crystal orientation grains having a deviation angle within 15 to 30 ° from the Cube orientation within a specific range, it is possible to achieve both excellent bending formability and high strength. .
- the present invention has been completed based on this finding. That is, the present invention is the following means.
- a copper alloy composition containing, by mass%, 0.8 to 5% of either or both of Ni and Co and 0.2 to 1.5% of Si, with the balance being Cu and unavoidable impurities
- the area ratio of crystal grains having a deviation angle of less than 15 ° from the Cube orientation is less than 10%, and the area ratio of crystal grains having a deviation angle of 15 to 30 ° from the Cube orientation is 15% or more.
- Copper alloy sheet material for electric and electronic parts having excellent strength and bendability which is controlled.
- the copper alloy sheet for electric and electronic parts according to (1) further containing 0.05 to 0.5% of Cr.
- the electric / electronic component according to (1) or (2) further containing 0.01 to 1.0% in total of one or more of Zn, Sn, Mg, Ag, Mn and Zr. Copper alloy sheet material.
- the copper alloy sheet material of the present invention has high strength, good bendability, and high conductivity. Moreover, the above-mentioned physical properties of the copper alloy sheet can be further improved by adding another additive element. Furthermore, it is possible to realize improvement in heat-resistant peelability and migration resistance at the time of soldering, and improvement in workability and stress relaxation characteristics at the time of hot rolling.
- copper alloy material means one obtained by processing a copper alloy material into a predetermined shape (e.g., plate, strip, foil, bar, wire, etc.).
- a plate material refers to a plate having a specific thickness, being stable in shape and having a spread in the surface direction, and in a broad sense, it includes a bar material.
- material surface layer means “plate surface layer”
- depth position of material means “position in the plate thickness direction”.
- the thickness of the plate is not particularly limited, but is preferably 8 to 800 ⁇ m, more preferably 50 to 70 ⁇ m, in consideration of the fact that the effects of the present invention are more apparent and suitable for practical applications.
- the copper alloy sheet material of the present invention defines its characteristic by the accumulation ratio of atomic planes in a predetermined direction of the rolled sheet, it is sufficient if it has such a characteristic as a copper alloy sheet material. That is, the shape of the copper alloy sheet is not limited to the sheet and the strip, and in the present invention, the pipe can be interpreted as a sheet and handled.
- the average grain size of the copper alloy sheet material of the present invention is preferably 50 ⁇ m or less.
- the average crystal grain size is equal to or less than the above upper limit value, it is preferable that a shear band causing a crack is hardly generated in bending in both Good Way (GW) bending and Bad Way (BW) bending.
- Good Way means the rolling parallel direction
- Bad Way means the rolling perpendicular direction.
- the crystal grain size was determined by JIS H 0501 (cutting method).
- the texture of the copper alloy sheet material of the present invention is, in particular, measured by the SEM-EBSD method (described later) in order to achieve both strength and bending workability, and the deviation angle (orientation difference) from the Cube orientation is 15 °.
- the area ratio of less than 10 crystal grains is less than 10%, and the area ratio of crystal grains having a deviation angle of 15 to 30 ° from the Cube orientation is 15% or more, preferably 20% or more and less than 50%. It is a thing.
- a copper alloy sheet mainly, as shown below, an aggregate structure called Cube orientation, Goss orientation, Brass orientation, Copper orientation, S orientation, etc. is formed, and a crystal plane corresponding to them is present.
- the formation of these textures differs even in the case of the same crystal system due to differences in processing and heat treatment methods.
- a texture of material such as a plate material by rolling, it is represented by a face and a direction, the face is represented by ⁇ ABC ⁇ , and the direction is represented by ⁇ DEF>.
- the crystal orientation display method in this specification is a material in which the rolling direction (RD) of the material is taken along the X axis, the sheet width direction (TD) is taken along the Y axis, and the rolling normal direction (ND) is taken along the Z axis orthogonal coordinate system.
- RD rolling direction
- TD sheet width direction
- ND rolling normal direction
- Each region in the figure is shown in the form of (hkl) [uvw] using the index (hkl) of the crystal face perpendicular to the Z-axis and the index [uvw] of the crystal direction parallel to the X-axis.
- Cube orientation ⁇ 001 ⁇ ⁇ 100> Goss azimuth ⁇ 011 ⁇ ⁇ 100> Rotated-Goss azimuth ⁇ 011 ⁇ ⁇ 011> Brass orientation ⁇ 011 ⁇ ⁇ 211> Copper azimuth ⁇ 112 ⁇ ⁇ 111> S direction ⁇ 123 ⁇ ⁇ 634> P direction ⁇ 011 ⁇ ⁇ 111>
- the texture of a normal copper alloy sheet consists of a large number of orientation factors.
- the plastic behavior of the material such as the sheet changes, and the workability such as bending etc. Changes.
- the texture of the conventional Corson-based high-strength copper alloy plate material when manufactured by the usual method, S orientation ⁇ 123 ⁇ ⁇ 634> other than Cube orientation ⁇ 001 ⁇ ⁇ 100>, as in the example described later
- the cube orientation ⁇ 011 ⁇ ⁇ 211> is the main component, and the proportion of cube orientation decreases. For this reason, particularly in the BW bending process, a shear band is easily generated and the bending processability is deteriorated.
