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 PDFInfo
- 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
- Authority
- US
- United States
- Prior art keywords
- copper
- solution
- spent
- concentration
- cucl
- 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.)
- Expired - Lifetime
Links
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Classifications
-
- 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.
Landscapes
- 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)
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 |
Family
ID=5855884
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
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)
Country | Link |
---|---|
US (1) | US3855141A (sl) |
JP (1) | JPS5549155B2 (sl) |
AT (1) | AT324065B (sl) |
CH (1) | CH606470A5 (sl) |
FR (1) | FR2199009B1 (sl) |
GB (1) | GB1416637A (sl) |
IT (1) | IT993886B (sl) |
SE (1) | SE387966B (sl) |
Cited By (9)
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)
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)
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 |
-
1973
- 1973-07-10 SE SE7309677A patent/SE387966B/xx unknown
- 1973-07-13 CH CH1023273A patent/CH606470A5/xx not_active IP Right Cessation
- 1973-08-09 AT AT700673A patent/AT324065B/de not_active IP Right Cessation
- 1973-08-22 US US00390553A patent/US3855141A/en not_active Expired - Lifetime
- 1973-09-05 GB GB4171273A patent/GB1416637A/en not_active Expired
- 1973-09-06 IT IT28632/73A patent/IT993886B/it active
- 1973-09-06 FR FR7332189A patent/FR2199009B1/fr not_active Expired
- 1973-09-07 JP JP10040073A patent/JPS5549155B2/ja not_active Expired
Patent Citations (2)
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)
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 |
---|---|
DE2244307B2 (de) | 1975-08-21 |
JPS50110948A (sl) | 1975-09-01 |
DE2244307A1 (de) | 1974-03-28 |
GB1416637A (en) | 1975-12-03 |
SE387966B (sv) | 1976-09-20 |
IT993886B (it) | 1975-09-30 |
FR2199009B1 (sl) | 1978-03-10 |
AT324065B (de) | 1975-08-11 |
CH606470A5 (sl) | 1978-10-31 |
FR2199009A1 (sl) | 1974-04-05 |
JPS5549155B2 (sl) | 1980-12-10 |
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