US20130092297A1 - Cu-Co-Si System Alloy Sheet and Method for Manufacturing Same - Google Patents

Cu-Co-Si System Alloy Sheet and Method for Manufacturing Same Download PDF

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US20130092297A1
US20130092297A1 US13/581,715 US201113581715A US2013092297A1 US 20130092297 A1 US20130092297 A1 US 20130092297A1 US 201113581715 A US201113581715 A US 201113581715A US 2013092297 A1 US2013092297 A1 US 2013092297A1
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mass
conducting
rolling
copper alloy
alloy sheet
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US13/581,715
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Hiroshi Kuwagaki
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Assigned to JX NIPPON MINING & METALS CORPORATION reassignment JX NIPPON MINING & METALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KUWAGAKI, HIROSHI
Assigned to JX NIPPON MINING AND METALS CORPORATION reassignment JX NIPPON MINING AND METALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KUWAGAKI, HIROSHI
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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
    • 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
    • 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 a Cu—Co—Si system alloy sheet which is a precipitation hardening copper alloy and suitable for use in a variety of electronic device components, in particular, to a Cu—Co—Si system alloy sheet which has excellent uniform adhesive property for plate.
  • a copper alloy for electronic materials that are used in a connector, switch, relay, pin, terminal, lead frame, and various other electronic components is required to satisfy both high strength and high electrical conductivity (or thermal conductivity) as basic characteristics.
  • high integration and reduction in size and thickness of an electronic component have been rapidly advancing, requirements for copper alloys used in these electronic components have been increasingly becoming severe.
  • precipitation-hardened copper alloys Because of considerations related to high strength and high electrical conductivity, the amount in which precipitation-hardened copper alloys are used has been increasing, replacing conventional solid-solution strengthened copper alloys typified by phosphor bronze and brass as copper alloys for electronic components. With a precipitation-hardened copper alloy, the aging of a solution-treated supersaturated solid solution causes fine precipitates to be uniformly dispersed and the strength of the alloys to increase. At the same time, the amount of solved elements in the copper is reduced and electrical conductivity is improved. For this reason, it is possible to obtain materials having excellent strength, spring property, and other mechanical characteristics, as well as high electrical and thermal conductivity.
  • Ni—Si system copper alloys commonly referred to as Corson alloys are typical copper alloys having relatively high electrical conductivity, strength, and bending workability, and are among the alloys that are currently being actively developed in the industry.
  • Corson alloys fine grains of Ni—Si system intermetallic compounds are precipitated in the copper matrix, thereby increasing strength and electrical conductivity.
  • Patent document 1 discloses that, with the aim of producing Ni—Si—Co system copper alloys having excellent bending workability, electrical conductivity, strength and stress relaxation resistance, amounts of Ni, Si and Co, and mutual relationships thereof are controlled. Further, it discloses average grain sizes being 20 ⁇ m or less. Its production process is characterized in that a first age annealing temperature is higher than a second age annealing temperature (paragraphs 0045 to 0047).
  • Patent document 2 discloses that, with the aim of improving bending workability of Ni—Si—Co system copper alloys, grain coarsening is inhibited by controlling distribution state of secondary-phase grains.
  • This Patent document explains a relationship of precipitates having an effect of inhibiting grain coarsening in high-temperature heat treatment, and distribution states, for copper alloys produced by adding cobalt to Corson alloys.
  • Strength, electrical conductivity, stress relaxation resistance and bending workability are improved by controlling grain size (paragraph 0016). The smaller the grain size is, the more desirable it is.
  • the Patent document discloses that bending workability will improve when the grain size is 10 ⁇ m or less (paragraph 0021).
  • Patent document 3 discloses copper alloys for electronic materials in which generation of coarse secondary-phase grains in Ni—Si—Co system copper alloys is inhibited. This Patent document explains that aimed excellent property can be given when generation of coarse secondary-phase grains is inhibited by conducting a hot rolling and a solution treatment under specific conditions (paragraph 0012).
  • Ni plate is generally formed as a ground plate.
  • the Ni ground plate becomes thinner in proportion to recent needs for being lighter and thinner in the components. Under these circumstances, a defect in Ni plate, which has not been thought as a problem in the past, such as a defect that Ni plate does not partially adhere uniformly, becomes obvious.
  • the object of the present invention is to provide Cu—Co—Si system alloy sheet having excellent uniform adhesive property for ground plate, in particular, Ni plate.
  • the inventors have diligently studied means for solving the problem, and eventually have found out that, in Cu—Ni—Si system alloy sheet, further improved adhesive property for ground plate can be pursued by using Cu—Co—Si system alloy, wherein Ni is replaced by Co in Cu—Ni—Si system. Further, the inventors have found out that, even when average grain size is totally small, uniform adhesive property for plate will deteriorate because grain size of the Cu—Co—Si system alloy sheet is more likely to coarsen in the surface layer locally than in the inward (in the center part of the sheet thickness), and the coarsened crystal exists in the surface.
