EP1685273B1 - Methode zur patinierung von kupfer - Google Patents

Methode zur patinierung von kupfer Download PDF

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Publication number
EP1685273B1
EP1685273B1 EP04797943A EP04797943A EP1685273B1 EP 1685273 B1 EP1685273 B1 EP 1685273B1 EP 04797943 A EP04797943 A EP 04797943A EP 04797943 A EP04797943 A EP 04797943A EP 1685273 B1 EP1685273 B1 EP 1685273B1
Authority
EP
European Patent Office
Prior art keywords
copper
article
weight
temperature
patination
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
EP04797943A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1685273A1 (de
Inventor
Jürgen LEUCHTE
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.)
Cunova GmbH
Original Assignee
KME Germany GmbH and Co KG
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 KME Germany GmbH and Co KG filed Critical KME Germany GmbH and Co KG
Priority to SI200431789T priority Critical patent/SI1685273T1/sl
Priority to PL04797943T priority patent/PL1685273T3/pl
Publication of EP1685273A1 publication Critical patent/EP1685273A1/de
Application granted granted Critical
Publication of EP1685273B1 publication Critical patent/EP1685273B1/de
Priority to CY20111101159T priority patent/CY1112119T1/el
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • C23C22/63—Treatment of copper or alloys based thereon
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • C23C22/77—Controlling or regulating of the coating process
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment

Definitions

  • the invention relates to a method for producing a patina on objects made of copper or copper alloys.
  • the US-3,497,401-A a method and a reaction solution for producing a patina.
  • a copper part is immersed in an acidic, aqueous solution containing potassium chlorate and copper sulfate.
  • the US-5,160,381-A describes the generation of a patina on a copper article
  • the copper to be patinated part is treated after cleaning with an aqueous solution containing copper, sodium, acetate, chlorine, sulfate, H + and OH - contains ions.
  • the copper piece is treated in a second operation with an aqueous solution of copper carbonate, ammonium chloride, copper acetate, arsenic trioxide, copper nitrate and hydrochloric acid.
  • the EP 0 943 701 A1 is concerned with the generation a patina, again by treatment of a copper object with an aqueous copper salt solution. This method is particularly suitable for pre-oxidized copper surfaces.
  • the EP 0 492 566 and the GB 697294 also have methods for producing an artificial patina to the content. According to these, an aqueous solution of copper salts is applied to the surface of a copper or copper alloy article. The treated objects are then removed at a defined temperature and humidity.
  • JP 08 120 460 discloses a similar process with a zinc containing patination solution.
  • an article of copper or a copper alloy is passed through an oxidizing copper salt solution.
  • the article thus treated is then moistened and aftertreated with a gaseous oxidizing agent.
  • the object of the invention is to provide a method which avoids the disadvantages of the prior art and solves as many of the described problems as possible.
  • articles made of copper or of a copper alloy are treated with a preferably aqueous patination solution containing copper ions and subsequently subjected to a so-called ripening process.
  • the ripening process involves individual ripening steps that include a choice of humidities and temperatures.
  • the setting and control of the two parameters temperature and humidity is well feasible especially in a designated climate chamber.
  • the ripening process includes the following ripening steps: After the article has been treated with the patination solution, in particular the application of the patinating solution to the object to be patinated, the article is allowed to rest for a first resting period at a first resting temperature and a first resting air humidity. This is followed by at least a one-time watering of the article at a watering temperature and a watering humidity over a washing period, followed by rest again at a second rest temperature and a second rest air humidity over a second rest period.
  • the temperature is in particular in the climatic chamber between 20 ° C and 70 ° C, in particular between 25 ° C and 55 ° C (first resting temperature).
  • the humidity is in the range between 30% and 90%, in particular between 40% and 50% (first resting air humidity). In essence, these preferred ranges for temperature and humidity given for the first rest phase also correspond to the preferred ranges for the second rest temperature and the second rest air humidity.
  • the temperature in the climatic chamber between 20 ° C and 70 ° C, in particular between 25 ° C and 55 ° C.
  • the humidity is maintained in the range between 30% to 95% during the washing process, in particular in the range between 65% to 80%.
  • the watering is done by spraying the treated article with water. This process is preferably repeated four to five times at a distance of 90 minutes to 2 hours.
  • the first rest period is up to one week, but a period of two to three days is preferred. The same applies to the second rest period.
  • the washing time is not more than one day, but preferably only 5 hours to 10 hours.
  • the patination solution used is a copper ion-containing solution, the preferred composition of which is discussed below. It should further be emphasized that it is particularly preferred if the object to be patinated is cleaned before the application of the patination solution and / or its surface is roughened. Any existing grease or oil residues or other impurities on the surface can adversely affect the adhesion of the resulting patina. This is encountered in particular by chemical degreasing and / or blasting of the surface to be patinated with broken glass spheres. Alternatively, for example, an eccentric grinder or a belt sander can be used.
  • the object to be patinated is, optionally after a described optional pre-treatment, subjected to the ripening process, preferably transferred to the already mentioned climatic chamber. It is not mandatory, but preferred, that the application of the Patinierttes takes place in the chamber.
  • the patination solution is preferably applied in finely divided form, particularly preferably sprayed on.
  • the temperature (preferably in the climatic chamber) is preferably between 30 ° C and 70 ° C, in particular it is between 40 ° C and 55 ° C.
  • the application of the Patinierains takes place in at least two, preferably in four to five treatment steps, in particular at intervals of about 1 hour.
  • a further treatment of the freshly patinated surface can be carried out. It is possible to either lighten or darken the surface. If appropriate, the surface can also be sealed, since the patina unsealed under certain circumstances may continue to react under natural weather conditions.
  • the described method is preferably provided for the patination of panel, strip or shingle material made of copper.
  • it is applicable in principle to all moldings or articles made of copper or copper alloys.
  • Supplementpatinierept of moldings such. B. gutters are possible. So z. B. in gutters of the bead area are heavily patinated, while only oxidized the outside of the watercourse. This gives the visual impression that the piece of copper has been exposed to atmospheric influences for years and decades. Such effects are common in the optical Design of new buildings, but especially in the restoration or repair of older, listed buildings used to preserve the historic overall impression.
  • the patina produced by the process of the present invention has good resistance to mechanical stress and excellent adhesive properties.
  • Patinierionat which is also an object of this invention. It consists of an aqueous solution in which a copper salt, preferably copper nitrate, in a proportion of up to 20 wt .-%, in particular in a proportion of 3 wt .-% to 5 wt .-%, is included.
  • the solution additionally contains a zinc salt, in particular zinc chloride, preferably in a proportion of 0.1% by weight to 5% by weight, in particular in a proportion of 0.2% by weight to 1% by weight. %.
  • the solution may contain various chloride and carbonate additives, including in particular sodium chloride, ammonium chloride, calcium chloride and ammonium carbonate.
  • the pH of the patination solution is preferably in the basic, in particular in the slightly basic range at pH 7-10.
  • the proportion of zinc salt is particularly noteworthy. Surprisingly, it has been found that the zinc salt addition has a positive effect on the adhesive properties of the resulting patina. In addition, such an addition causes a visual whitening in the green.
  • the patina usually has a layer thickness of 0.02 mm to 0.06 mm, in particular from 0.03 mm to 0.05 mm.
  • the climate chamber has a floor space of approx. 3 x 2.5 m.
  • a copper sheet the surface of which has been thoroughly sanded with an orbital sander and is free of grease and other contaminants, is placed in the climatic chamber.
  • the temperature in the climate chamber is set to 50 ° C.
  • the Patinierates is sprayed four times at intervals of one hour four times on the surface of the copper piece.
  • the temperature is maintained at about 45 ° C.
  • the humidity is regulated to about 45%.
  • a repeated watering of the treated copper part follows. A total of five times it is sprayed with water at intervals of 90 minutes.
  • the humidity in the climatic chamber is about 75% during this period, the temperature is about 50 ° C as with the treatment with patinating solution. Subsequently If the humidity and temperature are lowered again to 45% and 45 ° C, respectively, the copper sheet is allowed to rest for 3 more days. This completes the patination. The copper sheet is completely evenly covered by the artificial protective layer.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Physical Vapour Deposition (AREA)
  • Paints Or Removers (AREA)
  • Chemically Coating (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
EP04797943A 2003-11-17 2004-11-17 Methode zur patinierung von kupfer Expired - Lifetime EP1685273B1 (de)

Priority Applications (3)

Application Number Priority Date Filing Date Title
SI200431789T SI1685273T1 (sl) 2003-11-17 2004-11-17 Postopek za patiniranje bakra
PL04797943T PL1685273T3 (pl) 2003-11-17 2004-11-17 Sposób patynowania miedzi
CY20111101159T CY1112119T1 (el) 2003-11-17 2011-11-25 Μεθοδος για πατιναρισμα χαλκου

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10354527A DE10354527B4 (de) 2003-11-17 2003-11-17 Verfahren zur Patinierung von Kupfer
PCT/EP2004/013009 WO2005049889A1 (de) 2003-11-17 2004-11-17 Patinierung von kupfer

Publications (2)

Publication Number Publication Date
EP1685273A1 EP1685273A1 (de) 2006-08-02
EP1685273B1 true EP1685273B1 (de) 2011-10-05

