EP2256219A1 - Matériau d'alliage de cuivre - Google Patents

Matériau d'alliage de cuivre Download PDF

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Publication number
EP2256219A1
EP2256219A1 EP09712614A EP09712614A EP2256219A1 EP 2256219 A1 EP2256219 A1 EP 2256219A1 EP 09712614 A EP09712614 A EP 09712614A EP 09712614 A EP09712614 A EP 09712614A EP 2256219 A1 EP2256219 A1 EP 2256219A1
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Prior art keywords
mass
copper alloy
alloy material
rolling
compound
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EP09712614A
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German (de)
English (en)
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EP2256219A4 (fr
Inventor
Kiyoshige Hirose
Tatsuhiko Eguchi
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Furukawa Electric Co Ltd
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Furukawa Electric Co Ltd
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Publication of EP2256219A1 publication Critical patent/EP2256219A1/fr
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Withdrawn legal-status Critical Current

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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 copper alloy material.
  • the high mechanical strength alloys such as titanium-copper and beryllium-copper
  • copper alloys such as phosphor bronze
  • the beryllium-copper contains metallic beryllium which is harmful to human bodies
  • substitution materials are desired from the viewpoints of production process and environmental considerations.
  • a Cu-Ni-Si-based alloy (Corson alloy), which is relatively not expensive in the production cost and which is excellent in the balance between mechanical strength and electrical conductivity, has attracted attention and has come to be used as a copper alloy for connectors.
  • the Cu-Ni-Si-based alloy is a precipitation-type alloy in which a precipitate, which is comprised of Ni and Si, is to be formed and the resultant alloy is hardened, and the hardening ability is very high.
  • the fatigue property is enhanced concomitantly with an increase in tensile strength.
  • the Cu-Ni-Si-based alloy it is difficult to maintain a bending property as the tensile strength increases.
  • the stress relaxation resistance deteriorates, when a high processing rate is introduced for a material in order to obtain a tensile strength. Therefore, in order to obtain a mechanical strength and a bending property needed for achieving product functions, and to obtain reliability upon the use of products, there has been a demand to develop a Cu-Ni-Si alloy that satisfies both of a favorable stress relaxation resistance and a favorable fatigue property.
  • the present invention is contemplated for providing a copper alloy material, which has a high mechanical strength, is excellent in the bending property and the stress relaxation resistance, and is also excellent in the fatigue property, and which is suitable for terminals, connectors, switches, relays, and the like, for electric / electronic equipments.
  • the inventors have conducted investigations on copper alloy materials suitable for the use in electric / electronic parts, and have found that, upon an aging treatment, a precipitate free zone (PFZ) is formed in the vicinity of a grain boundary in a copper alloy, and since this precipitate free zone is lower in mechanical strength as compared with that of the inside of grains, when the copper alloy is subjected to processing or repeated stress, deformation occurs dominantly, causing deterioration of a bending property and a fatigue property, but when the width of the precipitate free zone is narrowed, the precipitate free zone can be rendered harmless.
  • PFZ precipitate free zone
  • the Cu-Ni-Si-based copper alloy material of the present invention is a copper alloy material which has a high mechanical strength and is excellent in all of the bending property, the stress relaxation resistance, and the fatigue property, as compared with conventional copper alloy materials.
  • the copper alloy material means a copper alloy processed into a particular shape, for example, a sheet material, a strip material, or a foil, by rolling.
  • Nickel (Ni) and silicon (Si) in a copper alloy form mainly a Ni 2 Si phase via an aging treatment, to enhance the mechanical strength and improve the electrical conductivity of the resultant copper alloy.
  • the content of Ni is 1.8 to 5.0 mass%, and preferably 2.0 to 4.8 mass%. The reason for defining as such is that, if the content is less than 1.8 mass%, a sufficient mechanical strength required of a copper alloy for the use in connectors cannot be obtained.
  • the content of Si is 0.3 to 1.7 mass%, and preferably 0.35 to 1.6 mass%.
