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WO2019215287A1 - Réseau de couches comprenant du nickel et son procédé de fabrication - Google Patents

Réseau de couches comprenant du nickel et son procédé de fabrication Download PDF

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Publication number
WO2019215287A1
WO2019215287A1 PCT/EP2019/061938 EP2019061938W WO2019215287A1 WO 2019215287 A1 WO2019215287 A1 WO 2019215287A1 EP 2019061938 W EP2019061938 W EP 2019061938W WO 2019215287 A1 WO2019215287 A1 WO 2019215287A1
Authority
WO
WIPO (PCT)
Prior art keywords
nickel
layer
chromium
array
porous
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.)
Ceased
Application number
PCT/EP2019/061938
Other languages
English (en)
Inventor
Berkem Özkaya
Philipp Wachter
Torsten Voss
Philip Hartmann
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.)
Atotech Deutschland GmbH and Co KG
Original Assignee
Atotech Deutschland GmbH and Co KG
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 Atotech Deutschland GmbH and Co KG filed Critical Atotech Deutschland GmbH and Co KG
Publication of WO2019215287A1 publication Critical patent/WO2019215287A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/623—Porosity of the layers
    • 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
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
    • 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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/06—Electroplating: Baths therefor from solutions of chromium from solutions of trivalent chromium
    • 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
    • C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/16—Acetylenic compounds
    • 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
    • C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/18—Heterocyclic compounds

