EP3584353A1 - Metallstoff für elektronische komponente, verfahren zur herstellung des besagten metallstoffs und anschlussklemme, steckverbinder und elektronische komponente, in der der besagte metallstoff verwendet wird - Google Patents

Metallstoff für elektronische komponente, verfahren zur herstellung des besagten metallstoffs und anschlussklemme, steckverbinder und elektronische komponente, in der der besagte metallstoff verwendet wird Download PDF

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Publication number
EP3584353A1
EP3584353A1 EP17896426.8A EP17896426A EP3584353A1 EP 3584353 A1 EP3584353 A1 EP 3584353A1 EP 17896426 A EP17896426 A EP 17896426A EP 3584353 A1 EP3584353 A1 EP 3584353A1
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EP
European Patent Office
Prior art keywords
metallic material
constituent element
layer
element group
electronic components
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP17896426.8A
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English (en)
French (fr)
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EP3584353A4 (de
EP3584353A9 (de
Inventor
Satoru Endo
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
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JX Nippon Mining and Metals Corp
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Publication of EP3584353A1 publication Critical patent/EP3584353A1/de
Publication of EP3584353A9 publication Critical patent/EP3584353A9/de
Publication of EP3584353A4 publication Critical patent/EP3584353A4/de
Withdrawn legal-status Critical Current

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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
    • C25D7/00—Electroplating characterised by the article coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/325—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with layers graded in composition or in physical properties
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/36—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including layers graded in composition or physical properties
    • 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
    • C25D5/48—After-treatment of electroplated surfaces
    • 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
    • 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
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/02—Electrolytic coating other than with metals with organic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/02—Contact members
    • H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D3/30—Electroplating: Baths therefor from solutions of tin
    • 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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • 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
    • C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting

Definitions

  • the present invention relates to a metallic material for electronic components, a method for producing the same, connector terminals, connectors and electronic components using the same.
  • Sn or Sn alloy plating is generally required to have properties such as low contact resistance and high solder wettability, and further, recently the reduction of the insertion force has also been required at the time of joining together a male terminal and a female terminal molded by press processing of plating materials.
  • Patent Literature 1 discloses a coating material comprising a conductive base material and a coating layer formed on the conductive base material.
  • the coating layer comprises intermetallic compounds of Sn and precious metals on at least its surface.
  • Patent Literature 1 discloses that, according to this, contact resistance is low and it has a low coefficient of friction and is effective for reducing insertion force.
  • Patent Literature 1 Japanese Patent Laid-Open No. 2005-126763
  • the coating layer comprises intermetallic compounds of Sn and precious metals, and a thickness of Ag-Sn alloy layer comprising intermetallic compounds (Ag 3 Sn) of Sn and precious metals is preferably 1 ⁇ m or more and 3 ⁇ m or less.
  • a thickness of Ag-Sn alloy layer comprising intermetallic compounds (Ag 3 Sn) of Sn and precious metals is preferably 1 ⁇ m or more and 3 ⁇ m or less.
  • the thickness could not reduce the insertion force sufficiently.
  • the alloy layer is in a state where intermetallic compound particles are dispersed in the Sn matrix, Sn is exposed.
  • a surface of the alloy layer can corrode in corrosive environments. This leads to an increase in electrical resistance.
  • the conventional metallic material for electronic components having the Sn-Ag alloy / Ni base plating structure still has a problem that the insertion force cannot be lowered sufficiently.
  • the present invention has been achieved in order to solve the above-described problems, and an object of the present invention is the provision of a metallic material for electronic components, and connector terminals, connectors and electronic components using the same, having a low adhesive wear.
  • the adhesive wear refers to a wear phenomenon that occurs due to the fact that an adhesive portion constituting the real contact area between solids is sheared by frictional motion. When the adhesive wear increases, the insertion force when the male terminal and the female terminal are fitted together increases.
  • a metallic material for electronic components having a low adhesive wear can be produced by disposing a lower layer, an intermediate layer and an upper layer on a base material by using a prescribed metals, and controlling an amount of oxide particles on a surface of the treated layer after heating.
  • a metallic material for electronic components comprising:
  • the treated layer further comprises one or more selected from the group consisting of S, P and N.
