EP2050841A1 - Bain galvanique alcalin doté d'une membrane de filtration - Google Patents
Bain galvanique alcalin doté d'une membrane de filtration Download PDFInfo
- Publication number
- EP2050841A1 EP2050841A1 EP09152660A EP09152660A EP2050841A1 EP 2050841 A1 EP2050841 A1 EP 2050841A1 EP 09152660 A EP09152660 A EP 09152660A EP 09152660 A EP09152660 A EP 09152660A EP 2050841 A1 EP2050841 A1 EP 2050841A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- anode
- filtration membrane
- cathode
- zinc
- bath
- 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.)
- Granted
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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
- C25D3/56—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
- C25D17/02—Tanks; Installations therefor
-
- 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
- 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
- C25D21/16—Regeneration of process solutions
- C25D21/22—Regeneration of process solutions by ion-exchange
Definitions
- the invention relates to an alkaline electroplating bath for applying zinc alloys to substrates, in which the anode space and the cathode space are separated from one another by a filtration membrane.
- zinc alloys can be deposited on substrates in a consistently high quality.
- the electroplating bath is operated with zinc alloy baths containing organic additives such as brighteners and wetting agents and complexing agents in addition to soluble zinc salts and optionally other metal salts selected from iron, nickel, cobalt and tin salts.
- Activated carbon treatment by stirring 0.5-2 g / l of activated carbon into the bath followed by filtration reduces the concentration of impurities by adsorption on the coal. Disadvantage of this method is that it is laborious is and causes only a relatively small reduction.
- Alkaline Zn baths contain a factor of 5 to 10 lower proportion of organic additives as acidic baths. Accordingly, contamination by decomposition products is generally less critical. In the case of alkaline alloy baths, however, the addition of significant amounts of organic complexing agents is required to complex the alloying additive (Fe, Co, Ni, Sn). These are oxidatively degraded at the anode and the accumulated decomposition products have a negative effect on the production process.
- the WO 00/06807 and WO 01/96631 describe electroplating baths for applying zinc-nickel coatings. To avoid the undesirable decomposition of additives at the anode, it is proposed to separate the anode from the alkaline electrolyte through an ion exchange membrane.
- the invention has for its object to provide an alkaline electroplating bath, which does not have the aforementioned disadvantages.
- the life of the bath is to be increased, the anodic decomposition of organic constituents of the bath to be minimized and, when it is used, a layer thickness of consistently high quality to be obtained on the coated substrate.
- filtration membranes are used.
- the size of the pores of these filtration membranes is generally in a range from 0.0001 to 1.0 ⁇ m and from 0.001 to 1.0 ⁇ m, depending on the type of membrane (nano- or ultrafiltration membrane).
- the pore size is in a range of 0.1 to 0.3 microns.
- filtration membranes made of polypropylene.
- the filtration membrane in the alkaline electroplating bath according to the invention is designed as a flat membrane.
- the alkaline electroplating bath according to the invention can also be realized with other membrane forms, examples being hoses, capillaries and hollow fibers.
- Such baths are for example in US 5,417,840 .
- US 4,421,611 US 4,877,496 or US 6,652,728 described.
- the alkaline electroplating bath according to the invention has the advantage that in it also baths for the deposition of zinc alloys can be used, which are suitable for use in the from WO 00/06807 and WO 01/96631 known alkaline zinc-nickel bath with an ion exchange membrane are not suitable.
- sold by the applicant bath "Protedur Ni-75" to call which is characterized by a particularly high efficiency.
- the previously used anodes can be used further. These are mostly nickel anodes.
- the use of these anodes is less expensive than that from the WO 00/06807 known electroplating bath, in which special platinum-plated titanium anodes must be used in addition.
- the anode space is preferably made smaller than the cathode space, since the essential processes take place there.
- Both baths were operated with and without filtration membrane in 5-liter tanks.
- the filtration membrane used was the Abwa-Tec polymer membrane P150F, which has a pore size of 0.12 ⁇ m.
- the membrane was placed in the anode to cathode bath with the anolyte and catholyte being identical, ie, no special anolyte was added.
- iron sheets (7 ⁇ 10 cm), which are usually used for Hull cell tests, were used as workpieces to be coated and coated at a current density of 2 A / dm 2 .
- the baths were operated in serial connection. The movement of the iron sheets was mechanical, at a speed of 1.4 m / min.
- a filtration membrane is produced after a throughput of> 1000 Ah / l introduced after a short time comparable to a new approach current efficiency.
- Table 3 shows the average consumption (1 / 10,000 Ah) of the electrolyte in the bath for filtration membrane electroplating baths according to the invention and baths which do not have this membrane.
- the organic consumption was reduced between 12 and 29% depending on the additive.
