WO2012121109A1 - ALLIAGE À BASE DE Cu-Ni-Si ET PROCÉDÉ POUR SA FABRICATION - Google Patents

ALLIAGE À BASE DE Cu-Ni-Si ET PROCÉDÉ POUR SA FABRICATION Download PDF

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Publication number
WO2012121109A1
WO2012121109A1 PCT/JP2012/055255 JP2012055255W WO2012121109A1 WO 2012121109 A1 WO2012121109 A1 WO 2012121109A1 JP 2012055255 W JP2012055255 W JP 2012055255W WO 2012121109 A1 WO2012121109 A1 WO 2012121109A1
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Prior art keywords
orientation
copper
mass
annealing
rolling
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PCT/JP2012/055255
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English (en)
Japanese (ja)
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波多野　隆紹
真之 長野
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Jx日鉱日石金属株式会社
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Priority to KR1020137026578A priority Critical patent/KR101808372B1/ko
Priority to CN201280012297.2A priority patent/CN103403202B/zh
Publication of WO2012121109A1 publication Critical patent/WO2012121109A1/fr

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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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/495—Lead-frames or other flat leads
    • H01L23/49579—Lead-frames or other flat leads characterised by the materials of the lead frames or layers thereon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/00013—Fully indexed content
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the present invention has excellent strength, bending workability, stress relaxation suitable as a lead frame material for conductive spring materials such as connectors, terminals, relays and switches, and semiconductor devices such as transistors and integrated circuits (ICs).
  • the present invention relates to a copper alloy having characteristics, conductivity, and the like, and a method for manufacturing the copper alloy.
  • a Cu-Ni-Si alloy which is one of the Corson alloys, is an alloy in which compound particles of Ni and Si are precipitated in a Cu matrix, and has high strength, high electrical conductivity, and good bending workability. Yes.
  • strength and bending workability are contradictory properties, and it is desired to improve bending workability while maintaining high strength even in Cu—Ni—Si based alloys.
  • the surface of the copper alloy plate is cut in advance, which is called notching, and the copper alloy is cut along the cut.
  • the plate may be bent (hereinafter also referred to as notch bending). This notch bending is frequently used, for example, in press working of a vehicle-mounted female terminal. Since the copper alloy is work-hardened and loses ductility by the notching process, the copper alloy is easily cracked in the subsequent bending process. Therefore, particularly good bending workability is required for the copper alloy used for notch bending.
  • Patent Document 1 Japanese Patent Laid-Open No. 2006-283059
  • (8) short-time annealing The bendability is improved by controlling the area ratio to 50% or more.
  • Patent Document 2 Japanese Patent Laid-Open No. 2011-17072
  • the area ratio of the Cube orientation is controlled to 5 to 60%, and at the same time, the area ratios of the Brass orientation and the Copper orientation are both controlled to 20% or less, so that bending workability is improved.
  • Manufacturing processes for this purpose include (1) casting, (2) hot rolling, (3) cold rolling (working degree 85 to 99%), (4) heat treatment (300 to 700 ° C, 5 minutes to 20 hours) (5) Cold rolling (working degree 5 to 35%), (6) Solution treatment, (7) Aging treatment, (8) Cold rolling (working degree 2 to 30%), (9) Temper annealing The best bendability is obtained when the steps are sequentially performed.
  • an object of the present invention is to provide a Cu—Ni—Si alloy having both high strength and high notch bendability and a method for producing the same.
  • EBSD Electron Back Scatter Diffraction: Electron Back Scattering Diffraction
  • SEM Sccanning Electron Microscope
  • the present inventors have found that it is necessary to control the crystal orientation inside the copper alloy plate for notch bending. This is because the inner angle of bending moves into the plate by notching. Then, the crystal orientation in the central part in the plate thickness direction was optimized for notch bending, and a manufacturing method for obtaining this crystal orientation was clarified.
  • the present invention completed on the basis of the above findings contains 0.8 to 4.5 mass% Ni and 0.2 to 1.0 mass% Si, with the balance being copper and inevitable impurities.