  • the reason for defining as such is that, if the amount of Si is less than 0.3 mass%, the enhancement of mechanical strength by the aging treatment is insufficiently achieved, and a sufficient mechanical strength cannot be obtained.
  • the content of Si is more than 1.7 mass%, it becomes a cause of lowering of electrical conductivity, in addition to occurrence of the above problems that are similar to the case where the amount of Ni is too large. Since Ni and Si form mainly the Ni 2 Si phase, there is an optimal ratio between Ni and Si in order to enhance the mechanical strength.
  • a ratio, Ni / Si, between Ni (mass%) and Si (mass%) is determined to be 4.2, in the case where the Ni 2 Si phase is formed regarding the amount of Si. Further, it is preferable to control the Ni/Si to be within a range of 3.0 to 6.0 with the above-mentioned value to be a central value, and more preferably within a range of 3.8 to 4.6.
  • S Sulfur
  • the content is specified to be less than 0.005 mass%, particularly preferably less than 0.002 mass%.
  • Mg magnesium
  • the amount is 0.01 to 0.20 mass%. Mg is able to improve the stress relaxation property largely, but affects as negatively to the bending property.
  • the amount of Mg is 0.01 mass% or more in order to improve the stress relaxation property, and the more the amount is, the better the improvement becomes to be. However, in the case where the amount is more than 0.20 mass%, it becomes unable to satisfy the required level of bending property.
  • the amount is preferably 0.05 to 0.15 mass%.
  • tin (Sn) into the copper alloy.
  • the amount is 0.05 to 1.5 mass%. Sn co-relating to Mg each other is able to improve the stress relaxation property further, but the effect is not so large with comparing to that according to Mg. In the case where Sn is less than 0.05 mass%, it is not able to obtain the effect sufficiently. On the other hand, in the case where the amount is more than 1.5 mass%, the electrical conductivity lowers conspicuously.
  • the amount is preferably 0.1 to 0.7 mass%.
  • Zn zinc
  • the amount is 0.2 to 1.5 mass%.
  • Zn is able to improve the bending property slightly. By containing Zn in an amount of 0.2 to 1.5 mass%, it becomes possible to obtain the bending property corresponding to the standard without any problem for a practical use even adding Mg with 0.20 mass% at the maximum.
  • Zn is able to improve, for example, adherence or migration of Sn plating or solder plating. In the case where the amount of Zn is less than 0.2 mass%, it is not able to obtain the effect sufficiently, and on the other hand, in the case where the amount is more than 1.5 mass%, the electrical conductivity becomes lowered.
  • the amount is preferably 0.3 to 1.0 mass%.
  • the copper alloy can contain any one or two or more selected from the group consisting of scandium (Sc), yttrium (Y), titanium (Ti), zirconium (Zr), hafnium (Hf), vanadium (V), molybdenum (Mo), and silver (Ag), in an amount of 0.005 to 0.3 mass% in total.
  • Sc, Y, Ti, Zr, Hf, V, and Mo respectively forms a compound together with Ni or Si, which is effective to restrict coarsening of grains in the grain size.
  • those may be added singly or in combination of two or more, within the above-mentioned range by which the properties, for example, mechanical strength or electrical conductivity, would not be worsened.
  • Ag is able to improve heat resistance and enhance mechanical strength, and is effective to restrict coarsening of grains in the grain size to improve the bending property.
  • the amount of Ag is less than 0.005 mass%, it is not able to obtain the effect sufficiently.
  • the amount is more than 0.3 mass%, it becomes a cause of a high cost of production, although there is no affect as negatively to be given to the properties of the resultant copper alloy.
  • the content of Ag is preferably within the above-mentioned range, from the viewpoints of those.
  • Manganese (Mn) has an effect to improve hot workability.
  • the addition in an amount of 0.01 to 0.5 mass% is effective in such a level that no deterioration would occur to the electrical conductivity.
  • Cobalt (Co) forms a compound with Si, which is similar to Ni, and has an effect to enhance the mechanical strength.
