EP2609232B1 - Bain électrolytique pour placage et procédé dudit placage - Google Patents

Bain électrolytique pour placage et procédé dudit placage Download PDF

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Publication number
EP2609232B1
EP2609232B1 EP11754998.0A EP11754998A EP2609232B1 EP 2609232 B1 EP2609232 B1 EP 2609232B1 EP 11754998 A EP11754998 A EP 11754998A EP 2609232 B1 EP2609232 B1 EP 2609232B1
Authority
EP
European Patent Office
Prior art keywords
nickel
electrolytic bath
concentration
bath
acid
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.)
Not-in-force
Application number
EP11754998.0A
Other languages
German (de)
English (en)
Other versions
EP2609232A1 (fr
Inventor
Matthias Kurrle
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.)
IPT - International Plating Technologies GmbH
Original Assignee
IPT - International Plating Technologies GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by IPT - International Plating Technologies GmbH filed Critical IPT - International Plating Technologies GmbH
Publication of EP2609232A1 publication Critical patent/EP2609232A1/fr
Application granted granted Critical
Publication of EP2609232B1 publication Critical patent/EP2609232B1/fr
Not-in-force 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
    • 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
    • C25D3/56—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

Definitions

  • the invention relates to an electrolytic bath for the electrodeposition and a process for its production, in particular for a galvanic deposition of a nickel-phosphorus layer.
  • NiP nickel-phosphorus
  • An electrolytic bath preferably allows a high quality coating at a high current density and deposition rate, and it is as cost effective as possible.
  • the WO 99/02765 A1 shows an electrolytic bath for NiP coating.
  • the bath contains nickel carbonate, phosphoric acid, hypophosphorous acid (H 3 PO 2 ) or phosphorous acid (H 3 PO 3 ), and methanesulfonic acid.
  • an electrolytic bath according to claim 1 a method according to claim 10 and a use according to claim 12.
  • Such an electrolytic bath is stable, allows a high current density, a high deposition rate, the generation of a good nickel-phosphorus Layer, and it is inexpensive.
  • saccharin is added in the process.
  • a typical electroplating plant has a bath in which there is a bath (electrolyte, galvanic bath).
  • the substrate to be coated eg cylinder liner of an engine block
  • the substrate to be coated is surrounded in the electrolyte and by a dimensionally stable, insoluble anode or a soluble anode.
  • a DC power source is connected to the anode with the plus terminal and the substrate (cathode) with the minus terminal, and the current is used to electrodeposit the layer on the substrate.
  • a circulation pump ensures a uniform distribution of the bath, and there may be a rotation of the substrate in the electrolyte. This is only an illustrative example, and other electroplating equipment may be used.
  • the composition of the bath determines what current densities and thus deposition rates are possible in the coating, and baths are available on the market for many applications.
  • NiP bath It is proposed a bath that is well suited for the galvanic coating with a layer of nickel and phosphorus and possibly other constituents, which is why the bath is referred to below as NiP bath.
  • a nickel-phosphor coating has a higher hardness compared to a pure nickel coating and thus opens up additional fields of application.
  • the nickel content in the nickel-phosphorus layer also affects the anti-wear properties and the corrosion properties of the alloy.
  • the phosphorus content in the layer determines the hardness, and a common mass fraction is e.g. 6-8% by weight of phosphorus, but depending on the requirements, higher mass fractions of e.g. 12 wt .-% may be required.
  • the nickel or more precisely the nickel ions are present in the solution predominantly as nickel (II) or Ni 2+ , but other oxidation states may also occur.
  • NiP bath may also contain saccharin and / or other additives.
  • H 3 PO 2 phosphinic acid
  • the combination of the constituents phosphoric acid, phosphonic acid and boric acid has proved to be advantageous, since the finished bath with this combination has proved to be relatively stable, in particular with regard to the pH.
  • the combination also allows a high current density and thus a high deposition rate.
  • the ingredients are relatively cheap.
  • the pH of the final bath preparation is preferably in the range of 1.6 to 2.3, more preferably in the range of 1.8 to 2.2.
