EP2706125A1 - Matériau de feuille en alliage de cuivre et son procédé de production - Google Patents

Matériau de feuille en alliage de cuivre et son procédé de production Download PDF

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Publication number
EP2706125A1
EP2706125A1 EP12779988.0A EP12779988A EP2706125A1 EP 2706125 A1 EP2706125 A1 EP 2706125A1 EP 12779988 A EP12779988 A EP 12779988A EP 2706125 A1 EP2706125 A1 EP 2706125A1
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Prior art keywords
rolling
mass
copper alloy
orientation
grains
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EP12779988.0A
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German (de)
English (en)
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EP2706125A4 (fr
Inventor
Takemi ISOMATSU
Hiroshi Kaneko
Koji Sato
Tatsuhiko Eguchi
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Furukawa Electric Co Ltd
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Furukawa Electric Co Ltd
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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
    • 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
    • C22C9/10—Alloys based on copper with silicon as the next major constituent
    • 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
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • 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
    • 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
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/02—Single bars, rods, wires, or strips

Definitions

  • the present invention relates to a copper alloy sheet material and a method of producing the same, which can be applied, for example, to lead frames, connectors, terminal materials, relays, switches, sockets, and the like, for electrical or electronic equipments.
  • Characteristics required for copper alloy materials that are used in applications for electrical or electronic equipments include, for example, electrical conductivity, proof stress (yield stress), tensile strength, bending property, and stress relaxation resistance.
  • the demanded levels for the characteristics become higher, concomitantly with the size reduction, weight reduction, enhancement of the performance, high density packaging, or the temperature rise in the use environment, of electrical or electronic equipments.
  • copper-based materials such as phosphor bronze, red brass, and brass
  • copper-based materials have also been widely used in general as the materials for electrical or electronic equipments.
  • These copper alloys are enhanced in the mechanical strength through a combination of solid solution strengthening of tin (Sn) or zinc (Zn) and work hardening through cold-working, such as rolling or drawing.
  • Sn tin
  • Zn zinc
  • cold-working such as rolling or drawing.
  • the electrical conductivity is insufficient, and the bending property and/or the stress relaxation resistance are also insufficient, due to that high mechanical strength is attained by making a working ratio high in the cold-working.
  • precipitation strengthening is available by which a fine second phase is precipitated in the material.
  • This strengthening method has advantages of enhancing the mechanical strength, as well as, simultaneously, enhancing the electrical conductivity, and thus this method has been applied to many alloy systems.
  • a copper alloy sheet material to be used therein a copper alloy-based material higher in the mechanical strength has become to be subjected to bending at a smaller radius, and there is a strong demand for a copper alloy sheet material excellent in the bending property.
  • the sheet material is subjected to micromachining in a pin type at a narrow width, and it is important that favorable characteristics are exhibited in any direction, in this case also.
  • Patent Literature 1 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material excellent in the bending property, which sheet material has a given grain size and a crystal orientation in which X-ray diffraction intensities I from the ⁇ 3 1 1 ⁇ , ⁇ 2 2 0 ⁇ , and ⁇ 2 0 0 ⁇ planes satisfy a certain condition.
  • Patent Literature 2 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material excellent in the bending property, which sheet material has a crystal orientation in which the X-ray diffraction intensities from the ⁇ 2 0 0 ⁇ and ⁇ 2 2 0 ⁇ planes satisfy a certain condition.
  • Patent Literature 3 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material excellent in the bending property, which sheet material is controlled on a ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> to 50% or less.
  • Patent Literature 4 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material favorable in the bending property, which sheet material has a recrystallized crystal structure from a distorted state due to strong cold working, whereby the crystal structure is converted into one whose anisotropy is small, and also elongation is improved.
  • Patent Literature 5 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material excellent in the bending property and small in strength anisotropy, which sheet material is controlled in a grain size, and a ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> to 20% to 60%.
  • Patent Literature 6 discloses, in a Cu-Ni-Si-based copper alloy, a copper alloy sheet material improved in fatigue property, without deteriorating mechanical strength, electrical conductivity, and bending property, by controlling a grain size, and a ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> to 5 to 50%.
  • Patent Literatures 1 and 2 only limited specific planes among the expansive distribution of crystal orientations are focused, in the analysis of crystal orientations with X-ray diffraction from the specific planes. Further, in the invention described in Patent Literature 3, the control of the crystal orientation is realized by a reduction of a working ratio in rolling after solution heat treatment. Further, the area and the dispersibility of the Cube orientation grains are not described in Patent Literature 3, and the bending property and the anisotropy in mechanical strength are not disclosed in Patent Literature 3.
  • Patent Literature 4 a crystal structure in a distorted state due to strong cold-rolling is recrystallized, to realize a crystal structure small in anisotropy, and to improve elongation, thereby to realize a favorable bending property.
  • improvement in characteristics by controlling crystal orientation is not carried out at all in Patent Literature 4.
  • a process e.g. a rolling reduction ratio in cold-rolling before a solution treatment, and a temperature rising speed in the solution treatment, is controlled, to accumulate the Cube orientation and to reduce anisotropy in mechanical strength and bending property.
  • a temperature rising speed in the solution treatment is slow, and thus the temperature rising time period is long.
  • the Cube orientation grains are coarsened, a homogeneous dispersibility of the Cube orientation grains is poor, and anisotropy in mechanical strength is also large.
  • cold-rolling before the solution treatment is conducted at a rolling reduction ratio as high as 85% to 99.8%, and a heating temperature and a holding time period in the subsequent solution treatment are controlled, to cause accumulation in the Cube orientation, and to improve the fatigue property.
