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WO2025079295A1 - Matériau en feuille d'alliage de cuivre, produit plié et produit étiré - Google Patents

Matériau en feuille d'alliage de cuivre, produit plié et produit étiré Download PDF

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Publication number
WO2025079295A1
WO2025079295A1 PCT/JP2024/022029 JP2024022029W WO2025079295A1 WO 2025079295 A1 WO2025079295 A1 WO 2025079295A1 JP 2024022029 W JP2024022029 W JP 2024022029W WO 2025079295 A1 WO2025079295 A1 WO 2025079295A1
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Prior art keywords
orientation
copper alloy
alloy sheet
mass
sheet material
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English (en)
Japanese (ja)
Inventor
雅也 東
亮佑 松尾
紳悟 川田
司 高澤
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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
    • 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
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/02—Single bars, rods, wires, or strips
    • 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
    • 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

Definitions

  • This disclosure relates to copper alloy sheet materials, bent products, and drawn products.
  • Cu-Ni-Si alloys have been used for bending in connectors, and various improvements have been made to them through crystal orientation control. However, there have been few reports of Cu-Ni-Si alloys with excellent drawing properties.
  • Patent Document 1 in crystal orientation analysis in EBSD measurement, BR orientation ⁇ 3 6 2 ⁇ ⁇ 8 5 3>, RD-Rotated-Cube orientation ⁇ 0 1 2 ⁇ ⁇ 1 0 0>, Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1>, Copper orientation ⁇ 1 2 1 ⁇ ⁇ 1 1 1>, S orientation ⁇ 2 3 1 ⁇ ⁇ 3 4 6>, Brass orientation ⁇ 1 1 0 ⁇ ⁇ 1 1 2>
  • a copper alloy sheet material is described that has excellent bending workability and strength, with a yield strength of 500 MPa or more and a conductivity of 30% IACS or more.
  • Patent Document 1 discusses bending workability but not drawing workability.
  • drawing processes are mainly divided into round drawing and square drawing.
  • square drawing the corners are drawn while the straight lines are bent, so it is necessary to achieve both bending workability and drawing workability.
  • bending workability and drawing workability have been studied separately up until now, and no copper alloy sheet material that achieves both bending workability and drawing workability has been reported.
  • the Cu-Ni-Si alloys for bending that have been reported so far have strong material anisotropy, so when they are subjected to drawing, the ears develop significantly.
  • the ears grow not only does it damage the shape of the processed product, but wrinkles occur in the valleys of the ears during processing, which can become the starting point of cracks.
  • an additional process is required to remove the ears after processing has been completed. Therefore, ear growth is undesirable, and suppressing ear growth is effective in improving drawing workability. For these reasons, it is not desirable to use Cu-Ni-Si alloys for bending that have been used so far in drawing as is.
  • the objective of this disclosure is to provide a copper alloy sheet material that combines excellent drawing and bending workability, as well as bent and drawn products made from the copper alloy sheet material.
  • FIG. 1 is a schematic diagram showing an example of a drawn product for explaining the ear ratio.
  • FIG. 2 is a schematic diagram showing an example of the bottom surface of a drawn product for explaining the ear ratio.
  • FIG. 3 is a graph showing the relationship between the ratio ⁇ and the earing ratio for the examples and comparative examples in which drawing was possible without generating cracks.
  • a copper alloy sheet material can achieve both excellent drawing workability and bending workability by having a specified alloy composition and controlling the ratio ⁇ of the area ratio of each crystal orientation measured by the EBSD method and the area ratio [W] of the Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1> within a specified range, and have completed the present disclosure based on this knowledge.
  • the copper alloy sheet material of the embodiment has an alloy composition containing 1.00 mass% or more and 5.00 mass% or less of Ni and 0.20 mass% or more and 1.50 mass% or less of Si, with the balance being Cu and unavoidable impurities, and has the following area ratios measured by the EBSD method: [BR] for the BR orientation ⁇ 3 6 2 ⁇ ⁇ 8 5 3>, [C] for the Copper orientation ⁇ 1 2 1 ⁇ ⁇ 1 1 1>, [S] for the S orientation ⁇ 2 3 1 ⁇ ⁇ 3 4 6>, [S] for the Brass orientation ⁇ 1 1 0 ⁇ ⁇ 1 1>, [S] for the Brass orientation ⁇ 1 1 0 ⁇ ⁇ 1 1>.
