EP3070726B1 - Silberplattierungsmaterial und verfahren zur herstellung davon - Google Patents

Silberplattierungsmaterial und verfahren zur herstellung davon Download PDF

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Publication number
EP3070726B1
EP3070726B1 EP14861043.9A EP14861043A EP3070726B1 EP 3070726 B1 EP3070726 B1 EP 3070726B1 EP 14861043 A EP14861043 A EP 14861043A EP 3070726 B1 EP3070726 B1 EP 3070726B1
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EP
European Patent Office
Prior art keywords
silver
coated material
conditions
carried out
heat treatment
Prior art date
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Application number
EP14861043.9A
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English (en)
French (fr)
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EP3070726A4 (de
EP3070726A1 (de
Inventor
Akihiro Aiba
Hirofumi Takahashi
Takashi Ouchi
Satoru Endo
Ryu Murakami
Satoshi Miyazawa
Masahiko ODASHIMA
Hiroyuki Tokuda
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
Alps Alpine Co Ltd
Original Assignee
JX Nippon Mining and Metals Corp
Alps Alpine Co Ltd
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Publication date
Application filed by JX Nippon Mining and Metals Corp, Alps Alpine Co Ltd filed Critical JX Nippon Mining and Metals Corp
Publication of EP3070726A1 publication Critical patent/EP3070726A1/de
Publication of EP3070726A4 publication Critical patent/EP3070726A4/de
Application granted granted Critical
Publication of EP3070726B1 publication Critical patent/EP3070726B1/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/46—Electroplating: Baths therefor from solutions of silver
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/021—Composite material
    • H01H1/025—Composite material having copper as the basic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/041—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by bonding of a contact marking face to a contact body portion
    • H01H2011/046—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by bonding of a contact marking face to a contact body portion by plating

