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WO2012124732A1 - FIL D'ALLIAGE DE Cu-Ni-Si À CAPACITÉ DE CINTRAGE EXCELLENTE - Google Patents

FIL D'ALLIAGE DE Cu-Ni-Si À CAPACITÉ DE CINTRAGE EXCELLENTE Download PDF

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Publication number
WO2012124732A1
WO2012124732A1 PCT/JP2012/056568 JP2012056568W WO2012124732A1 WO 2012124732 A1 WO2012124732 A1 WO 2012124732A1 JP 2012056568 W JP2012056568 W JP 2012056568W WO 2012124732 A1 WO2012124732 A1 WO 2012124732A1
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WIPO (PCT)
Prior art keywords
inclusions
alloy
maximum value
rolling
hot rolling
Prior art date
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Ceased
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PCT/JP2012/056568
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English (en)
Japanese (ja)
Inventor
真之 長野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JX Nippon Mining and Metals Corp
Original Assignee
JX Nippon Mining and Metals Corp
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Filing date
Publication date
Application filed by JX Nippon Mining and Metals Corp filed Critical JX Nippon Mining and Metals Corp
Priority to CN201280013438.2A priority Critical patent/CN103429771B/zh
Priority to KR1020137026858A priority patent/KR101590242B1/ko
Publication of WO2012124732A1 publication Critical patent/WO2012124732A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • 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
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • 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
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/02—Single bars, rods, wires, or strips