  • the area ratio of 2> is [B]
  • the area ratio of Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1> is [W]
  • the area ratio of RD-Rotated-Cube orientation ⁇ 0 1 2 ⁇ ⁇ 1 0 0> is [RDW]
  • the area ratio of Goss orientation ⁇ 0 1 1 ⁇ ⁇ 1 0 0> is [G]
  • the ratio of the area ratios of the crystal orientations ⁇ (([BR] + [C] + [S] + [B]) / ([W] + [RDW] + [G])) is 1.4 or more and 3.0 or less
  • [W] is 5.0% or more and 20.0% or less.
  • the copper alloy sheet material of the above embodiment has an alloy composition containing 1.00% by mass to 5.00% by mass of Ni, 0.20% by mass to 1.50% by mass of Si, and the remainder being Cu and unavoidable impurities.
  • the lower limit of the Ni content is 1.00% by mass or more, preferably 1.50% by mass or more, more preferably 2.00% by mass or more, and the upper limit is 5.00% by mass or less, preferably 4.50% by mass or less, more preferably 4.00% by mass or less.
  • Sn (tin) content is 0.10 mass% or more, the stress relaxation resistance of the copper alloy sheet material can be improved.
  • the Sn content is 0.30 mass% or less, the decrease in the electrical conductivity of the copper alloy sheet material can be suppressed. Therefore, the Sn content is preferably 0.10 mass% or more and 0.30 mass% or less.
  • the Zn (zinc) content is 0.10 mass% or more, the adhesion and migration properties of the Sn plating can be improved.
  • the Zn content is 0.50 mass% or less, the decrease in the electrical conductivity of the copper alloy sheet material can be suppressed. Therefore, the Zn content is preferably 0.10 mass% or more and 0.50 mass% or less.
  • ⁇ Fe 0.05% by mass or more and 0.30% by mass or less>
  • the content of Fe (iron) is 0.05% by mass or more, grain growth after dynamic recrystallization during hot rolling can be suppressed, and roughness of the drawn product can be suppressed.
  • the content of Fe is 0.30% by mass or less, the generation of coarse Fe-containing crystals during casting is suppressed, improving the drawing workability. The coarse Fe-containing crystals are likely to become the starting point of cracks during drawing. For this reason, the content of Fe is preferably 0.05% by mass or more and 0.30% by mass or less.
  • Cu and inevitable impurities The remainder other than the above-mentioned components is Cu (copper) and inevitable impurities.
  • Inevitable impurities refer to impurities at a level that are inevitably mixed in during the manufacturing process. Since the content of inevitable impurities may affect the properties of the copper alloy sheet material, it is preferable that the content of inevitable impurities is small. Examples of inevitable impurities include nonmetallic elements such as S (sulfur), C (carbon), and O (oxygen), and elements such as Sb (antimony).
  • the upper limit of the content of inevitable impurities is preferably 500 ppm or less for each of the above elements, and preferably 2000 ppm or less in total for the above elements.
  • the direction in which ears occur is correlated with the ratio ⁇ of the area ratio of the above crystal orientations, and the ear ratio can be suppressed by controlling the ratio ⁇ within a specified range.
  • FIG. 1 is a schematic diagram showing an example of a drawn product for explaining the ear ratio.
  • FIG. 2 is a schematic diagram showing an example of the bottom surface of a drawn product for explaining the ear ratio.
  • the direction parallel to the rolling direction of the copper alloy sheet material is set to 0°.
  • the heights from the bottom surface to the upper edge of the drawn product at positions of 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° are set to H0, H45, H90, H135, H180, H225, H270, and H315, respectively.
  • the ear ratio can be calculated from the following formula.
  • the ear ratio will be positive, and if the ears appear at the positions of 0°, 90°, 180°, and 270°, the ear ratio will be negative.