  • the present inventions comprise the following constitutions.
  • FIG. 1 is a micrograph (magnification ratio: ⁇ 200) of a plate surface of Ni-plated copper alloy sheet of the present invention (inventive example 1).
  • FIG. 2 is a micrograph (magnification ratio: ⁇ 200) of a plate surface of Ni-plated copper alloy sheet of comparative example (comparative example 11).
  • FIG. 3 is a magnified micrograph (magnification ratio: ⁇ 2,500) of a plate surface in FIG. 2 .
  • the additive amounts of Co and Si are such that Co is less than 0.5 mass % and Si is less than 0.1 mass % respectively, the desired strength cannot be achieved, and conversely, when the additive amount of Co and Si are such that Co is more than 3.0 mass % and Si is more than 1.0 mass % respectively, higher strength can be achieved, but electrical conductivity is dramatically reduced and hot workability furthermore deteriorates. Therefore, the additive amounts of Co and Si are such that Co is 0.5 to 3.0 mass % and Si is 0.1 to 1.0 mass % in the present invention.
  • the additive amounts of Co and Si are preferably such that Co is 0.5 to 2.0 mass % and Si is 0.1 to 0.5 mass %.
  • Cr preferentially precipitates along crystal grain boundaries in the cooling process at the time of casting. Therefore, the grain boundaries can be strengthened, cracking during hot rolling is less liable to occur, and a reduction in yield can be inhibited. That is, Cr, being precipitated along the grain boundaries during casting, is solved again by solution treatment and the like, resulting in producing precipitated grains or compounds with Si (silicide), having a bcc structure mainly composed of Cr in the subsequent aging precipitation. With an ordinary Ni—Si system copper alloy, the portion of the added Si, being not contributed to aging precipitation, remains solved in the matrix, and deteriorates electrical conductivity.
  • the Si content solved in the matrix can be reduced and deterioration of electrical conductivity can be inhibited without compromising strength by adding Cr as a silicide-forming element and causing Si, being not contributed to aging precipitation, to further precipitate as silicide.
  • Cr can be added in a maximum amount of 0.5 mass %.
  • the additive amount is preferably 0.01 to 0.5 mass %, and more preferably 0.09 to 0.3 mass %.
  • traces of Mg, Mn, Ag and P improves strength, stress relaxation characteristics, and other manufacturing characteristics without compromising electrical conductivity.
  • the effect of the addition is mainly produced by the formation of a solid solution in the matrix, but the effect can be further produced when the elements are contained in the second-phase grains.
  • the total concentration of Mg, Mn, Ag and P exceeds 2.0 mass %, the effect of improving the characteristics becomes saturated and manufacturability is compromised. Therefore, in the Cu—Co—Si system alloy sheet according to the present invention, a single element or two or more elements selected from Mg, Mn, Ag and P can be added in total in a maximum amount of 2.0 mass %.
  • the additive amount is preferably a total of 0.01 to 2.0 mass %, more preferably a total of 0.02 to 0.5 mass %, and typically a total of 0.04 to 0.2 mass %.
  • the addition of traces of Sn and Zn also improves the strength, stress relaxation characteristics, plating properties, and other product characteristics without compromising electrical conductivity.
  • the effect of the addition is mainly produced by the formation of a solid solution in the matrix.
  • the characteristics improvement effect becomes saturated and manufacturability is compromised. Therefore, in the Cu—Co—Si system alloy sheet according to the present invention, one or two elements selected from Sn and Zn can be added in total in a maximum amount of 2.0 mass %.
  • the additive amount is preferably a total of 0.05 to 2.0 mass %, and more preferably a total of 0.5 to 1.0 mass %.
  • the addition of As, Sb, Be, B, Ti, Zr, Al and Fe also improves electrical conductivity, strength, stress relaxation characteristics, plating properties, and other product characteristics, by adjusting the additive amount thereof, in accordance with the required product characteristics.
  • the effect of the addition is mainly produced by the formation of a solid solution in the matrix, but a further effect can be produced when the above-described elements are added to the second-phase grains or when second-phase grains having a new composition are formed. However, when the total concentration of these elements exceeds 2.0 mass %, the characteristics improvement effect becomes saturated and manufacturability is compromised.
  • the additive amount is preferably a total of 0.001 to 2.0 mass %, and more preferably a total of 0.05 to 1.0 mass %.
  • the total is preferably 2.0 mass % or less, and more preferably 1.5 mass % or less, and further more preferably 1.0 mass % or less.
  • the average grain size in the center part of the sheet thickness, in cross-section surface of rolling direction is 20 ⁇ m or less in the present invention.
  • the average grain size in the center part of the sheet thickness is measured on the basis of JIS H 0501 (cutting method).
  • the average grain size in the center part of the copper alloy sheet thickness of the present invention does not change relatively to a remarkable extent before and after the last rolling at a reduction ratio being 10 to 50%. Accordingly, if the average grain size is 20 ⁇ m or less before the last rolling, the alloy can maintain finer crystal structure than sample copper alloys having the copper average grain size being 20 ⁇ m, even after the last rolling.
  • the average grain size, being 20 ⁇ m or less, in the center part of the sheet thickness” of the present invention is the provision for securing the same high strength with prior art
  • the center part of the sheet thickness” of the present invention is the wording for indicating a measurement position.
