US3855141A - Method of processing a spent copper etching solution for reuse in an electroless copper recovery baths - Google Patents

Method of processing a spent copper etching solution for reuse in an electroless copper recovery baths Download PDF

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Publication number
US3855141A
US3855141A US00390553A US39055373A US3855141A US 3855141 A US3855141 A US 3855141A US 00390553 A US00390553 A US 00390553A US 39055373 A US39055373 A US 39055373A US 3855141 A US3855141 A US 3855141A
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United States
Prior art keywords
copper
solution
spent
concentration
cucl
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Expired - Lifetime
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US00390553A
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English (en)
Inventor
C Ruff
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.)
Loewe Opta GmbH
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Loewe Opta GmbH
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Publication date
Priority claimed from DE19722244307 external-priority patent/DE2244307C3/de
Application filed by Loewe Opta GmbH filed Critical Loewe Opta GmbH
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Publication of US3855141A publication Critical patent/US3855141A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper

Definitions

  • the spent solution is enriched by p l the addition of copper ions which are oxidized in the [57] Us Cl 252/792 156/19 252/794 presence of an alkaline complex component to in- 6 3 3/00 6 crease the concentration of CuCl in the solution and [58] Fie'ld 252/79 79 2 79 to thereby decrease the concentration of CuCl.
  • the spent solution is first enriched by the addition of copper ions to a predetermined specified concentration.
  • An oxidation medium such as hydrogen peroxide
  • an alkaline complex component illustrated as ethylenediaminetetraacetic acid, hereinafter called EDTA
  • EDTA ethylenediaminetetraacetic acid
  • FIGURE is a diagram showing facilities for preparing spent copper etching solution in accordance with the invention.
  • a copper etching operation carried out in a conventional etching tank 1 may typically employ a starting solution that includes copper chloride (CuCl having a copper concentration in the range of 30 grams.
  • CuCl copper chloride having a copper concentration in the range of 30 grams.
  • the spent solution from the etching tank 1 is conducted via a magnetic valve 2 and to a first mixing vessel 3 where it is enriched to a'prescribed copper concentration by theaddition of copper ions from a suitable source 11.
  • the concentration of CuCl in the enriched solution may be analytically determined.
  • an oxidizing agent (illustratively hydrogen peroxide) from a source 12 together with an alkaline complex component (illustratively EDTA) from a source 13 are then added to the enriched solution in a second mixing vessel 5.
  • the resulting oxidation of the added copper serves to increase the concentration of the unsaturated CuCl component in the solution, in accordance with the following equation:
  • the relative amounts of the oxidizing agent and the alkaline complex component are determined in a conventional way in accordance with the previously measured concentration of CuCl in the enriched solution, although it has been found that when the oxidization agent is added in excess of such predetermined amount, improved performance is obtained in some cases
  • the EDTA added during the same step preferably has a pH in the range of 11.5 to 12.5 to prevent hydroxide formation. Care must be taken to assure that the elevated temperatures generates in the vessel 5 generated during oxidation does not impair the efficiency of the EDTA.
  • oxygen e.g., a chlorate
  • free oxygen may be used as the oxidizing agent in the mixing vessel 5.
  • alkaline complex components other than EDTA e.g., nitriloessic acid or triethanolamine
  • EDTA nitriloessic acid or triethanolamine
  • the regenerated etching solution is applied through a filter 7 into an electroless copper recovery tank 8 (together with suitable stabilizers, if necessary.) whereupon efficient recovery of the etched copper from the regenerated, alkaline solution may be accomplished without the requirement of extraction of impurities and other contaminants as in electrolytic processes.
  • a method of preparing the spent etching solution for reuse in the separation of the etched copper by electroless means which comprises the steps of:
  • oxidizing agent is selected from the group consisting of hydrogen peroxide, free oxygen, and a chlorate.
  • alkaline complex component is selected from the group consisting of EDTA, nitriloessic acid and thriethanolamine.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Chemically Coating (AREA)
  • Manufacturing Of Printed Circuit Boards (AREA)
US00390553A 1972-09-09 1973-08-22 Method of processing a spent copper etching solution for reuse in an electroless copper recovery baths Expired - Lifetime US3855141A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19722244307 DE2244307C3 (de) 1972-09-09 Verfahren zur Herstellung von alkalischen Bädern zur autokatalytischen stromlosen Abscheidung von Kupfer

Publications (1)

Publication Number Publication Date
US3855141A true US3855141A (en) 1974-12-17

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ID=5855884

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US00390553A Expired - Lifetime US3855141A (en) 1972-09-09 1973-08-22 Method of processing a spent copper etching solution for reuse in an electroless copper recovery baths