  • the bending and drawing workability of copper alloy sheet material varies greatly depending on the anisotropy of the copper alloy sheet material, that is, the crystal orientation of the copper alloy sheet material. It is widely known that bending workability is improved by accumulation in the Cube orientation. However, accumulation in a specific orientation increases the material anisotropy, resulting in larger drawing ears. On the other hand, it is known that with respect to drawing, the less the Cube orientation, the less likely breakage occurs during processing and the better the drawing workability. Therefore, in order to achieve both drawing workability and bending workability, it is preferable to reduce accumulation in a specific crystal orientation and have various crystal orientations present to the same extent, and it is also preferable to introduce an appropriate amount of Cube orientation.
  • the ratio ⁇ When the ratio ⁇ is 1.4 or more and 3.0 or less, the ears become small, making it easier to perform uniform drawing.
  • the ratio ⁇ When the ratio ⁇ is less than 1.4, the 0° ears become very large, and the drawing workability of the copper alloy sheet material is significantly reduced.
  • the ratio ⁇ when the ratio ⁇ is less than 1.4, the Cube orientation, which has a negative effect on the drawing workability, is excessively formed, and breakage frequently occurs during drawing.
  • the ratio ⁇ when the ratio ⁇ is more than 3.0, the 45° ears become very large, and the drawing workability of the copper alloy sheet material is significantly reduced.
  • the lower limit of the ratio ⁇ is 1.4 or more, preferably 1.5 or more, and the upper limit is 3.0 or less, preferably 2.1 or less.
  • the area ratio [W] of the Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1> is 5.0% or more and 20.0% or less, the material anisotropy of the copper alloy sheet material is reduced and the copper alloy sheet material can exhibit excellent bending workability.
  • [W] is less than 5.0%, the bending workability of the copper alloy sheet material is insufficient.
  • the presence of excessive Cube orientation significantly reduces the drawing workability of the copper alloy sheet material.
  • [W] is more than 20.0%, the material anisotropy of the copper alloy sheet material is high, so that the ears become large, the drawing workability of the copper alloy sheet material is reduced, and in some cases, breakage during drawing is likely to occur.
  • the lower limit of [W] is 5.0% or more, preferably 10.0% or more, and the upper limit is 20.0% or less, preferably 18.0% or less.
  • the area ratio of each crystal orientation can be obtained from crystal orientation analysis data calculated using analysis software (OIM Analysis, manufactured by TSL) from crystal orientation data continuously measured using an EBSD detector attached to a high-resolution scanning analytical electron microscope (JSM-7001FA, manufactured by JEOL Ltd.).
  • EBSD Electron Backscatter Diffraction
  • the EBSD method is a crystal orientation analysis technique that uses reflected electron Kikuchi diffraction that occurs when an electron beam is irradiated on a copper alloy sheet material, which is a measurement sample, inside a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • OIM Analysis is analysis software that analyzes data measured by EBSD.
  • the average crystal grain size in the cross section perpendicular to the rolling direction of the copper alloy sheet is preferably 30 ⁇ m or less, and more preferably 25 ⁇ m or less.
  • the area ratio [W] of the Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1> may decrease. Therefore, the average crystal grain size in the cross section perpendicular to the rolling direction of the copper alloy sheet is preferably 5 ⁇ m or more.
  • the copper alloy sheet material of the embodiment has both excellent drawing workability and bending workability, and is therefore suitable as a copper alloy sheet material for bending and a copper alloy sheet material for drawing.
  • Bent products obtained by bending a copper alloy sheet material for bending which is a copper alloy sheet material before bending, i.e., bent products using copper alloy sheet material
  • drawn products obtained by drawing a copper alloy sheet material for drawing which is a copper alloy sheet material before drawing, i.e., drawn products using copper alloy sheet material
  • the ingot having the above alloy composition obtained by melting and casting [step 1] is sequentially subjected to reheating [step 2], hot rolling [step 3], intermediate annealing [step 4], first cold rolling [step 5], solution heat treatment [step 6], second cold rolling [step 7], aging heat treatment [step 8], third cold rolling [step 9], and low-temperature annealing [step 10] to manufacture the copper alloy sheet material of the above embodiment.