  • the inventors of the present invention have found out that Cu—Co—Si system alloy sheet for electronic materials, wherein plates can adhere uniformly to the surface of the alloy sheet, can be provided by decreasing crystal grains coarsened in the surface of the Cu—Co—Si system alloy sheet.
  • the number of the crystal grain being tangent to the surface of the sheet and having 45 ⁇ m or more of the length of major axis, is 5 or less in the area of 1 mm in a rolling direction.
  • the number of the crystal grain is preferably 4 or less, more preferably 2 or less. If the number of the crystal grain exceeds 5, the plates do not adhere to the surface of the alloy sheet uniformly, and the plated products will be defective products, wherein tarnish can be seen on the plates when observed by the unaided eye.
  • the number of the crystal grain being tangent to the cross-section surface of rolling direction and having 45 ⁇ m or more of the length of major axis, is measured by micrograph (magnification ratio: ⁇ 400).
  • the number of the crystal grain is divided by the total length of the measured grain sizes, in the surface area having 2,000 ⁇ m in length, provided by the multiple (10 times) measured views, and then indicated by the millimeter.
  • the copper alloy sheet of the present invention has excellent uniform adhesive property for plate because the number of the crystal grain, being tangent to the surface of the sheet and having 45 ⁇ m or more of the length of major axis, is 5 or less.
  • Various plate materials can be applied to the copper alloy sheet of the present invention.
  • the plate materials include, for example, Ni ground plate which is generally used for a ground plate for Au plate, Cu ground plate, Sn plate and the like.
  • the plate in the alloy sheet of the present inventions has enough uniform adhesive property in the thickness of 2 to 5 ⁇ m as well as 0.5 to 2.0 ⁇ m.
  • the method for manufacturing the copper alloy sheet of the present invention uses general manufacturing processes for the copper alloy sheet (melting and casting ⁇ hot rolling ⁇ intermediate cold rolling ⁇ intermediate solution treatment ⁇ last cold rolling ⁇ aging). However, intended copper alloy sheet is produced by adjusting the following conditions in those steps. If desired, the intermediate rolling and the intermediate solution treatment may be conducted repeatedly more than once.
  • electrolytic cathode copper, Si and Co, and other starting materials are melted to obtain a molten metal having the desired composition. Then the molten metal is cast in a mold to produce an ingot.
  • hot rolling step it is necessary to eliminate crystallized substances such as Co—Si, generated in casting step, to a maximum extent, by conducting heat treatment uniformly. For example, hot rolling is conducted after maintaining at 950 to 1050° C. for 1 hour or more. When the maintaining temperature before the hot rolling is less than 950° C., solubilization is not enough. On the other hand, when the maintaining temperature is more than 1050° C., materials may dissolve.
  • a temperature at the end of the hot rolling is less than 700° C.” means “processing treatments of the last pass or a few passes including the last pass in the hot rolling, are conducted at less than 700° C.”
  • the inward is in the state of recrystallization, while the surface layer ends in the state of being subjected to processing strain.
  • the temperature at the end of the hot rolling is preferably 700° C. or more, more preferably 850° C. or more, and it is preferable to conduct rapid cooling after the end of the hot rolling.
  • the rapid cooling can be achieved by water cooling.
  • an intermediate rolling and an intermediate solution treatment are conducted, by selecting frequency and order of them, within a scope of the purpose.
  • the reduction ratio of the last pass in the intermediate rolling is less than 5%, processing strain energy is accumulated only in the surface of materials. Accordingly, coarsened crystal grains are generated in the surface layer.
  • the reduction ratio of the last pass in the intermediate rolling is preferably 8% or more. Further, controlling viscosity of rolling oil used in the intermediate rolling and rate of the intermediate rolling is also effective for uniform load of the processing strain energy.
  • the intermediate solution treatment is sufficiently conducted, in order to eliminate precipitates such as coarsened Co—Si as much as possible, by dissolving crystallized grains generated at solution casting and precipitated grains generated after hot rolling.
  • the temperature of the solution treatment is less than 850° C.
  • the solution is not enough and then desired strength of alloys cannot be provided.
  • the temperature of the solution treatment is more than 1050° C.
  • materials may be dissolved. Therefore, it is preferable to conduct solution treatment where the materials are heated at 850 to 1050° C.
  • the solution treatment is preferably conducted for 0.5 minutes to 1 hour.
  • the heat time is preferably 1 to 2 minutes at 950° C., and 0.5 to 1 minute at 1000° C.
  • fine secondary-phase grains are precipitated uniformly by conducting aging treatment at temperature conditions of 400° C. or more and 600° C. or less.
  • the aging temperature is less than 400° C.
  • fine secondary-phase grains precipitate insufficiently, and then a problem that desired strength and electrical conductivity cannot be provided, is caused.
  • the aging temperature is more than 600° C.
  • the precipitated secondary-phase grains coarsen, and then a problem that desired strength cannot be provided, is caused.
  • the aging temperature is preferably 450° C. or more and 550° C. or less.
  • a reduction ratio of the last pass is preferably 10 to 50%, more preferably 30 to 50%. When the reduction ratio is less than 10%, desired strength cannot be provided. On the other hand, when the reduction ratio is more than 50%, bending workability deteriorates.