Definitions

  • the present invention relates to a Cu—Ni—Si alloy strip suitable as a material for connectors, terminals, relays, switches and the like.
  • precipitation strengthened copper alloys such as a Corson alloy having high strength and conductivity are used, and the demand is increasing.
  • Corson alloys Cu—Ni—Si alloys are alloys that have both high strength and relatively high electrical conductivity, and the strengthening mechanism is that Ni—Si intermetallic particles are precipitated in the Cu matrix. Thus, the strength and conductivity are improved.
  • Patent Document 1 the area ratio of ⁇ 001 ⁇ ⁇ 100> of the measurement result of EBSP analysis is set to 50% or more.
  • Patent Document 2 the area ratio of ⁇ 001 ⁇ ⁇ 100> of the measurement result of EBSP analysis is 50%.
  • the area ratio of ⁇ 110 ⁇ ⁇ 112> in the measurement result of EBSP analysis is 20% or less, and the area ratio of ⁇ 121 ⁇ ⁇ 111> is 20% or less.
  • ⁇ 001 ⁇ ⁇ 100> has an area ratio of 5 to 60% to improve bending workability.
  • an object of the present invention is to improve the bending workability of a Cu—Ni—Si based alloy, and in particular to improve the bending workability when notching is performed.
  • the present inventor has found ⁇ 001 ⁇ ⁇ 100> on the ⁇ 200 ⁇ positive electrode diagram in both the surface layer and the central portion. It has been found that bending workability is improved by controlling the maximum value of the X-ray random intensity ratio in the region including the azimuth, in particular, bending workability after notching is improved. Furthermore, in order to control the X-ray random intensity ratio of both the surface layer and the central part, it is cooled at a specific speed after hot rolling to allow a specific amount of inclusions having a particle diameter of 1 to 2 ⁇ m to exist, and after the hot rolling, It was found that adjusting the strain rate of hot rolling is effective.
  • the present invention relates to the following inventions.
  • the maximum value of the X-ray random intensity ratio in the range where the angle ⁇ around the axis perpendicular to the rotation axis of the diffraction goniometer specified in the Schulz method is 0 to 10 ° is 3.0 to 15.
  • FIG. 10 is a ⁇ 200 ⁇ positive dot diagram showing a range where the angle ⁇ around the axis perpendicular to the rotation axis of the diffraction goniometer specified in the Schulz method is 0 to 10 ° in gray (in the center circle). It is the schematic of a notching process. The arrows in the figure indicate the pressure direction. It is the schematic of a 90 degreeW bending process.
  • Ni and Si concentrations Ni and Si are precipitated as intermetallic compounds such as Ni 2 Si by performing an aging treatment. This compound improves the strength, and by precipitation, Ni and Si dissolved in the Cu matrix are reduced, so that the conductivity is improved.
  • the Ni concentration is less than 1.0 mass% (hereinafter referred to as “%”) or the Si concentration is less than 0.2%, the desired strength cannot be obtained, and conversely, when the Ni concentration exceeds 4.5%, or If the Si concentration exceeds 1.0%, the hot workability deteriorates.
  • the X-ray random intensity ratio of the region including the ⁇ 001 ⁇ ⁇ 100> orientation on the ⁇ 200 ⁇ positive electrode diagram It is effective to increase the maximum value of. Furthermore, it is effective for improving the bending workability after notching to increase both the X-ray random intensity ratios in both the surface layer and the central part.
  • the “surface layer” represents a portion from the front and back surfaces of the strip to the 1/6 depth in the thickness direction
  • the “central portion” represents a portion other than the surface layer.
  • the ⁇ 001 ⁇ ⁇ 100> orientation on the ⁇ 200 ⁇ positive point diagram is the angle ⁇ around the axis perpendicular to the rotation axis of the diffraction goniometer specified by the Schulz method, and the axis around the axis parallel to the rotation axis.
  • ⁇ 0 to 10 °
  • ⁇ 0 to 360 °.
  • the surface layer and the central portion are measured with an X-ray diffractometer (RINT2500 manufactured by Rigaku Corporation), and on the ⁇ 200 ⁇ positive pole figure, ⁇ is in the range of 0 to 10 ° (see FIG. 1).
  • the maximum value of the random strength ratio is 3.0 or more. If the maximum value is less than 3.0, the bending workability deteriorates. On the other hand, it is difficult for the maximum value to actually exceed 15.0. Therefore, the upper limit of the maximum value is 15.0. Preferably, the maximum value is 5.0 or more in both the surface layer and the central portion.
  • the reason for achieving excellent bending cracking resistance by adjusting the X-ray random strength of the ⁇ 001 ⁇ ⁇ 100> orientation is not clear, but the ⁇ 001 ⁇ ⁇ 100> orientation is the introduction of shear bands during plastic deformation. It is considered that cracks are unlikely to occur during bending because the orientation is suppressed from other orientations.
  • the present invention is not limited by the above theory. The ranges of ⁇ and ⁇ were determined in consideration of fluctuations in the peak position of the X-ray intensity ratio due to processing, heat treatment conditions, measurement errors, and the like.
  • Patent Documents 1 to 3 are all controlled by measuring the crystal orientation of the surface, and the crystal orientation of the central portion is not controlled (claims 1 to 3 of Patent Documents 1 to 3). Therefore, in the bending process after the notching process, a micro crack is generated in the central part of the plate thickness, and the bending processability is inferior.
  • inclusions refers to generally coarse crystallized products that occur during the solidification process during casting, oxides, sulfides, and the like that are generated by reaction in the molten metal during melting, This is a concept that includes precipitates generated by precipitation reaction in the solid phase matrix after the solidification process during casting, that is, the cooling process after solidification, the hot rolling, the cooling process after solution treatment, and the aging treatment.
  • the particles (so-called second phase particles) observed in the matrix by SEM observation of the copper alloy are included.
  • “Inclusion particle size” refers to the diameter of the smallest circle including the inclusion, measured under SEM observation.
  • Numberer of inclusions refers to a unit per square mm in which particles of components different from the parent phase are actually counted at a plurality of locations by SEM observation after etching in a cross section parallel to the rolling direction of the material and parallel to the plate thickness direction. Is the average number.
  • the inclusions of the present invention also include particles formed in the process after hot rolling, but it is the inclusion of a specific size that exists after hot rolling that mainly contributes to the intended function of the present invention. It is. Specifically, when there are 50 to 200 inclusions / mm 2 of particle diameters of 1 to 2 ⁇ m in the parallel rolling cross section after hot rolling, the maximum X-ray random intensity ratio of both the surface layer and the central portion is maximized. The value becomes 3.0 or more. If it is out of the range of 50 to 200 / mm 2 , the maximum value of the X-ray intensity ratio becomes less than 3.0, and the bending workability deteriorates.
  • the number of inclusions with a grain size exceeding 1 ⁇ m after hot rolling is the number of inclusions in the final product obtained through the manufacturing process of the Cu—Ni—Si alloy including cold rolling, solution treatment, and aging treatment. Almost identical. Specifically, after hot rolling, if cold rolling is performed on a material in which inclusions having a grain size of 1 to 2 ⁇ m are uniformly distributed in the thickness direction, processing strain accumulates around the inclusions. Strain is uniformly distributed in the thickness direction. When solution treatment is performed on the material, crystal grains with ⁇ 001 ⁇ ⁇ 100> orientation are recrystallized uniformly in the plate thickness direction, so that an X-ray intensity ratio within the above range can be obtained.
  • Patent Documents 1 to 3 pay attention to the conditions of the hot rolling process, and the crystal orientation of the rolling surface is adjusted by controlling only the degree of rolling processing or the solution treatment conditions.