  • the Cube orientation ⁇ 0 0 1 ⁇ The area ratio of ⁇ 1 0 ⁇ 0> is 10 to 80%, the area ratio of Brass orientation ⁇ 1 ⁇ 1 0 ⁇ ⁇ 1 1 2> is 20% or less, and the area ratio of Copper orientation ⁇ 1 1 2 ⁇ ⁇ 1 1> It is a Cu—Ni—Si alloy that is 20% or less.
  • the Cu—Ni—Si based alloy according to the present invention includes at least one of Sn, Zn, Mg, Fe, Ti, Zr, Cr, Al, P, Mn, Co, Cr and Ag in a total amount. 0.005 to 3.0% by mass is contained.
  • an ingot containing 0.8 to 4.5 mass% Ni and 0.2 to 1.0 mass% Si, the balance being copper and inevitable impurities is produced.
  • the ingot is hot-rolled at a temperature of 800-1000 ° C. to a thickness of 5-20 mm, then cold-rolled with a working degree of 30-99%, and subjected to a heat treatment with a softening degree of 0.25-0.75.
  • cold rolling with a workability of 7 to 50% is performed, followed by solution treatment at 700 to 900 ° C. for 5 to 300 seconds, and 350 to 550 ° C. In this method, the aging treatment is performed for 2 to 20 hours.
  • the ingot is made of Sn, Zn, Mg, Fe, Ti, Zr, Cr, Al, P, Mn, Co, Cr, and Ag.
  • One or more kinds are contained in a total amount of 0.005 to 3.0% by mass.
  • the present invention is a copper-drawn product provided with the above copper alloy.
  • the present invention is an electronic device component including the copper alloy.
  • Ni and Si are deposited as an intermetallic compound such as Ni 2 Si by performing an appropriate aging treatment.
  • the strength is improved by the action of the precipitates, and Ni and Si dissolved in the Cu matrix are reduced by precipitation, so that the conductivity is improved.
  • Ni is less than 0.8% by mass or Si is less than 0.2% by mass
  • the desired strength cannot be obtained, and conversely, when Ni exceeds 4.5% by mass or Si is 1.0% by mass When it exceeds, electrical conductivity will fall.
  • the addition amount of Ni is 0.8 to 4.5 mass% and the addition amount of Si is 0.2 to 1.0 mass%.
  • the addition amount of Ni is preferably 1.0 to 4.0% by mass
  • the addition amount of Si is preferably 0.25 to 0.90% by mass.
  • the Cu—Ni—Si based alloy according to the present invention preferably contains these elements in a total amount of 0.005 to 3.0 mass%, preferably 0.01 to 2.5 mass%. More preferred.
  • the Cube orientation is a state in which the (0 0 1) plane faces the rolling surface normal direction (ND) and the (1 0 0) plane faces the rolling direction (RD), and ⁇ 0 0 1 ⁇ It is indicated by an index of ⁇ 1 0 0>.
  • the Brass orientation is a state in which the (1 1 0) plane faces ND and the (1 1 2) plane faces RD, and is indicated by an index of ⁇ 1 1 0 ⁇ ⁇ 1 1 2>.
  • the Copper orientation is a state in which the (1 1 2) plane faces the ND and the (1 1 1) plane faces the RD, and is represented by an index of ⁇ 1 1 2 ⁇ ⁇ 1 1 1>.
  • the area ratio of the Cube orientation at the center of the plate thickness is less than 10%, the notch bendability is drastically lowered.
  • the area ratio of the Cube orientation in the central portion of the plate thickness exceeds 80%, the Young's modulus is rapidly lowered.
  • P spring force
  • E Young's modulus
  • d displacement
  • the area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is set to 10 to 80%.
  • a more preferable area ratio of the Cube orientation ⁇ 0 0 1 ⁇ ⁇ 1 0 0> is 15 to 60%. If any of the area ratio of the Copper azimuth and the area ratio of the Brass azimuth in the central portion of the plate thickness exceeds 20%, the notch bendability deteriorates rapidly. For this reason, the area ratio of the Copper azimuth and the area ratio of the Brass azimuth are set to 20% or less.
  • the lower limit of the area ratio of Copper orientation in the central portion of the plate thickness and the area ratio of Brass orientation is not restricted from the point of notch bendability, in the case of the alloy of the present invention, no matter how the manufacturing method is changed, Either the area ratio of the Copper azimuth or the area ratio of the Brass azimuth in the central portion of the plate thickness is never less than 1%.
  • the area ratio of the Copper azimuth and the area ratio of the Brass azimuth in the central portion of the plate thickness are preferably 15% or less.
  • the central portion of the plate thickness refers to a cross-sectional position of 45 to 55% with respect to the plate thickness.
  • pre-annealing heat treatment
  • cold rolling hereinafter also referred to as light rolling
  • the preliminary annealing is performed for the purpose of partially generating recrystallized grains in a rolled structure formed by cold rolling after hot rolling.
  • the ratio of recrystallized grains in the rolled structure there is an optimum value for the ratio of recrystallized grains in the rolled structure, and the above-mentioned crystal orientation cannot be obtained if the amount is too small or too large.