  • the amount is more than 2.0 mass%, a crystallized and/or precipitated product occurs even after a solution treatment which does not contribute to enhancement of the mechanical strength, thereby resulting in deterioration of the bending property.
  • Chromium (Cr) is precipitated finely into the copper, to contribute to enhancement of the mechanical strength, and Cr forms a compound with Si or with Ni and Si, which is effective to restrict coarsening of grains in the grain size, similar to the above-mentioned group of Sc, Y, Ti, Zr, Hf, V, and Mo.
  • the amount is less than 0.005 mass%, it is not able to obtain the effect sufficiently.
  • the amount is more than 1.0 mass%, the bending property is deteriorated.
  • the respective amount is determined within the range of 0.005 to 2.0 mass% in total, according to the required characteristics.
  • the tensile strength TS is defined, which is in the direction parallel to rolling (LD) of the copper alloy material having the composition mentioned above.
  • LD direction parallel to rolling
  • the rolling direction is identical.
  • a mechanical strength of the copper alloy material is required in order to maintain a springiness or spring property, but when the mechanical strength is markedly enhanced by working or the like, the bending property deteriorates.
  • the Si content has a region that is optimal for the ratio of contents of Ni and Si as described above, and the Si content can be representatively defined by the Ni content, C. If the tensile strength TS is too small, this implies that the contents of Ni and Si are large relative to the mechanical strength, and the cost increases.
  • TS is a value determined according to JIS Z 2241. TS is preferably such that (130 ⁇ C+350) ⁇ TS ⁇ (130 ⁇ C+600).
  • the average grain diameter d (mm) of the grains of the matrix of the copper alloy material is such that 0.001 ⁇ d ⁇ 0.020.
  • the reason for defining the average grain diameter d to be 0.001 mm or more and 0.020 mm or less is because, if the average grain diameter d is less than 0.001 mm, the recrystallized structure is apt to have mixed grains (which is a structure in which grains with different sizes are co-exist), and the bending property and stress relaxation resistance are deteriorated.
  • the grain diameter d is a value measured based on JIS H 0501 (cutting method).
  • the number of measurements for determining the grain diameter d is set at 1,000 or more.
  • the average grain diameter d (mm) is preferably such that 0.001 ⁇ d ⁇ 0.015.
  • the precipitate free zone (PFZ) is formed at the vicinity of the grain boundary in the course of the aging treatment, and is a region where no precipitate is present.
  • Fig. 1 is a transmission electron microscopic photograph at the vicinity of the grain boundary including the precipitate free zone of one example of the copper alloy material of the present invention. Since the precipitate free zone (PFZ) is a region where no precipitate is present, the precipitate free zone (PFZ) is relatively softer than the inside of grains. Therefore, when the copper alloy material is subjected to deformation or loaded with repeated stress, deformation progresses dominantly and the PFZ serves as an origin of cracks, and the PFZ serves as an origin of fatigue fracture due to accumulation of dislocations.
  • the width W of the PFZ is obtained, by taking transmission electron microscopic photographs of two visual fields at the vicinity of the grain boundary of a copper alloy sheet, with the incident direction of the beam aligned to the (100) plane, at a magnification of 50,000 times, measuring the width of PFZ at 5 sites per one visual field, and calculating an average value of 10 sites in total.
  • W is preferably from 0 to 100 nm.
  • the compound on the grain boundary is mainly an intermetallic compound, and is harder as compared with the inner part of the grain and the precipitate free zone.
  • the copper alloy material is subjected to deformation or repeated stress, there occurs a difference in mechanical strength between the hard compound and the structure surrounding the compound, and thus dislocations are apt to accumulate in the copper alloy structures near the compound and serve as the origin of cracks and the origin of fatigue fracture. Therefore, when the compound on the grain boundary is smaller, brittleness of the copper alloy structure is alleviated.
  • the average particle diameter L (nm) of the compound on the grain boundary is such that 10 ⁇ L ⁇ 800.
  • the average particle diameter L of the compound When the average particle diameter L of the compound is 800 nm or less, the compound does not much affect the deterioration of bending property and fatigue property.
