FI3607116T3 - Method for electrolytically depositing a chromium or chromium alloy layer on at least one substrate - Google Patents

Method for electrolytically depositing a chromium or chromium alloy layer on at least one substrate Download PDF

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Publication number
FI3607116T3
FI3607116T3 FIEP18714275.7T FI18714275T FI3607116T3 FI 3607116 T3 FI3607116 T3 FI 3607116T3 FI 18714275 T FI18714275 T FI 18714275T FI 3607116 T3 FI3607116 T3 FI 3607116T3
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Finland
Prior art keywords
total
range
current density
plating bath
substrate
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FIEP18714275.7T
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Finnish (fi)
Swedish (sv)
Inventor
Anke Walter
Oleksandra Yevtushenko
Franziska Paulig
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Atotech Deutschland Gmbh & Co Kg
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/04Electroplating: Baths therefor from solutions of chromium
    • C25D3/06Electroplating: Baths therefor from solutions of chromium from solutions of trivalent chromium
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10Electrodes, e.g. composition, counter electrode
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60Electroplating characterised by the structure or texture of the layers
    • C25D5/615Microstructure of the layers, e.g. mixed structure
    • C25D5/619Amorphous layers

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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)
  • Crystallography & Structural Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)

Claims (1)

MENETELMÄ KROMI- TAI KROMISEOSKERROKSEN PINNOITTAMISEKSI ELEKTRO- LYYTTISESTI AINAKIN YHDELLE ALUSTALLE PATENTTIVAATIMUKSETMETHOD FOR ELECTROLYTIC COATING OF CHROME OR CHROMIUM ALLOY LAYER ON AT LEAST ONE SUBSTRATE PATENT CLAIMS 1. Menetelmä kromi- tai kromiseoskerroksen pinnoittamiseksi elektrolyyttisesti ainakin yhdelle — alustalle, menetelmän käsittäessä vaiheet, joissa (a) tarjotaan käyttöön vesipitoinen pinnoitushaude, jonka pH on välillä, joka on 4,1 - 7,0, — joka käsittää trivalentteja kromi-ioneja, — joka käsittää 0 mg/l - 200 mg/l heksavalenttia kromia perustuen pinnoitushauteen kokonaisti- lavuuteen, ja —joka ei käsitä booria sisältäviä yhdisteitä, (b) tarjotaan käyttöön ainakin yksi alusta ja ainakin yksi anodi, ja (c) upotetaan kyseinen ainakin yksi alusta vesipitoiseen pinnoitushauteeseen ja kytketään tasa- virta niin, että kromi- tai kromiseoskerros pinnoittuu kyseiselle ainakin yhdelle alustalle, jossa kyseinen ainakin yksi alusta muodostaa katodin, jolla on katodin kokonaisvirtatiheys, ja kysei- — sellä ainakin yhdellä anodilla on anodin kokonaisvirtatiheys, edellyttäen, että — anodin kokonaisvirtatiheys on 6 A/dm? tai suurempi, jossa maksimaalinen anodin kokonaisvir- tatiheys on 50 A/dm?, — katodin kokonaisvirtatiheys on 18 A/dm? tai suurempi, jossa maksimaalinen katodin kokonais- — virtatiheys on 250 A/dm?, — katodin kokonaisvirtatiheys on korkeampi kuin anodin kokonaisvirtatiheys, ja — kyseinen ainakin yksi alusta ja kyseinen ainakin yksi anodi ovat läsnä pinnoitushauteessa niin, että trivalenttiset kromi-ionit ovat kosketuksissa kyseisen ainakin yhden anodin kanssa.1. A method for electrolytically plating a chromium or chromium alloy layer on at least one — substrate, the method comprising the steps of (a) providing an aqueous plating bath with a pH in the range of 4.1 to 7.0, — comprising trivalent chromium ions, — comprising 0 mg/l to 200 mg/l hexavalent chromium based on the total volume of the plating bath, and — not comprising boron-containing compounds, (b) providing at least one substrate and at least one anode, and (c) immersing said at least one substrate in an aqueous plating bath and direct current is applied so that a chromium or chromium alloy layer is deposited on said at least one substrate, where said at least one substrate forms a cathode with a total current density of the cathode, and said at least one anode has a total current density of the anode, provided that — the total current density of the anode is 6 A/dm? or greater, where the maximum total anode current density is 50 A/dm?, — the total cathode current density is 18 A/dm? or greater, wherein the maximum total cathode current density is 250 A/dm?, the total cathode current density is higher than the total anode current density, and said at least one substrate and said at least one anode are present in the plating bath such that the trivalent chromium ions are in contact with said with at least one anode. 2. Patenttivaatimuksen 1 mukainen menetelmä, jossa anodin kokonaisvirtatiheys on 8 A/dm? tai — suurempi, edullisesti 9 A/dm? tai suurempi, edullisemmin 10 A/dm? tai suurempi.2. The method according to claim 1, where the total current density of the anode is 8 A/dm? or — higher, preferably 9 A/dm? or larger, preferably 10 A/dm? or greater. 3. Patenttivaatimuksen 1 tai 2 mukainen menetelmä, jossa katodin kokonaisvirtatiheys on 30 A/dm? tai suurempi, edullisesti 35 A/dm? tai suurempi.3. The method according to claim 1 or 2, in which the total current density of the cathode is 30 A/dm? or higher, preferably 35 A/dm? or greater. 4. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa anodin kokonaisvirta- tiheyden suhde katodin kokonaisvirtatiheyteen on välillä, joka on 1:2 - 1:8, edullisesti välillä, joka on 1:2 - 1:6, edullisemmin välillä, joka on 1:3 - 1:6, vielä edullisemmin välillä, joka on 1:3 - 1:5.4. A method according to one of the preceding claims, wherein the ratio of the total current density of the anode to the total current density of the cathode is in the range of 1:2 to 1:8, preferably in the range of 1:2 to 1:6, more preferably in the range of 1: 3 to 1:6, even more preferably in the range of 1:3 to 1:5. 5. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa trivalenttien kromi- — jonien kokonaismäärä pinnoitushauteessa on välillä, joka on 10 g/l - 30 g/l perustuen pinnoitus- hauteen kokonaistilavuuteen, edullisesti välillä, joka on 17 g/l - 24 g/l.5. A method according to one of the preceding claims, wherein the total amount of trivalent chromium ions in the plating bath is in the range of 10 g/l to 30 g/l based on the total volume of the plating bath, preferably in the range of 17 g/l to 24 g/ l. 6. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa pinnoitushaude käsit- tää bromidi-ioneja edullisesti kokonaismääränä, joka on ainakin 0,06 mol/l perustuen pinnoitus- hauteen kokonaistilavuuteen, edullisesti ainakin 0,1 mol/l, edullisemmin ainakin 0,15 mol/l.6. The method according to one of the preceding claims, in which the plating bath preferably comprises bromide ions in a total amount that is at least 0.06 mol/l based on the total volume of the plating bath, preferably at least 0.1 mol/l, more preferably at least 0.15 mol /l. —7. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa pinnoitushauteen pH on välillä, joka on 4,5 - 6,5, edullisesti välillä, joka on 5,0 - 6,0, edullisimmin välillä, joka on 5,3 -—7. A method according to one of the preceding claims, wherein the pH of the coating bath is in the range of 4.5 to 6.5, preferably in the range of 5.0 to 6.0, most preferably in the range of 5.3 to 5,9.5.9. 8. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa pinnoitushaude sisäl- tää kupari-ioneja, sinkki-ioneja, nikkeli-ioneja ja rautaioneja, kutakin itsenäisesti kokonaismää- — ränä, joka on 0 mg/l - 40 mg/l perustuen pinnoitushauteen kokonaistilavuuteen, edullisesti kuta- kin itsenäisesti kokonaismääränä, joka on 0 mg/l - 20 mg/l, edullisimmin kutakin itsenäisesti kokonaismääränä, joka on 0 mg/l - 10 mg/l.8. A method according to one of the preceding claims, in which the plating bath contains copper ions, zinc ions, nickel ions and iron ions, each independently in a total amount of — 0 mg/l to 40 mg/l based on the total volume of the plating bath, preferably each independently in a total amount of 0 mg/l to 20 mg/l, most preferably each independently in a total amount of 0 mg/l to 10 mg/l. 9. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa pinnoitushaude ei kä- sitä glysiiniä, alumiini-ioneja ja tinaioneja tai käsittää niitä kokonaismääränä, joka on alle 10 mg/l — perustuen pinnoitushauteen kokonaistilavuuteen.9. A method according to one of the preceding claims, in which the plating bath does not handle glycine, aluminum ions and tin ions or comprises them in a total amount that is less than 10 mg/l — based on the total volume of the plating bath. 10. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa menetelmä toistetaan vesipitoisella pinnoitushauteella, joka saadaan vaiheen (c) jälkeen, ja toisella alustalla.10. A method according to one of the preceding claims, wherein the method is repeated with an aqueous coating bath obtained after step (c) and with another substrate. 11. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa kyseinen ainakin yksi alusta on metalli- tai metalliseosalustaa, edullisesti metalli- tai metalliseosalustaa, joka itsenäi- — sesti käsittää yhtä tai useampaa kuin yhtä metallia, joka valitaan ryhmästä, joka koostuu kupa- rista, raudasta, nikkelistä ja alumiinista.11. A method according to one of the preceding claims, wherein said at least one substrate is a metal or metal alloy substrate, preferably a metal or metal alloy substrate, which independently comprises one or more than one metal selected from the group consisting of copper, iron , nickel and aluminum. 12. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa kyseinen ainakin yksi anodi valitaan itsenäisesti ryhmästä, joka koostuu grafiittianodeista ja sekametallioksidianodeis- ta, edullisesti se valitaan itsenäisesti ryhmästä, joka koostuu grafiittianodeista ja sekametal- — lioksidianodeista titaanilla.12. A method according to one of the preceding claims, wherein said at least one anode is independently selected from the group consisting of graphite anodes and mixed metal oxide anodes, preferably it is independently selected from the group consisting of graphite anodes and mixed metal oxide anodes with titanium. 13. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa pinnoitushauteen lämpötila vaiheessa (c) on välillä, joka on 20 °C - 90 °C, edullisesti välillä, joka on 30 °C - 70 °C, edullisemmin välillä, joka on 40 °C - 60 °C, edullisimmin välillä, joka on 45 °C - 60 °C.13. A method according to one of the preceding claims, wherein the temperature of the plating bath in step (c) is in the range of 20°C to 90°C, preferably in the range of 30°C to 70°C, more preferably in the range of 40°C - 60°C, most preferably in the range of 45°C to 60°C. 14. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa vaiheessa (c) kromi- tai kromiseoskerros pinnoitetaan pinnoitusnopeudella, joka on välillä, joka on 0,3 um/min - 1,2 um/min perustuen katodin kokonaisvirtatiheyteen, joka on 40 A/dm?.14. A method according to any of the preceding claims, wherein in step (c) the chromium or chromium alloy layer is deposited at a deposition rate in the range of 0.3 µm/min to 1.2 µm/min based on a total cathode current density of 40 A/dm ?. 15. Jonkin edellä olevan patenttivaatimuksen mukainen menetelmä, jossa vaiheessa (c) pinnoi- tetun kromi- tai kromiseoskerroksen keskimääräinen kerrospaksuus on 1,0 um tai suurempi, edullisesti 2 um tai suurempi, edullisemmin 4 um tai suurempi, vielä edullisemmin 5 um tai suu- — rempi, edullisimmin keskimääräinen kerrospaksuus on välillä, joka on 5 um - 200 um, edullisesti 5 um - 150 pm.15. The method according to one of the preceding claims, wherein the average layer thickness of the chromium or chromium alloy layer coated in step (c) is 1.0 µm or greater, preferably 2 µm or greater, more preferably 4 µm or greater, even more preferably 5 µm or — more preferably, the average layer thickness is between 5 µm and 200 µm, preferably 5 µm and 150 µm.
FIEP18714275.7T 2017-04-04 2018-04-04 Method for electrolytically depositing a chromium or chromium alloy layer on at least one substrate FI3607116T3 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP17164736 2017-04-04
PCT/EP2018/058591 WO2018185154A1 (en) 2017-04-04 2018-04-04 Method for electrolytically depositing a chromium or chromium alloy layer on at least one substrate