  • Optimal ratio of recrystallized grains, so that the softening degree S T defined below is 0.25-0.75 is obtained by adjusting the pre-annealing conditions.
  • FIG. 1 illustrates the relationship between the annealing temperature and the tensile strength when the alloy according to the present invention is annealed at various temperatures.
  • a sample with a thermocouple attached was inserted into a tube furnace at 950 ° C., and when the sample temperature measured by the thermocouple reached a predetermined temperature, the sample was taken out of the furnace, cooled with water, and the tensile strength was measured. is there. Recrystallization progresses when the sample arrival temperature is 500 to 700 ° C., and the tensile strength is rapidly reduced. The gradual decrease in tensile strength on the high temperature side is due to the growth of recrystallized grains.
  • S T ( ⁇ 0 ⁇ T ) / ( ⁇ 0 ⁇ 900 )
  • ⁇ 0 is the tensile strength before annealing
  • ⁇ T and ⁇ 900 are the tensile strength after annealing at T ° C. and 900 ° C., respectively.
  • the temperature of 900 ° C. is adopted as a reference temperature for knowing the tensile strength after recrystallization because the alloy according to the present invention is stably completely recrystallized when annealed at 900 ° C.
  • the temperature, time and cooling rate of the pre-annealing are not particularly limited, and it is important to adjust ST and conductivity within the above ranges.
  • the furnace temperature ranges from 400 to 700 ° C. for 5 seconds to 10 minutes
  • the furnace temperature ranges from 350 to 600 ° C. for 30 minutes to 20 hours. Done in
  • the processing degree R (%) is defined by the following equation.
  • R (t 0 ⁇ t) / t 0 ⁇ 100 (t 0 : plate thickness before rolling, t: plate thickness after rolling) If the degree of work falls outside this range, the area ratio of the Cube orientation at the center of the plate thickness becomes less than 10%.
  • the strain relief annealing (10) is optionally performed in order to recover the spring limit value and the like which are lowered by the cold rolling when the cold rolling (9) is performed. Regardless of the presence or absence of strain relief annealing (10), the effect of the present invention is obtained in that the notch bendability is improved by controlling the crystal orientation at the center of the plate thickness.
  • the strain relief annealing (10) may or may not be performed.
  • general production conditions for the Cu—Ni—Si based alloy may be selected.
  • the Cu—Ni—Si based alloy of the present invention can be processed into various copper products such as plates, strips and foils. Furthermore, the Cu—Ni—Si based alloy of the present invention can be used for lead frames, connectors and pins. It can be used for electronic device parts such as terminals, relays, switches, and foil materials for secondary batteries.
  • Example 1 An alloy containing Ni: 2.6% by mass, Si: 0.58% by mass, Sn: 0.5% by mass, and Zn: 0.4% by mass with the balance being copper and inevitable impurities is used as an experimental material. The relationship between pre-annealing and light rolling conditions and crystal orientation, and the effect of crystal orientation on the bendability and mechanical properties of the product were investigated. In a high frequency melting furnace, 2.5 kg of electrolytic copper was melted using a graphite crucible having an inner diameter of 60 mm and a depth of 200 mm in an argon atmosphere.
  • Pre-annealing Insert the sample into an electric furnace adjusted to a predetermined temperature, hold it for a predetermined time, then place the sample in a water bath and cool (water cooling) or leave the sample in the atmosphere and cool (air cooling) Cooled under conditions.
  • Solution treatment The sample was inserted into an electric furnace adjusted to 800 ° C. and held for 10 seconds, and then the sample was placed in a water bath and cooled.
  • Aging treatment Heated in an Ar atmosphere at 450 ° C. for 5 hours using an electric furnace.
  • Cold rolling Cold rolled from 0.18 mm to 0.15 mm at a workability of 17%.
  • Strain relief annealing The sample was inserted into an electric furnace adjusted to 400 ° C. and held for 10 seconds, and then the sample was left in the air and cooled.
  • the area ratios of the Cube orientation, Copper orientation, and Brass orientation were measured by EBSD.
  • the sample surface was mechanically polished to remove minute irregularities due to a rolling pattern or the like, and then finished to a mirror surface using colloidal silica abrasive grains.
  • the resulting surface polishing depth was in the range of 2-3 ⁇ m.
  • a sample for analyzing the crystal orientation of the central part of the plate thickness from one surface to the central part of the plate thickness is removed by etching using a ferric chloride solution, and then mechanical polishing and colloidal silica abrasive grains are used.