Definitions

  • This invention relates to a silver-coated material and a method of manufacture thereof. More specifically, the invention relates to a silver-coated material suitable as a contact in connectors, switches, terminals and electronic components.
  • Japanese Patent Publication No. 2012-49041 discloses a silver-coated material for moving contact components which has an electrically conductive base material made of copper or a copper alloy or of iron or an iron alloy on which are superimposed, in order, an underlayer made of nickel, a nickel alloy, cobalt or a cobalt alloy, an intermediate layer made of copper, a copper alloy, tin or a tin alloy, and an outermost layer made of silver or a silver alloy, and in which an intermediate oxide layer is present as a second intermediate layer between the intermediate layer and the outermost layer.
  • the intermediate oxide layer is a layer of an oxide of the metal making up the intermediate layer.
  • making an intermediate oxide layer present between the intermediate layer and the outermost layer has the effect of keeping the intermediate layer ingredients from diffusing to the surface and forming an oxide within the surface layer, thus preventing a rise in the contact resistance, and moreover has the effect of suppressing peeling of the silver layer at the surface.
  • the intermediate oxide layer is formed by 5 to 60 minutes of heating in open air at a temperature of 250°C after the outermost layer has been formed.
  • Patent Application Publication US 2012/0301745 discloses a silver-coated material for electric contacts having a silver plating layer on a nickel underlayer, wherein crystals having a columnar structure and an average grain size of 0.5 ⁇ m are included in the plating layer.
  • the object of this invention is to provide a silver-coated material of excellent abrasion resistance in which, even when used as, for example, a moving contact and/or a fixed contact in a switch used over an extended period of time under conditions where switching is repeatedly carried out, the silver or silver alloy layer at the surface does not wear away and, moreover, the contact resistance does not rise.
  • the inventors have conducted extensive investigations, as a result of which they have discovered that the above problem is resolved by the use of plating to form, as an outermost layer on an electrically conductive base material, a layer made of at least silver or a silver alloy, and heat-treating under specific heating conditions. This discovery led ultimately to the present invention.
  • the silver-coated material according to (1) above characterized in that the coating loss in the abrasion resistance test is less than 30 mg.
  • a switch characterized by using the silver-coated material according to (1) or (2) above as a moving contact and/or fixed contact for the switch.
  • a silver-coated material of excellent abrasion resistance in which the silver or silver alloy layer at the surface does not wear away and, moreover, the contact resistance does not rise even when used as, for example, a moving contact and/or a fixed contact in a switch used over an extended period of time under conditions where switching is repeatedly carried out.
  • the silver-coated material of this invention is a silver-coated material that has, as an outermost layer on an electrically conductive base material, a layer made of at least silver or a silver alloy, and is characterized by having a coating loss in an abrasion resistance test of less than 40 mg, and having an initial contact resistance of less than 10 m ⁇ and a contact resistance of less than 10 m ⁇ after a sliding wear test carried out under the following conditions.
  • Contact resistance measurement conditions Apparatus: Yamasaki type CRS-1 Contact Simulator Conditions: contact load, 10 g (Au probe); sliding distance, 1 mm Sliding wear test conditions: [Load] 1.6 N [Sliding range] 0.2 mm [Sliding speed] 1 mm/s [Number of cycles] 50 000, wherein, the abrasion resistance test is carried out in accordance with JIS H 8682 under conditions of a load of 4.9 N (500 gf) (surface area of abrasion, 12 mm x 31 mm), with #1500 emery paper, and 200 back-and-forth cycles.
  • the conductive base material is a material having, for example, electrical conductivity, spring characteristics and durability.
  • it is preferably made of copper or a copper alloy, or iron or an iron alloy.
  • Copper alloys that can be preferably used include bronzes, phosphor bronzes, brasses, titanium coppers, copper-nickel-silicon (Corson) alloys and beryllium coppers.
  • Iron alloys that can be preferably used include stainless steels (SUS) and Alloy 42.
  • silver alloys such as Ag-Sn alloys, Ag-Cu alloys, Ag-In alloys and Ag-Se alloys have good contact characteristics and thus can be preferably used.
  • the silver alloy is preferably one having a silver content in excess of 50% by mass.
  • the outermost layer made of silver or a silver alloy is formed by plating using a known silver plating solution or silver alloy plating solution.
  • the plating solution is not particularly limited, although a plating solution that contains cyanide as a complex is preferred. Prior to plating with a plating solution containing the cyanide as a complex, silver strike plating may be carried out. By using plating to form the outermost layer made of silver or a silver alloy, the layer can be easily and conveniently formed at a low cost.
  • the outermost layer has a thickness of preferably from 0.05 to 5 ⁇ m, more preferably from 0.1 to 2 ⁇ m, and even more preferably from 0.2 to 2 ⁇ m.
  • the silver-coated material of the invention may have an underlayer between the base material and the outermost layer made of silver or a silver alloy.
  • the underlayer include a plated Ni layer, a plated copper layer and a plated cobalt layer. These may be formed with a known plating solution and under known plating conditions.
  • the plating solution used to form an underlying plated Ni layer is preferably a sulfamate bath.
