EP1865081A1 - Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise - Google Patents

Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise Download PDF

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Publication number
EP1865081A1
EP1865081A1 EP06291130A EP06291130A EP1865081A1 EP 1865081 A1 EP1865081 A1 EP 1865081A1 EP 06291130 A EP06291130 A EP 06291130A EP 06291130 A EP06291130 A EP 06291130A EP 1865081 A1 EP1865081 A1 EP 1865081A1
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EP
European Patent Office
Prior art keywords
substrate
stainless steel
chromium
heating zone
less
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.)
Withdrawn
Application number
EP06291130A
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English (en)
French (fr)
Inventor
Marc Mantel
Eric Chauveau
Christophe Vachey
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.)
Ugitech SA
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Ugitech SA
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 Ugitech SA filed Critical Ugitech SA
Priority to EP06291130A priority Critical patent/EP1865081A1/de
Publication of EP1865081A1 publication Critical patent/EP1865081A1/de
Withdrawn legal-status Critical Current

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    • 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
    • C23C22/06—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 acidic solutions with pH less than 6
    • C23C22/48—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 acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/54—Furnaces for treating strips or wire
    • C21D9/56—Continuous furnaces for strip or wire
    • 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
    • C23C22/06—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 acidic solutions with pH less than 6
    • C23C22/07—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 acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • 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
    • 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
    • C23C8/80—After-treatment