- the bendability is improved by increasing the accumulation of crystal grains having a displacement angle of less than 15 ° from the Cube orientation, there arises a problem that the strength is lowered.
- the texture of the copper alloy sheet material of the present invention has strength and bendability in which the area ratio of crystal grains having a displacement angle of 15 to 30% from the Cube orientation ⁇ 001 ⁇ ⁇ 100> is 15% or more. It shall have an excellent texture.
- the area ratio of crystal grains having a displacement angle of 15 to 30 ° from the Cube orientation is 15% or more, the presence of other orientations as sub-orientations is acceptable.
- Measurement of the degree of accumulation of oriented grains with a displacement angle of 15 to 30 ° from the Cube orientation ⁇ 001 ⁇ ⁇ 100> of the texture of the copper alloy sheet material is based on data obtained by measuring the electron microscopic structure by SEM using EBSD. It is obtained by conducting orientation analysis using an orientation distribution function (ODF).
- ODF orientation distribution function
- scanning was performed at 0.5 ⁇ m steps to analyze the orientation.
- direction distribution is changing to the thickness direction of material, it is preferable to analyze azimuth
- the SEM-EBSD method is an abbreviation of Scanning Electron Microscopy-Electron Back Scattered Diffraction Pattern method. That is, each crystal grain appearing on a scanning electron microscope (SEM) screen is irradiated with an electron beam, and its crystal orientation is identified from its diffracted electrons.
- SEM scanning electron microscope
- the rotation angle was calculated around the common rotation axis and used as the deviation angle.
- the S orientation (2 3 1) [6-4 3] (1 2 1) [1-1 1] rotates by 19.4 ° with the (20 10 17) direction as the rotation axis. This angle is taken as the offset angle.
- the common axis of rotation adopted what can be expressed by the smallest deviation angle.
- This deviation angle is calculated for all measurement points, and the first decimal place is regarded as an effective number, and the area of each crystal grain having an orientation less than 15 ° and 15 to 30 ° from the Cube orientation is the total measurement area Divide by the area ratio.
- the surface of the substrate was mirror-polished using colloidal silica abrasive grains, and then measurement was performed.
- the features of the EBSD measurement will be described as a comparison with the X-ray diffraction measurement.
- the first point is that X-ray diffraction can be measured by satisfying the Bragg's diffraction conditions and obtaining sufficient diffraction intensity.
- ND // (111), (200), (220 ), (311) and (420) planes, and the deviation angle from the Cube orientation is equivalent to 15 to 30 °, for example, ND // (511) plane or ND // (951) plane
- the crystal orientation expressed by high index can not be measured. That is, by adopting EBSD measurement, information on their orientation can be obtained, and the relationship between the identified alloy structure and the action can be clarified.
- the second point is that while X-ray diffraction measures the amount of crystal orientation included in ⁇ 0.5 ° or so of ND // ⁇ hkl ⁇ , according to EBSD measurement, the Kikuchi pattern is used,
- the information on the alloy structure is comprehensively obtained in an order of magnitude not limited to a specific crystal plane, and a state which becomes difficult to identify by X-ray diffraction as a whole of the alloy material becomes clear.
- the information obtained by EBSD measurement and X-ray diffraction measurement differs in the content and nature thereof.
- the result of EBSD is performed to the ND direction of a copper alloy plate material.
- Ni is an element which is contained together with Si described later, forms an Ni2Si phase precipitated by the aging treatment, and contributes to the improvement of the strength of the copper alloy sheet material.
- Ni2Si phase runs short, and the tensile strength of the copper alloy sheet can not be increased.
- the content of Ni is in the range of 0.5 to 5.0%, preferably 1.5 to 4.0%.
- the content of Co is 0.5 to 5.0%.
- Co is an element which is contained together with Si, forms a Co2Si phase precipitated similarly to Ni by aging treatment, and contributes to the improvement of the strength of the copper alloy sheet material.
- the content of Co is too small, the Co2Si phase runs short, and the tensile strength of the copper alloy sheet can not be increased.
- the content of Co is too large, the conductivity decreases. In addition, the hot rolling processability is deteriorated. Therefore, the content of Co is in the range of 0.5 to 5.0%, preferably 0.8 to 3.0%.
- Ni and Co may contain 0.5 to 5.0% in total.
- both Ni2Si and Co2Si can be precipitated during the aging treatment to enhance the aging strength. If the total content of Ni and Co is too small, the tensile strength can not be increased, and if too large, the conductivity and the hot-rolling processability decrease. Therefore, the total content of Ni and Co is in the range of 0.5 to 5.0%, preferably 0.8 to 4.0%. In particular, when high conductivity is required, it is preferable to make the addition amount of Co larger than the addition amount of Ni.
- Si is contained together with the above-mentioned Ni and Co, forms a Ni2Si or Co2Si phase precipitated by the aging treatment, and contributes to the improvement of the strength of the copper alloy sheet.
- the tensile strength of the copper alloy sheet can be increased, but an excessive amount of Si forms a solid solution in the copper matrix and the conductivity of the copper alloy sheet The rate drops.
