WO2001038610A1 - Process for the extended use of electrolytes - Google Patents
Process for the extended use of electrolytes Download PDFInfo
- Publication number
- WO2001038610A1 WO2001038610A1 PCT/US2000/030148 US0030148W WO0138610A1 WO 2001038610 A1 WO2001038610 A1 WO 2001038610A1 US 0030148 W US0030148 W US 0030148W WO 0138610 A1 WO0138610 A1 WO 0138610A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- electrolytes
- electrolyte
- extended use
- precipitation
- addition
- Prior art date
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
- 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
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
Definitions
- the invention refers to a process for the extended use of electrolytes, especially for depositing of non-glare metal coatings on a metal surface. It is understood that metal coatings also include metal alloy coatings, and metal surfaces also include metallized surfaces of non-metallic objects.
- the electrolytes used for plating generally are based on the customary, known composition components for the particular metal being plated.
- these would be nickel sulfate, nickel chloride and boric acid.
- Electrolytes based on chloride, sulfate, sulfamate, fluoroborate or mixtures thereof may be used for the metals nickel, copper, zinc, tin as well as for noble metals.
- the electrolytes may contain selected organic or inorganic base brighteners, grain improvers, brighteners or complexing agents. In order to achieve absence of glare, a finely dispersed system is generated in the electrolyte by the addition of inorganic or organic foreign materials, so that these additives during the precipitation are either built into the deposit and/or interrupt for a short time the precipitation of the cathode film locally.
- finely ground insoluble materials such as graphite, barium sulfate, aluminum oxide, glass etc. are added to the electrolyte. These products are maintained in suspension by strong agitation of the electrolyte and built into the deposit during the precipitation.
- the fine dispersal phase is generated in the electrolytes themselves.
- One or more surfactants are added to the solution which form a homogeneous solution below their cloud point, but form a finely dispersed emulsion above their cloud point.
- the stability of the fine dispersal phase is limited. Over time, the droplets increase in size and negatively affect the uniformity of the precipitation.
- the emulsion is stabilized in that an electrolyte is continuously cooled to below the cloud point temperature, whereby the surfactant again goes into complete solution in the electrolyte. Subsequently, the electrolyte is again brought to the working temperature.
- the heating / cooling circuit required causes substantial additional operating cost.
- the surfactant may subsequently be readjusted several times, so that a worsening of the appearance of the layers due to coagulation occurs only after a period of 12 - 14 hours.
- the electrolyte functions without a secondary circuit.
- the coagulate may be removed by filtration over activated charcoal.
- a fine dispersal phase may be generated by the reaction of soluble anionic and cationic combined with difficult-to-dissolve, higher-molecule salts in electrolytes.
- the foreign material after a working cycle of 8 - 10 hours the foreign material must be removed completely from the electrolytes by filtration due to coagulation effects.
- the dispersion phase For the next working cycle the dispersion phase must be rebuilt again each time by the addition of components.
- the higher-molecular compounds may also be directly added to the electrolytes.
- the invention deals with the technical problem to prepare a process for the extended use of electrolytes which ensures a high electrolyte quality with a low economic investment, without having to accept production interruptions for regeneration.
- a thorough cleaning of the electrolyte can be performed on weekends.
- the invention describes a process for the extended use of electrolytes for the precipitation of non-glare metal coatings which, in addition to the metal salt, may also contain conducting salts, base brighteners, grain improvers and complexing agents in which a finely dispersed colloidal phase is generated in order to achieve non-glare properties.
- This is characterized by a partial flow of the electrolyte in which coagulated particles and not yet coagulated particles are removed wholly or in part by means of filtration and that an appropriate quantity of the active substances is subsequently added prior to reintegration.
- a portion of the electrolyte can be directed into an overflow compartment for filtration.
- the overflow compartment should be able to contain between 5 and 25% of the actual bath volume.
- Any type of filtration capable of removing very finely dispersed, finely dispersed and more grossly dispersed particles, wholly or in part, from the electrolyte may be employed.
- the different porosity of the filter materials and the use of filtration aids and/or activated charcoal may serve to differentiate between the various particle sizes.
- Plate filters of defined porosity commonly employed in electroplating can be used, precoated with filtration aids and/or activated charcoal, as well as the common precoated multiple tube filters with defined porosity. Without precoating, wound tube filters may be used. Also, classical methods of fractionating colloidal systems, such as dialysis, ultra and membrane filtration may be employed.