  • the Cube orientation grains that are obtained as a result of the solution treatment are coarsened, the homogeneous dispersibility of the Cube orientation grains is poor, and anisotropy in mechanical strength is also large.
  • a low Young's modulus (modulus of longitudinal elasticity) is required, as one of the characteristics required for copper alloy materials for use in electrical or electronic equipments.
  • Young's modulus modulus of longitudinal elasticity
  • the tolerances in the size accuracy of terminals and in the press working have been becoming severe to achieve.
  • the Young's modulus of a copper alloy material By lowering the Young's modulus of a copper alloy material, the effects of variation in size, which affect to a contact pressure, can be decreased, and thus the designing of parts becomes readily.
  • Young's modulus With regard to measurement of Young's modulus, there are two methods including: a method in which Young's modulus is calculated from a gradient in an elastic region in a stress-strain curve obtained by a tensile test; and a method in which Young's modulus is calculated from a gradient in an elastic region in a stress-strain curve when a beam (cantilever beam) is bent.
  • the present invention is contemplated for providing a copper alloy sheet material, which is excellent in the bending property, which has an excellent mechanical strength, which is less in anisotropy in those characteristics in the parallel direction to rolling and the perpendicular direction to rolling, and which is suitable for lead frames, connectors, terminal materials, and the like in electrical or electronic equipments, for connectors, for example, to be mounted on automotive vehicles, and for terminal materials, relays, switches, and the like. Further, the present invention is also contemplated for providing a favorable method of producing the copper alloy sheet material.
  • the inventors of the present invention having keenly conducted investigations on copper alloys appropriate for electrical or electronic part applications, have found that there is a correlation between the accumulation ratio of the Cube orientation and the bending property, to largely improve the bending property, the mechanical strength, and the electrical conductivity, in Cu-Ni-Si-based copper alloy sheet materials. Further, the inventors have found a specific copper alloy composition to further enhance the mechanical strength, in copper alloy sheet materials having the above crystal orientation and characteristics. In addition, the inventors have also found copper alloy sheet materials to which are added additional alloying elements that act to enhance the mechanical strength, without impairing the electrical conductivity and the bending property in this alloy system.
  • the inventors have also found a production method comprising specific steps, based on the correlation between the accumulation ratio of the Cube orientation and the bending property, to attain the above specific crystal orientation.
  • the present invention is attained, as a result of studies based on those findings.
  • a copper alloy sheet material which is excellent in the bending property, which has an excellent mechanical strength, and which is less in anisotropy in those properties in the parallel direction to rolling and the perpendicular direction to rolling.
  • a copper alloy sheet material which has properties suitable for lead frames, connectors, terminal materials, and the like in electrical or electronic equipments, for connectors, for example, to be mounted on automotive vehicles, and for terminal materials, relays, switches, and the like.
  • the production method of the present invention can favorably produce the above copper alloy sheet material.
  • Fig. 1 is a diagram illustrating the homogeneous dispersibility in a case of at least four groups, each group including four blocks adjacent to each other.
  • the copper alloy sheet material of the present invention has the composition containing 1.0 mass% to 5.0 mass% of Ni, and 0.1 mass% to 2.0 mass% of Si, with the balance being copper and unavoidable impurities.
  • Ni is set to 3.0 mass% to 5.0 mass%
  • Si is set to 0.5 mass% to 2.0 mass%.
  • Ni is set to 4.0 mass% or more
  • Si is set to 1.0 mass% or more.
  • the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> (hereinafter, which may be referred to as a Cube orientation area ratio) is 5% to 50%, preferably 10% to 45%, more preferably 15% to 40%, and particularly preferably 20% to 35%.
  • the copper alloy sheet material may contain 1.0 mass% to 5.0 mass% of Ni, 0.1 mass% to 2.0 mass% of Si, and at least one selected from the group consisting of Sn, Zn, Ag, Mn, B, P, Mg, Cr, Zr, Fe, and Hf in a total amount of 0.005 mass% to 1.0 mass%.
  • the total amount of at least one selected from the group consisting of Sn, Zn, Ag, Mn, B, P, Mg, Cr, Zr, Fe, and Hf is preferably 0.01 mass% to 0.9 mass%, more preferably 0.03 mass% to 0.8 mass%, and particularly preferably 0.05 mass% to 0.5 mass%.
  • the preferable contents of Ni and Si, and particularly preferable contents thereof, and the preferable range of the Cube orientation area ratio, and particularly preferable range thereof are the same as described above.
  • the average grain area of the grains having the orientation in which deviation from the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is within 15° is preferably 1.8 ⁇ m 2 to 45.0 ⁇ m 2 , more preferably 3.8 ⁇ m 2 to 36.0 ⁇ m 2 , still more preferably 6.0 ⁇ m 2 to 28.8 ⁇ m 2 , and particularly preferably 10.0 ⁇ m 2 to 25.0 ⁇ m 2 .
  • the average grain area of the grains having the orientation in which deviation from the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is within 15° may be abbreviated to be referred to as a Cube orientation area ratio, an area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0>, or the like.
  • the grains having the orientation in which deviation from the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is within 15° may be abbreviated to as the Cube orientation grains, grains of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0>, or the like.
  • the average grain area of the matrix containing the Cube orientation grains is preferably 40 ⁇ m 2 or less, and more preferably 5 ⁇ m 2 to 30 ⁇ m 2 .
  • An average value of the grain area is calculated from EBSD measurement results within a range of 300 ⁇ m ⁇ 300 ⁇ m on a plane of a sheet material, and the average value is set as the average grain area.