  • the copper alloy sheet of the present invention has no coarsened crystal grains on the surface, and then can be used appropriately for lead frames, connectors, pins, terminals, relays, switches, foil material for secondary batteries, and other electronic components and the like.
  • Standard samples (Co: 1.0 mass %, Si: 0.66 mass %, the balance being Cu), wherein a solution treatment was finished, a last rolling was not finished, and the average grain size in the center part of the sheet thickness in a rolling direction is 20 ⁇ m, were produced.
  • the average grain size was measured according to JIS H 0501 (cutting process). With respect to the standard samples, the last cold rolling (reduction ratio 15%) was conducted, optical micrographs (magnification ratio: ⁇ 400) in the center part of the sheet thickness, in cross-section surface of rolling direction, were taken, and then used as a standard.
  • the grain size was defined to be more than 20 ⁇ m (>20 ⁇ m) when the grain size of the example is larger than that of the standard, and the grain size was defined to be 20 ⁇ m or less ( ⁇ 20 ⁇ m) when the grain size of the example is equal to or less than that of the standard.
  • a line parallel to the surface was drawn at a depth of 10 ⁇ m from the surface layer. Then the length of the line was measured, and at the same time, the number of the crystal grains, wherein at least a part of which was tangent to the surface and a grain size was 45 ⁇ m or more, was counted by line segment method in 10 observation fields. Next, the sum of the number of the crystal grains, having the grain size of 45 ⁇ m or more, was divided by the sum of the line segments, and then the number of the crystal grains, having the grain size of 45 ⁇ m or more, per millimeter, was calculated.
  • Samples are electrolytically degreased in alkaline aqueous solution, by using the samples as cathode.
  • Plating bath composition nickel sulfate 250 g/L, nickel chloride 45 g/L, boric acid 30 g/L
  • Ni plate having 1.0 ⁇ m in thickness was formed by controlling electrodeposition time.
  • the plate thickness was measured by using CT-1-type electrolysis plate thickness tester (DENSOKU INSTRUMENTS) and electrolyte R-54 (KOCOUR).
  • FIG. 1 is the optical micrograph of the plate surface of inventive example 1, and it corresponds to rank “S”.
  • FIG. 2 is the optical micrograph of the plate surface of comparative example 11, and it corresponds to rank “C”.
  • FIG. 3 is the magnified micrograph (magnification ratio: ⁇ 2,500) of “island shaped plate”, observed in the plate surface, and such an island shaped plate was deemed to be one plate. In this way, the number of the island shaped plates in the observation field was counted.
  • Electrical conductivity was determined by measuring volume resistivity with the aid of double bridge.
  • Copper alloys having the compositions shown in Table 1 were melted in a high-frequency melting furnace at 1300° C. and then cast in a mold to produce ingots having a thickness of 30 mm. Next, the ingots were heated for 3 hours, under the conditions shown in Table 1, hot rolled thereafter to a sheet thickness of 10 mm at the temperature when the hot rolling was finished (ending temperature), and soon after the hot rolling, water-cooled to a room temperature.
  • the metals were faced to a thickness of 9 mm in order to remove scales from the surface, and then sheets having a thickness of 0.15 mm were formed, by appropriately conducting cold rolling, wherein a reduction ratio of the last pass was 5 to 15%, and intermediate solution treatment for 0.5 minutes to 1 hour, wherein the temperature of material was 900° C. Soon after the solution treatment, the sheets were water-cooled to a room temperature. Next, the sheets were subjected to an aging treatment in an inert atmosphere at 520° C. for 3 hours, and then the last cold rolling at a reduction ratio being 15% was conducted to produce each test piece. Measurement result of each test piece is shown in Table 1.
  • inventive example 1 The reduction ratio of the intermediate rolling in the last pass, in inventive example 1, was 15%.
  • inventive example 2 having the same composition with inventive example 1, had lower reduction ratio of 10% and then coarsened grains generated in the surface. Accordingly, inventive example 2 was slightly inferior to inventive example 1 in uniformity of adhesive property for plate. The same was true in the relation between inventive examples 4 and 5.
  • inventive example 1 The ending temperature (temperature when hot rolling was completed), in inventive example 1, was 750° C.
  • inventive example 3 having the same composition with inventive example 1, had lower ending temperature of 700° C. Accordingly, inventive example 3 was much inferior to inventive example 1 in uniformity of adhesive property for plate. The same was true in the relation between inventive examples 4 and 6.
  • inventive example 1 the starting temperature in hot rolling was 950° C., and the ending temperature was 750° C.
  • comparative example 11 having the same composition with inventive example 1, had lower starting temperature of 800° C. and lower ending temperature of 500° C. Accordingly, coarsened grains generate in the surface, and therefore comparative example 11 was much inferior to inventive example 1 in uniformity of adhesive property for plate.
  • comparative example 11 The reduction ratio of the intermediate rolling in the last pass, in comparative example 11, was 15%.
  • inventive example 7 the starting temperature in hot rolling was 950° C., the ending temperature was 750° C., and the reduction ratio of the intermediate rolling in the last pass was 15%.
  • comparative example 17, having the same composition with inventive example 7 had lower starting temperature of 800° C., lower ending temperature of 500° C. and lower reduction ratio of 5%. Accordingly, coarsened grains generated in the surface, and therefore comparative example 17 was inferior to inventive example 7 in uniformity of adhesive property for plate.
US13/581,715 2010-06-03 2011-03-24 Cu-Co-Si System Alloy Sheet and Method for Manufacturing Same Abandoned US20130092297A1 (en)