  • the plating solution used to form an underlying plated copper layer is preferably a copper cyanide bath.
  • Preferred silver-coated materials of the invention are ones having an outermost layer made of silver or a silver alloy on an electrically conductive base material, and ones having a plated copper or a plated Ni layer as an underlayer between an electrically conductive base material and an outermost layer made of silver or a silver alloy.
  • the silver-coated material of the invention after the outermost layer has been formed, is heat-treated at 200 to 500°C for 1 to 299 seconds. At a low temperature in this temperature range, it is preferable to make the treatment time longer; at a high temperature, it is preferable to make the treatment time shorter. From the standpoint of productivity, heat treatment at 250 to 450°C for 1 to 59 seconds is preferred, heat treatment at 270 to 450°C for 1 to 30 seconds is more preferred, and heat treatment at 300 to 450°C for 1 to 10 seconds is especially preferred.
  • the spherical silver or silver alloy crystal grains in the outermost layer grow, enlarging to an average crystal grain size of 0.2 ⁇ m or more and becoming columnar in the plating thickness direction, and so the outermost layer includes crystals of a columnar structure that are made of silver or a silver alloy.
  • the silver-coated material of the present invention is further characterized in that the outermost layer has an average crystal grain size of 0.2 ⁇ m or more and 0.5 ⁇ m or less, and includes crystals having a columnar structure.
  • heat treatment may be carried out in an inert gas atmosphere.
  • heat treatment in open air is easy and desirable.
  • the heating method for heat treatment is not particularly limited. Heat treatment may be carried out using, for example, a hot plate or a circulating hot-air oven.
  • a silver-coated material with, as the outermost layer, a layer made of silver or a silver alloy, when heat-treated in this way, has a coating loss in an abrasion resistance test of less than 40 mg and has an initial contact resistance of less than 10 m ⁇ and a contact resistance of less than 10 m ⁇ after a sliding wear test has been carried out under the following conditions.
  • a coating loss in the abrasion resistance test of less than 30 mg is more preferred.
  • the coating loss can be made less than 30 mg by the heat treatment conditions.
  • the abrasion resistance test was carried out in accordance with JIS H 8682 under conditions of a load of 4.9 N (500 gf) (surface area of abrasion, 12 mm ⁇ 31 mm), with #1500 emery paper, and 200 back-and-forth cycles.
  • the silver-coated material of the invention has, as mentioned above, an excellent peel resistance and abrasion resistance, and the contact resistance does not rise, it can be suitably used in connectors and switches serving as connection components for electronic equipment.
  • This plated substrate was heat-treated in open air using a hot plate under the Example 1 conditions in Table 1.
  • the heat treatment temperature is the temperature of the plated substrate that has been set on a hot plate, as measured with a thermocouple.
  • phosphor bronze C5210, 25 mm ⁇ 20 mm ⁇ 0.2 mm (T): copper plating to a thickness of 3 ⁇ m in a copper cyanide bath, silver strike plating to a thickness of 0.05 ⁇ m, and silver plating in a high silver cyanide bath to a thickness of 0.4 ⁇ m, was used as the test material.
  • This plated substrate was heat-treated using a hot plate in open air under the Example 4 conditions in Table 1.
  • Example 2 Aside from changing the heat treatment conditions in Example 2 to the conditions indicated in Table 1 and heating in a nitrogen atmosphere (oxygen concentration of less than 1%), a heat-treated plated substrate was obtained in the same way as in Example 2.
  • Example 4 Aside from changing the heat treatment conditions in Example 4 to the conditions indicated in Table 1, a heat-treated plated substrate was obtained in the same way as in Example 4.
  • Example 2 Aside from changing the heat treatment conditions in Example 2 to the conditions indicated in Table 1, a heat-treated plated substrate was obtained in the same way as in Example 2.
  • Example 4 Aside from changing the heat treatment conditions in Example 4 to the conditions indicated in Table 1, a heat-treated plated substrate was obtained in the same way as in Example 4.
  • Example 2 Aside from changing the heat treatment conditions in Example 2 to the conditions indicated in Table 1, a heat-treated plated substrate was obtained in the same way as in Example 2.
  • Example 1 Aside from changing the heat treatment conditions in Example 1 to the conditions indicated in Table 1, a heat-treated plated substrate was obtained in the same way as in Example 1.
  • Example 4 Aside from changing the heat treatment conditions in Example 4 to the conditions indicated in Table 1, heat-treated plated substrates were obtained in the same way as in Example 4.
  • Abrasion resistance tests were carried out on the heat-treated plated substrates.
  • the abrasion resistance test was carried out in accordance with JIS H 8682 and using a Suga Abrasion Tester (NUS-IS03) under the conditions of a load of 4.9 N (500 gf) (surface area of abrasion, 12 mm ⁇ 31 mm), with #1500 emery paper, and 200 back-and-forth cycles. Rating Criteria:
  • the heat-treated plated substrate was FIB milled, following which the average crystal grain size and the shape of the crystals were determined from a cross-sectional SIM image (using an SMI3050SE system from SII Nanotechnologies).
  • FIGS. 1 to 3 Cross-sectional SIM images of the plated substrates obtained in Example 1, Comparative Example 1 and Comparative Example 3 are shown in, respectively, FIGS. 1 to 3 .
  • the plated silver layer includes silver crystals of a columnar structure. Such shapes were referred to as “columnar.”
  • the silver grains in the plated silver layer are rounded. Such shapes were referred to as “round.”
  • the silver crystals are horizontally elongated. Such shapes were referred to as “horizontally elongated.”