  • Another aspect of the present invention is a method for producing a metallic material for electronic components, comprising a step of placing a metallic material in a treatment solution containing 2.5 to 5.0 g/L of phosphate ester-based treatment solution and stirring ultrasonically to form a treated layer having C (carbon) content being 60at% or more and O (oxygen) content being 30at% or less on a surface of the metallic material, wherein the metallic material comprises:
  • the phosphate ester-based treatment solution contains at least one of phosphoric acid esters represented by the following general formulas [1] and [2], and at least one selected from a group of cyclic organic compounds represented by the following general formulas [3] and [4]: (wherein, in formulas [1] and [2], R1 and R2 each represent a substituted alkyl group and M represents a hydrogen atom or an alkali metal) (wherein, in formulas [3] and [4], R1 represents a hydrogen atom, an alkyl group or a substituted alkyl group; R2 represents an alkali metal, a hydrogen atom, an alkyl group or a substituted alkyl group; R3 represents an alkali metal or a hydrogen atom; R4 represents -SH, an alkyl group-substituted or aryl group-substituted amino group, or represents an alkyl-substitute
  • the present invention is, in yet another aspect thereof, a connector terminal comprising the metallic material for electronic components of the present invention in a contact portion thereof.
  • the present invention is, in yet another aspect thereof, a connector comprising the connector terminal of the present invention.
  • the present invention is, in yet another aspect thereof, an FFC terminal comprising the metallic material for electronic components of the present invention in a contact portion thereof.
  • the present invention is, in yet another aspect thereof, an FPC terminal comprising the metallic material for electronic components of the present invention in a contact portion thereof.
  • the present invention is, in yet another aspect thereof, an FFC comprising the FFC terminal of the present invention.
  • the present invention is, in yet another aspect thereof, an FPC comprising the FPC terminal of the present invention.
  • the present invention is, in yet another aspect thereof, an electronic component comprising the metallic material for electronic components of the present invention in an electrode thereof for external connection.
  • the present invention is, in yet another aspect thereof, an electronic component comprising the metallic material for electronic components of the present invention, in a push-in type terminal thereof for fixing a board connection portion to a board by pushing the board connection portion into a through hole formed in the board, wherein a female terminal connection portion and the board connection portion are provided respectively on one side and the other side of a mounting portion to be attached to a housing.
  • Figure 1 is a schematic diagram which shows the structure of the metallic material for electronic components according to the embodiments of the present invention.
  • the metallic material for electronic components according to the embodiments of the present invention are described.
  • the lower layer 12 is formed on the base material 11
  • the intermediate layer 13 is formed on the lower layer 12
  • the upper layer 14 is formed on the intermediate layer 13 in the metallic material 10 for electronic components according to the embodiments of the present invention.
  • the base material 11 can be, not particularly limited, but for example, metal substrates such as copper and copper alloys, Fe-based materials, stainless steel, titanium and titanium alloys, aluminum and aluminum alloys.
  • the base material 11 can be a composite of a metal base and a resin layer.
  • the composite of a metal base and a resin layer is, for example, electrode parts on FPC or FFC substrate.
  • the upper layer 14 is constituted with an alloy comprising one or two selected from a constituent element group B consisting of Sn and In and one or two or more selected from a constituent element group C consisting of Ag, Au, Pt, Pd, Ru, Rh, Os and Ir.
  • Sn and In are oxidizable metals, but are characterized by being relatively soft among metals. Accordingly, even when an oxide film is formed on the surface of Sn or In, for example at the time of joining together a male terminal and a female terminal by using a metallic material for electronic components as a contact material, the oxide film is easily scraped to result in contact between metals, and hence a low contact resistance is obtained.
  • Sn and In are excellent in the gas corrosion resistance against the gases such as chlorine gas, sulfurous acid gas and hydrogen sulfide gas; for example, when Ag poor in gas corrosion resistance is used for the upper layer 14, Ni poor in gas corrosion resistance is used for the lower layer 12, and copper or a copper alloy poor in gas corrosion resistance is used for the base material 11, Sn and In have an effect to improve the gas corrosion resistance of the metallic material for electronic components.
  • Sn and In Sn is preferable because In is severely regulated on the basis of the technical guidelines for the prevention of health impairment prescribed by the Ordinance of Ministry of Health, Labour and Welfare.