  • the crystal orientation analysis by the electron backscatter diffraction method 40 to 100 grains of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> are distributed within 60 ⁇ m square, to have the homogeneous dispersibility.
  • the grains of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> within 60 ⁇ m square, preferably 45 to 95 grains are distributed, to have the homogeneous dispersibility, and particularly preferably 50 to 90 grains are distributed, to have the homogeneous dispersibility.
  • the difference between the deflection coefficient in the parallel direction to rolling (//) and the deflection coefficient in the perpendicular direction to rolling ( ⁇ ) is preferably 10 GPa or less, more preferably 8 GPa or less, and particularly preferably 5 GPa or less, in terms of an absolute value thereof.
  • the difference between the proof stress in the parallel direction to rolling and the proof stress in the perpendicular direction to rolling is preferably 10 MPa or less, more preferably 8 MPa or less, and particularly preferably 5 MPa or less, in terms of an absolute value thereof.
  • each of these differences is 0 (zero), that is, most preferably the values in the parallel direction to rolling and the perpendicular direction to rolling are the same as each other.
  • the copper alloy sheet material of the present invention when each of the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> and the average grain area thereof, more preferably the average grain area of the matrix in addition to those two, are within the above-described ranges, no cracks occur at the vertex of the bent portion upon the 180° tight U-bending and the favorable bending property can be obtained, and further the deflection anisotropy and the proof stress anisotropy becomes small.
  • the copper alloy sheet material of the present invention contains 1.0 mass% to 5.0 mass% of Ni, and 0.1 mass% to 2.0 mass% of Si. Due to those, a Ni-Si-based compound (Ni 2 Si phase) precipitates in the Cu matrix, to enhance the mechanical strength and electrical conductivity. On the other hand, if the content of Ni is too small, the mechanical strength may not be obtained, and if the content is too large, precipitation, which does not contribute to enhancement of the mechanical strength, occurs upon casting or hot working, resulting in that any mechanical strength appropriate for an addition amount may not be obtained, and hot workability and bending property become worse. Furthermore, Si forms the Ni 2 Si phase in combination with Ni, and thus when the content of Ni is determined, the addition amount of Si is determined.
  • the addition amounts of Ni and Si be set within the above-described ranges.
  • the inventors of the present invention conducted detailed investigation and analysis on the cause of cracks occurred at a bent portion.
  • the cause is that, upon bending, plastic deformation locally develops to form a shear deformation zone, to cause occurrence and connection of microvoids via local work-hardening, resulting in reaching the growth limitation.
  • the inventors have found that it is effective to increase the ratio of crystal orientation by which work hardening is difficult to occur in bending deformation. That is, as described above, the present inventors have found that in a case where the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is 5% to 50%, a favorable bending property is exhibited.
  • the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is within the above-described range, the above-described action and effect are sufficiently exhibited. Further, within the above-described range, even when cold-rolling after a recrystallization treatment is not conducted at a low rolling reduction ratio, the mechanical strength does not be lowered conspicuously, and thus the range is preferable. That is, the cold-rolling after the recrystallization treatment may be conducted at a high rolling reduction ratio, without significantly deteriorating the mechanical strength. On the other hand, when the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is too low, the bending property deteriorates.
  • the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is set to 5% to 50%, a preferable range is 10% to 45%, a more preferable range is 15% to 40%, and a particularly preferable range is 20% to 35%.
  • the S orientation ⁇ 3 2 1 ⁇ ⁇ 4 3 6>, the Copper orientation ⁇ 1 2 1 ⁇ ⁇ 1 -1 1>, the D orientation ⁇ 4 11 4 ⁇ ⁇ 11 -8 11>, the Brass orientation ⁇ 1 1 0 ⁇ ⁇ 1 -1 2>, the Goss orientation ⁇ 1 1 0 ⁇ ⁇ 0 0 1>, the RDW orientation ⁇ 1 0 2 ⁇ ⁇ 0 1 0>, and the like are generated as crystal orientations, in addition to the Cube orientation. Any of these other orientation components may be present in the copper alloy sheet material of the present invention, as long as the area ratio of the Cube orientation is within the above-mentioned range to the areas of all of the observed orientations.
  • the EBSD method which stands for electron backscatter diffraction, is a technique of crystal orientation analysis using a reflected electron back-scattering pattern (EBSP) that occurs when one point of the surface of a sample is irradiated with an electron beam under a scanning electron microscope (SEM), to analyze a crystal orientation and a crystalline structure (texture) in a localized region of the sample.
  • EBSP reflected electron back-scattering pattern
  • a sample area which is measured 1 mm on each of the four sides and which contains 200 or more grains, is subjected to an analysis of the crystal orientation, by scanning in a stepwise manner at an interval of 0.1 ⁇ m.
  • a measurement area is set to 300 ⁇ m ⁇ 300 ⁇ m in consideration of the size of grains of the sample.
  • the area ratio of the respective orientation is a ratio of the area of grains having the orientation in which the deviation (deviation angle) from the ideal orientation of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is within 15°, i.e. ⁇ 15° or less, to the measured area.
  • the data obtained from the orientation analysis based on EBSD includes the orientation data to a depth of several tens nanometers, through which the electron beam penetrates into the sample. However, since the depth is sufficiently small as compared with the width to be measured, the data is described in terms of ratio of an area, i.e. area ratio, in the present specification. Further, since the orientation distribution changes in the sheet thickness direction, it is preferable to carry out the orientation analysis by EBSD at several arbitrary points along the sheet thickness direction, to calculate the average. In this application, a value measured in this way is referred to as an area ratio of a crystal plane having a certain crystal orientation, unless otherwise state.