  • the thickness of the sample after finishing was in the range of 45 to 55% with respect to the original plate thickness.
  • a sample area of 500 ⁇ m square containing 200 or more crystal grains was scanned in steps of 0.5 ⁇ m to analyze the orientation.
  • the rotation angle was calculated around the common rotation axis, and was taken as the deviation angle. For example, with respect to the S orientation (2 3 1) [6 -4 3], (1 2 1) [1 -1 1] is rotated by 19.4 ° with the (20 10 17) direction as the axis of rotation. This angle was taken as the deviation angle.
  • a common rotation axis that can be expressed at the smallest angle is adopted.
  • the total measurement area is the area of crystal grains having an orientation within 10 ° from each of the Cube orientation, Copper orientation, and Brass orientation. To obtain the area ratio.
  • the information obtained in the azimuth analysis by EBSD includes azimuth information up to a depth of several tens of nanometers in which the electron beam penetrates the sample, but is described as an area ratio because it is sufficiently small with respect to the measured width. .
  • pre-annealing and light rolling were performed under the conditions specified by the present invention, the crystal orientation at the center of the plate thickness satisfied the specifications of the present invention, and cracking occurred in both W bending and notch bending.
  • the tensile strength was as high as 800 MPa or higher, and a high Young's modulus exceeding 110 MPa was obtained.
  • Comparative Example 1 since the degree of softening during pre-annealing was less than 0.25, the Copper azimuth area ratio in the central portion of the plate thickness exceeded 20%, and the Cube azimuth area ratio was less than 10%.
  • Comparative Example 2 since the degree of softening in the pre-annealing exceeded 0.75, the Brass orientation area ratio in the central portion of the plate thickness exceeded 20%.
  • Comparative Example 3 the degree of softening in the pre-annealing exceeded 0.75, and the electrical conductivity after the pre-annealing was less than 20% IACS, so that the area ratio of the Copper orientation and the Brass orientation in the central portion of the plate thickness was 20% The Cube orientation area ratio was less than 10%.
  • Comparative Examples 5 and 6 the degree of work of light rolling deviated from the definition of the present invention, and the Cube orientation area ratio in the center portion of the plate thickness was less than 10%.
  • cracks did not occur in W bending, but cracks occurred in notch bending.
  • the preliminary annealing and light rolling of these comparative examples were performed within the range recommended by Patent Document 2, and the crystal orientation of the plate thickness surface layer satisfied the provisions of Patent Document 2.
  • Comparative Example 4 the conductivity after the pre-annealing exceeded 45% IACS, so the Cube orientation area ratio exceeded 80% and the Young's modulus was a low value of less than 100 MPa.
  • Comparative Example 7 is a sheet thickness of 9 mm after surface grinding after hot rolling, and rolled as it is to 0.18 mm without pre-annealing and light rolling. In both the central part and the surface layer part, the area ratios of Copper orientation and Brass orientation exceeded 20%, and the Cube orientation area ratio became less than 10%. As a result, cracks occurred in both W bending and notch bending.
  • Example 2 It was examined whether the notch bendability improving effect shown in Example 1 could be obtained with Cu—Ni—Si alloys having different components and production conditions.
  • Example 2 The same evaluation as in Example 1 was performed on the sample after the preliminary annealing and the product sample. Tables 2 and 3 show the evaluation results. When any one of rolling 1, rolling 2, and strain relief annealing is not performed, “none” is written in the column of the degree of processing or temperature.
  • Each of the inventive examples contains Ni and Si at a concentration specified by the present invention, and is subjected to pre-annealing and light rolling under the conditions specified by the present invention. Satisfactory, notch bending was possible, high tensile strength exceeding 650 MPa and high Young's modulus exceeding 110 MPa were obtained.
  • Invention Example 15 in which the workability of Rolling 2 exceeded 50% and Invention Example 16 in which the workability of Rolling 1 exceeded 60% although cracks occurred in the notch bending test, they were practically acceptable. Since it was a fine crack, it evaluated as (circle).
  • Comparative Example 8 the light rolling workability exceeds 50%.