Country Status (8)

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US (1) US3855141A (sv)
JP (1) JPS5549155B2 (sv)
AT (1) AT324065B (sv)
CH (1) CH606470A5 (sv)
FR (1) FR2199009B1 (sv)
GB (1) GB1416637A (sv)
IT (1) IT993886B (sv)
SE (1) SE387966B (sv)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3919100A (en) * 1974-04-24 1975-11-11 Enthone Alkaline etchant compositions
US4051001A (en) * 1974-08-26 1977-09-27 Hitachi, Ltd. Process for regenerating etching solution
US5013395A (en) * 1987-08-28 1991-05-07 International Business Machines Corporation Continuous regeneration of acid solution
US5145553A (en) * 1991-05-06 1992-09-08 International Business Machines Corporation Method of making a flexible circuit member
US5227010A (en) * 1991-04-03 1993-07-13 International Business Machines Corporation Regeneration of ferric chloride etchants
US6503363B2 (en) * 2000-03-03 2003-01-07 Seh America, Inc. System for reducing wafer contamination using freshly, conditioned alkaline etching solution
US20050145580A1 (en) * 2001-10-02 2005-07-07 Rotometrics Method and apparatus to clean particulate matter from a toxic fluid
US20110000884A1 (en) * 2007-07-11 2011-01-06 Harald Ottertun Method for Etching Copper and Recovery of the Spent Etching Solution
US20200039852A1 (en) * 2018-08-02 2020-02-06 Guangzhou Ultra Union Chemicals Ltd Method for treating electroless copper plating wastewater

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2917597A1 (de) * 1979-04-30 1980-11-13 Siemens Ag Verfahren zur regenerierung ammoniakalischer aetzloesungen zum aetzen von metallischem kupfer

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3438901A (en) * 1965-10-22 1969-04-15 Neiko I Vassileff Metal treating bath and chelating agent for metal reactive acid baths
US3600244A (en) * 1969-02-20 1971-08-17 Ibm Process of etching metal with recovery or regeneration and recycling

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3438901A (en) * 1965-10-22 1969-04-15 Neiko I Vassileff Metal treating bath and chelating agent for metal reactive acid baths
US3600244A (en) * 1969-02-20 1971-08-17 Ibm Process of etching metal with recovery or regeneration and recycling

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3919100A (en) * 1974-04-24 1975-11-11 Enthone Alkaline etchant compositions
US4051001A (en) * 1974-08-26 1977-09-27 Hitachi, Ltd. Process for regenerating etching solution
US5013395A (en) * 1987-08-28 1991-05-07 International Business Machines Corporation Continuous regeneration of acid solution
US5227010A (en) * 1991-04-03 1993-07-13 International Business Machines Corporation Regeneration of ferric chloride etchants
US5145553A (en) * 1991-05-06 1992-09-08 International Business Machines Corporation Method of making a flexible circuit member
US6503363B2 (en) * 2000-03-03 2003-01-07 Seh America, Inc. System for reducing wafer contamination using freshly, conditioned alkaline etching solution
US20050145580A1 (en) * 2001-10-02 2005-07-07 Rotometrics Method and apparatus to clean particulate matter from a toxic fluid
US7404904B2 (en) * 2001-10-02 2008-07-29 Melvin Stanley Method and apparatus to clean particulate matter from a toxic fluid
US20110000884A1 (en) * 2007-07-11 2011-01-06 Harald Ottertun Method for Etching Copper and Recovery of the Spent Etching Solution
US8236189B2 (en) * 2007-07-11 2012-08-07 Sigma Engineering Ab Method for etching copper and recovery of the spent etching solution
US20200039852A1 (en) * 2018-08-02 2020-02-06 Guangzhou Ultra Union Chemicals Ltd Method for treating electroless copper plating wastewater
US10577265B2 (en) * 2018-08-02 2020-03-03 Guangzhou Ultra Union Chemicals Ltd Method for treating electroless copper plating wastewater

Also Published As

Publication number Publication date
SE387966B (sv) 1976-09-20
FR2199009A1 (sv) 1974-04-05
JPS5549155B2 (sv) 1980-12-10
DE2244307B2 (de) 1975-08-21
GB1416637A (en) 1975-12-03
DE2244307A1 (de) 1974-03-28
IT993886B (it) 1975-09-30
AT324065B (de) 1975-08-11
JPS50110948A (sv) 1975-09-01
FR2199009B1 (sv) 1978-03-10
CH606470A5 (sv) 1978-10-31

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