- composition of the aforementioned baths were analyzed according to the tests described above. Of particular interest was their cyanide content. This was much lower when using the baths according to the invention with a filtration membrane as baths without membrane. As shown in Table 4 below, a bath without the membrane had a cyanide content of 680 mg / L (new batch) and 790 mg / L (bath of> 1000 Ah / L), respectively, while the corresponding membrane baths contained a cyanide Content of 96 mg / L or 190 mg / L.
- the cyanide content of an old batch ie a bath with> 1000 Ah / l can be reduced when it is provided with a filtration membrane and operated.
- the cyanide content was reduced from 670 mg / l to 190 mg / l.
- the color of the baths was also evaluated. It was found that the color of a freshly prepared bath without membrane changed from initially violet-orange to brown within 15 Ah / l, whereby it remained violet or violet-orange over the entire time when using a filtration membrane. The old batch remained brown without using a membrane and the color changed to orange-brown after 15 Ah / l using a filtration membrane. Violet is also the color of freshly applied baths, which then turn to orange (after a few Ah / l) and at high throughput in brown.
- the voltage between anode and cathode was measured. It was about 3 V and was only about 50-100 mV higher in both approaches using a filtration membrane. Is used instead of the filtration membrane an ion exchange membrane, as in the WO 00/06807 described is, the voltage is higher by at least 500 mV. This again shows the advantage of using a filtration membrane instead of an ion exchange membrane.
- the use of filtration membranes over the use of ion exchange membranes offers many advantages.
- the coating process carried out therewith is more cost-effective, since no platinized anodes have to be used, catholyte and anolyte can have the same composition, and thus no circulation for the anolyte is required.
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)
- Separation Using Semi-Permeable Membranes (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP09152660.8A EP2050841B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique alcalin doté d'une membrane de filtration |
ES09152660.8T ES2574158T3 (es) | 2005-04-26 | 2005-04-26 | Baño galvánico alcalino con una membrana de filtración |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP09152660.8A EP2050841B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique alcalin doté d'une membrane de filtration |
EP05009127A EP1717353B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique contenant une membrane de filtration |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP05009127A Division EP1717353B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique contenant une membrane de filtration |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2050841A1 true EP2050841A1 (fr) | 2009-04-22 |
EP2050841B1 EP2050841B1 (fr) | 2016-05-11 |
Family
ID=35530823
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP09152660.8A Revoked EP2050841B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique alcalin doté d'une membrane de filtration |
EP05009127A Active EP1717353B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique contenant une membrane de filtration |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP05009127A Active EP1717353B1 (fr) | 2005-04-26 | 2005-04-26 | Bain galvanique contenant une membrane de filtration |
Country Status (11)
Country | Link |
---|---|
US (1) | US8293092B2 (fr) |
EP (2) | EP2050841B1 (fr) |
JP (1) | JP4955657B2 (fr) |
KR (1) | KR101301275B1 (fr) |
CN (3) | CN101146934A (fr) |
AT (1) | ATE429528T1 (fr) |
BR (1) | BRPI0610765B1 (fr) |
CA (1) | CA2600273C (fr) |
DE (1) | DE502005007138D1 (fr) |
ES (2) | ES2574158T3 (fr) |
WO (1) | WO2006114305A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3168332B1 (fr) | 2015-03-13 | 2019-03-13 | Okuno Chemical Industries Co., Ltd. | Agent de décapage électrolytique pour enlever du palladium d'un gabarit |
Families Citing this family (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8084684B2 (en) * | 2006-10-09 | 2011-12-27 | Solexel, Inc. | Three-dimensional thin-film solar cells |