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU17550/01A AU1755001A (en) | 1999-11-25 | 2000-11-21 | Process for the extended use of electrolytes |
US10/148,090 US6797141B1 (en) | 1999-11-25 | 2000-11-21 | Removal of coagulates from a non-glare electroplating bath |
ES00980265T ES2304986T3 (en) | 1999-11-25 | 2000-11-21 | PROCEDURE FOR THE EXTENDED USE OF ELECTROLYTES. |
DE60038700T DE60038700T2 (en) | 1999-11-25 | 2000-11-21 | PROCESS FOR THE ADVANCED USE OF ELECTROLYTES |
EP00980265A EP1252374B1 (en) | 1999-11-25 | 2000-11-21 | Process for the extended use of electrolytes |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19956666.6 | 1999-11-25 | ||
DE19956666A DE19956666B4 (en) | 1999-11-25 | 1999-11-25 | Process for the continuous deposition of glare-free metal coatings on a metallic surface |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001038610A1 true WO2001038610A1 (en) | 2001-05-31 |
Family
ID=7930254
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2000/030148 WO2001038610A1 (en) | 1999-11-25 | 2000-11-21 | Process for the extended use of electrolytes |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP1252374B1 (en) |
CN (1) | CN1399690A (en) |
AT (1) | ATE393247T1 (en) |
AU (1) | AU1755001A (en) |
DE (2) | DE19956666B4 (en) |
ES (1) | ES2304986T3 (en) |
WO (1) | WO2001038610A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8475874B2 (en) | 2004-12-20 | 2013-07-02 | Atotech Deutschland Gmbh | Method for continuously operating acid or alkaline zinc or zinc alloy baths |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4462851B2 (en) * | 2003-06-13 | 2010-05-12 | 三洋電機株式会社 | Manufacturing method of conductive member |
DE102008058086B4 (en) * | 2008-11-18 | 2013-05-23 | Atotech Deutschland Gmbh | Method and device for cleaning electroplating baths for the deposition of metals |
DE102014208733A1 (en) | 2014-05-09 | 2015-11-12 | Dr. Hesse Gmbh & Cie Kg | Process for the electrolytic deposition of copper from water-based electrolytes |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3922208A (en) * | 1973-11-05 | 1975-11-25 | Ford Motor Co | Method of improving the surface finish of as-plated elnisil coatings |
US4102756A (en) * | 1976-12-30 | 1978-07-25 | International Business Machines Corporation | Nickel-iron (80:20) alloy thin film electroplating method and electrochemical treatment and plating apparatus |
US4102755A (en) * | 1973-06-01 | 1978-07-25 | Langbein-Pfanhauser Werke Ag | Method of and electrolytic bath for the electrodeposition of semibright nickel and nickel-cobalt coatings upon a metal surface |
US5312539A (en) * | 1993-06-15 | 1994-05-17 | Learonal Inc. | Electrolytic tin plating method |
US5573652A (en) * | 1994-02-28 | 1996-11-12 | Kawasaki Steel Corporation | Apparatus for continuously dissolving metal powder for use in plating and method of dissolving nickel metal using same |
US5840170A (en) * | 1992-11-30 | 1998-11-24 | Gould Electronics Inc. | Method for inhibiting the electrodeposition of organic particulate matter on copper foil |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2015739A1 (en) * | 1970-04-02 | 1971-10-14 | Vaw Ver Aluminium Werke Ag | Aluminium anodic oxidation baths regenerated by - electrodialysis |
FR2384037A1 (en) * | 1977-03-17 | 1978-10-13 | Nice Anodisation Sa | Electrolytic colouring of anodised aluminium and its alloys - using alternating current and bath contg. stannous sulphate |
JPS59107092A (en) * | 1982-12-08 | 1984-06-21 | Kawasaki Steel Corp | Method for adjusting concentration of zn-ni alloy plating solution |
US5393416A (en) * | 1993-01-26 | 1995-02-28 | Henkel Corporation | Apparatus for maintaining a stable bath for an autodeposition composition by periodically separating particular metal ions from the composition |
DE19506297A1 (en) * | 1995-02-23 | 1996-08-29 | Schloemann Siemag Ag | Process and plant for the regeneration of sulfate electrolyte in steel strip galvanizing |
-
1999
- 1999-11-25 DE DE19956666A patent/DE19956666B4/en not_active Expired - Fee Related
-
2000
- 2000-11-21 DE DE60038700T patent/DE60038700T2/en not_active Expired - Lifetime
- 2000-11-21 EP EP00980265A patent/EP1252374B1/en not_active Expired - Lifetime
- 2000-11-21 ES ES00980265T patent/ES2304986T3/en not_active Expired - Lifetime
- 2000-11-21 AU AU17550/01A patent/AU1755001A/en not_active Abandoned
- 2000-11-21 CN CN00816310.3A patent/CN1399690A/en active Pending
- 2000-11-21 AT AT00980265T patent/ATE393247T1/en not_active IP Right Cessation
- 2000-11-21 WO PCT/US2000/030148 patent/WO2001038610A1/en active Application Filing
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4102755A (en) * | 1973-06-01 | 1978-07-25 | Langbein-Pfanhauser Werke Ag | Method of and electrolytic bath for the electrodeposition of semibright nickel and nickel-cobalt coatings upon a metal surface |
US3922208A (en) * | 1973-11-05 | 1975-11-25 | Ford Motor Co | Method of improving the surface finish of as-plated elnisil coatings |
US4102756A (en) * | 1976-12-30 | 1978-07-25 | International Business Machines Corporation | Nickel-iron (80:20) alloy thin film electroplating method and electrochemical treatment and plating apparatus |
US5840170A (en) * | 1992-11-30 | 1998-11-24 | Gould Electronics Inc. | Method for inhibiting the electrodeposition of organic particulate matter on copper foil |
US5312539A (en) * | 1993-06-15 | 1994-05-17 | Learonal Inc. | Electrolytic tin plating method |
US5573652A (en) * | 1994-02-28 | 1996-11-12 | Kawasaki Steel Corporation | Apparatus for continuously dissolving metal powder for use in plating and method of dissolving nickel metal using same |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8475874B2 (en) | 2004-12-20 | 2013-07-02 | Atotech Deutschland Gmbh | Method for continuously operating acid or alkaline zinc or zinc alloy baths |
Also Published As
Publication number | Publication date |
---|---|
CN1399690A (en) | 2003-02-26 |
ES2304986T3 (en) | 2008-11-01 |
EP1252374A1 (en) | 2002-10-30 |
ATE393247T1 (en) | 2008-05-15 |
EP1252374A4 (en) | 2003-03-12 |
EP1252374B1 (en) | 2008-04-23 |
DE60038700D1 (en) | 2008-06-05 |
DE60038700T2 (en) | 2009-05-20 |
DE19956666B4 (en) | 2009-10-29 |
DE19956666A1 (en) | 2001-05-31 |
AU1755001A (en) | 2001-06-04 |
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