  • the alloy components are melted and cast to obtain a copper alloy ingot having the above alloy composition.
  • melting is carried out in air using a high-frequency melting furnace.
  • the type of alloy components, casting conditions, etc. are set appropriately.
  • step 4 In the intermediate annealing [step 4] performed after the hot rolling [step 3], a heat treatment is performed at a temperature of 400°C to 600°C for 30 seconds to 2 hours, and Ni 2 Si precipitates are precipitated, which changes the solid solution state and generates a pinning effect of the crystal grains.
  • the development of a specific crystal orientation can be suppressed.
  • the Cube orientation that is not developed in the conventional process appears, and various crystal orientations tend to develop.
  • the material anisotropy is reduced, and the ears during drawing are reduced.
  • step 7 cold rolling with a processing rate of 10% to 30% is performed.
  • step 6 various crystal orientations are formed, but the material anisotropy is still high, resulting in a high earing rate after drawing.
  • the area ratio of not only the Cube orientation but also the RDW orientation increases. Therefore, by performing this step, the material anisotropy is significantly suppressed by forming an appropriate amount of the Copper orientation and S orientation, which are the main rolling textures, and the earing rate is reduced. As a result, the RDW orientation and Goss orientation formed excessively in the solution heat treatment can be reduced.
  • the Cube orientation is less likely to rotate due to rolling due to the symmetry of the crystal orientation with respect to the plate material, so the Cube orientation, which is advantageous for bending workability, can be retained. Furthermore, this process refines the crystal grains that were coarsened during the solution heat treatment [Step 6], improving bending workability. If the processing rate is less than 10%, there is little change in crystal orientation and crystal grain size. If the processing rate is more than 30%, a strong rolling texture develops again, increasing material anisotropy and worsening earing.
  • cold rolling is performed with a processing rate of 5% to 20%. If the processing rate is less than 5%, the effect of increasing the material strength is small. If the processing rate is more than 40%, rolling textures such as Brass orientation and S orientation are likely to develop, and anisotropy is likely to increase, resulting in a decrease in the drawability of the copper alloy sheet material.
  • the temperature is kept at 200°C to 600°C for 10 seconds to 30 minutes.
  • each component was melted in the atmosphere using a high-frequency melting furnace and cast in a metal mold to obtain a copper alloy ingot having the copper alloy composition shown in Table 1.
  • the copper alloy ingot was reheated [step 2] by heat treating it at a temperature in the range of 900 ° C. to 1050 ° C.
  • Ratio of area ratio of crystal orientation ⁇ The area ratio of each crystal orientation was obtained from crystal orientation analysis data calculated using analysis software (TSL, OIM Analysis) from crystal orientation data continuously measured using an EBSD detector attached to a high-resolution scanning analytical electron microscope (JSM-7001FA, manufactured by JEOL Ltd.).
  • the measurement part was a surface (main surface) of a copper alloy sheet material mirror-finished by electrolytic polishing, the measurement area was 1000 ⁇ m ⁇ 1000 ⁇ m (1,000,000 ⁇ m 2 ), and the scan step size was 0.2 ⁇ m.
  • Figure 3 is a graph showing the relationship between the ratio ⁇ and the earing ratio for examples and comparative examples in which drawing was possible without cracking.
  • examples 1 to 24 had a specified alloy composition, and the ratio ⁇ and the area ratio [W] of the Cube orientation ⁇ 1 0 0 ⁇ ⁇ 0 0 1> were each controlled within a specified range, so both the drawing workability and bending workability were excellent.
  • at least one of the alloy composition, ratio ⁇ , and [W] was outside the specified range, so at least one of the drawing workability and bending workability was poor.
  • Example 4 the temperature of the intermediate annealing [Step 4] was higher than that of Example 1, so the area ratio of the Cube orientation was larger, ⁇ was smaller, and the earing ratio was improved compared to Example 1.
  • Example 5 the temperature of the intermediate annealing [Step 4] was even higher than that of Example 4, so the area ratio of the Cube orientation was even larger, ⁇ was even smaller, and the earing ratio was even more improved.