  • a bath according to the above boric acid concentration range contains boron (partly as a constituent of borate and partly as a constituent of boric acid) at a concentration in the range of 5.2 to 7.0 g / l.
  • NiP bath it is possible to coat different substrates.
  • substrates e.g. Copper, steel or stainless steel to be coated.
  • degreasing, activation and pickling of the substrate preferably takes place, as is known to the person skilled in the art.
  • NiP layer could be produced by electrodeposition.
  • the deposited NiP layer was nonporous, homogeneous, charcoal gray shiny and amorphous, whereby a recrystallization by annealing is possible.
  • the substrate used was a copper stud which had been pretreated (degreasing, activation and pickling).
  • the temperature was about 65 ° C, and the current density was up to 30 A / dm 2 .
  • the deposition rate is Depending on the current density, typical deposition rates of 0.5 ⁇ m / min to more than 2 ⁇ m / min were achieved, these values representing no technical limits.
  • Successful tests were carried out with layer thicknesses of up to 100 ⁇ m.
  • the NiP bath was composed as follows: attempt Nickel (II) phosphoric acid phosphonic boric acid saccharin I 100 g / l 75 g / l 30 g / l 35 g / l 2.6 g / l II 100 g / l 75 g / l 30 g / l 35 g / l 0g / l III 100 g / l 75 g / l 40 g / l 30 g / l 2.6 g / l IV 100 g / l 60 g / l 30 g / l 30 g / l 2.6 g / l V 100 g / l 45 g / l 10 g / l 30 g / l 2.6 g / l
  • the concentration of phosphoric acid or phosphonic acid can also be specified by the concentration of the phosphate (PO 4 3- ) or phosphite (PO 3 3- ).
  • concentration of the phosphate (PO 4 3- ) or phosphite (PO 3 3- ) For example, 75 g / l phosphoric acid corresponds to 73 g / l phosphate and 30 g / l phosphonic acid corresponds to 29 g / l phosphite.
  • saccharin is at NiP layer thicknesses of e.g. 5 - 10 microns not required, but has proved particularly at layer thicknesses of more than 40 microns as advantageous.
  • the electrodeposition works e.g. good at a temperature of about 65 ° C. There are also higher temperatures of e.g. 80-90 ° C possible, wherein when using organic additives such. Saccharin whose temperature sensitivity is to be considered.
  • a layer of NiP is a binary alloy with the components Ni and P.
  • other components to be deposited can also be added to the NiP bath.
  • a ternary (Ni-XP, eg Ni-Co-P) or quaternary alloy or it is also possible to deposit a dispersion layer in which additional particles are embedded in the NiP layer, eg silicon carbide (SiC ), Boron nitride (BN), boron carbide (B 4 C), titanium nitride (TiN), silicon nitride (Si 3 N 4 ), titanium carbide (TiC), tungsten carbide (WC) and / or alumina (Al 2 O 3 ).
  • a prerequisite for commercial electrodeposition is the ability to analyze the bath composition. While the nickel (II) concentration is measurable by titration, and the concentration of phosphoric acid and the phosphonic acid by measuring the concentration of the phosphate (PO 4 3- ) or phosphite (PO 3 3- ) is possible by means of ion chromatography, the Determination of the concentration of boric acid in the specified NiP bath more difficult or expensive.
  • nickel carbonate (NiCO 3 ) is added until the pH is increased to about 1.8.
  • This can be done, for example, by continuously measuring the pH during the addition of the nickel carbonate and stopping the addition as soon as the desired pH is reached.
  • additional nickel is supplied (about 5 g / l Ni 2+ )
  • the current efficiency is significantly increased by the increased pH.
  • Increasing the pH by adding nickel carbonate works well up to a pH of about 2.2. At a higher pH, saturation may occur in the bath.
  • the carbon dioxide (CO 2 ) escapes as gas.
  • the increase in the pH can e.g. also by adding alkalis (e.g., sodium hydroxide (NaOH)).
  • alkalis e.g., sodium hydroxide (NaOH)
  • NiOH sodium hydroxide
  • the use of nickel carbonate to increase the pH has the advantage that no cations of additional elements enter the bath, but the concentration of the nickel (II), which may have been lowered by the electrodeposition, is increased again.
  • the electrolytic bath is filled with demineralised water (deionized water) to the desired volume.
  • the preparation of the NiP bath works e.g. good at a temperature of about 40-65 ° C, which are not absolute limits.
  • nickel salts or combinations of nickel salts are possible (eg nickel sulfate and nickel chloride (NiCl 2 )), preferably at least 50% of the nickel (II) comes from the nickel sulfate in the preparation of the bath, more preferably at least 70%.
  • NiCl 2 nickel chloride

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Claims (12)