  • the strain rate is not controlled, the processing strains generated in the surface layer and the central portion are different, so the crystal orientations in the surface layer and the central portion are different.
  • the solution treatment the amount of heat received by the surface layer and the central portion is different, and the target crystal orientation is usually not achieved in the central portion where the influence of the heat amount is small. Therefore, in the production methods of these patent documents, the crystal orientation in the central portion cannot be controlled, and the maximum value of the X-ray random intensity ratio in the region including the ⁇ 001 ⁇ ⁇ 100> orientation has not increased in the central portion.
  • Manufacturing process In the manufacturing process of the present invention, first, an atmospheric melting furnace is used, and raw materials such as electrolytic copper, Ni, and Si are melted under charcoal coating to obtain a molten metal having a desired composition. This molten metal is cast into an ingot. After that, hot rolling is performed, cold rolling, solution treatment (700 to 1,000 ° C. for 10 to 300 seconds), aging treatment (350 to 550 ° C. for 2 to 20 hours), final cold rolling (working degree) 5-40%). Strain relief annealing may be performed after the final cold rolling. The strain relief annealing is usually performed at 250 to 600 ° C. for 5 to 300 seconds in an inert atmosphere such as Ar.
  • an inert atmosphere such as Ar.
  • cold rolling may be performed between the solution treatment and the aging treatment. Further, after the solution treatment, the final cold rolling and the aging treatment may be performed in this order, and the order of these steps may be changed.
  • aging treatment and final cold rolling conditions employed in the Cu-Ni-Si alloy manufacturing process and exemplified above The material that has undergone the cold rolling recrystallizes the crystal grains of the target orientation in both the surface layer and the central part by solution treatment, and the structure of the crystal orientation does not change essentially after the aging treatment and the final cold rolling.
  • (A) Hot rolling The ingot is heated at 800 to 1,000 ° C. for 1 to 20 hours, homogenized and annealed. After rolling, the cooling rate while lowering the material temperature from 600 to 300 ° C. is preferably 10 to 100 ° C./min, more preferably 20 to 80 ° C./min.
  • the cooling rate is out of the above range, inclusions having a particle diameter of 1 to 2 ⁇ m tend to be out of the range of 50 to 200 / mm 2 . That is, when the cooling rate is high, inclusions with a particle size of 1 to 2 ⁇ m are less than 50 / mm 2, and uniform strain cannot be generated in the thickness direction in the next cold rolling process, and when it is slow, the particle size is 1 to 2 ⁇ m.
  • the number of inclusions exceeds 200 / mm 2, and in the same way, uniform strain cannot be generated in the thickness direction in the next cold rolling step, and the bendability is lowered.
  • strain rate of cold rolling after hot rolling is preferably 1 ⁇ 10 ⁇ 6 to 1 ⁇ 10 ⁇ 4 / s, more preferably 5 ⁇ 10 ⁇ 5 to 8 0.0 ⁇ 10 ⁇ 5 / s.
  • strain rate is specified as rolling speed / roll contact arc length. When the strain rate is less than 1 ⁇ 10 ⁇ 6 / s, the maximum value of the X-ray intensity ratio of the obtained material is 3.0 or more at the surface layer, but less than 3.0 at the center.
  • the maximum value of the X-ray intensity ratio of the obtained material is 3.0 or more at the center, but it is not preferable because it becomes less than 3.0 at the surface layer.
  • Step 2 The oxidized scale on the plate surface after hot rolling was ground and removed with a grinder.
  • Step 3 Cold rolling was performed at a strain rate shown in Table 1 to a plate thickness of 0.180 mm. The strain rate was determined from rolling speed / roll contact arc length.
  • Step 4 As a solution treatment, the solution was heated in the air at 800 ° C. for 10 seconds and rapidly cooled in water.
  • Step 5 Using an electric furnace as an aging treatment, heating was performed in an Ar atmosphere at 450 ° C. for 5 hours.
  • Step 6 The final cold rolling was performed to a plate thickness of 0.15 mm.
  • Process 7) As strain relief annealing, it heated at 400 degreeC for 10 second in Ar atmosphere. The samples thus produced were evaluated for the following characteristics.
  • the maximum value of the X-ray random intensity ratio of the surface layer is the rolled surface, and the maximum value of the X-ray random intensity ratio of the central part is the central part of the plate thickness by spray etching of ferric chloride solution (1/2 of the plate thickness) Each of the exposed surfaces was measured. The measurement of the rolled surface was performed after the surface of the rolled surface was revealed by electrolytic polishing in a solution of 67% phosphoric acid + 10% sulfuric acid + water under conditions of 15 V 60 seconds, washed with water and dried.
  • FIG. 2A is used upside down in FIG. 2B.
  • the cross section of the bent part parallel to the rolling direction and parallel to the plate thickness direction was finished to a mirror surface by mechanical polishing and buffing, and the presence or absence of cracks was observed with an optical microscope (50 times magnification).
  • the case where no crack was observed by optical microscope observation was evaluated as ⁇ , and the case where crack was observed was evaluated as x.
  • excellent in bending workability means that when the above evaluation is performed on a sample having a plate thickness of 0.15 mm, no cracking is observed even in a notching process having a depth of 50 ⁇ m.
  • Comparative Example 1 had a low 0.2% proof stress because both the Ni and Si concentrations were low. In Comparative Example 2, cracks occurred during hot rolling because both Ni and Si concentrations were high. In Comparative Example 3, the concentration of additive elements other than Ni and Si was high, so the conductivity was low, and it was unsuitable as an electric / electronic component material. Comparative Example 4 is an example in which the number of inclusions was large because the cooling rate of hot rolling was slow. The maximum value of the X-ray random intensity ratio was less than 3.0 in both the surface layer and the central portion, and the bending workability was poor.
  • Comparative Examples 5 and 6 are examples of the prior art that are water-cooled after hot rolling. Since the cooling rate was high, the number of inclusions was small, and even when the strain rate of cold rolling was within an appropriate range, the maximum value of the X-ray random strength ratio was less than 3.0 in both the surface layer and the central portion, and the bending workability was It was bad. Comparative Examples 7 and 8 are examples in which the strain rate of cold rolling after hot rolling was high. The maximum value of the X-ray random intensity ratio at the center is 3.0 or more, but the surface layer is less than 3.0 and the bending workability is poor even when the notching depth is 25 ⁇ m (1/6 of the plate thickness). It was.
  • Comparative Examples 9 and 10 are examples in which the strain rate of cold rolling after hot rolling was slow. Although the maximum value of the X-ray random intensity ratio of the surface layer portion is 3.0 or more, the center portion is less than 3.0, and cracking did not occur at a notching depth of 25 ⁇ m, but 50 ⁇ m (1/1 of the plate thickness). 3) Cracks occurred and the bending workability was poor.
  • the maximum value of the X-ray random intensity ratio of the surface layer is increased to 3.0 or more by controlling the strain rate of the subsequent cold rolling by water cooling after hot rolling as in Patent Documents 1 to 3. This is an adjusted example. Since the maximum value of the X-ray random intensity ratio in the center was less than 3.0, cracking occurred at a notching depth of 50 ⁇ m or more, and bending workability after notching was poor.
  • the Cu—Ni—Si based copper alloy of the present invention does not generate cracks even if it is notched on the inner surface before press bending, and is excellent in bending workability. Suitable as a material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