  • Ag, Au, Pt, Pd, Ru, Rh, Os and Ir are characterized by being relatively heat-resistant among metals. Accordingly, these metals suppress the diffusion of the composition of the base material 11 and the lower layer 12 toward the side of the upper layer 14 to improve the heat resistance. These metals also form compounds with Sn or In in the upper layer 14 to suppress the formation of the oxide film of Sn or In, so as to improve the solder wettability.
  • Ag Au, Pt, Pd, Ru, Rh, Os and Ir
  • Ag is more desirable from the viewpoint of electrical conductivity. Ag is high in electrical conductivity. For example, when Ag is used for high-frequency wave signals, impedance resistance is made low due to the skin effect.
  • the ⁇ (zeta)-phase being a Sn-Ag alloy including Sn in a content of 11.8 to 22.9 at% is preferably present.
  • the gas corrosion resistance is improved, and the exterior appearance is hardly discolored even when the gas corrosion test is performed.
  • the ⁇ (zeta)-phase and the ⁇ (epsilon)-phase being Ag 3 Sn are preferably present.
  • the coating becomes harder and the adhesive wear is decreased.
  • the increase of the proportion of Sn in the upper layer 14 improves the gas corrosion resistance.
  • the coating becomes further harder and the adhesive wear is decreased as compared with the case where the ⁇ (zeta)-phase and the ⁇ (epsilon)-phase being Ag 3 Sn are present in the upper layer 14.
  • the more increase of the proportion of Sn in the upper layer 14 also improves the gas corrosion resistance.
  • the presence of the ⁇ (epsilon)-phase being Ag 3 Sn and the ⁇ -Sn being a Sn single phase in the upper layer 14 is preferable.
  • the gas corrosion resistance is improved with a furthermore increase of the proportion of Sn in the upper layer 14 as compared with the case where only the ⁇ (epsilon)-phase is present in the upper layer.
  • the ⁇ (zeta)-phase being a Sn-Ag alloy including Sn in a content of 11.8 to 22.9 at%
  • the ⁇ (epsilon)-phase being Ag 3 Sn and ⁇ -Sn being a Sn single phase
  • the gas corrosion resistance is improved, the exterior appearance is hardly discolored even when a gas corrosion test is performed, and the adhesive wear is decreased.
  • the composition concerned is created by diffusion and involves no structure in an equilibrium state.
  • the upper layer 14 should not be present as solely composed of ⁇ -Sn.
  • the adhesive wear is significant, whiskers occur and, for example, the heat resistance and the fine sliding wear resistance are degraded.
  • the upper layer 14 preferably includes the metal(s) of the constituent element group B in a content of 10 to 50 at%.
  • the content of the metal(s) of the constituent element group B is less than 10 at%, the gas corrosion resistance is poor, and sometimes the exterior appearance is discolored when a gas corrosion test is performed.
  • the content of the metal(s) of the constituent element group B exceeds 50 at%, the proportion of the metal(s) of the constituent element group B in the upper layer 14 is large, and hence the adhesive wear is increased and whiskers also tend to occur. Moreover, the fine sliding wear resistance is sometimes poor.
  • the treated layer having C (carbon) content being 60at% or more and O (oxygen) content being 30at% or less is provided on the upper layer 14.
  • the treated layer is formed by a surface treatment such as a sealing treatment performed after forming the upper layer 14.
  • C (carbon) contained in the treated layer is a component resulting from surface treatment such as sealing treatment.
  • the treated layer can further comprise one or more selected from the group consisting of S, P and N.
  • An area ratio of oxide particles adhering to a surface of the treated layer is controlled to be 0.1 % or less when the metallic material is heated at 250 °C for 30 seconds.
  • the oxide particles adhering to the surface of the treated layer after the heating adversely affects the adhesive wear of metallic material for electronic components. Accordingly, the metallic material for electronic components having a low adhesive wear can be provided by controlling the area ratio of oxide particles to be 0.1% or less.
  • the intermediate layer 13 consists of one or two or more selected from the constituent element group A consisting of Ni, Cr, Mn, Fe, Co and Cu and one or two selected from the constituent element group B consisting of Sn and In. According to such a configuration, it has an effect of improving heat resistance and solder wettability. Furthermore, in this case, the thickness of the intermediate layer 13 is preferably 0.01 ⁇ m or more and less than 0.40 ⁇ m.