ITTO20070704A1 (it) * | 2007-10-05 | 2009-04-06 | Create New Technology S R L | Sistema e metodo di placcatura di leghe metalliche mediante tecnologia galvanica |
US8177944B2 (en) | 2007-12-04 | 2012-05-15 | Ebara Corporation | Plating apparatus and plating method |
DE102008056776A1 (de) | 2008-11-11 | 2010-05-12 | Enthone Inc., West Haven | Galvanisches Bad und Verfahren zur Abscheidung von zinkhaltigen Schichten |
ES2404844T3 (es) | 2010-05-07 | 2013-05-29 | Dr.Ing. Max Schlötter Gmbh & Co. Kg | Regeneración de electrolitos de cinc-níquel alcalinos mediante la eliminación de iones cianuro |
IT1405319B1 (it) * | 2010-12-27 | 2014-01-03 | Fontana R D S R L | Procedimento di rivestimento di pezzi metallici filettati |
KR101420865B1 (ko) * | 2012-10-12 | 2014-07-18 | 주식회사 익스톨 | 금속 도금장치 |
EP2784189A1 (fr) | 2013-03-28 | 2014-10-01 | Coventya SAS | Bain d'électrodéposition d'alliages zinc-fer, procédé de dépôt d'alliage zinc-fer sur un dispositif et ledit dispositif |
US10156020B2 (en) | 2015-07-22 | 2018-12-18 | Dipsol Chemicals Co., Ltd. | Zinc alloy plating method |
CN106550607B (zh) * | 2015-07-22 | 2018-09-18 | 迪普索股份公司 | 锌合金镀敷方法 |
US11913131B2 (en) * | 2016-05-24 | 2024-02-27 | Macdermid, Incorporated | Ternary zinc-nickel-iron alloys and alkaline electrolytes or plating such alloys |
EP3491177A4 (fr) * | 2016-07-29 | 2020-08-12 | Simon Fraser University | Procédé de dépôt électrochimique |
EP3358045A1 (fr) * | 2017-02-07 | 2018-08-08 | Dr.Ing. Max Schlötter GmbH & Co. KG | Procédé de dépôt par placage de revêtements en zinc et en alliage de zinc à partir d'un bain de revêtement alcalin à élimination réduite des additifs de bain organiques |
DK3415665T3 (da) | 2017-06-14 | 2024-02-12 | Dr Ing Max Schloetter Gmbh & Co Kg | Fremgangsmåde til galvanisk udfældning af zink-nikkel-legeringsovertræk ud fra et alkalisk zink-nikkel-legeringsbad med reduceret nedbrydning af tilsætningsstoffer |
PL3461933T3 (pl) * | 2017-09-28 | 2020-03-31 | Atotech Deutschland Gmbh | Sposób elektrolitycznego osadzania warstwy stopu cynkowo-niklowego co najmniej na podłożu przeznaczonym do obróbki |
US11165091B2 (en) | 2018-01-23 | 2021-11-02 | City University Of Hong Kong | Battery system and a method of forming a battery |
ES2952069T3 (es) * | 2019-01-24 | 2023-10-26 | Atotech Deutschland Gmbh & Co Kg | Método para la deposición electrolítica una aleación de zinc-níquel usando un sistema de ánodo de membrana |
CN110462107A (zh) | 2019-02-15 | 2019-11-15 | 迪普索股份公司 | 锌或锌合金电镀方法和系统 |
RU2712582C1 (ru) * | 2019-07-16 | 2020-01-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Электролит для электроосаждения цинк-железных покрытий |
EP4273303A1 (fr) * | 2022-05-05 | 2023-11-08 | Atotech Deutschland GmbH & Co. KG | Procédé de dépôt d'un alliage zinc-nickel sur un substrat, bain de dépôt zinc-nickel aqueux, agent d'éclaircissement et son utilisation |
Citations (10)
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US3974049A (en) * | 1973-08-03 | 1976-08-10 | Parel. Societe Anonyme | Electrochemical process |
US4421611A (en) | 1982-09-30 | 1983-12-20 | Mcgean-Rohco, Inc. | Acetylenic compositions and nickel plating baths containing same |
US4877496A (en) | 1986-08-22 | 1989-10-31 | Nippon Hyomen Kagaku Kabushiki Kaisha | Zinc-nickel alloy plating solution |
US5417840A (en) | 1993-10-21 | 1995-05-23 | Mcgean-Rohco, Inc. | Alkaline zinc-nickel alloy plating baths |
WO2000006807A2 (fr) | 1998-07-30 | 2000-02-10 | Walter Hillebrand Gmbh & Co. Galvanotechnik | Bain alcalin de zinc-nickel |
WO2001096631A1 (fr) | 2000-06-15 | 2001-12-20 | Taskem Inc. | Electrodeposition zinc-nickel |
US6652728B1 (en) | 1998-09-02 | 2003-11-25 | Atotech Deutschland Gmbh | Cyanide-free aqueous alkaline bath used for the galvanic application of zinc or zinc-alloy coatings |
EP1365046A1 (fr) * | 2002-05-16 | 2003-11-26 | UNIVERSITE PAUL SABATIER (TOULOUSE III) Etablissement public a caractère scientifique, culturel et professionnel | Procédé de protection d'un substrat en acier ou alliage d'alumium contre la corrosion permettant de lui conferer des propriétés tribologiques, et substrat obtenu |