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Abstract

L'invention concerne : un alliage à base de Cu-Ni-Si qui combine une résistance élevée et de bonnes propriétés d'essai de pliage sur éprouvette entaillée; et un procédé pour sa fabrication. L'alliage à base de Cu-Ni-Si contient 0,8 à 4,5% en masse de Ni et 0,2 à 1,0% en masse de Si, le reste consistant en cuivre et en impuretés inévitables. En outre, l'alliage à base de Cu-Ni-Si présente une fraction de surface d'orientation Cube {001}<100> de 10 à 80%, une fraction de surface d'orientation Laiton {110}<112> de 20% ou moins et une fraction de surface d'orientation Cuivre {112}<111> de 20% ou moins, quand il est analysé en ce qui concerne l'orientation cristalline dans une partie centrale de l'épaisseur de la feuille par réalisation d'une mesure EBSD (diffraction en électrons rétrodiffusés) parallèlement à la direction de l'épaisseur de la feuille, ladite partie centrale de l'épaisseur de la feuille étant une partie qui se trouve à une profondeur de 45 à 55% de l'épaisseur de la feuille.
PCT/JP2012/055255 2011-03-09 2012-03-01 ALLIAGE À BASE DE Cu-Ni-Si ET PROCÉDÉ POUR SA FABRICATION WO2012121109A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020137026578A KR101808372B1 (ko) 2011-03-09 2012-03-01 Cu-Ni-Si 계 합금 및 그 제조 방법
CN201280012297.2A CN103403202B (zh) 2011-03-09 2012-03-01 Cu-Ni-Si系合金及其制造方法

Applications Claiming Priority (2)

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JP2011051975A JP4857395B1 (ja) 2011-03-09 2011-03-09 Ｃｕ−Ｎｉ−Ｓｉ系合金及びその製造方法
JP2011-051975 2011-03-09

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JP (1) JP4857395B1 (fr)
KR (1) KR101808372B1 (fr)
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TW (1) TWI447241B (fr)
WO (1) WO2012121109A1 (fr)

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CN103484719A (zh) * 2013-09-29 2014-01-01 苏州市凯业金属制品有限公司 一种白铜合金金属管
JP6050738B2 (ja) 2013-11-25 2016-12-21 Ｊｘ金属株式会社 導電性、成形加工性および応力緩和特性に優れる銅合金板
JP6355671B2 (ja) * 2016-03-31 2018-07-11 Ｊｘ金属株式会社 Ｃｕ−Ｎｉ−Ｓｉ系銅合金条及びその製造方法
JP2017014624A (ja) * 2016-09-05 2017-01-19 Ｊｘ金属株式会社 コルソン合金及びその製造方法
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