EP0751233B2 - Bande ou plaque en cuivre pourvue d'un revêtement brun et procédé de fabrication - Google Patents

Bande ou plaque en cuivre pourvue d'un revêtement brun et procédé de fabrication Download PDF

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Publication number
EP0751233B2
EP0751233B2 EP96109446A EP96109446A EP0751233B2 EP 0751233 B2 EP0751233 B2 EP 0751233B2 EP 96109446 A EP96109446 A EP 96109446A EP 96109446 A EP96109446 A EP 96109446A EP 0751233 B2 EP0751233 B2 EP 0751233B2
Authority
EP
European Patent Office
Prior art keywords
copper
layer
semi
strip
finished product
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
EP96109446A
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German (de)
English (en)
Other versions
EP0751233A1 (fr
EP0751233B1 (fr
Inventor
Christian Dipl.-Ing. Triquet
Wolfgang Denke
Stefan Dipl.-Ing. Hoveling
Stefan Dr. Priggemeyer
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.)
KM Europa Metal AG
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
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Application filed by KM Europa Metal AG filed Critical KM Europa Metal AG
Publication of EP0751233A1 publication Critical patent/EP0751233A1/fr
Publication of EP0751233B1 publication Critical patent/EP0751233B1/fr
Application granted granted Critical
Publication of EP0751233B2 publication Critical patent/EP0751233B2/fr
Anticipated expiration legal-status Critical
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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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the invention relates on the one hand to a copper strip or sheet with a reddish brown to dark brown Covering layer for use in the construction sector.
  • the invention is to preferred methods for Production of a brown cover layer on copper existing strip-shaped semifinished product, in particular on rolled strips and sheets for the roof covering and facade cladding, addressed.
  • the formation of the brown topcoat can be but under certain atmospheric conditions considerably delay but also speed up so that, as a rule, it takes a relatively long time to wait until a uniform discoloration of the copper surface is reached. Deviations from a uniform Coloring are especially in the initial stages to watch the weathering. On the copper surface often form unevenly at first dark spots and / or streaks. In the further course the weathering by atmospheric influences however, these color differences are becoming noticeable.
  • a process for producing uniform Layers of copper (I) oxide on the surface of Copper wire or tape is for example in Chemical Abstracts, Vol. 83, No. 2, July 1975, page 258, abstract No. 32184t mentioned.
  • this known Process is the copper oxide layer by an oxidizing Heat treatment at a temperature range formed from 300 to 1000 ° C lying temperature.
  • From US-PS 5,282,890 is a method for producing a brown Covering known on a copper strip or sheet, in which by a heat treatment with the treatment parameters ⁇ Treatment temperature 150 ° C to 650 ° C and treatment time 0.1 to 30 Minutes, especially at a treatment temperature between 150 ° C and 350 ° C, preferably about 275 ° C, and a gas atmosphere with a Oxygen content of about 25 vol.% In the treatment furnace and a Treatment time between 0.1 and 30 minutes a dark brown layer is produced from copper oxides on a copper strip.
  • the invention is based on the object, on the one hand a copper strip or sheet of the aforementioned To provide kind on the surface a uniform and firm brown cover layer (Brown patina) and that at reduced Solubility of copper ions easy to handle and is to be processed.
  • the invention is based on the object Method for producing a brown cover layer on copper existing band-shaped To create semi-finished products.
  • the two-layer covering layer consists of a first layer of Cu 2 O adhering to the base metal with a thickness lying in the range of 0.05 to 5 ⁇ m, preferably in the range of 0.1 to 1 ⁇ m, and a second layer of CuO arranged above it Thickness between 1 and 100 nm, preferably with a thickness between 10 and 50 nm.
  • Procedure prepared prepatinated Strips or sheets of copper have cover layers, which both have excellent adhesive strength as well as deformation or bending during bending stay, d. H. show no detachment. Even when installing roofing and cladding often inevitable finger marks remain largely on the pre-patinated surface unremarkable.