  • a region of 300 ⁇ m ⁇ 300 ⁇ m is scanned in a stepwise manner at an interval of 0.1 ⁇ m, to analyze total 25 blocks, in which 60 ⁇ m square is set as one block.
  • the area ratio, the number, and the average grain area of the Cube orientation grains per one block, and the average grain area of the matrix containing the Cube orientation grains are confirmed, to examine the dispersibility.
  • the Cube orientation area ratio is 5% to 50%
  • the number of Cube orientation grains is 40 to 100
  • the average grain area of each one of the Cube orientation grains is 1.8 ⁇ m 2 to 45.0 ⁇ m 2
  • the average grain area of the matrix containing the Cube orientation grains is 50 ⁇ m 2 or less
  • the thus-obtained value is the average grain area.
  • the "homogeneous dispersibility" referred to herein specifies the average grain area and the number of Cube orientation grains per one block.
  • the homogeneous dispersibility can be confirmed when seen in terms of the entirety of 300 ⁇ m ⁇ 300 ⁇ m in which 25 blocks are accumulated.
  • the Cube orientation groups are included in at least four or more blocks, and thus it can be said that the homogeneous dispersibility is present.
  • the dispersibility thereof is equivalent, and the anisotropy in the parallel direction to rolling and the perpendicular direction to rolling is small.
  • the homogeneous dispersibility of a case of at least four or more groups, in which adjacent four blocks are set as one group
  • the area of one block is set as 30 ⁇ m square
  • the area ratio of the grains of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> be 5% to 50%
  • the average grain area of the grains of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> be 1.8 ⁇ m 2 to 45.0 ⁇ m 2
  • the average grain area of grains of the matrix is preferably 40 ⁇ m 2 or less.
  • the average grain area of the Cube orientation grains In a case where the average grain area of the Cube orientation grains is too small, the solution heat treatment is insufficient, and thus non-crystallized structure remains. Thus, there is a possibility that the mechanical strength and the bending property may be deteriorated. On the other hand, in a case where the average grain area of the Cube orientation grains is too large, a possibility of occurrence of fracture (cracks) is high at a portion of grains having orientations other than the Cube orientation grains upon bending. Further, the anisotropy may occur depending on a bending direction in some cases. Thus, it is preferable that the average grain area of the Cube orientation grains be set within the above-described range.
  • the average grain area and the dispersibility of the Cube orientation grains are controlled. Specifically, in the intermediate warm-rolling before the recrystallization solution heat treatment, by heating to a temperature at which recrystallization does not occur, followed by rolling at a rolling reduction ratio of 5% or more under the temperature, it is possible to control introduction and release of a strain in the entirety of the thus-rolled material in an appropriate state. By conducting those, the homogeneous dispersibility of the Cube orientation can be realized. Further, the average grain area of each crystal orientation can be controlled simultaneously. By controlling the dispersibility, the bending property of the narrow-width pin enhances, and the strength anisotropy, such as the deflection anisotropy, and the proof stress anisotropy, are reduced.
  • At least one additional alloying element selected from the group consisting of Sn, Zn, Ag, Mn, B, P, Mg, Cr, Zr, Fe, and Hf may be contained, in addition to main alloying elements of Ni and Si.
  • the content of the additional alloying elements is 0.005 to 1.0 mass%, preferably 0.01 to 0.9 mass%, more preferably 0.03 mass% to 0.8 mass%, particularly preferably 0.05 mass% to 0.5 mass%, in the total amount of the additional alloying elements. If the content of the additional alloying elements is 1.0 mass% or less in total, any adverse affection to lower the electrical conductivity is less likely to occur.
  • Mg, Sn, and Zn when added, improve the stress relaxation resistance of the copper alloy sheet material.
  • the stress relaxation resistance is further improved by synergistic effects. Further, an effect of remarkably improving solder brittleness is obtained.
  • the stress relaxation resistance is measured, according to EMAS-3003, the former Technical Standard of the "Electronic Materials Manufacturer's Association of Japan", under the conditions of retaining the sample specimen at 150°C for 1,000 hours. An initial stress that is 80% of a yield stress (proof stress) is applied thereto, by a cantilever method, and an amount of displacement after the test at 150°C for 1,000 hours is determined as an index of the stress relaxation resistance.
  • Mn, Ag, B, and P when added, improve hot workability, and at the same time, enhance the mechanical strength, of the copper alloy sheet material.
  • Cr, Zr, Fe, and Hf each finely precipitate, in the matrix, in the form of a compound thereof or in the form of a simple elementary substance.
  • the simple elementary substance Cr, Zr, Fe, and Hf precipitate in a size of preferably 75 nm to 450 nm, more preferably 90 nm to 400 nm, and particularly preferably 100 nm to 350 nm, to contribute to precipitation hardening.
  • Cr, Zr, Fe, and Hf precipitate in a size of 50 nm to 500 nm.
  • those elements each have an effect of making the grain size fine, by suppressing the grain growth, and an effect of improving the bending property favorably, by making the dispersion state of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> grains better.
  • a test specimen subjected to the 90° W-bending is subjected to 180° tight bending by a compression test machine. At this test, it is preferable that cracks do not occur at the vertex of the resultant bent portion.
  • the copper alloy sheet material of the present invention with regard to the bending property in the parallel direction to rolling and the perpendicular direction to rolling, it is preferable that no crack occur in the bent surface at the 180° tight U-bending upon bending of a narrow width of 1 mm or less.
