US20070051442A1 - Copper alloy material and method of making same - Google Patents

Copper alloy material and method of making same Download PDF

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Publication number
US20070051442A1
US20070051442A1 US11/510,854 US51085406A US2007051442A1 US 20070051442 A1 US20070051442 A1 US 20070051442A1 US 51085406 A US51085406 A US 51085406A US 2007051442 A1 US2007051442 A1 US 2007051442A1
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mass
copper alloy
alloy material
cold
heat treatment
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US11/510,854
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Yoshiki Yamamoto
Hiroaki Takano
Koichi Kotoku
Chingping Tong
Katsumi Nomura
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Hitachi Cable Ltd
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Hitachi Cable Ltd
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Assigned to HITACHI CABLE, LTD. reassignment HITACHI CABLE, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KOTOKU, KOICHI, NOMURA, KATSUMI, TAKANO, HIROAKI, TONG, CHINGPING, YAMAMOTO, YOSHIKI
Publication of US20070051442A1 publication Critical patent/US20070051442A1/en
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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
    • C22C9/02—Alloys based on copper with tin 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
    • C22C9/04—Alloys based on copper with zinc 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

Definitions

  • This invention relates to a copper alloy material for electric parts such as a terminal, connector and lead frame and, in particular, to a copper alloy material that is excellent in mechanical strength such as tensile strength and yield strength, in elongation, in electric conductivity and in bending workability.
  • This invention also relates to a method of making the copper alloy material.
  • an electronic hardware such as a cellular phone or notebook PC is downsized, low-profiled and reduced in weight. Along with this, electric and/or electronic components used therein tend to be reduced in weight, length and thickness.
  • phosphor bronze is used as a material for a terminal, connector etc.
  • the phosphor bronze cannot satisfy sufficiently the updated characteristics required to the connector material.
  • the phosphor bronze has a low electric conductivity of about 20% IACS, it cannot be suited to an increase in applied current (i.e., it results in an increase of the generated Joule heat).
  • the phosphor bronze does not have an excellent characteristic in migration resistance.
  • the migration is a phenomenon that, when a condensation of moisture occurs between electrodes, the Cu atom in the positive electrode is dissolved (ionized) and precipitated on the negative electrode, so that the short circuit between the electrodes can be caused.
  • the phenomenon is a serious problem especially on the connector or lead frame that can be used in environment of high temperature and high humidity as in automobiles. Further, it should be considered for the connector or lead frame with an interelectrode pitch narrowed due to the downsizing.
  • a ratio, (Ni+Fe+Co)/(Si+P), between a total mass of Ni, Fe and Co and a total mass of Si and P is 4 or more and 10 or less.
  • a ratio, (Ni+Fe+Co)/(Si+P), between a total mass of Ni, Fe and Co and a total mass of Si and P is 4 or more and 10 or less.
  • a first cold rolling step that the copper alloy raw material is cold-rolled down to a thickness of 1.1 to 1.3 times a target thickness of a final product
  • a first heat treatment step that the cold-rolled material in the first cold rolling step is heated up to 700 to 850° C. and then cooled to 300° C. or less at a cooling rate of 25° C./min or more;
  • a second heat treatment step that the cold-rolled material in the second cold rolling step is heated up to 400 to 500° C. and held for 30 min. to 3 hrs.
  • a first cold rolling step that the copper alloy raw material is cold-rolled down to a thickness of 1.1 to 1.3 times a target thickness of a final product
  • a first heat treatment step that the cold-rolled material in the first cold rolling step is heated up to 700 to 850° C. and then cooled to 300° C. or less at a cooling rate of 25° C./min or more;
  • a second heat treatment step that the cold-rolled material in the second cold rolling step is heated up to 400 to 500° C. and held for 30 min. to 3 hrs.
  • a copper alloy material for electric parts such as a terminal, connector and lead frame, can be provided that is excellent in mechanical strength such as tensile strength and 0.2% yield strength (herein called simply “yield strength”), in elongation, in electric conductivity and in bending workability to show reduced anisotropy in the bending process.