- Si is excessively contained, the castability in casting and the rolling process in hot and cold also decrease, and casting cracks and rolling cracks easily occur.
- the precipitated phase of Ni2Si or Co2Si is insufficient, and the tensile strength of the plate can not be increased.
- the copper alloy may contain 0.01 to 0.5% of Cr.
- Cr has the effect of refining the crystal grains in the alloy, and contributes to the improvement of the strength and bending workability of the copper alloy sheet material. When the amount is too small, the effect is not obtained, and when the amount is too large, a crystallized product is formed during casting and the aging strength is reduced.
- the preferred content is 0.05 to 0.3%.
- Sn is an element mainly improving the strength of the copper alloy sheet, and is selectively contained when used for applications in which these properties are emphasized.
- the content of Sn is too small, the strength improvement effect is insufficient.
- the conductivity of the copper alloy sheet tends to decrease.
- the content of Sn is preferably in the range of 0.01 to 1.0%.
- the addition of Zn can improve the heat peelability and migration resistance at the time of soldering. If the content of Zn is too low, the effect is insufficient. On the other hand, when Zn is contained, the conductivity of the copper alloy plate tends to decrease, and when Zn is too large, it becomes difficult to make the conductivity of the copper alloy plate 20% IACS or more. Therefore, the Zn content is preferably in the range of 0.01 to 1.0%.
- the content of Ag contributes to the increase in the strength of the copper alloy sheet. If the content of Ag is too low, the effect is insufficient. On the other hand, excessive addition of Ag is not preferable because the effect is saturated. Therefore, when it is contained, the content of Ag is preferably in the range of 0.01 to 1.0%.
- Mn mainly improves the workability of the alloy in hot rolling. If the content of Mn is too low, the effect is insufficient. On the other hand, when the amount of Mn is too large, the fluidity of the copper alloy during casting deteriorates, and the casting yield decreases. Therefore, when it is contained, the content of Mn is in the range of 0.01 to 1.0%.
- Zr mainly refines crystal grains to improve the strength and bending workability of the copper alloy sheet. If the content of Zr is too low, the effect is insufficient. On the other hand, when the amount of Zr is too large, a compound is formed, and the workability such as rolling of a copper alloy sheet is reduced. Therefore, when it is contained, the content of Zr is in the range of 0.01 to 1.0%.
- Mg improves stress relaxation properties. Therefore, when stress relaxation properties are required, they are selectively contained in the range of 0.01 to 1.0%. If the amount of Mg is too small, the intended effect is insufficient. If the amount of Mg is too large, the conductivity is lowered, which is not preferable.
- the corson alloy sheet material of the present invention includes the following steps: casting, hot rolling, cold rolling 1, intermediate annealing, cold rolling 2, solution heat treatment, cold rolling 3, aging heat treatment, finish cold rolling, and low temperature annealing Manufactured through.
- the method of manufacturing the copper alloy sheet material of the present invention can be manufactured by the same method as that of the conventional Corson alloy. Although it is necessary to limit the manufacturing conditions of each process to the texture, it is preferable to strictly control the conditions of the intermediate annealing and the cold rolling 3 in particular for manufacturing the copper alloy sheet material of the present invention.
- the casting is performed by casting a copper alloy formed molten metal adjusted to the above composition range. Then, the ingot is subjected to facing processing, heated or homogenized heat treatment at 800 to 1000 ° C., and then hot rolled, and the sheet after hot rolling is water cooled. After hot rolling, the surface is chamfered and cold rolling 1 is performed. If the rolling reduction rate of this cold rolling 1 is sufficiently high, then even if the final product is manufactured, the brass orientation and S orientation do not develop too much, and the area ratio with a deviation angle of 15 to 30 ° from the Cube orientation is sufficient Can be raised. Therefore, the rolling reduction rate of the cold rolling 1 is preferably 70% or more.
- the copper alloy material of the present invention is subjected to an intermediate annealing at 300 to 800 ° C. for 5 seconds to 2 hours between cold rolling 1 and solution heat treatment, followed by cold rolling 2 having a rolling reduction of 3 to 80%. It is characterized by adding.
- the intermediate annealing can obtain a partially annealed sub-annealed structure without completely recrystallizing the material.
- microscopic nonuniform strain can be introduced into the material by rolling at a relatively low working ratio.
- a more preferable range of the intermediate annealing is 10 seconds to 1 minute at 400 to 700 ° C., and a further preferable range is 15 seconds to 45 seconds at 500 to 650 ° C.
- a more preferable range of the working ratio of the cold rolling 2 is 5 to 55%, and a further preferable range is 7 to 45%.
- a heat treatment such as the above-mentioned intermediate annealing is performed to recrystallize the material to reduce the strength in order to reduce the load in the rolling in the next step.
- the purpose of rolling is to reduce the plate thickness, and it is general to adopt a processing rate of over 80% if it is the capability of a normal rolling mill.
- the purpose of the intermediate annealing and cold working in the present invention is to give priority to the crystal orientation after recrystallization unlike the general contents.
