EP3868924A1 - Procédé de suppression d'augmentation de la concentration en zinc dans une solution de placage, et procédé de production d'élément de placage à base de zinc - Google Patents

Procédé de suppression d'augmentation de la concentration en zinc dans une solution de placage, et procédé de production d'élément de placage à base de zinc Download PDF

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Publication number
EP3868924A1
EP3868924A1 EP20886179.9A EP20886179A EP3868924A1 EP 3868924 A1 EP3868924 A1 EP 3868924A1 EP 20886179 A EP20886179 A EP 20886179A EP 3868924 A1 EP3868924 A1 EP 3868924A1
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EP
European Patent Office
Prior art keywords
plating
diaphragm
zinc
tank
contact
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.)
Withdrawn
Application number
EP20886179.9A
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German (de)
English (en)
Other versions
EP3868924A4 (fr
Inventor
Toshihiro Sugiura
Yasunori Aoki
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.)
Yuken Industry Co Ltd
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Yuken Industry Co Ltd
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Filing date
Publication date
Application filed by Yuken Industry Co Ltd filed Critical Yuken Industry Co Ltd
Publication of EP3868924A1 publication Critical patent/EP3868924A1/fr
Publication of EP3868924A4 publication Critical patent/EP3868924A4/fr
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C25D21/14—Controlled addition of electrolyte components
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/002—Cell separation, e.g. membranes, diaphragms
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/06—Filtering particles other than ions
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/10—Agitating of electrolytes; Moving of racks
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/18—Regeneration of process solutions of electrolytes
    • 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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/06—Suspending or supporting devices for articles to be coated