  • a difference between the deflection coefficient in the parallel direction to rolling (//) and the deflection coefficient in the perpendicular direction to rolling ( ⁇ ) is preferably 10 GPa or less in terms of an absolute value thereof, and in that case, the anisotropy in the deflection coefficient is small.
  • a difference between the proof stress in the parallel direction to rolling and the proof stress in the perpendicular direction to rolling is preferably 10 MPa or less in terms of an absolute value thereof, and in that case, the anisotropy in the proof stress is small.
  • the production method of the copper alloy sheet material of the present invention contains, in this order, the steps of: casting a copper alloy raw material to give an ingot, followed by subjecting to a heat treatment (homogenization treatment) and hot-rolling, cold-rolling to roll into a thin sheet, intermediate annealing at a temperature lower than the recrystallization temperature of the thin sheet, heating to 100°C to 400°C and warm-rolling (hereinafter, referred to as intermediate warm-rolling) at a rolling reduction ratio of 5% or more at the temperature, and then an intermediate solution heat treatment to form a solid solution of solute atoms in the thin sheet again, to produce the copper alloy sheet material.
  • a heat treatment homogenization treatment
  • hot-rolling cold-rolling to roll into a thin sheet
  • intermediate annealing at a temperature lower than the recrystallization temperature of the thin sheet
  • heating to 100°C to 400°C and warm-rolling hereinafter, referred to as intermediate warm-rolling
  • an intermediate solution heat treatment
  • the copper alloy raw material has a composition containing 1.0 mass% to 5.0 mass% of Ni, 0.1 mass% to 1.0 mass% of Si, and optionally at least one selected from the group consisting of Sn, Zn, Ag, Mn, B, P, Mg, Cr, Zr, Fe, and Hf in a total amount of 0.005 mass% to 1.0 mass%, with the balance being copper and unavoidable impurities.
  • the following production method may be exemplified as a preferred example.
  • the above copper alloy raw material is subjected to casting [Step 1], to give an ingot.
  • the resultant ingot is subjected to homogenization heat treatment [Step 2], followed by hot rolling [Step 3], and immediately cooling [Step 4] (for example, water cooling, water quenching).
  • the resultant sheet is subjected to face milling [Step 5], to remove an oxide layer on the surface thereof.
  • the resultant sheet is subjected to cold-rolling [Step 6], to roll at a rolling reduction ratio of 80% or more, to give a thin sheet.
  • the resultant thin sheet is subjected to intermediate annealing [Step 7] at a temperature of 400°C to 700°C, at which the thin sheet is partially recrystallized, for 5 seconds to 20 hours, followed by heating to 100°C to 400°C and intermediate warm-rolling [Step 8] under the temperature at a rolling reduction ratio of 5% to 50%.
  • the resultant thin sheet is subjected to the intermediate solution heat treatment [Step 9], to form a solid solution of solute atoms again.
  • the Cube orientation area ratio increases.
  • Step 9 After the intermediate solution heat treatment [Step 9], the aging-precipitation heat treatment [Step 10] is conducted, and then a finish cold-rolling [Step 11], and a temper annealing [Step 12] may be conducted, in this order.
  • a copper alloy raw material is subjected to: casting [Step 1] to give an ingot, and the resultant ingot is subjected to homogenization heat treatment [Step 2], followed by hot rolling [Step 3], cooling (water cooling) [Step 4], face milling [Step 5], and cold-rolling [Step 6], in this order, to give a thin sheet.
  • the resultant thin sheet is subjected to: intermediate solution heat treatment [Step 9] at a temperature in the range of 700 to 1,000°C, to thereby form a solid solution of solute atoms again, followed by aging-precipitation heat treatment [Step 10], finish cold-rolling [Step 11], and, if necessary, temper annealing [Step 12], to satisfy the required mechanical strength.
  • Step 9 intermediate solution heat treatment
  • Step 10 finish cold-rolling
  • Step 12 temper annealing
  • the copper alloy raw material containing at least Ni in an amount of 1.0 to 5.0 mass%, and Si in an amount of 0.1 to 1.0 mass%, and optionally containing other element(s) such that any of the additional alloying elements would be suitably contained, with the balance being Cu and unavoidable impurities, is melted in a high-frequency melting furnace, followed by cooling at a cooling speed of 0.1 to 100°C/sec, to obtain an ingot.
  • This ingot is subjected to the homogenization heat treatment [Step 2] at 800 to 1,020°C for 3 minutes to 10 hours, followed by the hot rolling [Step 3], and water quenching (this corresponds to the cooling [Step 4]).
  • the surface oxide layer is removed by the face milling [Step 5].
  • the cold-rolling [Step 6] is conducted at a rolling reduction ratio of 80% to 99.8%, to obtain the thin sheet.
  • the intermediate annealing [Step 7] is conducted at 400°C to 700°C for 5 seconds to 20 hours, followed by heating under the condition of 100°C to 400°C, and the intermediate warm-rolling [Step 8] under the temperature at a rolling reduction ratio of 5% to 50%.
  • the warm-rolling means that rolling is conducted at the temperature of 100°C to 400°C.
  • the intermediate solution heat treatment [Step 9] is conducted at 600 to 1,000°C for 5 seconds to 1 hour.
  • the aging-precipitation heat treatment [Step 10] at 400 to 700°C for 5 minutes to 10 hours, preferably under an inert gas atmosphere, such as Ni and Ar, is conducted, and then, the finish cold-rolling [Step 11] at a rolling reduction ratio of 3 to 25%, and the temper annealing [Step 12] at 200 to 600°C for 5 seconds to 10 hours may be conducted, in this order, to obtain the copper alloy sheet material of the present invention.
