EP0780495B1 - Verfahren zur Erzeugung von Brochantit-Patina auf einer aus Kupfer bestehenden Oberfläche - Google Patents

Verfahren zur Erzeugung von Brochantit-Patina auf einer aus Kupfer bestehenden Oberfläche Download PDF

Info

Publication number
EP0780495B1
EP0780495B1 EP96119420A EP96119420A EP0780495B1 EP 0780495 B1 EP0780495 B1 EP 0780495B1 EP 96119420 A EP96119420 A EP 96119420A EP 96119420 A EP96119420 A EP 96119420A EP 0780495 B1 EP0780495 B1 EP 0780495B1
Authority
EP
European Patent Office
Prior art keywords
sodium
starting material
electrolyte
copper
concentration
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
Application number
EP96119420A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0780495A2 (de
EP0780495A3 (de
Inventor
Dirk Dr.-Ing. Rode
Ruzica Dipl.-Chem. Luetic
Helmut Dr.-Ing. Protzer
Stefan Dipl.-Ing. Hoveling
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.)
KME Special Products GmbH and Co KG
Original Assignee
KM Europa Metal AG
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.)
Filing date
Publication date
Application filed by KM Europa Metal AG filed Critical KM Europa Metal AG
Publication of EP0780495A2 publication Critical patent/EP0780495A2/de
Publication of EP0780495A3 publication Critical patent/EP0780495A3/de
Application granted granted Critical
Publication of EP0780495B1 publication Critical patent/EP0780495B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32

Definitions

  • the invention relates to a method for producing brochantite patina on a surface made of copper a primary material according to the features in the preamble of the claim 1.
  • FR-PS 2 064 465 is one of the latter.
  • the copper primary material is first subjected to a pretreatment by degreasing and pickling.
  • the primary material then undergoes anodic electrolysis from a sodium hydrogen carbonate (NaHCO 3 ) electrolyte with additions of sulfates, nitrates or phosphates as well as chromates or dichromates.
  • NaHCO 3 sodium hydrogen carbonate
  • the process can be carried out continuously or batchwise at a bath temperature of about 20 ° C to 30 ° C.
  • a carbonate patina is created with parts of the additives used.
  • JP-A-56 130 495 Another electrolytic process is known from JP-A-56 130 495, with which can form a patina layer on copper substrates, an acidic carbonate and hydrosulfite-containing electrolyte is used.
  • the invention is based on the object Process for producing brochantite patina on a copper one To propose a surface with which even on an industrial scale a uniform, adherent and weatherproof, from environmentally relevant components free, largely nature-identical green patina can be produced from brochantite, which is also not noteworthy in the further processing of the input material used is damaged.
  • the invention provides a uniform continuous flow process in which Input material can be used both in the form of sheets and in the form of coils can.
  • the length of the primary material on a coil is in itself unlimited. However, coils with a weight between about 2 t are preferably used up to 12 t.
  • the width of the primary material (sheets or coils) is unlimited.
  • the breadth is one Copper plate or a coil made of copper sheet between 300 mm and 1,000 mm.
  • the primary material is a copper material with a strength of F20 to F37, in particular from F24, according to DIN 17 650 or DIN 17 670 part 1.
  • An essential part of the method according to the invention is the use of a suitable starting material with a technically low-fat surface and corresponding roughness.
  • the roughening can be done, for example, by grinding or brushing.
  • an electrolyte containing anodic circuit of the primary material to be patinated in a sodium hydrogen carbonate (NaHCO 3 ) and sodium sulfite (Na 2 SO 3 ) and / or sodium disulfite (Na 2 S 2 O 5 ) is already well on the Adhesive green carbonate-sulfite patina with a thickness of 15 ⁇ m to 35 ⁇ m. If sodium carbonate (Na 2 CO 3 ) is used in this connection, this takes place in a concentration of 40 g / l to 90 g / l, in particular 60 g / l to 80 g / l.
  • the electrolysis bath is operated at a temperature of 30 ° C. to 90 ° C., preferably 35 ° C. to 50 ° C., the current density being 1 to 20 A / dm 2 , preferably 3 to 10 A / dm 2 .
  • the residence time of the starting material in the electrolysis bath is set at 10 seconds to 12 minutes, in particular 2 to 6 minutes.
  • wetting agents can be added to the electrolyte in the form from non-foaming or non-ionic surfactants to one Percent are added.
  • the pre-patinated semi-finished product is then rinsed and in a subsequent step of post-oxidation in subjected to a fixing bath in which the initially formed Carbonate sulfite patina practically completely in basic Copper sulfate, which is converted into brochantite.
  • the oxidizing agents are preferred to the fixing bath added in a concentration of 10 g / l to 50 g / l.
  • the reaction time is extremely short, preferably about 10 to 120 sec, so that straight copper material from the coil is advantageous can be patinated.
  • the temperature of the fixer is between 35 ° C and 95 ° C.
  • the invention leads to the fact that a Brochantite patina is created that in appearance and Composition largely of the natural brochantite patina corresponds and at the same time permanent weather resistance having.
  • the artificial patina shows one Color range from lime green to turquoise, with the Layer contains about 6% to 8% sulfur and therefore typically the concentration range of about 7.1% sulfur, which has the natural brochantite patina.
  • From the beginning of one Outdoor weathering is the final state of a natural grown brochantits, which is particularly evident in shows permanent weather resistance.
  • the layer is firmly adhering to the respective surface, and that too with any further processing of the patinated raw material.
  • the patinated material is not just that for the arts and crafts application indoors, but especially in the industrial area for the occupancy of expansive areas.
  • the procedure is rational and simple. There are environmental and occupational safety requirements Chemicals used.
  • patination brochantite is produced as follows:
  • a largely fat-free SFCu tape F24 with a thickness of 0.7 mm and a width of 1000 mm and a roughness of about 9 ⁇ m is used as the coil with a weight of 10 t as the starting material.
  • the SFCu band is decoiled and passed horizontally through an electrolysis bath, which is composed of an aqueous solution with 60 g / l sodium carbonate (Na 2 CO 3 ) and 15 g / l sodium disulfite (Na 2 S 2 O 5 ).
  • the temperature of the electrolysis bath is 45 ° C.
  • the SFCu band stays in the electrolysis bath for two minutes. This is constantly kept in motion by a corresponding pump.
  • the pre-patinated tape is rinsed and then passed through a fixing bath with an aqueous solution of 50 g / l potassium chlorate (KClO 3 ), to which up to 10 g / l magnesium and / or zinc sulfate can be added.
  • the temperature of the fixing bath is 40 ° C.
  • the SFCu tape stays in the fixer for two minutes.
  • the typical layer thickness is 15 ⁇ m to 20 ⁇ m.
  • the SFCu belt runs through yet another rinse bath and is then subsequently used of an air stream dried. After drying the SFCu tape can be rewound and then further processed be fed.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Chemically Coating (AREA)
  • Physical Vapour Deposition (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Electroplating Methods And Accessories (AREA)
  • ing And Chemical Polishing (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
EP96119420A 1995-12-22 1996-12-04 Verfahren zur Erzeugung von Brochantit-Patina auf einer aus Kupfer bestehenden Oberfläche Expired - Lifetime EP0780495B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19548261A DE19548261A1 (de) 1995-12-22 1995-12-22 Verfahren zur Herstellung einer Bronchantitpatina auf Kupferhalbzeug
DE19548261 1995-12-22