Definitions

  • the present invention relates to a method for suppressing an increase in the zinc concentration of a plating solution, and a method for manufacturing a zinc-based plating member.
  • Patent literature 1 describes a zinc alloy electroplating method including energization in an alkali-zinc alloy electroplating bath equipped with a cathode and an anode, wherein a cathode region including the cathode and an anode region including the anode are separated from each other by a separator containing an electrolytic solution gel that can be energized.
  • Patent literature 2 describes a plating bath characterized in that an anode (2) is isolated from an alkaline electrolytic solution (plating bath) by an ion exchange membrane (6) in an alkaline plating bath (1) for zinc-nickel film electrodeposition which has the anode (2) and a cathode (3).
  • the present invention provides a method for suppressing an increase in the zinc concentration of a plating solution when an anode is soluble, and a method for manufacturing a zinc-based plating member.
  • the present invention includes the following aspects.
  • a method for suppressing an increase in the zinc concentration of a plating solution when an anode is soluble and a method for manufacturing a zinc-based plating member are provided.
  • FIG. 1 is an illustrative diagram of a zinc-based plating apparatus according to a first embodiment of the present invention.
  • a zinc-based plating apparatus 100 according to the first embodiment is used for manufacturing a zinc-based plating member.
  • Zinc-based plating is a general term for zinc plating and zinc alloy plating.
  • a specific example of the zinc alloy plating may be zinc-nickel plating.
  • the zinc-based plating apparatus 100 includes a plating tank 10, a first diaphragm tank 20, a cathode holding member 30, and a first anode holding member 40.
  • the plating tank 10 is capable of accommodating a plating solution PE, and in FIG. 1 , the plating solution PE is inside the plating tank 10.
  • a specific example of the material constituting the plating tank 10 may be polypropylene.
  • the plating tank 10 may be equipped with a stirring apparatus for stirring the plating solution PE, or may be equipped with a filter for removing insoluble substances generated in the plating solution PE.
  • the plating tank 10 may be equipped with a circulation pump for stirring the plating solution PE and removing the insoluble substances.
  • the composition of the plating solution PE is appropriately set according to the type of the zinc-based plating.
  • the plating solution PE is acidic. That is, in the embodiment, the plating solution PE is an acidic zinc-based plating solution.
  • the zinc-based plating solution is an electrolytic solution containing ions including zinc elements and is a liquid capable of forming a zinc-containing plating film on a member to be plated 31 that has been cathode-electrolyzed.
  • the zinc-based plating solution may contain insoluble components and may be in the form of a dispersion.
  • the first diaphragm tank 20 is capable of accommodating a first electrolytic solution E1, and in FIG. 1 , the first electrolytic solution E1 is inside the first diaphragm tank 20.
  • the first diaphragm tank 20 has a first diaphragm 21 including a first ion exchange membrane.
  • the first ion exchange membrane may include a cation exchange membrane or an anion exchange membrane. As described later, the first ion exchange membrane may preferably include a cation exchange membrane.
  • the first diaphragm tank 20 is located inside the plating tank 10, and the first diaphragm tank 20 is arranged in a manner that the first electrolytic solution E1 is in contact with one surface of the first diaphragm 21 (on the inner side of the first diaphragm tank 20) and the plating solution PE is in contact with the other surface of the first diaphragm 21 (on the outer side of the first diaphragm tank 20).
  • a specific example of the material constituting the first diaphragm tank 20 may be polypropylene.
  • the first diaphragm tank 20 may be equipped with a stirring apparatus for stirring the first electrolytic solution E1 inside the first diaphragm tank 20, or may be equipped with a filter for removing insoluble substances generated in the first electrolytic solution E1.
  • the first diaphragm tank 20 may be equipped with a circulation pump for stirring the first electrolytic solution E1 and removing the insoluble substances.
  • the first diaphragm tank 20 is arranged inside the plating tank 10, but a part of the inside of the plating tank 10 may be partitioned and the first diaphragm 21 may be arranged in the partition.
  • the inner side of the partitioned part becomes the first diaphragm tank 20
  • the first electrolytic solution E1 may be located inside the first diaphragm tank 20
  • the plating solution PE may be located on the outer side of the partitioned part inside the plating tank 10.
  • the cathode holding member 30 is used for cathode-electrolyzing the member to be plated 31 that is in contact with the plating solution PE inside the plating tank 10 during use. That is, the cathode holding member 30 has a function of holding the member to be plated 31 and a function of passing a cathode electrolytic current through the member to be plated 31.
  • a shape of the cathode holding member 30 is appropriately set according to a shape of the member to be plated 31 to be held. In FIG. 1 , the cathode holding member 30 has the shape of a clip that clamps the member to be plated 31 having a plate shape.
  • the cathode holding member 30 is connected to a cathode terminal 62 of a power supply apparatus 60 via wiring in order that the member to be plated 31 can be cathode-electrolyzed.
  • cathodic electrolysis means that electrolysis is performed at a negative potential relative to the potential of anodic electrolysis, and in relation to the ground potential, the potential of cathodic electrolysis may be a positive potential or a negative potential.
  • anodic electrolysis means that electrolysis is performed at a positive potential relative to the potential of cathodic electrolysis, and in relation to the ground potential, the potential of anodic electrolysis may be a positive potential or a negative potential.
  • the first anode holding member 40 is used for anode-electrolyzing a soluble zinc-containing member 41 that is in contact with the first electrolytic solution E1 inside the first diaphragm tank during use. That is, the first anode holding member 40 has a function of holding the soluble zinc-containing member 41 and a function of passing an anode electrolytic current through the soluble zinc-containing member 41.
  • a shape of the first anode holding member 40 is appropriately set according to a shape of the soluble zinc-containing member 41 to be held. In FIG. 1 , the first anode holding member 40 has the shape of a cage that holds the soluble zinc-containing member 41 composed of a plurality of zinc ingots (lumps).
  • the first anode holding member 40 is connected to an anode terminal 61 of the power supply apparatus 60 via wiring in order that the soluble zinc-containing member 41 can be anode-electrolyzed.
  • the first electrolytic solution E1 is an electrolytic solution containing ions including zinc elements, and when the soluble zinc-containing member 41 is anode-electrolyzed, the zinc contained in the soluble zinc-containing member 41 can be dissolved as an ion. Moreover, the first electrolytic solution E1 may contain insoluble components and may be in the form of a dispersion.