  • one or more of the steps of the face milling [Step 5], the finish cold-rolling [Step 11], and the temper annealing [Step 12] may be omitted and may not be conducted.
  • the hot-rolling [Step 3] is to conduct, at the temperature region from 700°C to the reheated temperature (1,020°C), working for breaking the cast structure and segregation to form a homogeneous structure, and working for making grains fine by dynamic recrystallization.
  • Step 7 a heating is conducted such that the microstructure of the resultant alloy would not be recrystallized in the whole. Then, heating at a temperature range at which recrystallization does not occur is conducted preferably at 100°C to 400°C, more preferably 120°C to 380°C, and particularly preferably 140°C to 360°C, and the intermediate warm-rolling [Step 8] is conducted under the temperature, at a rolling reduction ratio of preferably 5% to 50%, more preferably 7% to 45%, and particularly preferably 10% to 40%, to control introduction and release of a working strain.
  • the heating temperature in the intermediate warm-rolling [Step 8] is lower than 100°C, the release of working strain is less, and on the contrary, when this heating temperature is higher than 400°C, recrystallization is apt to progress along with the progress of the release of the working strain.
  • the homogeneous dispersibility of the Cube orientation grains at strain-induced grain boundary migration becomes not sufficient.
  • the resultant copper alloy sheet material is caused with the deflection anisotropy as the anisotropy in bending, and the proof stress anisotropy as the anisotropy in mechanical strength.
  • the Cube orientation area ratio increases in the resultant recrystallized texture.
  • the heat treatment temperature in the intermediate annealing [Step 7] before the intermediate solution heat treatment [Step 9] is set to be higher than a temperature within the above-described range, the surface oxide layer is formed, which is not preferable.
  • the heat treatment temperature in the intermediate annealing [Step 7] is preferably set to 400°C to 700°C.
  • the Cube orientation area ratio has a tendency to increase in the intermediate solution heat treatment [Step 9].
  • the aging-precipitation heat treatment [Step 10] is conducted, and then the finish cold-rolling [Step 11] and the temper annealing [Step 12] may be conducted.
  • the recrystallized texture formed upon the intermediate solution heat treatment [Step 9] it is effective to conduct a predetermined working in the intermediate warm-rolling [Step 8], to increase the Cube orientation area ratio, due to the strain-induced grain boundary migration. Further, when a crystal orientation is controlled to a certain direction in the intermediate warm-rolling [Step 8], this control contributes to development of the Cube orientation grains.
  • the mechanical strength can be enhanced, due to precipitation hardening.
  • the sheet thickness may be finally adjusted, by conducting the finish cold-rolling [Step 11].
  • the temper of the sheet material may be finally adjusted, by conducting the temper annealing [Step 12].
  • the object of the intermediate annealing [Step 7] is to obtain a sub-annealed structure, which is partially recrystallized without being completely recrystallized.
  • the object of the intermediate warm-rolling [Step 8] is to allow introduction and release of a microscopically nonuniform strain to progress, by rolling under the conditions of a heating temperature of 100°C to 400°C and a rolling reduction ratio of 5% or more.
  • the Cube orientation grains can be developed, by the introduction of the strain, and the Cube orientation grains can be made fine and the homogeneous dispersibility of the Cube orientation grains can be made higher, by the release of the strain.
  • the primary object of the heat treatment such as the intermediate solution treatment [Step 9] is to recrystallize a material so as to reduce a load in the subsequent step, thereby lowering the strength, but the object of the said heat treatment in the present invention is completely different from the above object in the conventional art.
  • the sheet thickness of the copper alloy sheet material of the present invention is not particularly limited, and the sheet thickness is generally 0.03 mm to 0.50 mm, and preferably 0.05 mm to 0.35 mm.
  • the copper alloy sheet material of the present invention satisfies the conditions described above, the following characteristics, for example, which are required for a copper alloy sheet material for use in connectors, can be satisfactorily exhibited, which is preferable.
  • the deflection coefficient as one of the characteristics is preferably 130 GPa or less. Detailed conditions thereof are set as described in the Examples section.
  • the lower limit of the deflection coefficient exhibited by the copper alloy sheet material of the present invention is not particularly limited, but the lower limit is generally 90 GPa or more.
  • the proof stress as one of the characteristics is preferably 700 MPa or more, and more preferably 750 MPa or more. Detailed measurement conditions thereof are set as described in the Examples section.
  • the upper limit of the proof stress exhibited by the copper alloy sheet material of the present invention is not particularly limited, but the upper limit is generally 900 MPa or less.
  • the copper alloy sheet material has an electrical conductivity of preferably 5%IACS or more, more preferably 10%IACS or more, and particularly preferably 20%IACS or more.
  • IACS is an abbreviation of international annealed copper standard. Unless otherwise specified, the specific measurement conditions are set as described in the Examples section.
  • the upper limit value of the electrical conductivity of the copper alloy sheet material of the present invention is not particularly limited, it is generally 50%IACS or less.
  • This resultant respective ingot was subjected to the homogenization heat treatment [Step 2] at 800 to 1,020°C for 3 minutes to 10 hours, followed by the hot rolling [Step 3] as a hot working at 700°C or higher and a reheated temperature of 1,020°C or lower, and then the water quenching (this corresponds to the water cooling [Step 4]), to obtain a hot-rolled sheet. Then, the hot-rolled sheet was subjected to the face milling [Step 5] of the surface, so as to remove an oxide layer. Then, the respective resultant sheet was subjected to the cold-rolling [Step 6] at a rolling reduction ratio of 80 to 99.8%, to obtain a thin sheet.