  • yield strength tensile strength and 0.2% yield strength
  • FIG. 1 is a flowchart showing a method of making a copper alloy material for electric parts in a preferred embodiment according to the invention.
  • the reasons for adding the alloy elements to compose the copper alloy material for electric parts and for limiting the content thereof are as follows.
  • Ni, Fe and Co can be dispersed and precipitated in the material while forming a Si compound or a P compound when it is added therein together with Si and P.
  • the conventional Cu—Ni—Si alloys have an enhanced mechanical strength by dispersing and precipitating a Ni—Si compound
  • this embodiment can have a further enhanced mechanical strength by the effects of precipitations, i.e., a Ni—P compound, and a Si compound and/or a P compound with Fe and Co in addition to the Ni—Si compound.
  • the mechanical strength and spring property can be enhanced by the enhanced dispersion effect of the precipitations while suppressing the amount of solid-solution element in the Cu matrix that may reduce the electric conductivity.
  • the composition ratio of Si is defined to be 0.2 to 1.0 mass %, preferably to be 0.4 to 0.7 mass %.
  • the composition ratio of P is defined to be 0.01 to 0.3 mass %, preferably to be 0.1 to 0.2 mass %.
  • the composition of Ni is 1.0 to 5.0 mass %
  • the total composition of Fe and Co is 0.05 to 1.0 mass %
  • the ratio (Ni+Fe+Co)/(Si+P) between a total mass of Ni, Fe and Co and a total mass of Si and P is 4 or more and 10 or less, so as to secure simultaneously a high mechanical strength and a high electric conductivity while forming effectively the compound in relation to the above composition of Si and P. If the content of Ni, Fe and Co is less than the lower limit of the above composition, the amount of the compound formed will be insufficient, which causes a lack of mechanical strength and spring property.
  • Ni, Fe and Co are more than the upper limit thereof, excessive Ni, Fe and Co will be dissolved into the Cu matrix as a solid solution to degrade the electric conductivity. Further, if the ratio (Ni+Fe+Co)/(Si+P) is less than 4, Si and P are excessive and if more than 10, Ni, Fe and Co are excessive by contrast. Since such an excessive component exists in solid-solution state in the Cu matrix, the electric conductivity will be degraded. It is preferably defined that the composition of Ni is 2.5 to 3.5 mass %, the total composition of Fe and Co is 0.3 to 0.7 mass %, and the ratio (Ni+Fe+Co)/(Si+P) is 4 or more and 7 or less.
  • the composition of Sn is preferably to be 0.05 to 2.0mass %, more preferably to be 0.3 to 1.0 mass %.
  • the Zn has an effect to enhance the mechanical strength and spring property. Further, it has a significant effect to enhance the migration resistance. Still further, it has an effect to improve the solder wettability and cohesion to a Sn plating which are needed in the material for electric and electronic parts. However, if the content thereof is less than 0.1 mass %, the effects are not sufficient. If it is added more than 5.0 mass %, it has a negative affection to degrade the electric conductivity.
  • the composition of Zn is preferably to be 0.1 to 5.0 mass %, more preferably to be 0.3 to 2.0 mass %.
  • the reasons for adding the alloy elements to compose the copper alloy material for electric parts and for limiting the content thereof are as follows.
  • the reason why at least one of Mg, Ti, Cr and Zr is added 0.01 to 1.0 mass % in total is that additional excellent properties can be obtained.
  • These elements have effects to improve further the mechanical strength, spring property, migration resistance, and heat resistance, and have only a small affection to lower the electric conductivity. Therefore, they are effective as an additive to facilitate the effects of the aforementioned elements in the first embodiment.
  • the total content thereof is less than 0.01 mass %, the sufficient effect cannot be expected. If it is added more than 1.0 mass %, a negative affection may appear such as deterioration in casting property in the process of forming a copper alloy raw material.
  • the composition of Mg, Ti, Cr and Zr is in total to be 0.01 to 1.0 mass %, more preferably to be 0.1 to 0.3 mass %.
  • FIG. 1 is a flowchart showing a method of making a copper alloy material for electric parts in the preferred embodiment according to the invention.