- the solution treatment is performed at 600 to 1000 ° C. for 5 seconds to 300 seconds. Since the necessary temperature conditions change depending on the concentrations of Ni and Co, it is necessary to select an appropriate temperature condition according to the Ni and Co concentrations.
- the strength is sufficiently maintained in the aging treatment step when the solution treatment temperature is above the lower limit value, and the material is not softened more than necessary when the solution treatment temperature is below the upper limit value, and shape control is preferably realized. . At this time, it is preferable to set the area ratio of crystal grains having a deviation angle of 15 to 30 ° from the Cube orientation to 15 to 50%.
- cold rolling 3 of 5 to 40% is performed.
- the texture is within the scope of the present invention, which is preferable.
- crystal grains with a displacement angle of less than 15 ° from the Cube orientation slightly rotate, and from the Cube orientation Can be integrated at an angle of 15 to 30 °. This is considered to be because in the differential friction rolling, the plastic constraint is different between the upper surface and the lower surface of the rolled material, and the shear deformation is slightly introduced due to the difference in the plastic constraint.
- the difference between the center line average roughness Ra of the upper roll and the lower roll is preferably 0.05 to 3.0 ⁇ m, and more preferably 2.4 to 2.8 ⁇ m.
- the roughness of the roll may be adjusted by roughening the roll with abrasive paper.
- the cold rolling 3 has an effect of increasing the amount of aging precipitation, and also contributes to the improvement of the strength.
- the aging treatment is performed at 400 to 600 ° C. for 0.5 to 8 hours. Since the necessary temperature conditions change depending on the concentrations of Ni and Co, it is necessary to select an appropriate temperature condition according to the Ni and Co concentrations. When the temperature of the aging treatment is equal to or higher than the above lower limit value, the amount of aging precipitation does not decrease and the strength is sufficiently maintained. In addition, when the temperature of the aging treatment is less than or equal to the above upper limit value, the precipitates are not coarsened, and the strength is maintained. It is preferable to set the working ratio of finish cold rolling after solution treatment to 0 to 20% or less.
- the Cube orientation grains may be rotated to the Brass, S and Copper orientation, etc., and the texture may be out of the scope of the present invention. Verification of the characteristic of the copper alloy sheet manufactured by this invention is possible by verification by EBSD analysis whether the structure of the copper alloy sheet is within a specified range.
- the copper alloy of each composition shown in the following Table 1 was cast to manufacture a copper alloy plate, and each characteristic such as strength, conductivity and bendability was evaluated.
- casting was performed by a DC (Direct Chill) method to obtain an ingot having a thickness of 30 mm, a width of 100 mm, and a length of 150 mm.
- these ingots were heated to 900 ° C., held at this temperature for 1 hour, hot-rolled to a thickness of 14 mm, and quickly cooled.
- cold rolling 1 with a rolling ratio of 90 to 98% was applied. Thereafter, heat treatment was performed at 600 to 700 ° C. for 1 hour, and cold rolling 2 was performed at a cold rolling ratio of 5 to 20%.
- solution treatment was performed under various conditions of 700 to 950 ° C., and immediately cooled at a cooling rate of 15 ° C./s or more.
- cold rolling 3 with a rolling ratio of 5 to 40% was applied.
- a roll having a surface roughness Ra difference of 0.05 to 3.0 ⁇ m was used.
- aging was performed at 400 to 600 ° C. for 2 hours, and then finish rolling was performed at a rolling reduction of 20% or less, and the final plate thickness was made 0.15 mm.
- various characteristics were evaluated using a material subjected to a low temperature annealing treatment at 400 ° C. for 30 seconds.
- the structure of the copper alloy plate sample, the area ratio of crystal orientation grains having a displacement angle of less than 15 ° from the Cube orientation, and the area ratio of crystal orientation grains within a displacement angle of 15 to 30 ° were measured by the method described above. These results are shown in the table.
- OIM 5.0 HIKARI manufactured by TSL company was used as an EBSD measuring device.
- each crystal orientation grain of the said copper alloy plate sample (2) tensile strength, (3) electric conductivity, and (4) bendability were evaluated.
- the area ratio of crystal orientation grain shows the area ratio of less than 15 ° of deviation angle from Cube orientation and of 15 to 30 ° of deviation angle of Cube orientation.
- the tensile strength was determined in accordance with JIS Z 2241 using a No. 5 test piece described in JIS Z 2201. The tensile strength is shown by rounding to an integral multiple of 5 MPa.
- the conductivity was determined in accordance with JIS H 0505.
- Examples 1 to 31 of Table 1 show examples of the present invention.
- the texture is within the scope of the present invention, and the strength and bending workability are excellent.
- Table 2 shows a comparative example to the present invention. Comparative Examples 1, 2 and 5 have significantly lower tensile strength because the content of Ni or Co is less than the range specified by the present invention. In Comparative Examples 3, 4, 6, and 7, since the content of Ni or Co was too large, cracking occurred at the time of hot rolling, and the production was stopped.
- Table 3 is an example which investigated the influence which the difference of average roughness Ra of the upper and lower rolling rolls of the cold rolling 3 exerts on the texture using the same ingot as the Example of Table 1.