Definitions

  • Nickel comprising layer array and a method for its manufacturing
  • the nickel comprising layer array comprises a semi-bright nickel layer.
  • the semi-bright nickel layer is located on the surface of the substrate. Preferably, it is located directly on the surface of the sub strate.
  • the surface of the substrate is preferably selected from those described hereinafter.
  • the semi-bright nickel layer is nobler than intermediate nickel layer selected from the bright nickel layer or a satin nickel layer; preferably, the electrical potential difference between the semi-bright nickel layer and the bright nickel layer or a satin nickel layer ranges from 80 to 250 mV.
  • This electrical potential difference allows for a further decrease of the nickel ion release.
  • the nickel comprising layer array comprises a non-porous nickel layer.
  • the non-porous nickel layer is located on the intermediate nickel layer.
  • the non-porous nickel layer is located direct ly on the intermediate nickel layer.
  • the non-porous nickel layer is free of particulate matter, especially free of non-conductive particulate matter. It is preferred that the particulate matter is free of particulate matter having a d50 (measured by X-ray diffraction) of 0.25 pm or greater.
  • the nickel comprising layer array comprises a chromium layer.
  • the chromium layer is located on the non-porous nickel layer.
  • the chromium layer is located directly on the non-porous nickel layer.
  • the chromium layer comprises 1000 pores per cm 2 or less, more preferably 100 per cm 2 or less and even more preferably 10 per cm 2 or less.
  • the chromium layer is (essentially) free of pores. Free of pores or having the mentioned small numbers of pores according to the invention mean that the pores where not intentionally generated within the chromium layer by using intentionally added particulate matter into the plating bath or special plating conditions during chromium plating or otherwise intentionally transferred into the chromium layer by e.g. underlying nickel layers, especially not by the underlying non-porous nickel layer.
  • chromium surfaces derived from chromium electroplating bath comprising chromium (VI) ions Dubpernell test method is preferred and for chromium surfaces derived from chromium electroplating bath comprising chromium (III) ions pore count test method is preferred.
  • the chromium layer is deposited from a chromium elec troplating bath.
  • the chromium layer is deposited from a hexava- lent chromium electroplating bath comprising chromium (VI) ions.
  • the chromium layer is deposited from a trivalent chromium electroplating bath comprising chromium (III) ions.
  • the nickel comprising layer array comprises a coating on the chromium layer derived from the trivalent chromium electroplating bath comprising chromium (III) ions.
  • the coating is located directly on the chromium layer.
  • the coating is selected from the group consisting of silica-based nanocoatings (sol-gel coatings) and UV-cured cathodic electrophoretic coatings, e.g. based on polyurethanes.
  • the thickness of the coating preferably ranges from 0.001 to 1.0 pm, more preferably from 0.005 to 0.5 pm, even more preferably from 0.01 to 0.4 pm.
  • the overall thickness of all nickel layers and the chromium layer ranges from 10.6 to 30 pm, preferably from 12.5 to 28 pm, more preferably from 15 to 25 pm. This allows for a very thin and cost-effective layer array to be obtained whose nickel ion release is very low and often meets the requirement of the new ECHA guideline in this regard.
  • the amount of nickel ion release is 0.88 pg/cm 2 /week or less, preferably 0.5 pg/cm 2 /week or less according to EN 1811 :201 1 +A1 :2015. Occasionally, it is reported that a nickel ion release of 0.88 pg/cm 2 /week would be sufficient to meet the requirements set out in the ECHA draft guideline, es pecially when error margins are considered.
  • the nickel comprising layer array is used as decorative coating on the surface of the substrate.
  • the nickel comprising layer array is used as decorative coating having a reduced nickel ion release, e.g. according to EN 1811 :2011 +A1 :2015.
  • the nickel ion release of the nickel comprising layer array is 0.5 pg/cm 2 /week or less according to EN 1811 :2011 +A1 :2015.
  • non-porous nickel layer wherein the non-porous nickel layer is free of particulate matter and wherein the non-porous nickel layer is nobler than the intermediate nickel layer; wherein the elec trical potential difference between the non-porous nickel layer and the intermediate nickel layer ranges from 10 to 150 mV, deposited from an electroplating bath for deposition of a non-porous nickel layer comprising nickel ions, boric acid, chloral hydrate and optionally, one or more of carri ers, brighteners and auxiliary brighteners;
  • the temperature of said electroplating bath for deposition of a non-porous nickel layer dur ing deposition ranges from 45 to 75 °C, preferably from 50 to 67.5 °C, more preferably from 52 to 62.5 °C;
  • the cathode density during deposition of the non-porous nickel layer preferably ranges from 1 to 8 A/dm 2 , more preferably from 1.5 to 7 A/dm 2 , even more preferably from 2 to 6 A/dm 2 ; and wherein the electroplating bath for deposition of a non-porous nickel layer is preferably free of particulate matter having a d 50 (measured by X-ray diffraction) of 0.25 pm or greater ; and
  • an intermediate nickel layer selected from bright nickel layers and satin nickel layers, preferably a satin nickel layer; and wherein the intermediate layer is preferably directly on the semi-bright nickel layer;
  • the cathode density during deposition of the non-porous nickel layer preferably ranges from 1 to 8 A/dm 2 , more preferably from 1 .5 to 7 A/dm 2 , even more preferably from 2 to 6 A/dm 2 ;
  • the semi-bright nickel electroplating bath comprises nickel ions, boric acid and one or more organic levelling agents.
  • Semi-bright nickel electroplating baths are typically free of sulfur- containing additives to avoid sulfur incorporation in the formed nickel layer.
  • Usual concentrations of nickel chloride in the semi-bright nickel electroplating bath range from 25 to 65 g/L, preferably from 30 to 60 g/L, more preferably from 35 to 54 g/L.
  • the bright nickel electroplating bath comprises nickel ions, boric acid and one or more of carriers, brighteners and auxiliary brighteners.
  • Auxiliary brighteners further increase the brightness and levelling when used with carriers and brighteners. They are preferably selected from the group consisting of allyl sulfonate; zinc ions; cobalt ions; cadmium ions; 1 ,4-butyne 2-diol; pyridinium propyl sulfonate; salts and mixtures of the aforementioned. Zinc ions, cobalt ions and cadmium ions may be provided as water-soluble salts of zinc, cobalt and cadmium, respectively.
  • the auxiliary brightener is selected from the group consisting of allyl sulfonate; 1 ,4-butyne 2-diol; pyri dinium propyl sulfonate; salts and mixtures of the aforementioned.
  • the temperature of the bright nickel electroplating bath ranges from 45 to 75 °C, prefera bly from 50 to 67.5 °C, more preferably from 55 to 62.5 °C during deposition.
  • the cathode density during deposition of the bright nickel layer preferably ranges from 0.5 to 8 A/dm 2 , more preferably from 1 to 6.5 A/dm 2 , even more preferably from 2 to 5 A/dm 2 .
  • sulfosuccinic acid compounds may be added to the bath without any other bath addi tives to be added too.
  • sufficient long-time stability of the baths can only be achieved if a combination of the sulfosuccinic acid compounds is used together with quaternary ammonium compounds and if necessary with additional basic brighteners. Under these circumstances an ex cellent satin-finish of nickel or nickel alloy surfaces is achieved over the entire current density range operable under practical conditions.
  • the pH value of the satin nickel electroplating bath preferably ranges from 3.7 to 4.7, more prefer ably from 3.8 to 4.5, even more preferably from 3.9 to 4.3.
  • the temperature of the satin nickel electroplating bath ranges from 45 to 65 °C, preferably from 47 to 60 °C, more preferably from 51 to 53 °C during deposition.
  • any duration necessary to achieve the desired thickness of the satin nickel layer can be employed.
  • Usually applied durations range from 3 to 40 min, preferably from 4.5 to 30 min, more preferably from 6 to 19 min.
  • the thickness of the intermediate nickel layer ranges from 5 to 15 pm, more preferably from 5.5 to 14, even more preferably from 6 to 13 pm.
  • a non-porous nickel layer is deposited, wherein the non-porous nickel layer is free of particulate matter and wherein the non-porous nickel layer is nobler than the intermediate nickel layer; wherein the electrical potential difference between the non-porous nickel layer and the intermediate nickel layer ranges from 10 to 150 mV.
  • the final electroplating bath comprises chloral hydrate in a concentration ranging from 0.001 to 2 g/L, preferably from 0.1 to 1 .5 g/L, more preferably from 0.2 to 1 g/L.
  • Auxiliary brighteners further increase the brightness and levelling of the non-porous nickel layer when used with carriers and brighteners. They are preferably selected from the group consisting of allyl sulfonate; zinc ions; cobalt ions; cadmium ions; 1 ,4-butyne 2-diol; pyridinium propyl sulfonate; salts and mixtures of the aforementioned. Zinc ions, cobalt ions and cadmium ions may be provid ed as water-soluble salts of zinc, cobalt and cadmium, respectively.
  • the pH value of the final nickel electroplating bath preferably ranges from 3.4 to 5.0, more prefera bly from 3.6 to 4.8, even more preferably from 3.8 to 4.6.
  • the nickel ion release of the thus obtained nickel comprising array was then tested in accordance with EN 1811 :2011 +A1 :2015.
  • the nickel ion release rate was ⁇ 0.2 pg /cm 2 /week. This value was in accordance with the requirement described by ECHA.
  • a coating (TriSeal 300, an electrolytically applied chromium passivation coating) was placed on the chromium layer. Thereby, the nickel ion release was further decreased.
  • Inventive example 8 deposition from a trivalent chromium plating bath
  • Inventive example 7 was repeated but for the chrome layer deposition a chloride-free trivalent chromium plating bath was used (TriChrome ICE, plating time: 5 minutes, current density: 5 [A/dm 2 ], temperature 50 °C, air agitation.
  • TriChrome ICE plating time: 5 minutes, current density: 5 [A/dm 2 ], temperature 50 °C, air agitation.
  • the layer thicknesses of the individual layers of the obtained nickel comprising array were:
  • the nickel ion release of the thus obtained nickel comprising array was then tested in accordance with EN 181 1 :201 1 +A1 :2015.
  • the nickel ion release rate was 1 .7 pg /cm 2 /week.
  • a porous nickel layer deposition as described in comparative example 2 was used, the nickel ion release was increased to 5.1 pg /cm 2 /week.
  • a coating (TriSeal 300, an electrolytically applied chromium passivation coating) was placed on the chromium layer. Thereby, the nickel ion release was further decreased.