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Contacts (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Manufacture Of Switches (AREA)

Claims (7)

  1. Silberplattiertes Material mit einer Silberplattierungsschicht auf einem elektrisch leitfähigen Grundmaterial, direkt und/oder über eine Zwischenschicht, wobei die Silberplattierungsschicht eine äußerste Schicht, hergestellt aus Silber oder einer Silberlegierung, ist, wobei Kristalle einer Stängelstruktur mit einer mittleren Kristallkomgröße von 0,2 µm oder mehr und 0,5 µm oder weniger, gemessen gemäß JIS H 0501, die aus Silber oder einer Silberlegierung hergestellt sind, in der Schicht eingeschlossen sind, welche aus Silber oder einer Silberlegierung hergestellt ist, und wobei das silberplattierte Material einen Plattierungsverlust in einem Abriebbeständigkeitstest von weniger als 40 mg aufweist und einen anfänglichen Kontaktwiderstand von weniger als 10 mΩ und einen Kontaktwiderstand von weniger als 10 mΩ nach einem Gleitverschleißtest, durchgeführt unter den folgenden Bedingungen, aufweist:
    Kontaktwiderstand-Messbedingungen: Gerät: Yamasaki Typ CRS-1 Contact Simulator Bedingungen: Kontaktbeladung, 10 g (Au-Sonde); Gleitdistanz, 1 mm
    Gleitverschleiß-Testbedingungen:
    [Beladung] 1,6 N
    [Gleitbereich] 0,2 mm
    [Gleitgeschwindigkeit] 1 mm/s
    [Anzahl von Zyklen] 50 000,
    wobei der Abriebbeständigkeitstest gemäß JIS H 8682 unter Bedingungen einer Beladung von 4,9 N (500 gf) (Oberfläche von Abrieb, 12 mm x 31 mm) mit Nr. 1500 Sandpapier und 200 Hin-und-Her-Zyklen durchgeführt wird.
  2. Silberplattiertes Material gemäß Anspruch 1, dadurch gekennzeichnet, dass der Plattierungsverlust in dem Abriebbeständigkeitstest weniger als 30 mg beträgt.
  3. Schalter, gekennzeichnet durch Verwenden des silberplattierten Materials gemäß Anspruch 1 oder 2 als ein beweglicher Kontakt und/oder fester Kontakt für den Schalter.
  4. Verfahren zum Herstellen des silberplattierten Materials gemäß Anspruch 1 oder 2 mit einer Silberplattierungsschicht auf einem elektrisch leitfähigen Grundmaterial, direkt und/oder über eine Zwischenschicht, wobei die Silberplattierungsschicht eine äußerste Schicht, hergestellt aus Silber oder einer Silberlegierung, ist, und wobei das Verfahren einen Schritt von Bilden der Schicht, die aus Silber oder einer Silberlegierung hergestellt ist, durch Plattieren und Wärmebehandeln derselben bei 200 bis 500°C 1 bis 299 Sekunden lang einschließt.
  5. Verfahren zum Herstellen des silberplattierten Materials gemäß Anspruch 4, dadurch gekennzeichnet, dass die Wärmebehandlung bei 250 bis 450°C 1 bis 59 Sekunden lang durchgeführt wird.
  6. Verfahren zum Herstellen des silberplattierten Materials gemäß Anspruch 4, dadurch gekennzeichnet, dass die Wärmebehandlung bei 270 bis 450°C 1 bis 30 Sekunden lang durchgeführt wird.
  7. Verfahren zum Herstellen des silberplattierten Materials gemäß Anspruch 4, dadurch gekennzeichnet, dass die Wärmebehandlung bei 300 bis 450°C 1 bis 10 Sekunden lang durchgeführt wird.
EP14861043.9A 2013-11-11 2014-11-10 Silberplattierungsmaterial und verfahren zur herstellung davon Active EP3070726B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2013233244 2013-11-11
JP2013264021 2013-12-20
PCT/JP2014/079705 WO2015068835A1 (ja) 2013-11-11 2014-11-10 銀被覆材及びその製造方法

Publications (3)

Publication Number Publication Date
EP3070726A1 EP3070726A1 (de) 2016-09-21
EP3070726A4 EP3070726A4 (de) 2017-08-02
EP3070726B1 true EP3070726B1 (de) 2019-05-15

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EP (1) EP3070726B1 (de)
JP (1) JP6162817B2 (de)
KR (1) KR101751167B1 (de)
CN (1) CN105247642B (de)
MY (1) MY178336A (de)
SG (1) SG11201509591VA (de)
TW (1) TWI651744B (de)
WO (1) WO2015068835A1 (de)

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JP6579425B2 (ja) * 2015-06-16 2019-09-25 富士電機機器制御株式会社 基板用スイッチ
JP7359046B2 (ja) * 2020-03-11 2023-10-11 株式会社オートネットワーク技術研究所 金属材、接続端子、および金属材の製造方法

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JP2915623B2 (ja) * 1991-06-25 1999-07-05 古河電気工業株式会社 電気接点材料とその製造方法
JP3874621B2 (ja) * 2001-03-30 2007-01-31 株式会社神戸製鋼所 嵌合型接続端子用Ｓｎめっき銅合金材料及び嵌合型接続端子
JP3772240B2 (ja) * 2003-06-11 2006-05-10 東洋精箔株式会社 押しボタンスイッチに用いる電気接点用ばね材およびその製造方法
JP4728571B2 (ja) * 2003-10-31 2011-07-20 古河電気工業株式会社 可動接点用銀被覆ステンレス条の製造方法
JP4367457B2 (ja) * 2006-07-06 2009-11-18 パナソニック電工株式会社 銀膜、銀膜の製造方法、ｌｅｄ実装用基板、及びｌｅｄ実装用基板の製造方法
CN102667989B (zh) * 2010-02-12 2016-05-04 古河电气工业株式会社 可动接点部件用银包覆复合材料、其制造方法以及可动接点部件
JP2012049041A (ja) 2010-08-27 2012-03-08 Furukawa Electric Co Ltd:The 可動接点部品用銀被覆材およびその製造方法

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Publication number Publication date
JP6162817B2 (ja) 2017-07-19
TW201523668A (zh) 2015-06-16
EP3070726A4 (de) 2017-08-02
CN105247642B (zh) 2017-08-18
WO2015068835A1 (ja) 2015-05-14
KR20160007650A (ko) 2016-01-20
TWI651744B (zh) 2019-02-21
CN105247642A (zh) 2016-01-13
JPWO2015068835A1 (ja) 2017-03-09
MY178336A (en) 2020-10-08
EP3070726A1 (de) 2016-09-21
KR101751167B1 (ko) 2017-06-27
SG11201509591VA (en) 2015-12-30

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