  • Sn and In are excellent in the gas corrosion resistance against the gases such as chlorine gas, sulfurous acid gas and hydrogen sulfide gas; for example, when Ni poor in gas corrosion resistance is used for the lower layer 12, and copper or a copper alloy poor in gas corrosion resistance is used for the base material 11, Sn and In have an effect to improve the gas corrosion resistance of the metallic material for electronic components.
  • Ni, Cr, Mn, Fe, Co and Cu provide a harder coating as compared with Sn and In, accordingly make the adhesive wear hardly occur, prevent the diffusion of the constituent metal(s) of the base material 11 into the upper layer 14, and thus improve the durability in such a way that the degradation of the heat resistance or the degradation of the solder wettability is suppressed.
  • the thickness of the intermediate layer 13 is less than 0.01 ⁇ m, there is a possibility that a coating becomes hard and adhesive wear decreases. On the other hand, when the thickness of the intermediate layer 13 is 0.40 ⁇ m or more, there is a possibility that bending workability decreases, mechanical durability decreases, and plating scraping occurs.
  • Sn is preferable because In is severely regulated on the basis of the technical guidelines for the prevention of health impairment prescribed by the Ordinance of Ministry of Health, Labour and Welfare.
  • Ni, Cr, Mn, Fe, Co and Cu Ni is preferable because Ni is hard, adhesive wear hardly occurs, and sufficient bending workability is obtained.
  • the intermediate layer 13 preferably includes the metal(s) of the constituent element group B in a content of 35 at% or more.
  • the content of Sn is 35 at% or more, there is a possibility that a coating becomes hard and adhesive wear decreases.
  • the intermediate layer 13 can consist of Ni 3 Sn and Ni 3 Sn 2 , and can consist of only Ni 3 Sn 2 or only Ni 3 Sn 4 .
  • the presence of Ni 3 Sn, Ni 3 Sn 2 , and Ni 3 Sn 4 may improve heat resistance and solder wettability.
  • Ni 3 Sn 4 and ⁇ -Sn being a Sn single phase in the intermediate layer 13 is preferable. By the presence of these, a heat resistance and a solder wettability are improved compared to the case where Ni 3 Sn 4 and Ni 3 Sn 2 are present.
  • the thickness of the upper layer 14 is preferably 0.02 ⁇ m or more and less than 1.00 ⁇ m.
  • the thickness of the upper layer 14 is less than 0.02 ⁇ m, the gas corrosion resistance is poor, and the exterior appearance is discolored when the gas corrosion test is performed.
  • the thickness of the upper layer 14 is 1.00 ⁇ m or more, the thin film lubrication effect by the hard base material 11 or the lower layer 12 is lowered and adhesive wear may be increased. Furthermore, mechanical durability decreases, and plating scraping is likely to occur.
  • the thickness of the upper layer 14 is preferably less than 0.50 ⁇ m.
  • the lower layer 12 is constituted with one or two or more selected from a constituent element group A consisting of Ni, Cr, Mn, Fe, Co and Cu. Such a configuration prevents a diffusion of the constituent metal(s) of the base material 11 into the intermediate layer 13 or the upper layer 14.
  • the thickness of the lower layer 12 is preferably 0.05 ⁇ m or more.
  • the thickness of the lower layer 12 is less than 0.05 ⁇ m, the thin film lubrication effect by the hard lower layer is lowered and adhesive wear may be increased. Furthermore, the constituent metal(s) of the base material 11 is likely to diffuse into the upper layer 14, and a heat resistance and a solder wettability may deteriorate.
  • the thickness of the lower layer 12 is preferably less than 5.00 ⁇ m. When the thickness of the lower layer 12 is 5.00 ⁇ m or more, a bending workability may be poor.
  • the lower layer 12 can have a composition in which a total amount of metal(s) of the constituent element group A is 50 mass% or more, and a total amount of metal(s) of one or two or more selected from a group consisting of B, P, Sn and Zn is less than 50 mass%. Because the alloy composition of the lower layer 12 has such a configuration, the lower layer 12 is further hardened, the thin film lubricating effect is further improved, and the adhesive wear is further reduced. The alloying of the lower layer 12 further prevents the constituent metals of the base material 11 from diffusing into the upper layer, and may improve durability such as heat resistance and solder wettability.
