EP0752484A1 - Elektrolytisches Verfahren zur Beschichtung eines Metallelements mit Messung - Google Patents

Elektrolytisches Verfahren zur Beschichtung eines Metallelements mit Messung Download PDF

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Publication number
EP0752484A1
EP0752484A1 EP96201786A EP96201786A EP0752484A1 EP 0752484 A1 EP0752484 A1 EP 0752484A1 EP 96201786 A EP96201786 A EP 96201786A EP 96201786 A EP96201786 A EP 96201786A EP 0752484 A1 EP0752484 A1 EP 0752484A1
Authority
EP
European Patent Office
Prior art keywords
brass
layer
zinc
copper
bath
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.)
Granted
Application number
EP96201786A
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English (en)
French (fr)
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EP0752484B1 (de
Inventor
Federico Pavan
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.)
Pirelli Tyre SpA
Original Assignee
Pirelli Coordinamento Pneumatici SpA
Pirelli SpA
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Application filed by Pirelli Coordinamento Pneumatici SpA, Pirelli SpA filed Critical Pirelli Coordinamento Pneumatici SpA
Priority to SI9630096T priority Critical patent/SI0752484T1/xx
Publication of EP0752484A1 publication Critical patent/EP0752484A1/de
Application granted granted Critical
Publication of EP0752484B1 publication Critical patent/EP0752484B1/de
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    • D—TEXTILES; PAPER
    • D07—ROPES; CABLES OTHER THAN ELECTRIC
    • D07B—ROPES OR CABLES IN GENERAL
    • D07B1/00—Constructional features of ropes or cables
    • D07B1/06—Ropes or cables built-up from metal wires, e.g. of section wires around a hemp core
    • D07B1/0606—Reinforcing cords for rubber or plastic articles
    • D07B1/0666—Reinforcing cords for rubber or plastic articles the wires being characterised by an anti-corrosive or adhesion promoting coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
    • D—TEXTILES; PAPER
    • D07—ROPES; CABLES OTHER THAN ELECTRIC
    • D07B—ROPES OR CABLES IN GENERAL
    • D07B2205/00—Rope or cable materials
    • D07B2205/30—Inorganic materials
    • D07B2205/3021—Metals
    • D07B2205/3085—Alloys, i.e. non ferrous
    • D07B2205/3089—Brass, i.e. copper (Cu) and zinc (Zn) alloys