Publications (3)

Publication Number Publication Date
EP0780495A2 EP0780495A2 (de) 1997-06-25
EP0780495A3 EP0780495A3 (de) 1997-08-27
EP0780495B1 true EP0780495B1 (de) 2001-05-09

Family

ID=7781097

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96119420A Expired - Lifetime EP0780495B1 (de) 1995-12-22 1996-12-04 Verfahren zur Erzeugung von Brochantit-Patina auf einer aus Kupfer bestehenden Oberfläche

Country Status (9)

Country Link
US (1) US5714052A (da)
EP (1) EP0780495B1 (da)
AT (1) ATE201059T1 (da)
CA (1) CA2190419C (da)
DE (2) DE19548261A1 (da)
DK (1) DK0780495T3 (da)
ES (1) ES2156248T3 (da)
GR (1) GR3036263T3 (da)
PT (1) PT780495E (da)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812715A (zh) * 2010-03-24 2010-08-25 西安北方光电有限公司 一种钛合金黑色阳极氧化工艺

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19809904A1 (de) * 1998-03-07 1999-09-09 Km Europa Metal Ag Verfahren und Reaktionslösung zur Erzeugung einer Patina
JP4121217B2 (ja) 1999-06-30 2008-07-23 株式会社スーパーブラストシステムズ 人工緑青発生法
AT413668B (de) * 2003-05-13 2006-04-15 Fronius Int Gmbh Gasdüse für einen schweissbrenner und schweissbrenner mit einer derartigen gasdüse
CN101805917B (zh) * 2010-03-24 2011-12-07 西安北方光电有限公司 一种钛合金黑色阳极氧化处理液的配制方法
CN103014815B (zh) * 2012-11-28 2016-05-04 常州大学 铜导线辊式快速阳极氧化处理方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3497401A (en) * 1967-09-20 1970-02-24 Intern Copper Research Ass Inc Patination of copper
FR2064465A5 (en) 1969-09-12 1971-07-23 Trefimetaux Artificial patina prodn on copper (alloy)objects
JPS607038B2 (ja) * 1980-03-19 1985-02-21 積水化学工業株式会社 銅もしくは銅合金材の着色方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812715A (zh) * 2010-03-24 2010-08-25 西安北方光电有限公司 一种钛合金黑色阳极氧化工艺
CN101812715B (zh) * 2010-03-24 2011-12-07 西安北方光电有限公司 一种钛合金黑色阳极氧化工艺

Also Published As

Publication number Publication date
CA2190419C (en) 2000-11-07
EP0780495A2 (de) 1997-06-25
US5714052A (en) 1998-02-03
CA2190419A1 (en) 1997-06-23
ES2156248T3 (es) 2001-06-16
GR3036263T3 (en) 2001-10-31
DE19548261A1 (de) 1997-06-26
PT780495E (pt) 2001-09-27
EP0780495A3 (de) 1997-08-27
DK0780495T3 (da) 2001-06-11
DE59606874D1 (de) 2001-06-13
ATE201059T1 (de) 2001-05-15

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