  • the zinc-based plating apparatus 100 further includes a second anode holding member 50 for anode-electrolyzing a soluble metal-containing member 51 that is electrically connected to the plating solution PE during use. That is, the second anode holding member 50 has a function of holding the soluble metal-containing member 51 and a function of passing an anode electrolytic current through the soluble metal-containing member 51.
  • a shape of the second anode holding member 50 is appropriately set according to a shape of the soluble metal-containing member 51 to be held.
  • the first anode holding member 40 has the shape of a cage that holds the soluble metal-containing member 51 composed of a plurality of nickel ingots (lumps).
  • the second anode holding member 50 is connected to the anode terminal 61 of the power supply apparatus 60 via wiring in order that the soluble metal-containing member 51 can be anode-electrolyzed.
  • the soluble metal-containing member 51 is held by the second anode holding member 50 and located inside the plating tank 10, and is electrically connected to the plating solution PE in a manner of being in direct contact with the plating solution PE.
  • the soluble metal-containing member 51 can be a source of alloy elements in the zinc alloy plating. As described above, when the soluble metal-containing member 51 is composed of the plurality of nickel ingots (lumps), the zinc alloy plating can be zinc-nickel plating.
  • the soluble metal-containing member 51 may contain a metal nobler than zinc as a soluble metal, such as the nickel described above.
  • first anode holding member 40 and the second anode holding member 50 are connected to the same anode terminal 61, but the present invention is not limited hereto.
  • the anodic electrolysis potential of the first anode holding member 40 and the anodic electrolysis potential of the second anode holding member 50 may be different from each other.
  • FIG. 2 is an illustrative diagram of a zinc-based plating apparatus according to a second embodiment of the present invention.
  • a zinc-based plating apparatus 101 according to the second embodiment has the same basic configuration as the zinc-based plating apparatus 100 according to the first embodiment.
  • the difference of the zinc-based plating apparatus 101 according to the second embodiment when compared with the zinc-based plating apparatus 100 according to the first embodiment is that the second anode holding member 50 is located inside a second diaphragm tank 70 which accommodates a second electrolytic solution E2.
  • the zinc-based plating apparatus 101 includes the second diaphragm tank 70 having a second diaphragm 71 including a second ion exchange membrane.
  • the second diaphragm tank 70 is arranged in a manner that the second electrolytic solution E2 is in contact with one surface of the second diaphragm 71 (on the inner side of the second diaphragm tank 70) and the plating solution PE is in contact with the other surface of the second diaphragm 71 (on the outer side of the second diaphragm tank 70).
  • the second electrolytic solution E2 is in contact with the soluble metal-containing member 51 held by the second anode holding member 50 inside the second diaphragm tank 70.
  • a specific example of the material constituting the second diaphragm tank 70 may be polypropylene.
  • the second diaphragm tank 70 may be equipped with a stirring apparatus for stirring the second electrolytic solution E2 inside the second diaphragm tank 70, or may be equipped with a filter for removing insoluble substances generated in the second electrolytic solution E2.
  • the second diaphragm tank 70 may be equipped with a circulation pump for stirring the second electrolytic solution E2 and removing the insoluble substances.
  • the second diaphragm tank 70 is arranged inside the plating tank 10, but a part of the inside of the plating tank 10 may be partitioned and the second diaphragm 71 may be arranged in the partition.
  • the inner side of the partitioned part becomes the second diaphragm tank 70
  • the second electrolytic solution E2 may be located inside the second diaphragm tank 70
  • the plating solution PE may be located on the outer side of the partitioned part inside the plating tank 10.
  • the second electrolytic solution E2 is an electrolytic solution, and when the soluble metal-containing member 51 is anode-electrolyzed, the metal contained in the soluble metal-containing member 51 can be dissolved as an ion. Moreover, the second electrolytic solution E2 may contain insoluble components and may be in the form of a dispersion.
  • the second ion exchange membrane may include a cation exchange membrane or an anion exchange membrane.
  • the second ion exchange membrane may have the same configuration as the first ion exchange membrane, or may have a different configuration.
  • the first diaphragm tank 20 may have a plurality of first diaphragms 21 having different configurations
  • the second diaphragm tank 70 may have a plurality of second diaphragms 71 having different configurations.
  • Acidic zinc-nickel plating solution having the composition shown in Table 1 was prepared.
  • Acidic zinc-nickel plating solution Metas ANK-10 manufactured by Yuken Kogyo Co., Ltd. Zinc chloride 73 g/L (Zn: 35 g/L) Nickel chloride 81g/L (Ni: 20 g/L) Potassium chloride 206 g/L Metas ANK-10K 125 ml/L Metas ANK-10D 12 ml/L Metas ANK-10M 30 ml/L Metas ANK-10G 2 ml/L Bath temperature 40°C pH 5.4
  • the above acidic zinc-nickel plating solution was put into the plating tank 10 as the plating solution PE, and any one of the following electrolytic solutions was put into the first diaphragm tank 20 as the first electrolytic solution E1 (internal solution).
  • electrolytic solution A zinc chloride concentration 50 g/L
  • electrolytic solution B zinc chloride concentration 500 g/L
  • electrolytic solution C zinc chloride concentration 0 g/L
  • any one of the ion exchange membranes shown in Table 2 was used as the first diaphragm 21 of the first diaphragm tank 20.
  • Table 2 Type of ion exchange membrane Product name Maker Type Selemion CMVN AGC Engineering Co., Ltd. Cation Neosepta CMB Astom Co., Ltd. Cation Neosepta AHA Astom Co., Ltd. Anion
  • Plating was performed under the conditions shown in Table 3. Moreover, the unit of energization time in Table 3 is hour. [Table 3] No. Ion exchange membrane Membrane type Energization time (hr) Internal solution Plating solution Zn before energization (g/L) Zn after energization (g/L) Zn before energization (g/L) Zn after energization (g/L) 1 None --- 25 --- --- 35.0 40.2 ⁇ 2 Neocepta AHA Anion 25 0 43.1 ⁇ 35.0 20.5 ⁇ 3 Neosepta CMB Cation 25 25.0 39.5 ⁇ 35.0 30.1 ⁇ 4 Neosepta CMB Cation 25 250.0 257.0 ⁇ 35.0 32.5 ⁇ 5 Selemion CMVN Cation 25 25.0 28.5 ⁇ 35.0 34.0 ⁇ 6 Selemion CMVN Cation 25 250.0 251.3 ⁇ 35.0 34.5 ⁇
  • the nickel concentration when the second diaphragm 71 is an anion membrane (anion exchange membrane) (Experiment No.7) was 16.7 g/L
  • the nickel concentration when the second diaphragm 71 is a cation membrane (cation exchange membrane) (Experiment No.8) was 18.5 g/L.
  • an increase in the nickel concentration could be suppressed compared with the case where the second diaphragm tank 70 was not used.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
EP20886179.9A 2019-11-28 2020-08-21 Procédé de suppression d'augmentation de la concentration en zinc dans une solution de placage, et procédé de production d'élément de placage à base de zinc Withdrawn EP3868924A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2019214897A JP6750186B1 (ja) 2019-11-28 2019-11-28 めっき液の亜鉛濃度の上昇を抑制する方法および亜鉛系めっき部材の製造方法
PCT/JP2020/031629 WO2021106291A1 (fr) 2019-11-28 2020-08-21 Procédé de suppression d'augmentation de la concentration en zinc dans une solution de placage, et procédé de production d'élément de placage à base de zinc