  • the improved adhesion of the cover layer and the even more uniform browning of the prepatinized copper surface can be achieved both by carrying out a second heat treatment under oxidizing conditions to form a CuO layer immediately after the first heat treatment under a mixed gas atmosphere containing defined oxygen.
  • the Cu 2 O intermediate layer serves as a bonding agent for the CuO layer.
  • the Cu 2 O layer protects the copper sheet from local corrosion, while the CuO layer is responsible for reducing surface corrosion (copper ion solubility) from acid rainwater or other media aggressive to copper.
  • a chemical also performs Post-oxidation with an aqueous solution of a alkaline salt alone or in combination with a salt of the inorganic peroxide, organic peroxides and hydrochloric acid Group to the same result.
  • a cold rolled and optionally degreased strip of SF copper according to DIN 1787 with a thickness of 0.6 mm and a width of 100 mm (sample 1) was roughened uniformly by means of a rough work roll. The average roughness of the surface of the copper strip was 5 ⁇ m.
  • the copper strip was then fed to a laboratory furnace for heat treatment, the operating temperature of which was set at about 480 ° C.
  • a controlled gas atmosphere of nitrogen with 2 vol.% Oxygen content was set in the furnace chamber and the copper strip was held for 5 minutes under these conditions.
  • the sample 1 was cooled to room temperature in a cooling chamber under inert gas, for example, argon.
  • the heat-treated copper tape showed a regular red about 1 micron thick Cu 2 O oxide layer whose crystals had a mean grain size of 0.05 microns.
  • the sample 1 was subjected to a second heat treatment at a temperature of 300 ° C. in a mixed gas atmosphere having a higher oxygen content than in the first heat treatment, for example, atmospheric air.
  • a second heat treatment a thin dark brown CuO oxide layer having a thickness of about 0.05 ⁇ m (50 nm) grew on the surface of the Cu 2 O intermediate layer.
  • CuO layers on copper surfaces are black and consist of tenorite crystals.
  • the color values of the two oxide layers add up to the desired reddish brown to dark brown cover layer.
  • the thickness of the Cu 2 O intermediate layer is below 0.05 ⁇ m, the proportion of the red color is too small to obtain a dark brown color of the cover layer together with the CuO layer.
  • the thickness of the Cu 2 O intermediate layer copper oxide
  • the adhesion of this intermediate layer is disadvantageously reduced and the deformability of the layer is no longer guaranteed.
  • the best properties in terms of color, adhesion and deformability in the thickness range of the intermediate layer from 0.2 to 0.7 .mu.m.
  • sample 2 a copper plate referred to as sample 2 after the first Heat treatment cold worked by 20% and then a second 10 minute heat treatment at 350 ° C to produce a thin dark brown Subjected to CuO layer.
  • a copper sheet designated sample 3 was first subjected to a heat treatment for 1.5 minutes at 550 ° C. to form the Cu 2 O intermediate layer and then to form a thin CuO layer at 350 ° C. under oxidizing conditions subjected. After these two heat treatments, sample 3 was cold worked about 10% to increase strength.
  • a cold-rolled strip of SF-Cu (hard-rolled state) according to DIN 1787 with a thickness of 0.63 mm and a width of 1000 mm was subjected to recrystallization annealing with simultaneous surface oxidation in a continuous furnace.
  • the heat treatment took place above the recrystallization temperature of the copper strip in a controlled gas atmosphere with about 5% oxygen.
  • the copper strip was passed through an oxidizing bath heated to about 70 ° C., which consists of a mixture of about 40 g / l of sodium hydroxide solution and about 20 g / l of potassium peroxodisulfate. Subsequently, the copper tape was rinsed with water and dried with hot air.
  • the residence times of the copper strip in the continuous furnace and in the chemical oxidation bath can be determined by the time required for soft annealing.
  • the copper strip had a uniform, reddish brown to dark brown top layer after these treatment steps.
  • the thickness of the Cu 2 O layer was determined to be 0.7 ⁇ m, while the thickness of the CuO layer was about 0.05 ⁇ m.
  • the copper strip then rolled semi-hard. Neither here even with additional bending or bending operations showed damage or detachment the topcoat.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Laminated Bodies (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemically Coating (AREA)