Family

ID=34609209

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04797943A Expired - Lifetime EP1685273B1 (de) 2003-11-17 2004-11-17 Methode zur patinierung von kupfer

Country Status (17)

Country Link
US (1) US20070079906A1 (pl)
EP (1) EP1685273B1 (pl)
JP (1) JP2007511668A (pl)
KR (1) KR20060107784A (pl)
CN (1) CN1906328A (pl)
AT (1) ATE527396T1 (pl)
AU (1) AU2004291674B2 (pl)
BR (1) BRPI0416664A (pl)
CA (1) CA2548291C (pl)
CY (1) CY1112119T1 (pl)
DE (1) DE10354527B4 (pl)
DK (1) DK1685273T3 (pl)
ES (1) ES2374817T3 (pl)
PL (1) PL1685273T3 (pl)
PT (1) PT1685273E (pl)
SI (1) SI1685273T1 (pl)
WO (1) WO2005049889A1 (pl)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100890607B1 (ko) * 2007-07-02 2009-03-27 김부현 산화 녹청 동판의 제조방법
KR101143687B1 (ko) * 2011-12-07 2012-05-09 김부현 산화 녹청 동판 및 그 제조방법
US10119038B2 (en) 2015-05-08 2018-11-06 PatinaNow, LLC Patina solution, method for producing patina on object, and patina kit
JP6354814B2 (ja) 2016-09-30 2018-07-11 ダイキン工業株式会社 配管の製造方法及び銅管内面の酸化皮膜形成方法
JP6421892B1 (ja) * 2017-10-26 2018-11-14 住友化学株式会社 熱可塑性樹脂組成物

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB697294A (en) * 1950-09-05 1953-09-16 Ici Ltd Improvements in or relating to the colouring of copper and its alloys
US3497401A (en) * 1967-09-20 1970-02-24 Intern Copper Research Ass Inc Patination of copper
US3669766A (en) * 1969-11-28 1972-06-13 Mitsunosuke Fukawa Formation of coating on copper containing materials
US3725138A (en) * 1971-03-15 1973-04-03 Anaconda American Brass Co Production of synthetic patina
JPS52110235A (en) * 1976-03-03 1977-09-16 Nippon Paint Co Ltd Industrial process for forming patina
JPH06102837B2 (ja) * 1990-02-14 1994-12-14 日鉱金属株式会社 緑青の形成方法
DE4041854A1 (de) * 1990-12-24 1992-06-25 Kabelmetal Ag Verfahren zur herstellung einer gruenen patina auf aus kupfer bestehendem halbzeug
JPH04329884A (ja) * 1991-05-02 1992-11-18 Kanebo Ltd 人工緑青液
US5160381A (en) * 1991-06-26 1992-11-03 Fumigation Maritime Ltee Method for forming artificially and rapidly patina on copper, products thereof and solutions therefor
JPH0718485A (ja) * 1993-07-01 1995-01-20 Furukawa Electric Co Ltd:The 緑青を形成した材料及びその製造方法
JP2640432B2 (ja) * 1994-10-20 1997-08-13 三井金属鉱業株式会社 人工緑青用化成液および人工緑青処理方法
JP2920610B2 (ja) * 1995-08-31 1999-07-19 元旦ビューティ工業株式会社 緑青皮膜の形成方法及び形成装置
DE19809904A1 (de) * 1998-03-07 1999-09-09 Km Europa Metal Ag Verfahren und Reaktionslösung zur Erzeugung einer Patina
JP3696139B2 (ja) * 2001-09-14 2005-09-14 元旦ビューティ工業株式会社 緑青発色組成液及び緑青形成方法

Also Published As

Publication number Publication date
KR20060107784A (ko) 2006-10-16
DE10354527A1 (de) 2005-06-23
AU2004291674A1 (en) 2005-06-02
US20070079906A1 (en) 2007-04-12
JP2007511668A (ja) 2007-05-10
CY1112119T1 (el) 2015-11-04
DE10354527B4 (de) 2008-08-28
ES2374817T3 (es) 2012-02-22
PL1685273T3 (pl) 2012-03-30
CA2548291C (en) 2012-03-13
CN1906328A (zh) 2007-01-31
DK1685273T3 (da) 2012-01-16
EP1685273A1 (de) 2006-08-02
CA2548291A1 (en) 2005-06-02
SI1685273T1 (sl) 2012-01-31
PT1685273E (pt) 2011-11-03
ATE527396T1 (de) 2011-10-15
BRPI0416664A (pt) 2007-01-16
AU2004291674B2 (en) 2009-08-27
WO2005049889A1 (de) 2005-06-02

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