Definitions

  • the present invention relates to an electrolytic process for coating a metal element with a layer of brass, the metal element thus coated and the use of some metal elements thus coated in reinforcing structures of articles made of vulcanized elastomeric material.
  • the present invention relates to the electrolytic codeposition of a layer of copper and zinc on a metal element such as, for example, a steel wire.
  • steel that is the preferred material due to its mechanical properties, has the disadvantage of not adhering sufficiently to the vulcanized elastomeric material.
  • the steel In order to obtain a good adhesion to the elastomeric material the steel is therefore usually coated with a layer of a suitable material.
  • the preferred coating material is brass.
  • adhesion is enhanced by the formation, during the vulcanizing process, of disulfide bridges (-S-S-) between the elastomeric matrix and the copper that coats, as a component of brass, the reinforcing metal element.
  • the brass layer on the metal element must be as compact and homogeneous as possible both to ensure a uniform formation of disulfide bridges, and thus a uniform adhesion of the elastomeric matrix to the reinforcing metal structure, and to prevent the triggering of corrosive reactions in the possible areas of the reinforcing metal structure that are not sufficiently coated.
  • the codeposition processes are characterized by the electrolytic codeposition of copper and zinc.
  • a second way by which attempts have been made to replace the cyanide process are that of the diffusion processes. These methods comprise the electrodeposition of one or two layers of copper on steel, followed by the electrodeposition of a layer of zinc and by a heat treatment whose purpose is to diffuse zinc in the layers of copper, thus forming a layer of brass.
  • a first drawback is that each electrodeposition step requires its own tank and this involves a costly and bulky plant.
  • a second drawback is that this process requires a careful selection and control of several parameters in a plurality of tanks.
  • a third drawback is the cost of the energy required in the heat treatment that causes the diffusion.
  • a fourth drawback is that the heat treatment causes some worsenings in the mechanical properties of steel; in particular the ultimate tensile strength shows a reduction of some 5 percent.
  • a second object of the present invention is to provide a metal element coated with a brass layer that, while not having been deposited with the cyanide process, has properties at least equal to those of a similar metal element that has been coated with brass according to the cyanide process.
  • a third object of the present invention is to provide an article of manufacture comprising a reinforcing metal element embedded in a vulcanized elastomeric matrix wherein said reinforcing element consists of at least a steel wire coated with a layer of brass that, while not having been deposited with the cyanide process, has properties at least equal to those of a similar wire that has been coated with brass according to the cyanide process.
  • the expression "metal element” means any metal article that can be coated with a layer of brass by an electrolytic method such as, for example, articles for bathroom, sanitary and electrical use, door and window frames and articles for personal use. Specific examples of such articles are: taps, handles, small metal items, chandeliers, spectacle frames and the like.
  • the metal element consists of iron and alloys thereof, aluminium and zinc.
  • the metal element consists of a steel wire having a carbon content of from 0.6 to 0.95%.
  • said steel wire is suitable for being corded into cords and forming internal reinforcing structures for articles made of vulcanized elastomeric material such as tires, conveyor belts, transmission belts and flexible pipes of natural or synthetic rubber or mixtures thereof.
  • brass means a metal composition, as homogeneous as possible, consisting of from 10% to 50% by weight of zinc and from 90% to 50% by weight of copper, preferably from 20% to 40% by weight of zinc and from 80% to 60% by weight of copper and, even more preferably, from 30% to 40% by weight of zinc and from 70% to 60% by weight of copper.
  • cord means a cord obtained by cording, according to conventional techniques, of steel wires coated with a layer of brass that, before drawing, is from 1 to 3 microns thick while, after drawing, it is from 0.1 to 0.4 microns thick.
  • the diameter of said wires is about 1-3 mm before drawing and 0.1-0.5 mm after drawing.
  • a cord commonly used in reinforcing structures of giant radial tires consists of 7 strands, each of 4 wires with a diameter of about 0.175 mm, round which a wire is wound, known as wrapper, having a diameter of 0.15 mm.
  • cathodic efficiency means the percent ratio between the amount of metal actually deposited and the theoretical amount of metal that should have been deposited according to the Faraday's rule.
  • the present invention relates to a process of electrolytic codeposition of copper and zinc on a metal element wherein the electrolytic bath consists of an aqueous solution of at least a bivalent copper salt, at least a zinc salt and an alkali pyrophosphate, characterized in that
  • a preferred meaning of Y is NR 3 .
  • R 1 , R 2 and R 3 are hydrogen, methyl and ethyl.
  • amino acid compound of formula (I) is histidine hydrochloride.
  • the deposit of brass obtained with the process of the present invention is characterized by a substantially constant content of copper and of zinc throughout the depth of the deposit.
  • said article of manufacture is a vehicle tire, a transmission belt, a belt for a conveyor or a pipe.
  • Fig. 4 shows a cord made of metal wires of the present invention embedded in a vulcanized elastomeric matrix.
  • Fig. 5 shows a cross-sectional view of a tire reinforced with cords made of metal wires of the present invention.
  • Fig. 6 shows a cross-sectional perspective view of a conveyor belt reinforced with cords made of metal wires of the present invention.
  • Fig. 7 shows a cross-sectional perspective view of a transmission belt reinforced with cords made of metal wires of the present invention.
  • Fig. 8 shows a cross-sectional perspective view of a flexible pipe reinforced with cords made of metal wires of the present invention.
  • the metal element Before being dipped in the galvanic bath to be coated with a layer of brass according to the process of electrolytic codeposition of the present invention, the metal element is pickled according to conventional techniques, to remove any possible surface layer of oxides.