- the texture of Examples 10-2, 10-3, 22-2, 22-3, 29-2 and 29-3 in Table 3 is within the range of the inventive example, and is excellent in strength and bending workability.
- Comparative Examples 10-2, 22-2, and 29-2 since the difference in Ra is small, the area ratio of less than 15 ° from the Cube orientation is high, and the strength is lowered.
- Comparative Example 101 Condition of JP 2009-007666 A metal element similar to that of the invention example 1-1 was blended, and an alloy composed of Cu and incidental impurities with the balance was melted in a high frequency melting furnace, This was cast at a cooling rate of 0.1 to 100 ° C./sec to obtain an ingot. After holding this at 900 ° C. to 1020 ° C. for 3 minutes to 10 hours, it was hot-worked and then water-quenched to carry out facing for oxide scale removal. In the subsequent steps, a copper alloy c01 was produced by the treatment of steps A-3 and B-3 described below.
- the manufacturing process includes one or more solution heat treatment, in which the steps are classified before and after the last solution heat treatment, and the steps up to intermediate solution treatment are designated as A-3, It was designated as B-3 step in the step after intermediate solution treatment.
- Step A-3 Cold work with a reduction in area of 20% or more, heat treatment for 5 minutes to 10 hours at 350 to 750 ° C., cold work with a reduction in area of 5 to 50%, 800 A solution heat treatment is performed at about 1000 ° C. for 5 seconds to 30 minutes.
- Step B-3 Apply cold working (no differential friction) with a reduction in area of 50% or less, heat treatment at 400 to 700 ° C for 5 minutes to 10 hours, and cold work with a reduction in area of 30% or less And temper annealing at 200 to 550 ° C. for 5 seconds to 10 hours.
- test body c01 was different from the above example in terms of the presence or absence of differential friction rolling with respect to manufacturing conditions, and the result was that the tensile strength did not satisfy the required characteristics.
- Comparative Example 102 Condition of Japanese Patent Application Laid-Open No. 2006-283059
- the copper alloy having the composition of the above-mentioned inventive example 1-1 was dissolved in the atmosphere with an electric furnace under charcoal coating, and the possibility of casting was judged. .
- the molten ingot was hot-rolled and finished to a thickness of 15 mm.
- cold rolling and heat treatment (cold rolling 1 ⁇ solution annealing continuous annealing ⁇ cold rolling 2 (without different friction) ⁇ aging treatment ⁇ cold rolling 3 ⁇ short time annealing) are applied to the hot-rolled material.
- a copper alloy thin plate (c02) of a predetermined thickness was produced.
- test body c02 was different from the above-mentioned Example 1 in terms of production conditions with respect to the presence or absence of intermediate annealing and cold rolling 2 and the presence or absence of differential friction rolling, and resulted in that the bending workability was not satisfied.
- Comparative Example 103 Condition of JP-A-2006-152392 The alloy having the composition of the above-mentioned invention example 1-1 is melted under charcoal covering in the atmosphere in a krypton furnace and cast in a cast iron book mold. Thus, an ingot having a thickness of 50 mm, a width of 75 mm and a length of 180 mm was obtained. Then, after the surface of the ingot was chamfered, it was hot rolled at a temperature of 950 ° C. to a thickness of 15 mm, and quenched into water from a temperature of 750 ° C. or more. Next, after removing the oxide scale, cold rolling was performed to obtain a plate having a predetermined thickness.
- test body c03 was different from the above-mentioned Example 1 in terms of production conditions with respect to the presence or absence of intermediate annealing and cold rolling 2 and the presence or absence of differential friction rolling, and the result was that the bending workability was not satisfied.
- Comparative Example 104 Condition of JP-A-2008-223136 The copper alloy shown in Example 1 was melted and cast using a vertical continuous casting machine. A sample of 50 mm in thickness was cut out from the obtained slab (180 mm in thickness), heated to 950 ° C., extracted, and hot rolling was started. At this time, the pass schedule was set so that the rolling reduction in the temperature range of 950 ° C. to 700 ° C. was 60% or more, and the rolling was performed in the temperature range of less than 700 ° C. The final pass temperature for hot rolling is between 600 ° C and 400 ° C. The total hot-rolling rate from the slab is about 90%. After hot rolling, the surface oxide layer was removed by mechanical polishing (face grinding).
- the aging treatment temperature was set to 450 ° C., and the aging time was adjusted to a time at which the hardness peaked at 450 ° C. aging depending on the alloy composition.
- the optimum solution treatment conditions and aging treatment time are grasped by preliminary experiments according to such alloy composition.
- finish cold rolling was performed at a rolling ratio.
- the final cold-rolled product was further subjected to low-temperature annealing for 5 minutes in a 400 ° C. furnace.
- the test material c04 was obtained.
- the main production conditions are described below.
- the obtained test body c04 was different from the above-mentioned Example 1 in the production conditions under the presence or absence of the intermediate annealing and the cold rolling 2 and the presence or absence of the differential friction rolling, and the result was that the bending workability was not satisfied.