  • the upper layer 14 can have a composition in which a total amount of metal(s) of the constituent element group B and the constituent element group C is 50 mass% or more, and a total amount of metal(s) of one or two or more selected from a group consisting of As, Bi, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, W and Zn is less than 50 mass%. Because the alloy composition of the upper layer 14 has such a configuration, adhesive wear may be reduced, whisker generation may be suppressed, and furthermore, durability such as heat resistance and solder wettability may be improved.
  • the intermediate layer 13 can have a composition in which a total amount of metal(s) of the constituent element group C is 50 mass% or more, and a total amount of metal(s) of one or two or more selected from a group consisting of Bi, Cd, Co, Cu, Fe, In, Mn, Mo, Ni, Pb, Sb, Se, Sn, W, Tl and Zn is less than 50 mass%. Because the alloy composition of the intermediate layer 13 has such a configuration, adhesive wear may be reduced, whisker generation may be suppressed, and furthermore, durability such as heat resistance and solder wettability may be improved.
  • a metallic material is prepared.
  • the metallic material comprises the base material, on the base material, the lower layer constituted with one or two or more selected from the constituent element group A consisting of Ni, Cr, Mn, Fe, Co and Cu, on the lower layer, an intermediate layer, on the intermediate layer, an upper layer constituted with an alloy comprising one or two selected from the constituent element group B consisting of Sn and In and one or two or more selected from the constituent element group C consisting of Ag, Au, Pt, Pd, Ru, Rh, Os and Ir.
  • the intermediate layer consists of one or two or more selected from the constituent element group A and one or two selected from the constituent element group B.
  • the metallic material can be produced by Wet (electrical, electroless) plating, dry (sputtering, ion plating, etc.) plating, etc.
  • the upper layer 14, the intermediate layer 13 and the lower layer 12 may be formed, by forming a film of one or two or more selected from the constituent element group A on the base material 11, then forming a film of one or two selected from the constituent element group B, then forming a film of one or two or more selected from the constituent element group C, and by diffusion of the respective selected elements of the constituent element group B and the constituent element group C.
  • the metal from the constituent element group B is Ag
  • the metal from the constituent element group C is Sn
  • the diffusion of Ag into Sn is fast, and thus a Sn-Ag alloy layer is formed by spontaneous diffusion.
  • the formation of the alloy layer can further reduce the adhesion force of Sn, and the low degree of whisker formation and the durability can also be further improved.
  • a heat treatment may be applied for the purpose of further suppressing the adhesive wear and further improving the low degree of whisker formation and the durability.
  • the heat treatment allows the metal(s) of the constituent element group B and the metal(s) of the constituent element group C of the upper layer 14 to diffuse to form an alloy layer more easily, further reduces the adhesion force of Sn, and can further improve the low degree of whisker formation and the durability.
  • the heat treatment may be performed in a reducing atmosphere or a non-oxidizing atmosphere.
  • treatment conditions temperature ⁇ time
  • the heat treatment is not particularly required to be applied.
  • the heat treatment performed at a temperature equal to or higher than the melting point of the metal(s) selected from the constituent element group B allows the metal(s) of one or two selected from the constituent element group B and the metal(s) of one or two or more selected from the constituent element group A to form an alloy layer more easily, and also allows the metal(s) of one or two selected from the constituent element group B and the metal(s) of one or two or more selected from the constituent element group C to form an alloy layer more easily.
  • the heat treatment performed at a temperature equal to or higher than the melting point of the metal(s) selected from the constituent element group B allows the metal(s) of one or two or more selected from the constituent element group C and the metal(s) of one or two selected from the constituent element group B to form an alloy layer more easily.
  • a post-treatment may be applied for the purpose of further decreasing the adhesive wear and improving the low degree of whisker formation and the durability to produce the treated layer.
  • the post-treatment is to place the metallic material in a treatment solution containing 2.5 to 5.0 g/L of phosphate ester-based treatment solution and stir ultrasonically to form the treated layer having C (carbon) content being 60at% or more and O (oxygen) content being 30at% or less on a surface of the metallic material.
  • a strong sealing membrane is produced by finely dispersing a sealing component in a treatment solution containing phosphate ester-based treatment solution at a high concentration of 2.5 to 5.0 g/L with stirring ultrasonically.
  • a treatment solution containing phosphate ester-based treatment solution at a high concentration of 2.5 to 5.0 g/L with stirring ultrasonically.