  1. Bain électrolytique pour l'électrodéposition, lequel contient en solution :
    a) un sel de nickel,
    b) de l'acide phosphorique,
    c) de l'acide phosphonique,
    d) de l'acide borique.
  2. Bain électrolytique selon la revendication 1,
    lequel contient en solution de l'acide phosphorique dans une concentration comprise entre 60 et 90 g/l.
  3. Bain électrolytique selon la revendication 1 ou 2,
    lequel contient en solution de l'acide phosphonique dans une concentration comprise entre 20 et 40 g/l.
  4. Bain électrolytique selon une des revendications précédentes,
    lequel contient en solution de l'acide borique dans une concentration comprise entre 30 et 40 g/l.
  5. Bain électrolytique selon une des revendications précédentes,
    lequel contient en solution du nickel(II) dans une concentration comprise entre 90 et 13 0 g/l.
  6. Bain électrolytique selon une des revendications précédentes,
    lequel contient en solution de 0 à 4 g/l de saccharine.
  7. Bain électrolytique selon une des revendications précédentes,
    lequel a un pH compris entre 1,6 et 2,3.
  8. Bain électrolytique selon une des revendications précédentes,
    dans lequel le sel de nickel comprend du sulfate de nickel, et dans lequel le nickel(II) dans le bain vient à plus de 50 % du sulfate de nickel.
  9. Bain électrolytique selon une des revendications précédentes,
    lequel contient en solution du sulfate dans une concentration comprise entre 147 et 213 g/l.
  10. Procédé de fabrication d'un bain électrolytique, lequel procédé présente les étapes suivantes :
    A) un sel de nickel, de l'acide phosphorique, de l'acide phosphonique et de l'acide borique sont mélangés ;
    B) du carbonate de nickel est ajouté pour élever le pH.
  11. Procédé selon la revendication 10,
    dans lequel le pH du bain est mesuré, et dans lequel du carbonate de nickel est ajouté pour élever le pH jusqu'à ce qu'un pH prédéfini soit atteint, le pH prédéfini étant de préférence compris entre 1,6 et 2,3.
  12. Utilisation d'un bain électrolytique selon une des revendications 1 à 9 pour l'électrodéposition d'une couche contenant du nickel sur une pièce.
EP11754998.0A 2010-08-27 2011-08-24 Bain électrolytique pour placage et procédé dudit placage Not-in-force EP2609232B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010035661A DE102010035661A1 (de) 2010-08-27 2010-08-27 Elektrolytisches Bad für die galvanische Abscheidung und Verfahren zu dessen Herstellung
PCT/EP2011/004244 WO2012025226A1 (fr) 2010-08-27 2011-08-24 Bain électrolytique pour le dépôt galvanique et son procédé de fabrication

Publications (2)

Publication Number Publication Date
EP2609232A1 EP2609232A1 (fr) 2013-07-03
EP2609232B1 true EP2609232B1 (fr) 2013-12-04

Family

ID=44645049

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11754998.0A Not-in-force EP2609232B1 (fr) 2010-08-27 2011-08-24 Bain électrolytique pour placage et procédé dudit placage

Country Status (5)

Country Link
US (1) US9340888B2 (fr)
EP (1) EP2609232B1 (fr)
DE (1) DE102010035661A1 (fr)
ES (1) ES2450052T3 (fr)
WO (1) WO2012025226A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015209887A1 (de) * 2015-05-29 2016-12-01 Mahle International Gmbh Kolben für einen Zylinder einer Brennkraftmaschine

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180363159A1 (en) * 2015-12-18 2018-12-20 Rolex Sa Method for producing a timepiece component
IT201700079843A1 (it) * 2017-07-14 2019-01-14 Metalcoating S R L Processo elettrolitico per il rivestimento di superfici metalliche allo scopo di conferire alta resistenza alla corrosione e all'abrasione.

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2643221A (en) * 1950-11-30 1953-06-23 Us Army Electrodeposition of phosphorusnickel and phosphorus-cobalt alloys
US3355267A (en) * 1964-02-12 1967-11-28 Kewanee Oil Co Corrosion resistant coated articles and processes of production thereof
US4673468A (en) * 1985-05-09 1987-06-16 Burlington Industries, Inc. Commercial nickel phosphorus electroplating
US4767509A (en) * 1983-02-04 1988-08-30 Burlington Industries, Inc. Nickel-phosphorus electroplating and bath therefor
US6099624A (en) * 1997-07-09 2000-08-08 Elf Atochem North America, Inc. Nickel-phosphorus alloy coatings
WO2002063070A1 (fr) * 2001-02-08 2002-08-15 The University Of Alabama In Huntsville Electrodeposition d'alliages phosphoreux de nickel et de cobalt a faible contrainte
JP4217778B2 (ja) * 2003-04-11 2009-02-04 古河電気工業株式会社 抵抗層付き導電性基材、抵抗層付き回路基板及び抵抗回路配線板
KR100546212B1 (ko) * 2003-09-18 2006-01-24 한국원자력연구소 Ｎｉ-Ｐ-Ｂ 합금 전해도금방법 및 그 도금액

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015209887A1 (de) * 2015-05-29 2016-12-01 Mahle International Gmbh Kolben für einen Zylinder einer Brennkraftmaschine

Also Published As

Publication number Publication date
US9340888B2 (en) 2016-05-17
EP2609232A1 (fr) 2013-07-03
WO2012025226A1 (fr) 2012-03-01
US20130168259A1 (en) 2013-07-04
DE102010035661A1 (de) 2012-03-01
ES2450052T3 (es) 2014-03-21

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