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Abstract
Description
しかし、このコルソン合金においても、銅合金板材の強度を向上させると、導電性や曲げ加工性は低下する。即ち、高強度のコルソン合金において、良好な導電率及び曲げ加工性とすることは非常に困難な問題である。
上記のような問題点に鑑み、本発明の目的は、曲げ加工性に優れ、かつ優れた強度を有し、電気・電子機器用のリードフレーム、コネクタ、端子材等、特に自動車車載用などのコネクタや端子材、リレー、スイッチなどに適した電気・電子機器用銅合金板材を提供することにある。
すなわち、本発明は、以下の手段である。
(1)質量%で、NiまたはCoのいずれか一方または両方を0.8~5%、Siを0.2~1.5%を含有し、残部Cuおよび不可避的不純物からなる銅合金組成よりなる銅合金板材であって、Cube方位からずれ角度15°未満の結晶粒の面積率を10%未満、かつCube方位から15~30°のずれ角度をもつ結晶粒の面積率を15%以上に制御した、優れた強度と曲げ加工性とを有する電気電子部品用銅合金板材。
(2)さらに、Crを0.05~0.5%含有する(1)に記載の電気電子部品用銅合金板材。
(3)さらに、Zn、Sn、Mg、Ag、MnおよびZrのうち1種又は2種以上を合計で0.01~1.0%含有する(1)又は(2)に記載の電気電子部品用銅合金板材。
(4)溶体化処理の後、異摩擦冷間圧延処理が施された(1)~(3)のいずれか1項に記載の電気電子部品用銅合金板材
(5)質量%で、NiまたはCoのいずれか一方または両方を0.8~5%、Siを0.2~1.5%を含有し、残部Cuおよび不可避的不純物からなる銅合金組成よりなる銅合金溶湯を鋳造する工程、加熱または均質化熱処理する工程、異摩擦熱間圧延処理を施す工程、冷間圧延処理を施す工程、中間焼鈍を施す工程、溶体化処理を施す工程、異摩擦冷間圧延処理を施す工程、及び時効処理を施す工程を有する電気電子部品用銅合金板材の製造方法。
(6)前記異摩擦冷間圧延を、上下のロールについて表面粗さが互いに異なるものを用いて行う(5)に記載の電気電子部品用銅合金板材の製造方法。
なお、本発明の銅合金板材は、その特性を圧延板の所定の方向における原子面の集積率で規定するものであるが、これは銅合金板材としてそのような特性を有していれば良いのであって、銅合金板材の形状は板材や条材に限定されるものではなく、本発明では、管材も板材として解釈して取り扱うことができるものとする。
本発明の銅合金板材の平均結晶粒径は50μm以下にすることが好ましい。平均結晶粒径が上記上限値以下である場合、Good Way(GW)曲げ加工、Bad Way (BW)曲げ加工の場合ともに曲げ加工において、割れの原因となるせん断帯が生成しにくく好ましい。ここで、Good Way とは圧延平行方向、Bad Way とは圧延垂直方向を意味する。なお、結晶粒径はJIS H 0501(切断法)により求めた。
本発明の銅合金板材の集合組織は、特に、強度と曲げ加工性を両立するために、SEM-EBSD法(後述する)による測定結果で、Cube方位からのずれ角度(方位差)が15°未満の結晶粒の面積率が10%未満で、かつCube方位からのずれ角度が15~30°の結晶粒の面積率が15%以上、好ましくは20%以上50%未満である集合組織を有するものである。
これらの集合組織の形成は同じ結晶系の場合でも加工、熱処理方法の相違により異なる。圧延による板材などの材料の集合組織の場合は、面と方向で表されており、面は{ABC}で表現され、方向は<DEF>で表現される。本明細書における結晶方位の表示方法は、材料の圧延方向(RD)をX軸、板幅方向(TD)をY軸、圧延法線方向(ND)をZ軸の直角座標系をとり、材料中の各領域がZ軸に垂直な結晶面の指数(hkl)とX軸に平行な結晶方向の指数[uvw]とを用いて(hkl)[uvw]の形で示す。上述の表記に伴い、各方位は下記のように表現される。
Cube方位 {001}<100>
Goss方位 {011}<100>
Rotated-Goss方位 {011}<011>
Brass方位 {011}<211>
Copper方位 {112}<111>
S方位 {123}<634>
P方位 {011}<111>
従来のコルソン系高強度銅合金板材の集合組織は、通常の方法によって製造した場合、後述する実施例の通り、Cube方位{001}<100>以外の、S方位{123}<634>、やBrass方位{011}<211>が主体となり、Cube方位の割合は減少する。このため、特に、BW曲げ加工において、せん断帯が生成し易く曲げ加工性が悪化する。一方、Cube方位からのずれ角度15°未満の結晶粒の集積を高めて曲げ性を改善した場合、強度が低下するという問題が生じる。
EBSD測定にあたっては、鮮明な菊池線回折像を得るために、機械研磨の後に、コロイダルシリカの砥粒を使用して、基体表面を鏡面研磨した後に、測定を行った。