Definitions

  • the present invention relates to a continuous dyeing process for a stainless steel or nickel base alloy substrate containing chromium.
  • Stainless steels have corrosion resistance properties, and are now widely used in the building market for decorative applications (facades, roofs, furniture etc .). For these applications, there is a market demand to have colored products while maintaining the metallic appearance of the surface. Products with good cleanability, good resistance to UV aging and good fire resistance are also sought.
  • Physical deposits include sputter deposition, an alternative vacuum deposition process. From a target, subjected to the action of an ionic bombardment of energetic particles, the atoms of the material to be colored are deposited on a material carrier. The ions are obtained by a glow discharge between two electrodes.
  • Chemical deposits consist of converting the surface of the metal into a stable oxide by immersion in an aqueous solution containing chromium (Cr 6+ ) salts.
  • the metal is oxidized under anodic polarization.
  • a current generator and a cell adapted to the type of sample are used so as to obtain a good distribution of the current lines.
  • the stainless steel sample is placed in anode, the cathode consists of a lead plate.
  • the object of the present invention is therefore to overcome the disadvantages of the processes of the prior art by providing a method of staining substrates of stainless steel or chromium-containing nickel base alloy, which has improved productivity, stable coloring , matt or glossy, retaining a metallic appearance and which further has a corrosion resistance equivalent to the uncolored base metal.
  • a method is also sought that makes it possible to obtain a colored surface that is not very sensitive to fingerprints and scratches, having the most homogeneous coloration possible, as well as good cleanability, good resistance to UV and fire.
  • a first object of the present invention is constituted by a method of continuously dyeing a substrate made of stainless steel or chromium-containing nickel base alloy, according to which said substrate is passed through a heating zone set to a set temperature between 800 and 1500 ° C, in order to obtain a surface oxidized layer having a thickness of less than 200 nm and a ratio between the chromium and iron contents greater than 0.02 in said oxidized layer, and then said substrate is cooled to a temperature of less than or equal to 70 ° C.
  • a third object of the invention is constituted by a substrate made of stainless steel or chromium-containing nickel base alloy, comprising a surface-oxidized layer having a thickness of less than 200 nm and a ratio between the chromium and iron contents greater than 0.02 in said oxidized layer.
  • the high temperature of the furnace makes it possible to diffuse the chromium of the base metal towards the surface and thus to improve the resistance to corrosion by increasing the ratio Cr / Fe of the oxide film.
  • XPS photoelectron spectroscopy
  • the method according to the invention has the essential advantage of allowing continuous operation. It applies perfectly to a wire or a profile, but also to a coil of strips of cold rolled material, or even to a bar.
  • yarn will be referred to when the substrate has a diameter of less than 32 mm and is wound into a reel and bar when the product will have a diameter greater than 2 mm with a finished length less than or equal to 12 m.
  • austenitic stainless steels such as type 304, 304L, 306, 316 and 316L steels.
  • the optional first step of the process according to the invention consists in improving the homogeneity of the surface of the substrate even before it is colored.
  • the inventors have indeed found that the brightness and the shade of the final color are influenced by the homogeneity of the surface state. It is therefore advantageous to integrate a surface preparation of the substrate to be colored. However, it is quite possible to carry out this operation prior to the implementation of the method according to the invention, on a separate line.
  • a cold plastic deformation operation such as drawing or cold rolling with a reduction rate greater than 4% or else a preparation of the surface condition by abrasion, shot blasting, sandblasting, annealing stripping or any other method to control and homogenize the surface condition.
  • the heating zone is preferably a furnace comprising an enclosure and electrical resistances, but it is also possible to form the desired oxide film with a combustion furnace or by other heating systems that do not necessarily require enclosures. scrolling, like induction heating.
  • the passage furnace preferentially used for coloring the substrate by oxidation is set to operate at a set temperature of between 800 and 1500 ° C., and preferably between 800 and 1300 ° C.
  • the setting of the oven temperature is a function of the speed of the line and the color that is to be obtained.
  • the line speed which depends on the length of the furnace, the operating temperature and the desired color is preferably greater than 1 m / min and more preferably greater than or equal to 10 m / min.
  • the method according to the invention makes it possible to obtain different colors by playing on the one hand on the temperature of the furnace and on the other hand on the running speed of the wire.
  • a series of tests were carried out on a laboratory cyclic oven (see FIG. 1), comprising a 610 mm heating zone by treating 304L type stainless steel wires.
  • FIG. 2 shows a number of additional tests in which the residence times in the oven at fixed temperature have been varied. We see that by playing on this time, we can get the full range of colorations.
  • the atmosphere used in the oven may be oxidizing or inert.
  • an oxidizing atmosphere it will be possible in particular to use air in order to maintain the highest possible line speed and to have good productivity.
  • inert gases such as nitrogen, hydrogen or a nitrogen / hydrogen mixture.
  • the dew point will preferably be controlled in a range of -20 ° C to + 30 ° C depending on the target color and the speed of the line.
  • a cooling system is provided to bring the temperature of the substrate to a value less than or equal to 70 ° C.
  • an anti-corrosion treatment of the substrate according to the invention is carried out after coloring and cooling.
  • This treatment consists in placing the substrate in contact with an aqueous solution of mineral acid until the oxidized layer formed during the coloration is partially dissolved, followed by rinsing with water.
  • the anti-corrosion treatment greatly improves the resistance to pitting corrosion in a chloride medium. This gives a pitting corrosion resistance close to that of the base metal.
  • mineral acids such as nitric acid or preferably phosphoric acid
  • the anti-corrosion treatment is preferably carried out at ambient temperature, but it is especially possible to work between 20 and 70 ° C., in particular if it is desired to increase the speed of the line and therefore the productivity of the coloring process.
  • the maximum temperature of use of the solutions will also depend on the nature of the acids used as well as their concentrations. The optimal parameters of this treatment have been defined using different tests.
  • Tests were carried out on 316 type austenitic stainless steel wires, which had previously been colored at an oven temperature of 920 ° C to 930 ° C, with an oven residence time of 32 seconds.
  • the bath used for the anti-corrosion treatment contained an aqueous nitric acid solution at 20% by volume and at a temperature of 60 ° C.
  • the tests were carried out on 316 type austenitic stainless steel wire, which had previously been colored at an oven temperature between 920 ° C and 930 ° C, with a residence time in the oven of 32s.
  • the samples were immersed in an acid bath for 30 seconds. Since nitric acid can pose health and environmental problems, the effectiveness of phosphoric acid has also been tested.
  • a cold plastic deformation treatment of the substrate which has just been cooled is carried out so as to obtain a degree of deformation of between 5 and 15%.
  • this operation may consist of a skin-pass (cold-rolled wire and strip), stretching (bars) or even profiling.
  • the present inventors have indeed found that this operation made it possible to improve, and surprisingly, various properties of the surface of the treated substrate, such as sensitivity to fingerprints, sensitivity to scratching, and corrosion resistance. . In addition, the homogeneity of the coloration and the corrosion resistance is also improved.
  • the tests for evaluating the homogeneity of the coloration were carried out on threads identical to those used for the fingerprint sensitivity test. The evaluation is performed visually by an operator.
  • this variant of the process according to the invention improves the homogeneity of the coloration, in particular when the oxidation temperature exceeds 900 ° C.
  • Corrosion resistance was measured by the pitting potential measured against a saturated calomel electrode on AISI 316L grade in 0.02M NaCl solution at 23 ° C. The results are collated in Table 8. ⁇ u> Table 8 Pitting potential measurements ⁇ / u> Potential for puncture NaCl 0.02M 23 ° C 316L naked 658 mV Colored 316L 900 ° C 253 mV Colored 316L 900 ° C + Skin Pass 5% 602 mV
  • the contact angle of the yarn according to the invention is significantly increased compared to that which has not been subjected to the process according to the invention, which means that the surface of this yarn has an improved hydrophobicity, which makes it easier to clean and less reactive to contamination.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
EP06291130A 2006-06-06 2006-06-06 Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise Withdrawn EP1865081A1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP06291130A EP1865081A1 (de) 2006-06-06 2006-06-06 Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise

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Application Number Priority Date Filing Date Title
EP06291130A EP1865081A1 (de) 2006-06-06 2006-06-06 Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise

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EP1865081A1 true EP1865081A1 (de) 2007-12-12

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EP06291130A Withdrawn EP1865081A1 (de) 2006-06-06 2006-06-06 Verfahrensweise ununterbrochener Färbung eines Substrates aus rostfreiem Stahl oder aus Legierung basiert Nickel das Chrom enthält, und Vorrichtung der Umsetzung der Verfahrensweise

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014009727A1 (en) * 2012-07-10 2014-01-16 Kts Wire Ltd Method for treating elongated metal product by heating and oxidizing the surface in a controlled environment

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59232233A (ja) * 1983-06-16 1984-12-27 Kawasaki Steel Corp ステンレス冷延鋼帯の焼鈍方法
JPH0211784A (ja) * 1988-06-29 1990-01-16 Nippon Steel Corp 鋼伸線材の表面清浄処理方法
EP0453321A1 (de) * 1990-04-20 1991-10-23 Kawasaki Steel Corporation Verfahren zum Entzundern warmgewalzter Bänder aus nichtrostendem Stahl
JPH06271938A (ja) * 1993-03-23 1994-09-27 Koyo Tetsusen Kk 耐食性に優れたなまし鉄線の製造方法
JP2001234371A (ja) * 2000-02-21 2001-08-31 Bridgestone Corp ゴムとの接着性に優れた銅合金めっき付きスチールワイヤ、コードおよびゴム物品
CN1519065A (zh) * 2003-09-02 2004-08-11 黄 澄 轴承钢丝的生产方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59232233A (ja) * 1983-06-16 1984-12-27 Kawasaki Steel Corp ステンレス冷延鋼帯の焼鈍方法
JPH0211784A (ja) * 1988-06-29 1990-01-16 Nippon Steel Corp 鋼伸線材の表面清浄処理方法
EP0453321A1 (de) * 1990-04-20 1991-10-23 Kawasaki Steel Corporation Verfahren zum Entzundern warmgewalzter Bänder aus nichtrostendem Stahl
JPH06271938A (ja) * 1993-03-23 1994-09-27 Koyo Tetsusen Kk 耐食性に優れたなまし鉄線の製造方法
JP2001234371A (ja) * 2000-02-21 2001-08-31 Bridgestone Corp ゴムとの接着性に優れた銅合金めっき付きスチールワイヤ、コードおよびゴム物品
CN1519065A (zh) * 2003-09-02 2004-08-11 黄 澄 轴承钢丝的生产方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014009727A1 (en) * 2012-07-10 2014-01-16 Kts Wire Ltd Method for treating elongated metal product by heating and oxidizing the surface in a controlled environment

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