  • the average particle diameter L of the compound is preferably 500 nm or less.
  • the compound present on the grain boundary has an effect of suppressing the movement of grains and thereby maintaining the grain diameter fine. For that reason, the particle diameter L is 10 nm or more, and preferably 30 nm or more.
  • the average particle diameter L of the compound on the grain boundary is determined, by taking transmission electron microscopic photographs of five visual fields of the grain boundary of the copper alloy material, with the incident direction of the beam aligned to (100) plane, at a magnification of 50,000 times, measuring the major axis and the minor axis for an individual compound to take an average of the axes as the particle diameter of the compound, and averaging the particle diameters of 20 pieces of compounds.
  • Fig. 2 is an explanatory diagram schematically showing the method of determining the width W of the precipitate free zone and the particle diameter L of the compound on the grain boundary, according to the present invention.
  • reference numeral 1 represents the grain boundary
  • reference numeral 2 represents the compound on the grain boundary
  • reference numeral 3 represents a Ni 2 Si precipitate in the grain.
  • the width W of the precipitate free zone can be determined, by measuring the distance from the grain boundary 1 to the boundary of a region (where no precipitates are present) formed by one grain.
  • the average particle diameter L of the compound on the grain boundary can be determined, by measuring the major axis and the minor axis of the compound 2 on the grain boundary, calculating the average of the axes as the particle diameter of the compound, and averaging the particle diameters of 20 compounds.
  • the grain, the precipitate free zone, and the grain boundary compound interact with each other when the copper alloy is subjected to deformation or repeated stress.
  • the average grain diameter d, the width W of the precipitate free zone, or the average particle diameter L of the grain boundary compound respectively satisfy the definitions described above, and only when all of the definitions are satisfied, brittleness of the copper alloy structure can be alleviated.
  • Casting is conducted by a general semi-continuous casting method, a so-called DC (direct chill) casting method, or the like. Then, the resultant ingot is subjected to a homogenization treatment, for example, at a temperature of 850 to 1,000°C for 0.5 to 6 hours, and then the resultant homogenized ingot is immediately subjected to a hot-rolling at a temperature of 600 to 1,000°C. After the hot-rolling, a cold-rolling is conducted appropriately.
  • a homogenization treatment for example, at a temperature of 850 to 1,000°C for 0.5 to 6 hours
  • the precipitate formed upon cooling after the hot-rolling is apt to become coarse, and coarse compounds of size 1,000 nm or more may often remain on the grain boundary of the final products, causing deterioration of bending property and fatigue property.
  • cloth rolling after face milling the oxide layer it is preferable to conduct cloth rolling after face milling the oxide layer. The cloth rolling is preferably conducted such that said rolling would be conducted to a sheet thickness with which a predetermined working ratio in the cold-rolling of the subsequent steps can be given.
  • a solution treatment is conducted by determining the temperature according to the Ni content, C. It is preferable that the solution treatment is conducted to the extent that the actual (substance's) temperature Tst (°C) of the material satisfies the formula (5). 54 ⁇ C + 625 ⁇ Tst ⁇ 54 ⁇ C + 725 As the temperature of the solution treatment is raised, the average particle diameter L of the precipitate on the grain boundary is decreased, and the width W of the precipitate free zone is narrowed. Then, a satisfactory solid solution state can be obtained, and it is possible to obtain a high mechanical strength upon the aging treatment in the subsequent steps.
  • the Tst when the Tst is in a range that exceeds the upper limit of the formula shown above, the grains are coarsened and the average grain diameter d does not fall in the above range, possibly resulting in deterioration of bending property.
  • the Tst is below the lower limit of the formula, dislocation structures resulting from a cold-working of plain rolling may remain behind, possibly causing deterioration of bending property.
  • an aging treatment causes the Ni 2 Si compound uniformly dispersed and precipitated in the copper alloy, thereby enhancing the mechanical strength and the electrical conductivity. It is preferable to maintain the copper alloy at an actual substance temperature of 350 to 600°C for 0.5 to 12 hours, using a batch-type furnace. If the temperature at the aging treatment is lower than 350°C, a longer period of time is required to obtain a sufficient precipitation amount of Ni 2 Si, and the costs increase, or the tensile strength and electrical conductivity may become insufficient.