次に、本発明の銅合金板材における化学成分組成の限定理由を説明する(記載の含有量%は全て質量%である)。
Niの含有量は0.5~5.0%とする。Niは後述するSiと共に含有されて、時効処理で析出したNi2Si相を形成して、銅合金板材の強度の向上に寄与する元素である。Niの含有量が少なすぎる場合は、前記Ni2Si相が不足し、銅合金板の引張強さを高めることができない。一方、Niの含有量が多すぎると、導電率が低下し、また、熱間圧延加工性が悪化する。したがって、Niの含有量は0.5~5.0%、好ましくは1.5~4.0%の範囲とする。
この範囲から外れ、Siが各々過剰に含まれた場合、銅合金板材の引張強さを高くすることができるが、過剰な分のSiが銅のマトリックス中に固溶し、銅合金板材の導電率が低下する。また、Siが過剰に含まれた場合、鋳造での鋳造性や、熱間および冷間での圧延加工も低下し、鋳造割れや圧延割れが生じやすくなる。一方、この範囲から外れ、Siの含有量が少な過ぎる場合は、Ni2SiやCo2Siの析出相が不足し板の引張強さを高くすることができない。
上記組成に加えて、銅合金はCrを0.01~0.5%含有してもよい。Crは合金中の結晶粒を微細化する効果があり、銅合金板材の強度や曲げ加工性の向上に寄与する。少なすぎるとその効果はなく、多すぎると鋳造時に晶出物を形成し時効強度が低下する。好ましい含有量は0.05~0.3%である。
次に、本発明の銅合金板材の好ましい製造方法(好ましい実施態様)について以下に説明する。
本発明のコルソン合金板材は、鋳造、熱間圧延、冷間圧延1、中間焼鈍、冷間圧延2、溶体化熱処理、冷間圧延3、時効熱処理、仕上げ冷間圧延、低温焼鈍の各工程を経て製造される。本発明の銅合金板材の製造方法自体は、従来のコルソン合金の場合と同一の方法で製造できる。集合組織には、各工程の製造条件を限定する必要があるが、特に本発明の銅合金板材を製造するには、中間焼鈍と冷間圧延3の条件を厳しく管理することが好ましい。
熱間圧延後、表面を面削し、冷間圧延1を行う。この冷間圧延1の圧延率が十分に高ければ、その後最終製品まで製造してもBrass方位やS方位などが発達しすぎず、Cube方位からのずれ角度が15~30°の面積率を十分に高めることができる。そのため、冷間圧延1の圧延率は70%以上であることが好ましい。
従来、上記中間焼鈍のような熱処理は、次工程の圧延での荷重を低減するために材料を再結晶させて強度を落とすために行われている。また、圧延は板厚を薄くすることが目的であり、通常の圧延機の能力であれば80%を超える加工率を採用するのが一般的である。本発明における中間焼鈍および冷間加工の目的は、これら一般的な内容とは異なり、再結晶後の結晶方位に優先性を持たせるためである。
溶体化処理後の仕上げ冷間圧延の加工率を0~20%以下とするのが好ましい。加工率が高すぎると、Cube方位粒がBrass、SおよびCopper方位などへと方位回転し、集合組織が本発明の範囲外となることがある。
本発明で製造された銅合金板の特性の確認は、銅合金板の組織が規定範囲内であるかどうか、EBSD解析による検証により可能である。
なお、EBSD測定装置として、TSL社製OIM5.0 HIKARIを用いた。
(1)結晶方位粒の面積率は、Cube方位からのズレ角度15°未満の面積率とCube方位からのズレ角度15~30°の面積率を示した。
(2)引張強さはJIS Z 2201記載の5号試験片を用い、JIS Z 2241に準拠して求めた。引張強度は5MPaの整数倍に丸めて示した。
(3)導電率はJIS H 0505に準拠して求めた。
(4)曲げ加工性は曲げ試験片幅wを5mmで行い、曲げR=0~0.6で90°曲げを行い、割れの生じない最小の曲げ半径(R)と板厚(t)の比をR/tとして定義した。
なお、ロールの表面粗さRaはJIS B 0601に準拠して測定した。
上記本発明例1-1と同様の金属元素を配合し、残部がCuと不可避不純物から成る合金を高周波溶解炉により溶解し、これを0.1~100℃/秒の冷却速度で鋳造して鋳塊を得た。これを900~1020℃で3分から10時間の保持後、熱間加工を行った後に水焼き入れを行い、酸化スケール除去のために面削を行った。この後の工程は、次に記載する工程A-3,B-3の処理を施すことによって銅合金c01を製造した。
製造工程には、1回または2回以上の溶体化熱処理を含み、ここでは、その中の最後の溶体化熱処理の前後で工程を分類し、中間溶体化までの工程でA-3工程とし、中間溶体化より後の工程でB-3工程とした。
工程B-3:断面減少率が50%以下の冷間加工(異摩擦なし)を施し、400~700℃で5分~10時間の熱処理を施し、断面減少率が30%以下の冷間加工を施し、200~550℃で5秒~10時間の調質焼鈍を施す。
上記本発明例1-1の組成の銅合金を、電気炉により大気中にて木炭被覆下で溶解し、鋳造可否を判断した。溶製した鋳塊を熱間圧延し、厚さ15mmに仕上げた。つづいてこの熱間圧延材に対し、冷間圧延及び熱処理(冷間圧延1→溶体化連続焼鈍→冷間圧延2(異摩擦なし)→時効処理→冷間圧延3→短時間焼鈍)を施し、所定の厚さの銅合金薄板(c02)を製造した。