L'invention concerne un alliage de Cu-Ni-Si montrant une capacité de cintrage améliorée même lorsqu'il est entaillé. L'invention concerne un fil d'alliage composé de 1,0 à 4,5% de Ni, 0,2 à 1,0% de Si, du cuivre, le reste étant des impuretés inévitables. Sur la couche de surface et le centre, la valeur maximum du rapport d'intensité aléatoire de rayons X sur la figure de pôle {200} est comprise entre 3,0 et 15,0 à l'intérieur d'une plage dans laquelle l'angle de rotation α de l'axe perpendiculaire à l'axe de rotation du goniomètre pour diffraction spécifiée par la méthode Shultz est compris dans une plage entre 0 et 10º; le nombre d'inclusions présentant une granulométrie de 1 à 2 µm est de préférence 50 à 200 inclusions/mm2 ; et l'alliage contient éventuellement un total de 0,005 à 2,5% d'un élément ou plus sélectionné dans le groupe constitué par Sn, Zn, Mg, Fe, Ti, Zr, Cr, Al, P, Mn, Co, Cr et Ag. L'alliage est produit par laminage à chaud, refroidissement de 600 à 300ºC à une vitesse de 10 à 100ºC/minute, puis laminage à froid à une vitesse de déformation de 1 x 10-6 à 1 x 10-4/s, traitement de la solution, vieillissement et laminage à froid final, avec un recuit possible.
PCT/JP2012/056568 2011-03-16 2012-03-14 FIL D'ALLIAGE DE Cu-Ni-Si À CAPACITÉ DE CINTRAGE EXCELLENTE Ceased WO2012124732A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201280013438.2A CN103429771B (zh) 2011-03-16 2012-03-14 弯曲加工性优异的Cu-Ni-Si系合金条
KR1020137026858A KR101590242B1 (ko) 2011-03-16 2012-03-14 굽힘 가공성이 우수한 Cu-Ni-Si 계 합금조