  • the thin sheet was subjected to the intermediate annealing [Step 7] in heating for 5 seconds to 20 hours at 400°C to 700°C, followed by subjected to further heating to 100°C to 400°C and the intermediate warm-rolling [Step 8] at a rolling reduction ratio of 5 to 50% under the temperature.
  • the intermediate solution treatment [Step 9] was conducted at 600 to 1,000°C for 5 seconds to 1 hour.
  • the respective resultant sheet was subjected to the aging-precipitation heat treatment [Step 10] at 400°C to 700°C for 5 min to 1 hours, under an inert gas atmosphere, followed by the finish cold-rolling [Step 11] at a rolling reduction ratio of 3% to 25%, and the temper annealing [Step 12] at 200°C to 600°C for 5 seconds to 10 hours, to give the respective sample specimen (Examples 1 to 14 and Comparative Examples 1 to 4) of the copper alloy sheet material.
  • the final sheet thickness of the respective sample specimen was set to be 0.08 mm.
  • compositions and characteristics of the resultant Examples 1 to 14, and Comparative Examples 1 to 4 are shown in Tables 1 and 2.
  • the measurement was conducted with the EBSD method in a measurement region of 0.09 ⁇ m 2 (300 ⁇ m ⁇ 300 ⁇ m), under the conditions of a scan step of 0.1 ⁇ m. Further, with regard to the measurement area, 60 ⁇ m ⁇ 60 ⁇ m was set as one block, and the measurement area was set to measure total 25 blocks (5 blocks ⁇ 5 blocks) at one visual field. In this case, the scanning step was set to 0.1 ⁇ m step as described above, to measure fine grains. In analysis, EBSD measurement results in the measurement area of 300 ⁇ m ⁇ 300 ⁇ m were divided to the above-described 25 blocks.
  • the Cube orientation area ratio, the average grain area, the number of grains, and the average grain area of the matrix containing the Cube orientation grains in each block were confirmed.
  • a thermoelectron from a tungsten filament of a scanning electron microscope was utilized as a generation source.
  • Test specimens with width 0.25 mm and length 1.5 mm were taken out, by press punching in a direction perpendicular to the rolling direction.
  • a W-bent test specimen in which a bending axis was perpendicular to the rolling direction was set as GW (Good Way)
  • a W-bent test specimen in which the bending axis was parallel to the rolling direction was set as BW (Bad Way).
  • the test specimens were subjected to 90° W-bending according to the Technical Standard JCBA-T307 (2007) by the Japan Copper and Brass Association, followed by 180° tight U-bending by a compression test machine without any inner radius.
  • the resultant bent-surface was observed with a scanning electron microscope with a magnification of 100x, to examine whether or not cracking occurred.
  • a test specimen without any cracks was indicated by "o (good)", and a test specimen having cracks was indicated by "x (poor)”.
  • o good
  • x poor
  • the maximum width was 30 ⁇ m to 100 ⁇ m
  • the maximum depth was 10 ⁇ m or more.
  • test specimen was taken out, by press punching to have a width of 0.25 mm in a direction perpendicular to the rolling direction, and a length of 1.5 mm in a direction parallel to the rolling direction.
  • the front surface and backing surface of the test specimen was measured ten times, respectively, by a cantilever beam, and an average value thereof is shown.
  • the electrical conductivity was calculated by using the four-terminal method to measure the specific resistance of the respective sample specimen in a thermostat bath that was maintained at 20°C ( ⁇ 0.5°C).
  • the spacing between terminals was set to 100 mm.
  • Example 1 to 14 As shown in Table 2, with the production conditions of Example 1 to 14, the intermediate warm-rolling [Step 8] was carried out by heating to 100°C to 400°C, followed by rolling at a rolling reduction ratio at 5% or more.
  • the Cube orientation area ratio was 5% to 50%
  • the average grain area of the Cube orientation grains was 1.8 ⁇ m 2 to 45.0 ⁇ m 2
  • the number of Cube orientation grains per one block 60 ⁇ m ⁇ 60 ⁇ m) was 40 to 100
  • the average grain area of the matrix containing the Cube orientation grains was 50 ⁇ m 2 or less.
  • all of the results of the 180° tight U-bending, the deflection anisotropy, and the proof stress anisotropy were excellent.
  • the deflection coefficient anisotropy was 10 GPa or less, and in the proof stress property, the proof stress anisotropy was 10 MPa or less. Both of the deflection coefficient anisotropy and the proof stress anisotropy were small.
  • the copper alloy sheet material of the present invention can be provided as a copper alloy sheet material suitable for lead frames, connectors, terminal materials, and the like for electrical or electronic equipments, and for connectors, for example, to be mounted on automotive vehicles, for terminal materials, relays, switches, and the like.
  • copper alloy sheet materials were produced under the conventional production conditions, and evaluations of the same characteristic items as described above were conducted.
  • the working ratio was adjusted so that, unless otherwise specified, the thickness of the respective sheet material would be the same as the thickness in the Examples described above.
  • a copper alloy having a composition containing 3.2 mass% of Ni, 0.7 mass% of Si, 1.0 mass% of Zn, and 0.2 mass% of Sn was melted and casted.
  • the resultant ingot was subjected to face milling, followed by a homogenization heat treatment, and hot-rolling in which a termination temperature was set to 550°C to 850°C.
  • a termination temperature was set to 550°C to 850°C.