  • the above mentioned copper alloy material of the first and second embodiments can be made, after preparing the copper alloy raw material with the average composition as defined earlier, by conducting: the first cold rolling step that the copper alloy raw material thus formed is cold-rolled down to 1.1 to 1.3 times thicker than a target thickness of a final product; the first heat treatment step that the material after the first cold rolling step is heated up to 700 to 850° C. and then cooled to less than 300° C. at a cooling rate of 25° C./min or more; the second cold rolling step that the material after the first heat treatment step is cold-rolled down to the target thickness of the final product; and the second heat treatment step that the material after the second cold rolling step is heated up to 400 to 500° C. and kept for 30 minutes to 3 hours.
  • the copper alloy raw material can be, for example, prepared by conducting an alloy casting step and then a hot working step.
  • the copper alloy raw material prepared is cold-rolled down to 1.1 to 1.3 times thicker than the target thickness of the final product.
  • This process (step) promotes the recrystallization in the following first heat treatment and allows the formation of the grain structure with equalized grain size after the recrystallization.
  • the reason why the material thickness after the rolling is defined to be 1.1 to 1.3 times the target thickness of final product is to introduce a proper amount of lattice defect such as a dislocation in the cold rolling (i.e., the second cold rolling step) after the first heat treatment step as described later.
  • the material thickness is more than the defined thickness, excessive lattice defects will be introduced by the cold rolling (i.e., the second cold rolling step) after the first heat treatment step and, therefore, the elongation property of the final product is lowered and the anisotropy of the elongation property is arisen depending on the rolling direction in the bending process, that causes to degrade the bending workability of the product.
  • the lattice defect will be insufficiently introduced in the cold rolling (i.e., the second cold rolling step) after the first heat treatment step and, therefore, the mechanical strength such as tensile strength and yield strength is lowered.
  • the copper alloy material after the first cold rolling step is heated up to 700 to 850° C. and then cooled to less than 300° C. at a cooling rate of 25° C./min or more.
  • it is heated up to 770 to 850° C. and then cooled to less than 300° C. at a cooling rate of 150° C./min or more.
  • the holding time of the heating is not defined, it is preferably shorter in consideration of the productivity and the material only has to be held at the defined temperature substantially for 1 sec. or more.
  • the solution heat treatment in this step is intended to disperse (dissolve) uniformly the alloy component into the copper matrix so as to disperse and precipitate uniformly and finely the alloy component in the final product.
  • the nonuniform precipitation that may be formed in the process of preparing the copper alloy raw material can be dissolved again in the copper matrix by the solid solution heat treatment.
  • the heating temperature to be 700° C. or more
  • the formation of solid solution can be sufficiently progressed.
  • the cooling rate to be 25° C./min or more, a coarse precipitation (grain growth of the precipitation) can be prevented from being formed again during the cooling process.
  • the grain distorted by the intensive cold working i.e., the first cold rolling step
  • the heating temperature is more than 850° C.
  • a coarsening of the grain i.e., excessive recrystallization or exaggerated grain growth
  • the upper limit of the heating temperature is defined to be 850° C.
  • the copper alloy material after the first heat treatment is cold-rolled until having the target thickness of final product.
  • the lattice defect which becomes a starting point (i.e., a nucleation site) for forming the precipitation in the heat treatment (i.e., the second heat treatment step) as described later can be introduced suitably into the material.
  • the formation of uniform and fine precipitation can be promoted in the following heat treatment (i.e., the second heat treatment step), and the mechanical strength can be enhanced.
  • the copper alloy material after the second cold rolling step is heated up to 400 to 500° C. and held for 30 minutes to 3 hours. Preferably, it is heated up to 430 to 480° C. and held for 1 to 2 hours.
  • the Ni, Fe and Co can form compounds with Si and P, which can be dispersed and precipitated in the copper matrix to have simultaneously the high mechanical strength and good electric conductivity.
  • the treatment conditions are higher and longer than the defined range, 400 to 500° C. and 30 minutes to 3 hours, the precipitation may be coarsened to fail to have the sufficient mechanical strength. If the treatment conditions are lower and shorter than the defined range, the precipitation may be insufficiently progressed to fail to have the sufficient electric conductivity and mechanical strength.