EP1369505A2 (fr) | 2002-06-06 | 2003-12-10 | Goema Ag | Procédé et dispositif de recirculation de l'eau de rincage et de nettoyage d'un bain |
WO2005073438A1 (fr) | 2003-12-31 | 2005-08-11 | Coventya Sas | Installation de depot de zinc ou d’alliages de zinc |
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US7442286B2 (en) * | 2004-02-26 | 2008-10-28 | Atotech Deutschland Gmbh | Articles with electroplated zinc-nickel ternary and higher alloys, electroplating baths, processes and systems for electroplating such alloys |
-
2005
- 2005-04-26 DE DE502005007138T patent/DE502005007138D1/de active Active
- 2005-04-26 AT AT05009127T patent/ATE429528T1/de not_active IP Right Cessation
- 2005-04-26 EP EP09152660.8A patent/EP2050841B1/fr not_active Revoked
- 2005-04-26 ES ES09152660.8T patent/ES2574158T3/es active Active
- 2005-04-26 ES ES05009127T patent/ES2324169T3/es active Active
- 2005-04-26 EP EP05009127A patent/EP1717353B1/fr active Active
-
2006
- 2006-04-26 KR KR1020077019889A patent/KR101301275B1/ko active IP Right Grant
- 2006-04-26 JP JP2008508150A patent/JP4955657B2/ja active Active
- 2006-04-26 US US11/912,591 patent/US8293092B2/en active Active
- 2006-04-26 CN CNA2006800094924A patent/CN101146934A/zh active Pending
- 2006-04-26 BR BRPI0610765A patent/BRPI0610765B1/pt active IP Right Grant
- 2006-04-26 CA CA2600273A patent/CA2600273C/fr active Active
- 2006-04-26 WO PCT/EP2006/003883 patent/WO2006114305A1/fr active Application Filing
- 2006-04-26 CN CN201510173915.7A patent/CN104911651A/zh active Pending
- 2006-04-26 CN CN201510173898.7A patent/CN104911676B/zh active Active
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3974049A (en) * | 1973-08-03 | 1976-08-10 | Parel. Societe Anonyme | Electrochemical process |
US4421611A (en) | 1982-09-30 | 1983-12-20 | Mcgean-Rohco, Inc. | Acetylenic compositions and nickel plating baths containing same |
US4877496A (en) | 1986-08-22 | 1989-10-31 | Nippon Hyomen Kagaku Kabushiki Kaisha | Zinc-nickel alloy plating solution |
US5417840A (en) | 1993-10-21 | 1995-05-23 | Mcgean-Rohco, Inc. | Alkaline zinc-nickel alloy plating baths |
WO2000006807A2 (fr) | 1998-07-30 | 2000-02-10 | Walter Hillebrand Gmbh & Co. Galvanotechnik | Bain alcalin de zinc-nickel |
US6652728B1 (en) | 1998-09-02 | 2003-11-25 | Atotech Deutschland Gmbh | Cyanide-free aqueous alkaline bath used for the galvanic application of zinc or zinc-alloy coatings |
WO2001096631A1 (fr) | 2000-06-15 | 2001-12-20 | Taskem Inc. | Electrodeposition zinc-nickel |
EP1365046A1 (fr) * | 2002-05-16 | 2003-11-26 | UNIVERSITE PAUL SABATIER (TOULOUSE III) Etablissement public a caractère scientifique, culturel et professionnel | Procédé de protection d'un substrat en acier ou alliage d'alumium contre la corrosion permettant de lui conferer des propriétés tribologiques, et substrat obtenu |
EP1369505A2 (fr) | 2002-06-06 | 2003-12-10 | Goema Ag | Procédé et dispositif de recirculation de l'eau de rincage et de nettoyage d'un bain |
WO2005073438A1 (fr) | 2003-12-31 | 2005-08-11 | Coventya Sas | Installation de depot de zinc ou d’alliages de zinc |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3168332B1 (fr) | 2015-03-13 | 2019-03-13 | Okuno Chemical Industries Co., Ltd. | Agent de décapage électrolytique pour enlever du palladium d'un gabarit |
US11649558B2 (en) | 2015-03-13 | 2023-05-16 | Okuno Chemical Industries Co., Ltd. | Electrolytic stripping agent for jig |
Also Published As
Publication number | Publication date |
---|---|
BRPI0610765A2 (pt) | 2010-07-20 |
CN104911651A (zh) | 2015-09-16 |
US20090107845A1 (en) | 2009-04-30 |
BRPI0610765B1 (pt) | 2017-04-04 |
ES2574158T3 (es) | 2016-06-15 |
JP2008539329A (ja) | 2008-11-13 |
EP1717353B1 (fr) | 2009-04-22 |
EP2050841B1 (fr) | 2016-05-11 |
ATE429528T1 (de) | 2009-05-15 |
JP4955657B2 (ja) | 2012-06-20 |
KR20070122454A (ko) | 2007-12-31 |
DE502005007138D1 (de) | 2009-06-04 |
CA2600273A1 (fr) | 2006-11-02 |
CA2600273C (fr) | 2014-08-12 |
ES2324169T3 (es) | 2009-07-31 |
CN101146934A (zh) | 2008-03-19 |
US8293092B2 (en) | 2012-10-23 |
CN104911676A (zh) | 2015-09-16 |
WO2006114305A1 (fr) | 2006-11-02 |
CN104911676B (zh) | 2017-11-17 |
KR101301275B1 (ko) | 2013-08-29 |
EP1717353A1 (fr) | 2006-11-02 |
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