  • the galvanic bath of the present invention is characterized by:
  • Suitable copper salts are hydrate or anhydrous cupric sulfate.
  • Suitable zinc salts are hydrate or anhydrous zinc sulfate.
  • Typical examples of an alkali pyrophosphate are sodium and potassium pyrophosphate.
  • a typical example of an amino acid compound is histidine, preferably in the form of an acid addition salt such as, for example, hydrochloride.
  • the density of cathodic current is of from 2 to 40 A/dm 2 .
  • it is of from 10 to 40 A/dm 2 , even more preferably it is of from 20 to 30 A/dm 2 .
  • a galvanic bath for depositing a brass layer comprising from 60% to 70% of copper and from 40% to 30% of zinc has the following composition: mols/litre Cu ++ 0.18 - 0.26 Zn ++ 0.087 - 0.14 alkali pyrophosphate 0.9 - 1.09 amino acid compound 0.09 - 0.011
  • Suitable materials to prepare the abovementioned bath are: grams/litre cupric sulfate pentahydrate 45 - 65 zinc sulfate heptahydrate 25 - 40 potassium pyrophosphate 300 - 360 histidine monohydrochloride 1.8 - 2.2 Bath temperature 40 - 55°C; preferably 45°C. Bath pH 8.5 - 9.7; preferably 8.8 - 9. Density of cathode current 10 - 40 A/dm 2 .
  • Both soluble anodes and insoluble anodes may be used.
  • brass anodes are used, having the same copper percent as that desired in the deposit.
  • Example of a suitable material for insoluble anodes is titanium, possibly coated with oxides of suitable materials such as iridium and tantalum.
  • the anodes may be placed parallel to the wire or on the bottom of the cups.
  • the metal element is preferably treated on its surface with a phosphating bath consisting of a 30 - 50 g/l solution of phosphoric acid at a temperature of 30°C - 50°C, for an immersion time of from 3 to 5 seconds.
  • a phosphating bath consisting of a 30 - 50 g/l solution of phosphoric acid at a temperature of 30°C - 50°C, for an immersion time of from 3 to 5 seconds.
  • the metal element is a steel wire coated with a layer of brass (1 - 2 microns), it is preferably drawn using a conventional emulsion lubricant.
  • the wire can then be used to produce cord of the type shown in Fig. 4.
  • a further advantage of the present invention is that the density of the cathode current does not have a significant effect on the percent of deposited copper.
  • the distribution of the current itself (depending on different cell forms, different bath stirring, and the like) also has no significant effect on the percent of deposited copper.
  • the cathode efficiency of the process of the present invention is about 70% while, in the case of the cyanide bath it is, for the same cathode current, substantially less.
  • the amount of copper deposited with the process of the present invention is a linear function of the copper/zinc ratio.
  • This further advantage of the present invention allows the composition of the bath to be preselected very easily in accordance with the brass composition that it is desired to deposit.
  • Fig. 5 shows a tire produced in a known way but using cords made of steel wires coated with brass deposited according to the present invention.
  • the tire is fitted on a rim 13 and consists of a bead 10, a bead ring 12, a carcass ply 14, belt strips 15, tread 16 and sidewalls 17.
  • the strips 15 are formed by cords of steel wire coated with brass with the process of the present invention.
  • Figs. 6-8 show a conveyor belt 20, a transmission belt 30 and a flexible pipe 40 made of vulcanized natural or synthetic rubber, respectively, each reinforced with cords made of steel wire coated with brass according to the process of the present invention.
  • a galvanic bath capable of depositing a layer of brass consisting of about 90% of copper and about 10% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.15 Zn ++ 0.06 alkali pyrophosphate 1 histidine 0.01
  • a galvanic bath capable of depositing a layer of brass consisting of about 80% of copper and about 20% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.1 Zn ++ 0.05 alkali pyrophosphate 1 histidine 0.01
  • a galvanic bath capable of depositing a layer of brass consisting of about 67% of copper and about 33% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.24 Zn ++ 0.13 alkali pyrophosphate 1 histidine 0.01
  • a galvanic bath capable of depositing a layer of brass consisting of about 64% of copper and about 36% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.2 Zn ++ 0.118 alkali pyrophosphate 1 histidine 0.01
  • Working conditions are: Bath temperature 45°C Bath pH 9 Density of cathode current 25 A/dm 2 .
  • a galvanic bath capable of depositing a layer of brass consisting of about 60% of copper and about 40% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.1 Zn ++ 0.07 alkali pyrophosphate 1 histidine 0.01
  • the materials used to prepare the abovementioned bath were: grams/litre cupric sulfate pentahydrate 25 zinc sulfate heptahydrate 20 potassium pyrophosphate 330 histidine monohydrochloride 2
  • a galvanic bath capable of depositing a layer of brass consisting of about 50% of copper and about 50% of zinc on a steel wire has the following composition: mols/litre Cu ++ 0.1 Zn ++ 0.1 alkali pyrophosphate 1 histidine 0.01
  • This morphological feature sharply distinguishes the brass deposits of to the present invention over those obtained by diffusion which, before drawing, show a highly irregular surface with holes of a size of from 0.1 to 0.5 microns.
  • the brass deposits according to the present invention are characterized by a substantially constant content of copper and zinc throughout the depth of the deposit while those obtained by diffusion show, before the drawing step, deviations of some 10%, as gradient of diffusion (diffusion % of Cu between the outside and the inside).
  • the surfaces of the brass deposits obtained by diffusion show, before the drawing step, some amounts of oxides, particularly of zinc, evaluated by detecting the content of oxygen, [estimated as the ratio O/(Cu+Zn)], which is of from about 5% to about 10%.
  • the surface of deposits obtained according to the present invention have a content of oxygen equal to or less than about 3%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electrolytic Production Of Metals (AREA)
EP96201786A 1995-07-07 1996-06-27 Elektrolytisches Verfahren zur Beschichtung eines Metallelements mit Messing Expired - Lifetime EP0752484B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SI9630096T SI0752484T1 (en) 1995-07-07 1996-06-27 Electrolytic process for coating a metal element with a layer of brass