  • the concentration of the phosphate ester-based treatment solution exceeds 5.0 g/L, an adhesive wear becomes high.
  • the concentration of the phosphate ester-based treatment solution is preferably 3.0 to 4.0 g/L.
  • An electrolytic potential for forming the treated layer is preferably 2.0 to 3.5 V. When the electrolytic potential is less than 2.0 V, the strong sealing membrane cannot be produced and there may be a problem in corrosion resistance and heat resistance. When the electrolytic potential exceeds 3.5 V, there may be a problem of discoloration.
  • the electrolytic potential is preferably 3.0 to 3.5 V.
  • the post-treatment reduces adhesive wear properties, improves lubricity, and improves durability such as heat resistance and solder wettability.
  • a specific post-treatment includes phosphate treatment using an inhibitor, and further includes lubrication treatment and silane coupling treatment.
  • the treatment conditions temperature x time
  • the treatment conditions can be selected as appropriate.
  • the oxide Prior to the post-treatment, it is desirable to remove the oxide on the surface oxidized by the heat treatment.
  • the oxide may be removed by pickling or reverse electrolysis with the same solution as the post-treatment solution. This exposes a fresh, unoxidized alloy surface.
  • post-treatment components are adsorbed. More organic materials with a specific structure adhere to the surface where the alloy is exposed than the surface where the oxide is exposed. Accordingly, further improvement in lubricity and durability is expected.
  • the oxide removal treatment may not be performed.
  • the post-treatment is preferably performed for the surface of the upper layer 14 by using an aqueous solution (referred to as the phosphoric acid ester-based solution) including one or two or more phosphoric acid esters and one or two or more cyclic organic compounds.
  • the phosphoric acid ester(s) added to the phosphoric acid ester-based solution plays the functions as an antioxidant and a lubricant for plating.
  • the phosphoric acid esters used in the present invention are represented by the general formula [1] and [2]. Examples of the preferable compounds among the compounds represented by the general formula [1] include lauryl acidic phosphoric acid monoester. Examples of the preferable compounds among the compounds represented by the general formula [2] include lauryl acidic phosphoric acid diester. (wherein, in formulas [1] and [2], R1 and R2 each represent a substituted alkyl group and M represents a hydrogen atom or an alkali metal)
  • the cyclic organic compound added to the phosphoric acid ester-based solution plays the function as an antioxidant for plating.
  • the group of the cyclic organic compounds used in the present invention are represented by the general formula [3] and [4].
  • Examples of the preferable compounds among the cyclic organic compounds represented by the general formulas [3] and [4] include: mercaptobenzothiazole, Na salt of mercaptobenzothiazole, K salt of mercaptobenzothiazole, benzotriazole, 1-methyltriazole, tolyltriazole and triazine-based compounds.
  • R1 represents a hydrogen atom, an alkyl group or a substituted alkyl group
  • R2 represents an alkali metal, a hydrogen atom, an alkyl group or a substituted alkyl group
  • R3 represents an alkali metal or a hydrogen atom
  • R4 represents -SH, an alkyl group-substituted or aryl group-substituted amino group, or represents an alkyl-substituted imidazolylalkyl group
  • R5 and R6 each represent -NH 2 , -SH or-SM (M represents an alkali metal).
  • the post-treatment is furthermore preferably performed in such a way that both P and N are present on the surface of the upper layer 14.
  • P is absent on the plating surface
  • the solderability tends to be degraded, and the lubricity of the plating material is also degraded.
  • N is absent on the Sn or Sn alloy plating surface, sometimes the contact resistance of the plating material tends to be increased in a high temperature environment.
  • the maximum height (Rz) of the surface of the upper layer 14 is preferably 3 ⁇ m or less.
  • the maximum height (Rz) of the surface of the upper layer 14 being 3 ⁇ m or less reduces the raised portions relatively tending to be corroded, thus smoothes the surface and improves the gas corrosion resistance.
  • Examples of the application of the metallic material for electronic components of the present invention include, without being particularly limited to: a connector terminal using, in the contact portion thereof, the metallic material for electronic components, an FFC terminal or an FPC terminal using, in the contact portion thereof, the metallic material for electronic components, and an electronic component using, in the electrode thereof for external connection, the metallic material for electronic components.
  • the terminal does not depend on the connection mode on the wiring side as exemplified by a crimp-type terminal, a soldering terminal and a press-fit terminal.