Publications (2)

Publication Number Publication Date
EP3868924A1 true EP3868924A1 (fr) 2021-08-25
EP3868924A4 EP3868924A4 (fr) 2022-03-09

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EP20886179.9A Withdrawn EP3868924A4 (fr) 2019-11-28 2020-08-21 Procédé de suppression d'augmentation de la concentration en zinc dans une solution de placage, et procédé de production d'élément de placage à base de zinc

Country Status (6)

Country Link
US (1) US20220298668A1 (fr)
EP (1) EP3868924A4 (fr)
JP (1) JP6750186B1 (fr)
CN (1) CN113195798A (fr)
MX (1) MX2021007195A (fr)
WO (1) WO2021106291A1 (fr)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2084191A (en) * 1980-09-23 1982-04-07 Vandervell Products Ltd Electro-deposition of alloys
DE19834353C2 (de) 1998-07-30 2000-08-17 Hillebrand Walter Gmbh & Co Kg Alkalisches Zink-Nickelbad
US8377283B2 (en) * 2002-11-25 2013-02-19 Coventya, Inc. Zinc and zinc-alloy electroplating
US7135103B2 (en) * 2003-10-20 2006-11-14 Waseda University Preparation of soft magnetic thin film
JP4822268B2 (ja) * 2005-04-19 2011-11-24 ユケン工業株式会社 回収型電気亜鉛めっき方法および装置
JP4738910B2 (ja) * 2005-06-21 2011-08-03 日本表面化学株式会社 亜鉛−ニッケル合金めっき方法
EP1870495A1 (fr) * 2006-06-21 2007-12-26 Atotech Deutschland Gmbh Bain aqueux alcalin, exempt de cyanide, pour la déposition galvanique de couches de Zinc et alliages de Zinc
DE102008056776A1 (de) * 2008-11-11 2010-05-12 Enthone Inc., West Haven Galvanisches Bad und Verfahren zur Abscheidung von zinkhaltigen Schichten
CN105189831A (zh) * 2013-03-21 2015-12-23 安美特德国有限公司 用于在工件上电解沉积金属层的装置和方法

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Publication number Publication date
CN113195798A (zh) 2021-07-30
JP2021085068A (ja) 2021-06-03
WO2021106291A1 (fr) 2021-06-03
JP6750186B1 (ja) 2020-09-02
US20220298668A1 (en) 2022-09-22
EP3868924A4 (fr) 2022-03-09
MX2021007195A (es) 2022-03-18

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