  • a copper alloy which comprises Ni: 3.0 mass %, Si: 0.5 mass %, P: 0.15 mass %, Fe: 0.15 mass %, Co: 0.15 mass %, Sn: 1.0 mass %, and Zn: 1.5 mass % in an oxygen-free copper matrix is molten in a RF melting furnace and then cast into an ingot with a diameter of 30 mm and a length of 250 mm.
  • the ingot is heated to 850° C. and extruded (hot-worked) into a plate-like copper alloy raw material with a width of 20 mm and a thickness of 8 mm. Then, it is cold-rolled down to a thickness of 0.36 mm (the first cold rolling step). Then, the cold-rolled material is held at 800° C. for 10 min. and then is quenched in water to be cooled down to a room temperature (about 20° C.) at a rate of about 300° C./min (the first heat treatment step). Then, the cooled material is cold-rolled down to a thickness of 0.3 mm (the second cold rolling step), and then heated at 470° C. for 2 hours (the second heat treatment step) (Sample No. 1).
  • Sample No. 1 thus made is measured in relation to the properties of tensile strength, yield strength, elongation and electric conductivity.
  • the tensile strength, yield strength and elongation are measured based on JIS Z 2241 and the electric conductivity is measured based on JIS H 0505.
  • the measurement results are shown in Table 2.
  • Sample No. 1 has good properties, i.e., a tensile strength of 740 N/mm 2 , a yield strength of 684 N/mm 2 , an elongation of 12% and an electric conductivity of 42% IACS, which are suited to the object of the invention.
  • Sample Nos. 2 to 9 have good properties suited to the object of the invention. Further, it is confirmed that Sample Nos. 6 to 9, each of which contains 0.1 mass % of Mg, Ti, Cr or Zr in addition to the composition of Sample No. 1, all have a tensile strength and yield strength higher than Sample No. 1 and that, thus, the additive elements are effective.
  • Sample No. 4 which is slightly lower than the more preferred composition ratio described earlier in relation to the Ni content, Si content and the total content of Fe and Co, has a tensile strength and yield strength slightly lower than Sample No. 1 while it has an elongation and electric conductivity higher than Sample No. 1.
  • Sample No. 5 which is slightly higher than the more preferred composition ratio described earlier in relation to the Ni content, has an elongation and electric conductivity slightly lower than Sample No. 1 while it has a tensile strength and yield strength higher than Sample No. 1.
  • both of Sample Nos. 4 and 5 can sufficiently secure the expected effects (i.e., a tensile strength of 700 N/mm 2 or more, a yield strength of 650 N/mm 2 or more, an elongation of 10% or more, and an electric conductivity of 40% IACS or more).
  • Sample Nos. 10 to 15 are out of the invention-defined range in relation to the content of Ni and Si.
  • Sample Nos. 10 and 14 a crack is observed in the ingot since the content of Si is too large.
  • Sample No. 12 due to the excessive content of Ni, the electric conductivity is degraded even though the tensile strength is high.
  • Sample Nos. 18 and 19 are out of the invention-defined range in relation to the ratio, (Ni+Fe+Co)/(Si+P), of the total mass of Ni, Fe and Co and the total mass of Si and P.
  • the ratio is smaller than the invention-defined range, the electric conductivity is degraded and both the tensile strength and yield strength are not high.
  • Sample No. 19 that the ratio is larger than the invention-defined range, the electric conductivity is degraded and both the tensile strength and yield strength are not high.
  • Sample Nos. 23 to 28 (which correspond to Comparative examples 14 to 19, respectively) are made such that the copper alloys with the same composition as Sample No. 1 in Example 1 are processed in similar processes to Example 1, where the thickness ratio of the cold-rolled material in the first cold rolling step and the final product, and the heating conditions of the first and second heat treatment steps are shown in Table 3.
  • a bending test is conducted to evaluate the bending workability.
  • the bending test is based on a W-bending test as set forth in JIS H 3110 and is conducted such that the sample is bent at an angle of 90 degrees with a bend radius of 0 mm and then the surface of bent portion is observed to check the existence of a crack.