  • the temperature at the aging treatment is higher than 600°C, coarsened Ni 2 Si is formed at the inside of the grains, thus lowering the mechanical strength, and since the width W of the precipitate free zone is broadened at the vicinity of the grain boundary, the bending property and the fatigue property may deteriorate.
  • the treatment period of time if it is less than 0.5 hours, sufficient properties may not be obtained, and if it is longer than 12 hours, not only the costs increase but also the width W of the precipitate free zone is broadened, possibly causing deterioration of the bending property and fatigue property.
  • a cold-rolling may be conducted in mid course of from the solution treatment to the aging treatment.
  • the dislocations introduced by this cold-rolling serve to accelerate precipitation of the Ni 2 Si compound, and also have a function of decreasing the width of the precipitate free zone W. If the cold-working ratio at this is too high, the bending property deteriorates, and thus it is preferable to conduct the cold-rolling at 50% or less.
  • the aging treatment functions to reduce the width W of the precipitate free zone
  • the aging treatment may also be conducted twice.
  • it is preferable to conduct the aging treatments by dividing the aging treatment temperature mentioned above into a temperature region 1: 350 to 450°C and a temperature region 2: 450 to 600°C, and conducting the treatment once each at the temperature region 1 and at the temperature region 2.
  • the order of conducting the treatments at the temperature region 1 and the temperature region 2 may be such that any one temperature region may precede the other.
  • a cold-rolling may be carried out at 50% or less, to accelerate precipitation of the Ni 2 Si compound.
  • a finish cold-rolling is conducted for the purpose of enhancing the tensile strength.
  • the finish cold-rolling may not be introduced. If the rolling ratio of the finish cold-rolling is too high, the bending property deteriorates, and the stress relaxation resistance also deteriorates. Therefore, it is preferable to set the rolling ratio of the finish rolling at 50% or less.
  • a low-temperature annealing is conducted for the purpose of restoring the elongation, the bending property, and the spring limit value, while maintaining the mechanical strength to a certain extent.
  • the step of low-temperature annealing may be omitted. It is preferable to conduct the annealing at an actual substance temperature of 300 to 600°C for a short time period of 5 to 60 seconds. If the temperature at the annealing is lower than 300°C, restoration of the elongation, the bending property, and the spring limit value may be insufficient. If the temperature at the annealing is higher than 600°C, a decrease in mechanical strength may occur.
  • each of the copper alloy materials in the Examples according to the present invention and the Comparative Examples was formed of a copper alloy (Alloy Nos. 1 to 25) which had a chemical composition (the balance of Cu), as shown in Table 1, respectively.
  • Each of those copper alloys was dissolved with a high-frequency melting furnace, and then the melt was cast into an ingot of thickness 30 mm, width 120 mm, and length 150 mm. Then, each of those ingots were heated to 980°C, and maintained at this temperature for one hour, followed by a hot-rolling to thickness 12 mm, and a cooling quickly.
  • the oxide layer was removed by face-milling the both sides at 1.5 mm each. Then, the resultant respective alloy was worked to thickness 0.16 to 0.50 mm by a cold-rolling. At this time, regarding Alloy No. 22 due to the too high amount of Sn, cobber cracks occurred upon the cold-rolling, and the subsequent steps were stopped in the production of this. Then, the resultant respective alloy was subjected to a heat treatment at 800°C to 950°C for 30 sec, followed immediately by a cooling with a cooling rate of 15°C/sec or more.
  • the thus-cooled respective alloy was subjected to a cold-rolling at various rolling ratios of 0 to 50% (when the rolling ratio was 0%, without conducting any cold-rolling) before an aging treatment, and the thus-rolled alloy was subjected to the aging treatment at 500°C for 2 hours under an inert gas atmosphere.
  • a rolling ratio of 0% means that no rolling was conducted.