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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)
  • Electroplating Methods And Accessories (AREA)

Abstract

La présente invention concerne un nouveau réseau de couches comprenant du nickel ayant de préférence une libération d'ions nickel réduite et un procédé pour sa fabrication. En outre, l'invention concerne l'utilisation du réseau de couches comme revêtement décoratif sur une surface du substrat. L'utilisation du nouveau réseau de couches réduit le risque de dermatite provoquée par le nickel due à la libération plus faible d'ions nickel par rapport aux revêtements décoratifs classiques.
PCT/EP2019/061938 2018-05-09 2019-05-09 Réseau de couches comprenant du nickel et son procédé de fabrication Ceased WO2019215287A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP18171635 2018-05-09
EP18171635.8 2018-05-09

Publications (1)

Publication Number Publication Date
WO2019215287A1 true WO2019215287A1 (fr) 2019-11-14

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PCT/EP2019/061938 Ceased WO2019215287A1 (fr) 2018-05-09 2019-05-09 Réseau de couches comprenant du nickel et son procédé de fabrication

Country Status (1)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210317589A1 (en) * 2018-07-03 2021-10-14 Jcu Corporation Trivalent chromium plating solution and chromium plating method using same
EP4239108A1 (fr) * 2022-03-01 2023-09-06 Jomoo Kitchen & Bath Co., Ltd. Couche de placage composite stérilisante et respectueuse de l'environnement, son procédé de préparation et produit stérilisant et respectueux de l'environnement
EP4239107A1 (fr) * 2022-03-01 2023-09-06 Jomoo Kitchen & Bath Co., Ltd. Couche de placage composite antivirale et écologique, son procédé de préparation et produit antiviral et écologique associé
US20240263334A1 (en) * 2023-02-03 2024-08-08 Luxshare Precision Industry(Chuzhou), Ltd. Process method for controlling glossiness of electroplated nickel-layer