  • an oxide layer on the surface was removed by mechanical grinding (face milling).
  • rolling to a predetermined sheet thickness was conducted by cold-rolling, followed by subjecting to cold-rolling at a working ratio of 90% or more.
  • heating was conducted to a temperature of 800°C to 900°C at a temperature rising speed of 0.1°C/s or less, followed by subjecting to a solution treatment.
  • an aging treatment was conducted at 500°C.
  • the time period for the aging treatment was adjusted to a time period in which the hardness reached a peak by aging at 460°C, depending on the composition of the copper alloy.
  • an optimal time period for the aging treatment was obtained by a preliminary experiment depending on the composition of the alloy of this Example 1 of JP-A-2011-162848 .
  • the sheet material after the above aging treatment was further subjected to finish cold-rolling at a rolling reduction ratio of 40%. Further, the resultant sheet material was subjected to low-temperature annealing at 480°C for 30 seconds. Where necessary, grinding and face milling were conducted in the mid course, and the sheet thickness was set to 0.10 mm.
  • the intermediate annealing [Step 7] was not conducted, and the intermediate warm-rolling [Step 8] under a heating temperature before the solution heat treatment [Step 9] was also not conducted. Further, since the temperature rising speed in the solution heat treatment was slow, grain growth in the vicinity of the reached temperature was significant, to coarsen grains. In the resultant texture, the area of the Cube orientation grains was as conspicuously large as 150 ⁇ m 2 or more. Further, the anisotropy in the deflection coefficient was as conspicuously large as more than 10 GPa, and the anisotropy in the strength was as conspicuously large as more than 15 MPa. Thus, Sample specimen c01 in Comparative Example 101 was poor in the results, in which the characteristics required for the present invention were not satisfied.
  • a coreless furnace high-frequency electrically-induction melting furnace
  • an SUS rod with a diameter of 3 mm ⁇ was inserted in a vertical direction from a molten metal surface located at an upper end portion of the casting mold, at an intersection position between a width 155-mm position and a thickness 125-mm position of the casting mold, to measure the depth of a non-solidified portion.
  • the casting was conducted, by adjusting a casting speed within a range of 50 mm/min/ to 200 mm/min, to obtain the ingots, respectively.
  • a block of 250 mm ⁇ 620 mm ⁇ 300 mm of a constant region was cut to take out, and a slice (250 mm ⁇ 15 mm ⁇ 300 mm) of a cross-section parallel with the casting direction was collected at the central portion of the width of 620 mm.
  • the slice was immersed and etched in nitric acid for 0.5 hours to 1 hour, and a columnar crystal in a [100] axis direction was obtained from the macro structure that was obtained after etching.
  • An angle made by a face perpendicular to the casting direction and the direction of the [100] axis of the columnar crystal was measured. Specifically, the angle was 13° (Example 1 of JP-A-2011-12321 ) and 11° (Example 4 of JP-A-2011-12321 ), respectively.
  • a temperature of the resultant ingot was adjusted to 500°C to 1,000°C, followed by rolling at a total working ratio of 60% to 96%, and then directly cooling the rolled material with water, to obtain a coil with thickness approximately 10 mm.
  • the surface of the rolled material was subjected to face-milling, to remove oxide scale. A proportion of the Cube orientation of the rolled material at this point of time was 5% to 95%.
  • the specimens were indicated as a sample d01 (Example 1 of JP-A-2011-12321 ) and a sample d02 (Example 4 of JP-A-2011-12321 ), respectively.
  • the intermediate annealing [Step 7] was not conducted, and the intermediate warm-rolling [Step 8] under a heating temperature before the solution heat treatment [Step 9] was also not conducted.
  • the area ratio of the Cube orientation grains was 35% for the sample d01 (Example 1 of JP-A-2011-12321 ), and 7% for the sample d02 (Example 4 of JP-A-2011-12321 ).
  • the average grain area of the matrix containing the Cube orientation grains was 254 ⁇ m 2 for the sample d01 (Example 1 of JP-A-2011-12321 ) and 201 ⁇ m 2 for the sample d02 (Example 4 of JP-A-2011-12321 ), and the grains were coarsened, respectively.
  • the anisotropy in the deflection coefficient was as large as more than 10 GPa, and the anisotropy in the strength was as large as more than 15 MPa, resulting in that the characteristics required for the present invention were not satisfied.

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US10294554B2 (en) 2013-12-27 2019-05-21 Furukawa Electric Co., Ltd. Copper alloy sheet material, connector, and method of producing a copper alloy sheet material

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KR102370860B1 (ko) * 2014-03-25 2022-03-07 후루카와 덴키 고교 가부시키가이샤 구리합금 판재, 커넥터, 및 구리합금 판재의 제조방법
KR101935987B1 (ko) * 2014-05-30 2019-01-07 후루카와 덴키 고교 가부시키가이샤 구리합금 판재, 구리합금 판재로 이루어지는 커넥터, 및 구리합금 판재의 제조방법
CN105088008A (zh) * 2015-07-26 2015-11-25 邢桂生 一种微合金化铜合金框架带材及其制备方法
CN105088009A (zh) * 2015-07-26 2015-11-25 邢桂生 一种铜合金框架带材及其制备方法
CN113215439A (zh) * 2021-04-16 2021-08-06 安徽绿能技术研究院有限公司 一种高强度铜合金板材及其生产工艺

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US10294554B2 (en) 2013-12-27 2019-05-21 Furukawa Electric Co., Ltd. Copper alloy sheet material, connector, and method of producing a copper alloy sheet material

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