  • Example 6 the processing time of the intermediate annealing [step 4] was longer than that of Example 1, so that the area ratio of the Cube orientation was larger, ⁇ was smaller, and the earing ratio was improved compared to Example 1.
  • Example 15 to 23 the Ni content, Si content, and optional component content were different from those of Examples 1 to 14, but were within the specified range, so that both the drawing workability and bending workability were excellent.
  • Example 24 the optional component content was not within the preferred range, but the drawing and bending workability was superior to Comparative Examples 1 to 11.
  • Comparative Example 8 since the Ni content was low, the area ratio of the Cube orientation was high and the specimen broke during drawing. In Comparative Example 9, since the Si content was low, the area ratio of the Cube orientation was high, the ratio ⁇ was small, and the ear ratio was deteriorated. In Comparative Example 10, since the Si content was high and the elongation was reduced, the specimen broke during drawing, and since the Cube orientation was low, the bending workability was also deteriorated. In Comparative Example 11, since both the Ni content and the Si content were low, the area ratio of the Cube orientation was high, the specimen broke during drawing, the average crystal grain size became coarse, and the bending workability was also deteriorated.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Abstract

Le matériau en feuille d'alliage de cuivre de la présente invention a une composition d'alliage contenant 1,00 à 5,00 % en masse de Ni et 0,20 à 1,50 % en masse de Si, la partie restante étant du Cu et des impuretés inévitables, et conduit à un rapport de pourcentage de superficie d'orientation cristalline γ (([BR]+[C]+[S]+[B])/([W]+[RDW]+[G])) de 1,4 à 3,0 et [W] de 5,0 à 20,0 %, lorsque, tels que mesurés par un procédé EBSD, [BR] représente le pourcentage de superficie d'orientation BR {3 6 2}<8 5 3>, [C] représente le pourcentage de superficie d'orientation du cuivre {1 2 1}<1 1 1>, [S] représente le pourcentage de superficie d'orientation S {2 3 1}<3 4 6>, [B] représente le pourcentage de superficie d'orientation du laiton {1 1 0}<1 1 2>, [W] représente le pourcentage de superficie d'orientation cubique {1 0 0}<0 0 1>, [RDW] représente le pourcentage de superficie d'orientation cubique à rotation RD {0 1 2}<1 0 0>, et [G] représente le pourcentage de superficie d'orientation Goss {0 1 1}<1 0 0>.
PCT/JP2024/022029 2023-10-10 2024-06-18 Matériau en feuille d'alliage de cuivre, produit plié et produit étiré Pending WO2025079295A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011068135A1 (fr) * 2009-12-02 2011-06-09 古河電気工業株式会社 Feuille d'alliage de cuivre et son procédé de fabrication
JP2012197503A (ja) * 2011-03-09 2012-10-18 Jx Nippon Mining & Metals Corp Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法
JP2013047360A (ja) * 2011-08-29 2013-03-07 Jx Nippon Mining & Metals Corp Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法
JP2021046590A (ja) * 2019-09-19 2021-03-25 Ｊｘ金属株式会社 銅合金、伸銅品及び電子機器部品
JP7328472B1 (ja) * 2022-02-04 2023-08-16 古河電気工業株式会社 銅合金板材、および銅合金板材を用いて作製された絞り加工部品

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011068135A1 (fr) * 2009-12-02 2011-06-09 古河電気工業株式会社 Feuille d'alliage de cuivre et son procédé de fabrication
JP2012197503A (ja) * 2011-03-09 2012-10-18 Jx Nippon Mining & Metals Corp Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法
JP2013047360A (ja) * 2011-08-29 2013-03-07 Jx Nippon Mining & Metals Corp Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法
JP2021046590A (ja) * 2019-09-19 2021-03-25 Ｊｘ金属株式会社 銅合金、伸銅品及び電子機器部品
JP7328472B1 (ja) * 2022-02-04 2023-08-16 古河電気工業株式会社 銅合金板材、および銅合金板材を用いて作製された絞り加工部品

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