EP0137123A2 - Solution de décapage contenant du sulfate d'ammonium et procédé pour sa régénération - Google Patents

Solution de décapage contenant du sulfate d'ammonium et procédé pour sa régénération Download PDF

Info

Publication number: EP0137123A2
Authority: EP; European Patent Office
Prior art keywords: etching solution; etching; ammonium sulfate; solution; weight
Prior art date: 1983-07-07
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

Application number

EP84107605A

Other languages

German (de)

English (en)

Other versions

EP0137123A3 (en

EP0137123B1 (fr

Inventor

Leander Fürst

Walter Holzer

Bertel Prof. Dr. Kastening

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.)

Elo Chem Atztechnik GmbH

Forschungszentrum Juelich GmbH

Original Assignee

Elo Chem Atztechnik GmbH

Forschungszentrum Juelich GmbH

Kernforschungsanlage Juelich GmbH

Priority date (The priority date 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 date listed.)

1983-07-07

Filing date

1984-06-30

Publication date

1985-04-17

1984-06-30 Application filed by Elo Chem Atztechnik GmbH, Forschungszentrum Juelich GmbH, Kernforschungsanlage Juelich GmbH filed Critical Elo Chem Atztechnik GmbH

1985-04-17 Publication of EP0137123A2 publication Critical patent/EP0137123A2/fr

1986-05-07 Publication of EP0137123A3 publication Critical patent/EP0137123A3/de

1988-06-01 Application granted granted Critical

1988-06-01 Publication of EP0137123B1 publication Critical patent/EP0137123B1/fr

Status Expired legal-status Critical Current

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Images

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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/34—Alkaline compositions for etching copper or alloys thereof
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions

Definitions

the invention relates to an ammoniacal etching solution specified in the preamble of claim 1 and to a regeneration process of the; Art.
Alkaline etchants such as ammoniacal copper tetrammine salt solutions, are used for etching metallic objects, in particular for the production of printed circuit boards, which are also known under the name “printed circuits”, especially when the printed circuit boards to be etched are metal parts that are not resistant to acidic etching media, for example made of lead, tin or nickel.
a re-oxidation of the alkaline etching solution after etching off the metal is carried out with the addition of ammonia gas and / or ammonium salt in the presence of oxygen or air.
the object of the invention is to provide an ammoniacal etching solution in which, without the addition of suspended catalyst particles, the regeneration of the etching solution is accelerated as well as the deposition - etched copper in an electrolysis cell is made possible with extensive oxygen development at the anode, whereby the electrolyte is degraded and one C hlorinal to be substantially avoided.
An etching solution having the chlorine ion concentration specified in claim 2 is preferably used.
a solution of 150 g of ammonium sulfate and 50 g of copper per liter was adjusted to a pH of 9.5 by adding gaseous ammonia.
the solution was gassed with air for oxidation.
the potential the solution was measured at room temperature using a platinum pen against a mercury / mercury oxide reference electrode.
etching solutions containing ammonium sulfate the invention is also applicable to etching solutions which, like the aforementioned etching solution, contain oxygen-containing anions, such as, for example, etching solutions containing ammonium nitrate or ammonium carbonate.
Another embodiment shows that the addition of chlorine ions also increases the etching rate that can be achieved with the etching solution.
copper-coated circuit boards were etched at a temperature of 40 ° C. using an etching solution of 150 g per liter of ammonium sulfate and 80 g per liter of copper in the form of copper tetramine sulfate, which was adjusted to a pH of 9.2 by gassing with ammonia.
the mean etching rate achieved with this starting solution was 7.8 ⁇ m per minute.
ammonium chloride an additional 0.2% by weight of chlorine ions were dissolved in the etching solution. With this etching solution, the etching speed could be increased to 11.7 ⁇ m per minute.
a further increase in the chlorine ion concentration by adding ammonium chloride to a total of 0.4% by weight increases the etching rate only slightly. The etching rate at this concentration was 12.3 ⁇ m per minute.