  • Examples of the electrode for external connection include a connection component prepared by applying a surface treatment to a tab, and material surface treated for use in under bump metal of a semiconductor.
  • Connectors may also be prepared by using such connector terminals formed as described above, and an FFC or an FPC may also be prepared by using an FFC terminal or an FPC terminal.
  • the metallic material for electronic components of the present invention may also be used in a push-in type terminal for fixing a board connection portion to a board by pushing the board connection portion into the through hole formed in the board, wherein a female terminal connection portion and the board connection portion are provided respectively on one side and the other side of a mounting portion to be attached to a housing.
  • both of the male terminal and the female terminal may be made of the metallic material for electronic components of the present invention, or only one of the male terminal and the female terminal may be made of the metallic material for electronic components of the present invention.
  • the use of the metallic material for electronic components of the present invention for both of the male terminal and the female terminal further improves the low degree of insertion/extraction force.
  • the heat treatment was performed by placing the sample on a hot plate, and verifying that the surface of the hot plate reached the predetermined temperature.
  • the sample after the heat treatment was immersed in dilute sulfuric acid (10 g/1 L) for 5 seconds. Thereafter, it was immersed in pure water for 5 seconds.
  • anodic electrolysis electrolytic potential and constant voltage electrolysis described in Table 2
  • a surface treatment was performed on the plating surface.
  • an ultrasonic stirring was performed at the time of initial make-up of electrolytic bath, and then the electrolysis was performed.
  • the ultrasonic stirring conditions for the treatment solution were stirring by an ultrasonic disperser (ultrasonic frequency: 20 kHz, ultrasonic output: 500 W, 10 minutes). After these treatments, the sample was immersed for 2 seconds and then dried with warm air.
  • the measurement of the thicknesses of the upper layer and the intermediate layer, and the determination of compositions and structures of the upper layer, of each of the obtained samples, were performed by the line analysis based on the STEM (scanning transmission electron microscope) analysis.
  • the analyzed elements are the elements in the compositions of the upper layer, the intermediate layer and the lower layer, and C, S and O. These elements are defined as the specified elements.
  • the concentrations (at%) of the respective elements were analyzed.
  • the thickness corresponds to the distance determined from the line analysis (or area analysis).
  • the STEM apparatus the JEM-2100F manufactured by JEOL Ltd. was used.
  • the acceleration voltage of this apparatus is 200 kV.
  • the determination of the structure of the upper layer is performed by checking the composition determined by STEM against the phase diagram.
  • the thickness of the lower layer was measured with a fluorescent X-ray film thickness meter (Seiko Instruments, SEA5100, collimator 0.1 mm ⁇ ).
  • the measurement of the thickness of the upper layer, the intermediate layer and the lower layer and the determination of the composition and the structure of the upper layer were performed by averaging 10 arbitrary points.
  • the concentration of C (carbon) of the treated layer was measured by the following method.
  • the area ratio of oxide particles adhering to the surface of the treated layer after heating at 250 °C for 30 seconds was measured by the following method.
  • the sample was placed on a hot plate and heated for 30 seconds after the surface of the hot plate reached 250 °C.
  • Adhesive wear property was evaluated by performing insertion / extraction test with a plated male terminal using a commercially available Sn reflow plating female terminal (090 type Sumitomo TS / Yazaki 090II series female terminal non-waterproof / F090-SMTS).
  • the measuring device used for the test was 1311NR made by Aikoh Engineering, and the evaluation was performed with a male spin sliding distance of 5 mm. The number of samples was 5, and adhesive wear was evaluated using the insertion force. As the insertion force, a value obtained by averaging the maximum values of the respective samples was adopted. As a blank material for adhesive wear, the sample of Comparative Example 1 was adopted, and the adhesive wear property with respect to the sample of Comparative Example 1 was evaluated.
  • Tables 1 and 2 show the test conditions and the test results.
  • Examples 1 to 7 were metallic materials for electronic components having excellently low adhesive wear.

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EP17896426.8A 2017-02-15 2017-10-26 Metallstoff für elektronische komponente, verfahren zur herstellung des besagten metallstoffs und anschlussklemme, steckverbinder und elektronische komponente, in der der besagte metallstoff verwendet wird Withdrawn EP3584353A4 (de)

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