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EP (2) EP3607116B1 (en)
CN (2) CN110446802B (en)
ES (1) ES2940623T3 (en)
FI (1) FI3607116T3 (en)
LT (1) LT3607116T (en)
PL (1) PL3607116T3 (en)
WO (1) WO2018185154A1 (en)

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Publication number Priority date Publication date Assignee Title
FI129158B (en) 2019-03-15 2021-08-13 Savroc Ltd An object comprising a chromium-based coating on a substrate
WO2021122932A1 (en) 2019-12-18 2021-06-24 Atotech Deutschland Gmbh Electroplating composition and method for depositing a chromium coating on a substrate
BR112022008879A2 (en) * 2019-12-18 2022-08-23 Atotech Deutschland Gmbh & Co Kg METHOD TO REDUCE THE CONCENTRATION OF IRON IONS IN A TRIVALENT CHROME GALVANIZING BATH

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NL75772C (en) 1948-03-20
US4392922A (en) 1980-11-10 1983-07-12 Occidental Chemical Corporation Trivalent chromium electrolyte and process employing vanadium reducing agent
RU2139369C1 (en) 1999-01-25 1999-10-10 Виноградов Сергей Станиславович Method of electrochemical chrome plating of metals and their alloys
EP2899299A1 (en) * 2014-01-24 2015-07-29 COVENTYA S.p.A. Electroplating bath containing trivalent chromium and process for depositing chromium
CO7190036A1 (en) 2014-02-11 2015-02-19 Garcia Carlos Enrique Muñoz Continuous trivalent chrome plating process
EP3146091B1 (en) * 2014-05-21 2019-08-21 Tata Steel IJmuiden BV Method for manufacturing chromium-chromium oxide coated substrates
US11198944B2 (en) * 2018-09-26 2021-12-14 Toyoda Gosei Co., Ltd. Black plated resin part and method for producing the same
CN110512240A (en) * 2019-09-04 2019-11-29 广东涂乐师新材料科技有限公司 A kind of white chromium electrodeposit liquid of salt acid type highly corrosion resistant trivalent

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LT3607116T (en) 2023-06-12
EP4170071A1 (en) 2023-04-26
CN110446802A (en) 2019-11-12
CN115961315A (en) 2023-04-14
PL3607116T3 (en) 2023-08-07
EP3607116B1 (en) 2022-12-21
EP3607116A1 (en) 2020-02-12
ES2940623T3 (en) 2023-05-09
WO2018185154A1 (en) 2018-10-11
CN110446802B (en) 2023-02-28

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