Claims (13)

  1. Ruban ou tôle de cuivre avec une couche de recouvrement brun rouge à brun foncé pour utilisation dans le domaine de la construction,
    caractérisé en ce que
    la couche de recouvrement se compose d'une première couche de Cu2O adhérant au métal de base avec une épaisseur se situant dans l'intervalle de 0,05 à 5 µm, de préférence dans l'intervalle de 0,1 à 1 µm et d'une deuxième couche de CuO appliquée sur la première avec une épaisseur comprise entre 1 et 100 nm, de préférence avec une épaisseur comprise entre 10 et 50 nm.
  2. Ruban ou tôle de cuivre selon la revendication 1,
    caractérisé en ce que
    les cristaux de Cu2O ont une grandeur de grain se situant dans la zone de 0,005 à 0,5 µm, de préférence une grandeur de grain moyenne d'environ 0,05 µm.
  3. Procédé de fabrication d'une couche de recouvrement brune sur un produit semi-fini en forme de ruban se composant de cuivre, en particulier des rubans ou tôles laminés pour la couverture d'un toit et le revêtement de façades,
    caractérisé par
    la combinaison des étapes de procédé suivantes :
    le produit semi-fini en cuivre en forme de ruban est soumis à une température se situant dans le domaine de 250 à 750°C pendant une durée de 0,1 à 5 minutes dans une atmosphère gazeuse mixte contenant jusqu'à 15 % en volume d'oxygène, lors d'un premier traitement thermique pour former une couche de Cu2O ;
    suite au premier traitement thermique selon la phase de procédé a) le semi-produit en cuivre en forme de ruban est soumis à un deuxième traitement thermique dans des conditions oxydantes pour la formation d'une couche de CuO, le deuxième traitement thermique étant réalisé pendant une durée de 1 à 30 minutes dans l'intervalle de températures de 200 à 450°C et l'atmosphère gazeuse mixte ayant une teneur en oxygène comprise entre 10 et 21 % en volume.
  4. Procédé selon la revendication 3,
    caractérisé en ce que
    le traitement thermique selon l'étape de procédé a) s'effectue à une température comprise entre 450 et 600°C.
  5. Procédé selon la revendication 3 ou 4,
    caractérisé en ce que
    la teneur en oxygène de l'atmosphère gazeuse mixte selon l'étape de procédé a) est de 3 à 10 % en volume.
  6. Procédé de fabrication d'une couche de recouvrement brune sur un produit semi-fini en forme de ruban composé de cuivre, en particulier des rubans ou tôles laminés pour la couverture d'un toit et le revêtement de façades,
    caractérisé par
    la combinaison des étapes de procédé suivantes :
    on traite thermiquement le produit semi-fini de cuivre en forme de ruban à une température se situant dans l'intervalle de températures de 450 à 600°C pendant une durée de 0,1 à 5 minutes dans une atmosphère gazeuse mixte contenant de l'oxygène, dont la teneur en oxygène est de 3 à 10 % en volume;
    suite au traitement thermique selon l'étape de procédé c), le produit semi-fini en forme de ruban est traité avec une solution aqueuse de sel à réaction alcaline en association avec au moins un sel du groupe comprenant les peroxydes inorganiques, la solution de traitement aqueuse présentant un pH supérieur à 8 et une température de 30 à 90°C et le traitement s'effectuant dans un intervalle de temps compris entre 15 et 120 secondes.
  7. Procédé selon l'une quelconque des revendications 3 à 6,
    caractérisé en ce qu'
    au moins une surface du produit semi-fini en forme de ruban est structurée avant l'étape de procédé a) ou c) au moyen de cylindres texturés.
  8. Procédé selon la revendication 6, caractérisé en ce que le pH de la solution de traitement se situe entre 10 et 14.
  9. Procédé selon au moins l'une des revendications 6 à 8, caractérisé en ce que le produit semi-fini en forme de ruban est en plus traité par voie électrolytique dans la solution aqueuse, le produit semi-fini étant raccordé comme anode.
  10. Procédé selon la revendication 9, caractérisé en ce que par l'anode, un courant électrique s'écoule avec une densité de courant de 1 à 20 A/dm2.
  11. Procédé selon l'une quelconque des revendications 3 à 8, caractérisé en ce que le produit semi-fini en forme de ruban selon l'étape de procédé a) ou c) et/ou selon l'étape de procédé b) ou d) est soumis à une déformation mécanique allant jusqu'à 40 %.
  12. Procédé selon la revendication 11, caractérisé en ce que la déformation se monte à 5 jusqu'à 7 %.
  13. Procédé selon la revendication 11 ou 12, caractérisé en ce que la déformation est réalisée au moyen de cylindre de travail texturé.
EP96109446A 1995-06-29 1996-06-13 Bande ou plaque en cuivre pourvue d'un revêtement brun et procédé de fabrication Expired - Lifetime EP0751233B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19523646A DE19523646A1 (de) 1995-06-29 1995-06-29 Kupferband oder -blech mit brauner Deckschicht und Verfahren zu seiner Herstellung
DE19523646 1995-06-29