上記本発明例1-1の組成をもつ合金について、クリプトル炉において大気中で木炭被覆下で溶解し、鋳鉄製ブックモールドに鋳造し、厚さが50mm、幅が75mm、長さが180mmの鋳塊を得た。そして、鋳塊の表面を面削した後、950℃の温度で厚さが15mmになるまで熱間圧延し、750℃以上の温度から水中に急冷した。次に、酸化スケールを除去した後、冷間圧延を行い、所定の厚さの板を得た。
溶体化処理温度: 900℃
人工時効硬化処理温度×時間: 450℃×4時間
板厚: 0.6mm
実施例1に示す銅合金を溶製し、縦型連続鋳造機を用いて鋳造した。得られた鋳片(厚さ180mm)から厚さ50mmの試料を切り出し、これを950℃に加熱したのち抽出して、熱間圧延を開始した。その際、950℃~700℃の温度域での圧延率が60%以上となり、かつ700℃未満の温度域でも圧延が行われるようにパススケジュールを設定した。熱間圧延の最終パス温度は600℃~400℃の間にある。鋳片からのトータルの熱間圧延率は約90%である。熱間圧延後、表層の酸化層を機械研磨により除去(面削)した。
次いで、冷間圧延を行った後、溶体化処理に供した。試料表面に取り付けた熱電対により溶体化処理時の温度変化をモニターし、昇温過程における100℃から700℃までの昇温時間を求めた。溶体化処理後の平均結晶粒径(双晶境界を結晶粒界とみなさない)が10~60μmとなるように到達温度を合金組成に応じて700~850℃の範囲内で調整し、700~850℃の温度域での保持時間を10sec~10minの範囲で調整した。続いて、上記溶体化処理後の板材に対して、圧延率で中間冷間圧延(異摩擦なし)を施し、次いで時効処理を施した。時効処理温度は材温450℃とし、時効時間は合金組成に応じて450℃の時効で硬さがピークになる時間に調整した。このような合金組成に応じて最適な溶体化処理条件や時効処理時間は予備実験により把握してある。次いで、圧延率で仕上げ冷間圧延を行った。仕上げ冷間圧延を行ったものについては、その後さらに、400℃の炉中に5min装入する低温焼鈍を施した。このようにして供試材c04を得た。なお、必要に応じて途中で面削を行い、供試材の板厚は0.2mmに揃えた。主な製造条件は下記に記載してある。
700℃未満~400℃での熱間圧延率: 56%(1パス)
溶体化処理前 冷間圧延率: 92%
中間冷間圧延 冷間圧延率: 20%
仕上げ冷間圧延 冷間圧延率: 30%
100℃から700℃までの昇温時間: 10秒
Claims (7)
- 質量%で、NiまたはCoのいずれか一方または両方を0.8~5%、Siを0.2~1.5%を含有し、残部Cuおよび不可避的不純物からなる銅合金組成よりなる銅合金板材であって、Cube方位からずれ角度15°未満の結晶粒の面積率を10%未満、かつCube方位から15~30°のずれ角度をもつ結晶粒の面積率を15%以上に制御した、優れた強度と曲げ加工性とを有する電気電子部品用銅合金板材。
- さらに、Crを0.05~0.5%含有する請求項1に記載の電気電子部品用銅合金板材。
- さらに、Zn、Sn、Mg、Ag、MnおよびZrのうち1種又は2種以上を合計で0.01~1.0%含有する請求項1又は2に記載の電気電子部品用銅合金板材。
- 溶体化処理の後、異摩擦冷間圧延処理が施された請求項1~3のいずれか1項に記載の電気電子部品用銅合金板材。
- 請求項1~4の合金板材からなるコネクタ。
- 質量%で、NiまたはCoのいずれか一方または両方を0.8~5%、Siを0.2~1.5%を含有し、残部Cuおよび不可避的不純物からなる銅合金組成よりなる銅合金溶湯を鋳造する工程、加熱または均質化熱処理する工程、異摩擦熱間圧延処理を施す工程、冷間圧延処理を施す工程、中間焼鈍を施す工程、溶体化処理を施す工程、異摩擦冷間圧延処理を施す工程、及び時効処理を施す工程を有する電気電子部品用銅合金板材の製造方法。
- 前記異摩擦冷間圧延を、上下のロールについて表面粗さが互いに異なるものを用いて行う請求項5に記載の電気電子部品用銅合金板材の製造方法。
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KR20120104548A (ko) | 2012-09-21 |
EP2508632A4 (en) | 2013-12-18 |
CN102639732B (zh) | 2017-08-04 |
EP2508632A1 (en) | 2012-10-10 |
CN102639732A (zh) | 2012-08-15 |
KR101419149B1 (ko) | 2014-07-11 |
JPWO2011068124A1 (ja) | 2013-04-18 |
JP4934759B2 (ja) | 2012-05-16 |
EP2508632B1 (en) | 2015-05-20 |
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