Landscapes

Chemical & Material Sciences (AREA)
Chemical Kinetics & Catalysis (AREA)
General Chemical & Material Sciences (AREA)
Engineering & Computer Science (AREA)
Materials Engineering (AREA)
Mechanical Engineering (AREA)
Metallurgy (AREA)
Organic Chemistry (AREA)
ing And Chemical Polishing (AREA)
Manufacturing Of Printed Circuit Boards (AREA)

EP84107605A 1983-07-07 1984-06-30 Solution de décapage contenant du sulfate d'ammonium et procédé pour sa régénération Expired EP0137123B1 (fr)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
DE3324450		1983-07-07
DE3324450A DE3324450A1 (de)	1983-07-07	1983-07-07	Ammoniumsulfathaltige aetzloesung sowie verfahren zur regeneration der aetzloesung

Publications (3)

Publication Number	Publication Date
EP0137123A2 true EP0137123A2 (fr)	1985-04-17
EP0137123A3 EP0137123A3 (en)	1986-05-07
EP0137123B1 EP0137123B1 (fr)	1988-06-01

Family

ID=6203349

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP84107605A Expired EP0137123B1 (fr)	1983-07-07	1984-06-30	Solution de décapage contenant du sulfate d'ammonium et procédé pour sa régénération

Country Status (4)

Country	Link
US (1)	US4564428A (fr)
EP (1)	EP0137123B1 (fr)
JP (1)	JPH07100875B2 (fr)
DE (2)	DE3324450A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
DE3429902A1 (de) *	1984-08-14	1986-02-27	Hans Höllmüller Maschinenbau GmbH & Co, 7033 Herrenberg	Verfahren zum aetzen von kupferfilmen auf leiterplatten unter elektrolytischer rueckgewinnung von kupfer aus der aetzloesung
US4784785A (en) *	1987-12-29	1988-11-15	Macdermid, Incorporated	Copper etchant compositions
US5248398A (en) *	1990-11-16	1993-09-28	Macdermid, Incorporated	Process for direct electrolytic regeneration of chloride-based ammoniacal copper etchant bath
US5085730A (en) *	1990-11-16	1992-02-04	Macdermid, Incorporated	Process for regenerating ammoniacal chloride etchants
CN102019430B (zh) *	2009-09-18	2012-09-05	福建师范大学福清分校	一种碱性蚀刻废液回收铜及碱性蚀刻液的回收方法
US11037792B2 (en) *	2018-10-25	2021-06-15	Taiwan Semiconductor Manufacturing Company Ltd.	Semiconductor structure etching solution and method for fabricating a semiconductor structure using the same etching solution

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
BE789944A (fr) *	1971-10-12	1973-02-01	Shipley Co	Regeneration d'une solution usagee d'attaque du cuivre
DE2216269A1 (de) *	1972-04-05	1973-10-18	Hoellmueller Maschbau H	Verfahren zum aetzen von kupfer und kupferlegierungen
CH568225A5 (fr) *	1973-06-22	1975-10-31	Sulzer Ag
US3999564A (en) *	1976-01-09	1976-12-28	Pesek Engineering & Mfg. Co.	Continuous etching and etched material recovery system
DE2850564C2 (de) *	1978-11-22	1982-12-23	Kernforschungsanlage Jülich GmbH, 5170 Jülich	Verfahren und Vorrichtung zum Regenerieren einer Kupfer(II)-Chlorid und/oder Eisen(III)-Chlorid enthaltenden Ätzlösung in einer Elektrolysezelle
DE2917597A1 (de) *	1979-04-30	1980-11-13	Siemens Ag	Verfahren zur regenerierung ammoniakalischer aetzloesungen zum aetzen von metallischem kupfer
JPS5610677A (en) *	1979-07-06	1981-02-03	Tokyo Shibaura Electric Co	Refrigerating plant
DE3031567A1 (de) *	1980-08-21	1982-04-29	Elochem Ätztechnik GmbH, 7758 Meersburg	Verfahren zum regenerieren einer ammoniakalischen aetzloesung

1983
- 1983-07-07 DE DE3324450A patent/DE3324450A1/de not_active Withdrawn
1984
- 1984-06-26 US US06/624,585 patent/US4564428A/en not_active Expired - Lifetime
- 1984-06-30 EP EP84107605A patent/EP0137123B1/fr not_active Expired
- 1984-06-30 DE DE8484107605T patent/DE3471693D1/de not_active Expired
- 1984-07-07 JP JP59139788A patent/JPH07100875B2/ja not_active Expired - Lifetime

Also Published As

Publication number	Publication date
JPH07100875B2 (ja)	1995-11-01
EP0137123A3 (en)	1986-05-07
EP0137123B1 (fr)	1988-06-01
DE3471693D1 (en)	1988-07-07
US4564428A (en)	1986-01-14
JPS6052600A (ja)	1985-03-25
DE3324450A1 (de)	1985-01-17