Publications (3)

Publication Number Publication Date
EP0751233A1 EP0751233A1 (fr) 1997-01-02
EP0751233B1 EP0751233B1 (fr) 1999-01-07
EP0751233B2 true EP0751233B2 (fr) 2005-12-07

Family

ID=7765548

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96109446A Expired - Lifetime EP0751233B2 (fr) 1995-06-29 1996-06-13 Bande ou plaque en cuivre pourvue d'un revêtement brun et procédé de fabrication

Country Status (8)

Country Link
US (1) US5962116A (fr)
EP (1) EP0751233B2 (fr)
AT (1) ATE175450T1 (fr)
CA (1) CA2179097C (fr)
DE (2) DE19523646A1 (fr)
DK (1) DK0751233T4 (fr)
ES (1) ES2128810T5 (fr)
GR (1) GR3029669T3 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013101696A1 (de) 2013-02-20 2014-08-21 Von Ardenne Anlagentechnik Gmbh Verfahren zum Bearbeiten eines thermisch leitfähigen Werkstücks, Kühlanordnung und Vakuumanordnung
US9988713B2 (en) * 2013-03-12 2018-06-05 Arizona Board Of Regents On Behalf Of Arizona State University Thin film devices and methods for preparing thin film devices
DE102014010711B4 (de) * 2014-07-19 2019-08-29 Wieland-Werke Ag Verfahren zur Glühbehandlung von zinkhaltigen Kupferlegierungsbändern

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3152927A (en) † 1960-02-11 1964-10-13 Svenska Metallverken Ab Method for applying green patina to objects, preferably made from copper or copper alloys

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB309966A (en) * 1927-12-14 1929-04-15 Hanovia Chemical & Mfg Co Improvements in and relating to processes for the production of crystalline cuprous oxide upon copper surfaces
US3398028A (en) * 1965-03-31 1968-08-20 Olin Mathieson Process of forming a red, cuprous oxide coating on copper
US3434889A (en) * 1965-12-27 1969-03-25 Budd Co Copper foil surface treatment
JPS5841349B2 (ja) * 1976-10-08 1983-09-12 古河電気工業株式会社 熱伝導性に優れた低温用導電材料の製造方法
US4189331A (en) * 1978-06-22 1980-02-19 Canada Wire And Cable Limited Oxidation resistant barrier coated copper based substrate and method for producing the same
SE8303976L (sv) * 1983-10-05 1985-04-06 Thermacore Ab Patineringsforfarande
JPH03260074A (ja) * 1990-03-12 1991-11-20 Mitsubishi Electric Corp 銅系金属材料の製造方法
DE4034249A1 (de) * 1990-10-27 1992-04-30 Kabelmetal Ag Verfahren zur herstellung von braunen deckschichten auf kupfer
DE69112181T2 (de) * 1990-11-30 1996-05-09 Toppan Printing Co Ltd Verfahren zur Herstellung einer Mehrschichtverdrahtungsplatine.
JPH05222471A (ja) * 1991-12-16 1993-08-31 Toshiba Corp 装飾用銅鉄合金

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3152927A (en) † 1960-02-11 1964-10-13 Svenska Metallverken Ab Method for applying green patina to objects, preferably made from copper or copper alloys

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Journal of the Institute of Metals, October 1960, p. 65-70, Rönnquist et al †

Also Published As

Publication number Publication date
ATE175450T1 (de) 1999-01-15
CA2179097C (fr) 2001-01-23
EP0751233A1 (fr) 1997-01-02
EP0751233B1 (fr) 1999-01-07
ES2128810T3 (es) 1999-05-16
DK0751233T4 (da) 2006-04-18
CA2179097A1 (fr) 1996-12-30
DE59601100D1 (de) 1999-02-18
US5962116A (en) 1999-10-05
DE19523646A1 (de) 1997-01-02
GR3029669T3 (en) 1999-06-30
ES2128810T5 (es) 2006-06-16
DK0751233T3 (da) 1999-08-30

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