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITMI951457A IT1275490B (it) 1995-07-07 1995-07-07 Procedimento elettrolitico per ricoprire un elemento metallico con uno strato di ottone
ITMI951457 1995-07-07

Publications (2)

Publication Number Publication Date
EP0752484A1 true EP0752484A1 (de) 1997-01-08
EP0752484B1 EP0752484B1 (de) 1999-08-18

Family

ID=11371937

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96201786A Expired - Lifetime EP0752484B1 (de) 1995-07-07 1996-06-27 Elektrolytisches Verfahren zur Beschichtung eines Metallelements mit Messing

Country Status (6)

Country Link
EP (1) EP0752484B1 (de)
AT (1) ATE183558T1 (de)
DE (1) DE69603799T2 (de)
ES (1) ES2137621T3 (de)
IT (1) IT1275490B (de)
SI (1) SI0752484T1 (de)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003012174A1 (en) * 2001-07-27 2003-02-13 Pirelli Pneumatici S.P.A. Electrolytic process for depositing a layer of copper on a steel wire
EP1535515A1 (de) * 2002-08-26 2005-06-01 Riken KUPFERPRûPARAT ZUR BEKûMPFUNG VON PFLANZENKRANKHEITEN
JP2009127097A (ja) * 2007-11-26 2009-06-11 Bridgestone Corp 銅−亜鉛合金電気めっき浴およびこれを用いためっき方法
US20100243466A1 (en) * 2007-11-26 2010-09-30 Bridgestone Corporation Copper-zinc alloy electroplating bath and plating method using the copper-zinc alloy electroplating bath
EP2287365A1 (de) * 2008-05-12 2011-02-23 Bridgestone Corporation Galvanisierungsbad aus kupfer-zink-legierung und plattierungsverfahren damit
EP2405034A4 (de) * 2009-03-04 2015-05-06 Bridgestone Corp Elektroplattierungsbad aus einer kupfer-zink-legierung und plattierungsverfahren damit

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITTO20110018U1 (it) * 2011-03-08 2012-09-09 Redaelli Tecna Spa Fune in acciaio a contrasto elevato

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63203790A (ja) * 1987-02-17 1988-08-23 Oosakashi シアン化合物を含まない光沢銅−亜鉛合金電気めつき浴
US5100517A (en) * 1991-04-08 1992-03-31 The Goodyear Tire & Rubber Company Process for applying a copper layer to steel wire

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63203790A (ja) * 1987-02-17 1988-08-23 Oosakashi シアン化合物を含まない光沢銅−亜鉛合金電気めつき浴
US5100517A (en) * 1991-04-08 1992-03-31 The Goodyear Tire & Rubber Company Process for applying a copper layer to steel wire

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Week 8839, Derwent World Patents Index; AN 88276038, XP002002660, "bright copper-zinc alloy electroplating bath" *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003012174A1 (en) * 2001-07-27 2003-02-13 Pirelli Pneumatici S.P.A. Electrolytic process for depositing a layer of copper on a steel wire
EP1535515A1 (de) * 2002-08-26 2005-06-01 Riken KUPFERPRûPARAT ZUR BEKûMPFUNG VON PFLANZENKRANKHEITEN
EP1535515A4 (de) * 2002-08-26 2005-09-14 Riken KUPFERPRûPARAT ZUR BEKûMPFUNG VON PFLANZENKRANKHEITEN
US7297349B2 (en) 2002-08-26 2007-11-20 Riken Copper-containing formulation for plant disease control
JP2009127097A (ja) * 2007-11-26 2009-06-11 Bridgestone Corp 銅−亜鉛合金電気めっき浴およびこれを用いためっき方法
US20100243466A1 (en) * 2007-11-26 2010-09-30 Bridgestone Corporation Copper-zinc alloy electroplating bath and plating method using the copper-zinc alloy electroplating bath
EP2218804A4 (de) * 2007-11-26 2011-08-24 Bridgestone Corp Galvanisierungsbad aus kupfer-zink-legierung und plattierungsverfahren mit dem galvanisierungsbad aus kupfer-zink-legierung
EP2287365A1 (de) * 2008-05-12 2011-02-23 Bridgestone Corporation Galvanisierungsbad aus kupfer-zink-legierung und plattierungsverfahren damit
EP2287365A4 (de) * 2008-05-12 2012-04-04 Bridgestone Corp Galvanisierungsbad aus kupfer-zink-legierung und plattierungsverfahren damit
EP2405034A4 (de) * 2009-03-04 2015-05-06 Bridgestone Corp Elektroplattierungsbad aus einer kupfer-zink-legierung und plattierungsverfahren damit

Also Published As

Publication number Publication date
SI0752484T1 (en) 1999-12-31
ITMI951457A1 (it) 1997-01-07
ITMI951457A0 (it) 1995-07-07
IT1275490B (it) 1997-08-07
ES2137621T3 (es) 1999-12-16
ATE183558T1 (de) 1999-09-15
EP0752484B1 (de) 1999-08-18
DE69603799D1 (de) 1999-09-23
DE69603799T2 (de) 2000-03-02

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