  • the copper alloy sheet was either subjected to a heat treatment of applying the two aging treatments, or subjected to a heat treatment of heating at 400°C for 4 hours and then heating at 500°C for 2 hours in an inert gas atmosphere, or subjected to a heat treatment of heating at 500°C for 2 hours and then heating at 400°C for 4 hours. The details on those will be described in the below. Then, a finish rolling was conducted at various rolling ratios, and finally the sheet thickness was adjusted to 0.15 mm. After the finish rolling, the copper alloy sheet was subjected to a low-temperature annealing at 400 to 600°C for 30 seconds. In the above-manner, copper alloy materials of Examples and Comparative Examples were produced, and the following various property evaluations were carried out thereon.
  • Examples 1-1 to 1-6 and Comparative Examples 1-7 to 1-10 are the cases in which Alloy No. 1 was subjected to the heat treatment and rolling in the different conditions each other within the ranges mentioned above, and Examples 2-1 to 2-2 are the cases in which Alloy No. 2 was subjected to those similarly in the above. Further, Nos. 3 to 18 are samples produced from Alloys Nos. 3 to 18, respectively.
  • Example 1-1 to 1-6 and Comparative Examples 1-7 to 1-10 are described.
  • the conditions not described in Examples 1-2 to 1-6 and Comparative Examples 1-7 to 1-10 were the same as the corresponding conditions utilized in Example 1-1.
  • the copper alloy materials of Examples 1-1 to 1-6, 2-1, 2-2, and 3 to 13 each are high in the mechanical strength and good in the bending property, and are excellent in the fatigue property.
  • Comparative Example 1-7 since the value of the grain diameter d was too large, the bending property was poor. In Comparative Example 1-8, since the value of the width W of the precipitate free zone was too large, the bending property and fatigue property were poor. In Comparative Example 1-9, since the particle diameter L of the compound on the grain boundary was too large, the bending property and fatigue property were poor. In Comparative Example 1-10, since the tensile strength was too high, the bending property was poor.
  • Comparative Example 14 since the Ni concentration and the Si concentration were too low, the fatigue life was conspicuously short, and the stress relaxation resistance was also poor.
  • Comparative Example 15 since the Mg concentration was too high, the bending property was poor.
  • Comparative Example 16 and 17 since the Mg concentration or the Zn concentration was too high, respectively, the electrical conductivity was poor.
  • Comparative Example 18 since the Co concentration was too high, the bending property was poor, and the fatigue life was also poor.
  • the copper alloy material of the present invention can be favorably used as a material, for example, for lead frames, connectors, terminal materials, relays, and switches, of electric / electronic equipments.
EP09712614A 2008-02-18 2009-02-17 Matériau d'alliage de cuivre Withdrawn EP2256219A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008036694 2008-02-18
PCT/JP2009/052718 WO2009104615A1 (fr) 2008-02-18 2009-02-17 Matériau d'alliage de cuivre

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EP2256219A1 true EP2256219A1 (fr) 2010-12-01
EP2256219A4 EP2256219A4 (fr) 2012-06-27

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US (2) US20100310413A1 (fr)
EP (1) EP2256219A4 (fr)
JP (1) JPWO2009104615A1 (fr)
CN (1) CN101946014A (fr)
WO (1) WO2009104615A1 (fr)

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RU2691823C1 (ru) * 2018-05-14 2019-06-18 Федеральное государственное бюджетное образовательное учреждение высшего образования Балтийский государственный технический университет "ВОЕНМЕХ" им. Д.Ф. Устинова (БГТУ "ВОЕНМЕХ") Способ термической обработки заготовки или изделия (пружин) из бронзы БрНХК 2,5-0,7-0,6
JP2021098887A (ja) * 2019-12-20 2021-07-01 Ｊｘ金属株式会社 積層造形用金属粉末及び該金属粉末を用いて作製した積層造形物

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US20110259480A1 (en) 2011-10-27
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WO2009104615A1 (fr) 2009-08-27
CN101946014A (zh) 2011-01-12

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