  • the bending test is conducted in both cases that the direction of bending axis is orthogonal to the rolling direction, and that the direction of bending axis is parallel to the rolling direction.
  • the sample is evaluated matter as “Good”.
  • When a crack formation is observed in either direction the sample is evaluated as “Not good”.
  • the measurement/observation results are shown in Table 4.
  • Sample Nos. 23 and 24 are out of the invention-defined range in relation to the thickness ratio between the cold-rolled material in the first cold rolling step and the final product. If the cold-rolled material in the first cold rolling step is too thin (i.e., the thickness ratio is less than 1.1) (Sample No. 23), the defects introduced in the second cold rolling step is reduced and, therefore, the yield strength of the final product remains low and the tensile strength is also low. By contrast, if the cold-rolled material in the first cold rolling step is too thick (i.e., the thickness ratio is more than 1.3) (Sample No.
  • the defects introduced in the second cold rolling step is excessive and, therefore, the elongation of the final product is degraded and anisotropy in the bending appears to deteriorate the bending workability (i.e., a crack is formed when the sample is bent with the bending axis parallel to the rolling direction).
  • Sample Nos. 25 and 26 are out of the invention-defined range in relation to the heating temperature of the first heat treatment step. If the heating temperature is too low or high, both the tensile strength and the yield strength are low. If the heating temperature is too high (Sample No. 26), the elongation, the electric conductivity and the bending workability are low as well as the tensile strength and the yield strength.
  • Sample Nos. 27 and 28 are out of the invention-defined range in relation to the heating temperature of the second heat treatment step. If the heating temperature is too low (Sample No. 27), the electric conductivity is low, the tensile strength, the yield strength and the elongation are insufficient, and the bending workability is lowered. If the heating temperature is too high (Sample No. 28), the tensile strength and the yield strength are insufficient even though the electric conductivity is high. TABLE 3 Thickness ratio of first cold-rolled material and First heat treatment Second heat treatment kind Sample No. final product heating conditions heating conditions Remarks Example 1 1 1.20:1 800° C. ⁇ 10 min 470° C. ⁇ 2 h — Comparative 14 23 1.07:1 800° C.

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JP2005-255502 2005-09-02
JP2005255502A JP4655834B2 (ja) 2005-09-02 2005-09-02 電気部品用銅合金材とその製造方法

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US20080298998A1 (en) * 2007-05-31 2008-12-04 The Furukawa Electric Co., Ltd. Copper alloy for electric and electronic equipments
US20090320964A1 (en) * 2003-03-03 2009-12-31 Mitsubishi Shindoh Co., Ltd. Heat resistance copper alloy materials
US20100037996A1 (en) * 2005-09-02 2010-02-18 Hitachi Cable, Ltd. Copper alloy material and method of making same
US20110056596A1 (en) * 2007-12-21 2011-03-10 Mitsubishi Shindoh Co., Ltd. High strength and high thermal conductivity copper alloy tube and method for producing the same
US20110100676A1 (en) * 2008-02-26 2011-05-05 Mitsubishi Shindoh Co., Ltd. High strength and high conductivity copper alloy rod or wire
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US9455058B2 (en) 2009-01-09 2016-09-27 Mitsubishi Shindoh Co., Ltd. High-strength and high-electrical conductivity copper alloy rolled sheet and method of manufacturing the same
US10311991B2 (en) 2009-01-09 2019-06-04 Mitsubishi Shindoh Co., Ltd. High-strength and high-electrical conductivity copper alloy rolled sheet and method of manufacturing the same
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US10266917B2 (en) 2003-03-03 2019-04-23 Mitsubishi Shindoh Co., Ltd. Heat resistance copper alloy materials
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US8287669B2 (en) 2007-05-31 2012-10-16 The Furukawa Electric Co., Ltd. Copper alloy for electric and electronic equipments
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US20080298998A1 (en) * 2007-05-31 2008-12-04 The Furukawa Electric Co., Ltd. Copper alloy for electric and electronic equipments
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