Legal Events

Date	Code	Title	Description
1985-02-16	PUAI	Public reference made under article 153(3) epc to a published international application that has entered the european phase	Free format text: ORIGINAL CODE: 0009012
1985-04-17	AK	Designated contracting states	Designated state(s): DE FR GB IT NL SE
1986-03-19	PUAL	Search report despatched	Free format text: ORIGINAL CODE: 0009013
1986-05-07	AK	Designated contracting states	Kind code of ref document: A3 Designated state(s): DE FR GB IT NL SE
1986-12-17	17P	Request for examination filed	Effective date: 19861017
1987-12-02	17Q	First examination report despatched	Effective date: 19871013
1988-04-16	GRAA	(expected) grant	Free format text: ORIGINAL CODE: 0009210
1988-06-01	AK	Designated contracting states	Kind code of ref document: B1 Designated state(s): DE FR GB IT NL SE
1988-07-07	REF	Corresponds to:	Ref document number: 3471693 Country of ref document: DE Date of ref document: 19880707
1988-07-13	RBV	Designated contracting states (corrected)	Designated state(s): DE FR GB IT
1988-07-20	GBT	Gb: translation of ep patent filed (gb section 77(6)(a)/1977)
1988-08-24	ITF	It: translation for a ep patent filed
1988-09-01	NLXE	Nl: other communications concerning ep-patents (part 3 heading xe)	Free format text: IN PAT.BUL.14/88,PAGE 1588:SHOULD BE DELETED
1988-10-07	ET	Fr: translation filed
1989-04-07	PLBE	No opposition filed within time limit	Free format text: ORIGINAL CODE: 0009261
1989-04-07	STAA	Information on the status of an ep patent application or granted ep patent	Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT
1989-05-24	26N	No opposition filed
1991-06-30	ITTA	It: last paid annual fee
1992-04-30	PGFP	Annual fee paid to national office [announced via postgrant information from national office to epo]	Ref country code: GB Payment date: 19920430 Year of fee payment: 9
1992-06-16	PGFP	Annual fee paid to national office [announced via postgrant information from national office to epo]	Ref country code: FR Payment date: 19920616 Year of fee payment: 9
1993-06-30	PG25	Lapsed in a contracting state [announced via postgrant information from national office to epo]	Ref country code: GB Effective date: 19930630
1994-02-23	GBPC	Gb: european patent ceased through non-payment of renewal fee	Effective date: 19930630
1994-02-28	PG25	Lapsed in a contracting state [announced via postgrant information from national office to epo]	Ref country code: FR Effective date: 19940228
1994-04-29	REG	Reference to a national code	Ref country code: FR Ref legal event code: ST
2001-06-06	PGFP	Annual fee paid to national office [announced via postgrant information from national office to epo]	Ref country code: DE Payment date: 20010606 Year of fee payment: 18
2003-01-01	PG25	Lapsed in a contracting state [announced via postgrant information from national office to epo]	Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030101

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DE2449588C2 (de)	1985-03-28	Verfahren zur Zersetzung einer wäßrigen, radioaktiven Abfallösung mit gelösten, anorganischen und organischen Inhaltsstoffen
DE2364162B2 (de)	1976-12-23	Saure waessrige metallbehandlungsloesung
DE1771381A1 (de)	1972-01-27	Regenerierung verbrauchter Ammoniumpersulvat-AEtzloesungen
DE2537757A1 (de)	1976-03-11	Verfahren zum regenerieren einer aetzloesung
CH633497A5 (de)	1982-12-15	Verfahren zur reduktion von reduzierbaren schadstoffen in waessrigen loesungen.
EP0046522B1 (fr)	1986-10-15	Procédé pour la régénération d'une solution ammoniacale de gravure
DE2850564A1 (de)	1980-06-04	Verfahren und vorrichtung zum regenerieren einer kupfer(ii)-chlorid und/oder eisen(iii)-chlorid enthaltenden aetzloesung in einer elektrolysezelle
EP0011800B1 (fr)	1982-02-03	Procédé de décapage de surfaces en cuivre ou alliages de cuivre
EP0178347B1 (fr)	1988-09-07	Procédé de régénération automatique de solutions de découpage à base de chlorure cuivrique
EP0137123B1 (fr)	1988-06-01	Solution de décapage contenant du sulfate d'ammonium et procédé pour sa régénération
DE2428380B2 (de)	1978-10-19	Wässrige Lösung zum Entfernen von Nickelabscheidungen
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