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2011-058054 2011-03-16
JP2011058054A JP5417366B2 (ja) 2011-03-16 2011-03-16 曲げ加工性に優れたＣｕ−Ｎｉ−Ｓｉ系合金

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WO2012124732A1 true WO2012124732A1 (fr) 2012-09-20

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JP (1) JP5417366B2 (fr)
KR (1) KR101590242B1 (fr)
CN (1) CN103429771B (fr)
TW (1) TWI453288B (fr)
WO (1) WO2012124732A1 (fr)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN103205600A (zh) * 2013-04-18 2013-07-17 大连理工大学 一种高强导电Cu-Ni-Si-M合金

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WO2015146981A1 (fr) * 2014-03-25 2015-10-01 古河電気工業株式会社 Matériau en feuille en alliage de cuivre, connecteur et procédé pour la fabrication de matériau en feuille en alliage de cuivre
CN104561649B (zh) * 2015-02-08 2016-08-31 江西省首诺铜业有限公司 一种高强度铜镍硅合金的生产工艺
JP6385383B2 (ja) * 2016-03-31 2018-09-05 Ｊｘ金属株式会社 銅合金板材および銅合金板材の製造方法
JP6762333B2 (ja) * 2018-03-26 2020-09-30 Ｊｘ金属株式会社 Ｃｕ−Ｎｉ−Ｓｉ系銅合金条
KR102052502B1 (ko) 2019-02-22 2019-12-05 김기찬 디스크 교체가 용이한 그라인더
JP2020158817A (ja) 2019-03-26 2020-10-01 Ｊｘ金属株式会社 強度と圧延平行方向および圧延直角方向の曲げ加工性に優れたＣｕ−Ｎｉ−Ｓｉ系合金条
CN111500893A (zh) * 2020-06-10 2020-08-07 铜陵高铜科技有限公司 超高强度铜合金板带材及其制造方法
CN114934204B (zh) * 2022-05-07 2022-12-20 陕西斯瑞新材料股份有限公司 一种电气化铁路接触网零部件用Cu-Ni-Si线材制备方法及其应用

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JP2007092135A (ja) * 2005-09-29 2007-04-12 Nikko Kinzoku Kk 強度と曲げ加工性に優れたＣｕ−Ｎｉ−Ｓｉ系合金
JP2010222618A (ja) * 2009-03-23 2010-10-07 Nippon Mining & Metals Co Ltd Ｃｕ−Ｎｉ−Ｓｉ系銅合金圧延板及びそれを用いた電気部品

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103205600A (zh) * 2013-04-18 2013-07-17 大连理工大学 一种高强导电Cu-Ni-Si-M合金

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KR20140002001A (ko) 2014-01-07
JP5417366B2 (ja) 2014-02-12
TW201247909A (en) 2012-12-01
JP2012193408A (ja) 2012-10-11
KR101590242B1 (ko) 2016-01-29
CN103429771B (zh) 2015-08-26
CN103429771A (zh) 2013-12-04
TWI453288B (zh) 2014-09-21

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