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001088227A1 (fr) 2000-05-19 2001-11-22 Atotech Deutschland Gmbh Revetement en nickel satine ou en alliage de nickel
JP2009235456A (ja) 2008-03-26 2009-10-15 Okuno Chem Ind Co Ltd ３価クロムめっき皮膜用電解処理液
JP2010209456A (ja) 2008-08-21 2010-09-24 Okuno Chem Ind Co Ltd クロムめっき皮膜の防錆用浸漬処理液及び防錆処理方法
EP2396455A1 (fr) 2009-02-13 2011-12-21 Nissan Motor Co., Ltd. Pièce chromée et son procédé de fabrication
WO2012150198A2 (fr) 2011-05-03 2012-11-08 Atotech Deutschland Gmbh Bain et procédé d'électroplacage pour la production de couches de chrome noir
DE102014207778B3 (de) * 2014-04-25 2015-05-21 Kiesow Dr. Brinkmann GmbH & Co. KG Verwendung einer Mischung zur Verwendung in einem galvanischen Bad oder eines galvanischen Bades zur Herstellung einer Glanznickelschicht sowie Verfahren zur Herstellung eines Artikels mit einer Glanznickelschicht
EP3067443A1 (fr) * 2015-03-11 2016-09-14 Jiaxing Minhui Automotive Parts Co.,Ltd Élément nickelé ou chromé et son procédé de fabrication
EP3159436A1 (fr) * 2014-06-23 2017-04-26 Okuno Chemical Industries Co., Ltd. Film multicouche de placage et objet présentant un film multicouche de placage
DE102016013792A1 (de) 2016-11-21 2018-05-24 Atotech Deutschland Gmbh Verfahren zur Bewertung des Korrosionsverhaltens eines Prüfkörpers

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001088227A1 (fr) 2000-05-19 2001-11-22 Atotech Deutschland Gmbh Revetement en nickel satine ou en alliage de nickel
JP2009235456A (ja) 2008-03-26 2009-10-15 Okuno Chem Ind Co Ltd ３価クロムめっき皮膜用電解処理液
JP2010209456A (ja) 2008-08-21 2010-09-24 Okuno Chem Ind Co Ltd クロムめっき皮膜の防錆用浸漬処理液及び防錆処理方法
EP2396455A1 (fr) 2009-02-13 2011-12-21 Nissan Motor Co., Ltd. Pièce chromée et son procédé de fabrication
US20120052319A1 (en) * 2009-02-13 2012-03-01 Atotech Deutschland Gmbh Chrome-plated part and manufacturing method of the same
WO2012150198A2 (fr) 2011-05-03 2012-11-08 Atotech Deutschland Gmbh Bain et procédé d'électroplacage pour la production de couches de chrome noir
DE102014207778B3 (de) * 2014-04-25 2015-05-21 Kiesow Dr. Brinkmann GmbH & Co. KG Verwendung einer Mischung zur Verwendung in einem galvanischen Bad oder eines galvanischen Bades zur Herstellung einer Glanznickelschicht sowie Verfahren zur Herstellung eines Artikels mit einer Glanznickelschicht
EP3159436A1 (fr) * 2014-06-23 2017-04-26 Okuno Chemical Industries Co., Ltd. Film multicouche de placage et objet présentant un film multicouche de placage
EP3067443A1 (fr) * 2015-03-11 2016-09-14 Jiaxing Minhui Automotive Parts Co.,Ltd Élément nickelé ou chromé et son procédé de fabrication
DE102016013792A1 (de) 2016-11-21 2018-05-24 Atotech Deutschland Gmbh Verfahren zur Bewertung des Korrosionsverhaltens eines Prüfkörpers

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"Modern Electroplating", 2000, JOHN WILEY & SONS, INC., pages: 147 - 150
"Modern Electroplating", JOHN WILEY & SONS, INC., pages: 147,149 - 151
"Modern Electroplating", JOHN WILEY & SONS, INC., pages: 298 - 311

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210317589A1 (en) * 2018-07-03 2021-10-14 Jcu Corporation Trivalent chromium plating solution and chromium plating method using same
EP4239108A1 (fr) * 2022-03-01 2023-09-06 Jomoo Kitchen & Bath Co., Ltd. Couche de placage composite stérilisante et respectueuse de l'environnement, son procédé de préparation et produit stérilisant et respectueux de l'environnement
EP4239107A1 (fr) * 2022-03-01 2023-09-06 Jomoo Kitchen & Bath Co., Ltd. Couche de placage composite antivirale et écologique, son procédé de préparation et produit antiviral et écologique associé
US20240263334A1 (en) * 2023-02-03 2024-08-08 Luxshare Precision Industry(Chuzhou), Ltd. Process method for controlling glossiness of electroplated nickel-layer
US12276038B2 (en) * 2023-02-03 2025-04-15 Luxshare Precision Industry(Chuzhou), Ltd. Process method for controlling glossiness of electroplated nickel-layer

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