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JP2010-127943 2010-06-03
JP2010127943A JP4708497B1 (ja) 2010-06-03 2010-06-03 Ｃｕ−Ｃｏ−Ｓｉ系合金板及びその製造方法
PCT/JP2011/057216 WO2011152104A1 (fr) 2010-06-03 2011-03-24 Tôle en un alliage à base de cu-co-si et son procédé de production

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EP (1) EP2578708A4 (fr)
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CN (1) CN102666890B (fr)
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WO (1) WO2011152104A1 (fr)

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US10998108B2 (en) 2014-05-30 2021-05-04 Furukawa Electric Co., Ltd. Electrical contact material, method of producing an electrical contact material, and terminal

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JP5437519B1 (ja) 2013-07-31 2014-03-12 Ｊｘ日鉱日石金属株式会社 Ｃｕ−Ｃｏ−Ｓｉ系銅合金条及びその製造方法
JP5437520B1 (ja) * 2013-07-31 2014-03-12 Ｊｘ日鉱日石金属株式会社 Ｃｕ−Ｃｏ−Ｓｉ系銅合金条及びその製造方法
JP6294037B2 (ja) * 2013-09-18 2018-03-14 株式会社Maruwa 複合型ノイズフィルタ
JP6306632B2 (ja) 2016-03-31 2018-04-04 Ｊｘ金属株式会社 電子材料用銅合金

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US10998108B2 (en) 2014-05-30 2021-05-04 Furukawa Electric Co., Ltd. Electrical contact material, method of producing an electrical contact material, and terminal

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EP2578708A1 (fr) 2013-04-10
WO2011152104A1 (fr) 2011-12-08
JP4708497B1 (ja) 2011-06-22
JP2011252216A (ja) 2011-12-15
TWI422693B (zh) 2014-01-11
CN102666890A (zh) 2012-09-12
CN102666890B (zh) 2014-05-07
EP2578708A4 (fr) 2014-04-09

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