EP2171116B1 - Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff - Google Patents

Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff Download PDF

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EP2171116B1
EP2171116B1 EP08762800A EP08762800A EP2171116B1 EP 2171116 B1 EP2171116 B1 EP 2171116B1 EP 08762800 A EP08762800 A EP 08762800A EP 08762800 A EP08762800 A EP 08762800A EP 2171116 B1 EP2171116 B1 EP 2171116B1
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Prior art keywords
steel sheet
oxide
temperature
process according
zinc
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German (de)
English (en)
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EP2171116A1 (fr
Inventor
Jean-Michel Mataigne
Florence Bertrand
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ArcelorMittal France SA
Nippon Steel Corp
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ArcelorMittal France SA
Nippon Steel Corp
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    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/34—Methods of heating
    • C21D1/52—Methods of heating with flames
    • 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
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • 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
    • C21D9/561—Continuous furnaces for strip or wire with a controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/11—Making amorphous alloys
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
    • C23C2/0222—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating in a reactive atmosphere, e.g. oxidising or reducing atmosphere
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
    • C23C2/0224—Two or more thermal pretreatments
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/06—Zinc or cadmium 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/261—After-treatment in a gas atmosphere, e.g. inert or reducing atmosphere
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
    • C23C2/36—Elongated material
    • C23C2/40—Plates; Strips

Definitions

  • the present invention relates to a process for manufacturing a hot-dip galvannealed steel sheet having a TRIP microstructure.
  • TRIP steels (the term TRIP standing for transformation-induced plasticity), which combine very high mechanical strength with the possibility of very high levels of deformation.
  • TRIP steels have a microstructure comprising ferrite, residual austenite and optionally martensite and/or bainite, which allows them to achieve tensile strength from 600 to 1000 MPa.
  • This type of steel is widely used for production of energy-absorbing parts, such as for example structural and safety parts such as longitudinal members and reinforcements.
  • TRIP steel sheets are obtained by adding a large amount of silicon to steel. Silicon stabilizes the ferrite and the austenite at room temperature, and prevents residual austenite from decomposing to form carbide.
  • TRIP steel sheets containing more than 0.2% by weight of silicon are galvanized with difficulty, because silicon oxides are formed on the surface of the steel sheet during the annealing taking place just before the coating. These silicon oxides show a poor wettability toward the molten zinc, and deteriorate the plating performance of the steel sheet.
  • TRIP steel having low silicon content (less than 0.2% by weight).
  • this has a major drawback: a high level of tensile strength, that is to say about 800 MPa, can be achieved only if the content of carbon is increased. But, this has the effect to lower the mechanical resistance of the welded points.
  • the TRIP effect is observed when the TRIP steel sheet is being deformed, as the residual austenite is transformed into martensite under the effect of the deformation, and the strength of the TRIP steel sheet increases.
  • the purpose of the present invention is therefore to remedy the aforementioned drawbacks and to propose a process for hot-dip galvannealing a steel sheet having a high silicon content (more than 0.5% by weight) and a TRIP microstructure showing high mechanical characteristics, that guarantees a good wettability of the surface steel sheet and no non-coated portions, and thus guarantees a good adhesion and a nice surface appearance of the zinc alloy coating on the steel sheet, and that preserves the TRIP effect.
  • the first subject of the invention is a process for manufacturing a hot-dip galvannealed steel sheet having a TRIP microstructure comprising ferrite, residual austenite and optionally martensite and/or bainite, said process comprising the steps consisting in:
  • the balance of the composition consists of iron and other elements that are usually expected to be found and impurities resulting from the smelting of the steel, in proportions that have no influence on the desired properties.
  • the steel sheet having the above composition is first subjected to an oxidation followed by a reduction, before being hot-dip galvanized in a bath of molten zinc and heat-treated to form said galvannealed steel sheet.
  • the aim is to form an oxidized steel sheet having an outer layer of iron oxide with a controlled thickness which will protect the steel from the selective outer oxidation of silicon, manganese and aluminium, while the steel sheet is annealed before the hot-dip galvanization.
  • Said oxidation of the steel sheet is performed under conditions that allow the formation, on the surface of the steel sheet, of a layer of iron oxide containing no superficial oxides selected from the group consisting of silicon oxide, manganese oxide, aluminium oxide, complex oxide comprising silicon and/or manganese and/or aluminium.
  • a layer of iron oxide containing no superficial oxides selected from the group consisting of silicon oxide, manganese oxide, aluminium oxide, complex oxide comprising silicon and/or manganese and/or aluminium.
  • a layer of an internal oxide of at least one type of oxide selected from the group consisting of silicon oxide, manganese oxide, aluminium oxide, complex oxide comprising Si and Mn, complex oxide comprising Si and Al, complex oxide comprising Mn and Al and complex oxide comprising Si, Mn and Al is thus formed.
  • the oxidation is preferably performed by heating said steel sheet from ambient temperature to a heating temperature T1 which is between 680 and 800°C, in a direct flame furnace where the atmosphere comprises air and fuel, with a ratio air-to-fuel preferably between 1 and 1.2.
  • the iron oxide layer formed on the surface of the steel sheet will contain manganese coming from the steel, and the wettability will be impaired. If the temperature T1 is below 680°C, the internal oxidation of silicon, manganese and aluminium will not be favoured, and the galvanizability of the steel sheet will be insufficient.
  • An atmosphere having a ratio air-to-fuel less than 1 leads to the formation of superficial oxidation of silicon, manganese and aluminium, and thus a superficial layer of oxides selected from the group consisting of silicon oxide, manganese oxide, aluminium oxide, and complex oxide comprising silicon and/or manganese and/or aluminium, possibly in combination with iron oxide is formed, and the wettability is impaired.
  • a ratio air-to-fuel above 1.2 the layer of iron oxide is too thick, and will not be completely reduced. Thus, the wettability will also be impaired.
  • the oxidized steel sheet When leaving the direct flame furnace, the oxidized steel sheet is reduced in conditions permitting the achievement of the complete reduction of the iron oxide into iron.
  • This reduction step can be performed in a radiant tube furnace or in a resistance furnace.
  • Said oxidized steel sheet is thus heat treated in an atmosphere comprising preferably more than 15% by volume of hydrogen, the balance being nitrogen and unavoidable impurities. Indeed, if the content of hydrogen in the atmosphere is less than 15% by volume, the layer of iron oxide can be insufficiently reduced and the wettability is impaired.
  • Said oxidized steel sheet is heated from the heating temperature T1 to a soaking temperature T2, then it is soaked at said soaking temperature T2 for a soaking time t2, and is finally cooled from said soaking temperature T2 to a cooling temperature T3.
  • Said soaking temperature T2 is preferably between 770 and 850°C.
  • T2 When the steel sheet is at the temperature T2, a dual phase microstructure composed of ferrite and austenite is formed.
  • T2 When T2 is above 850°C, the volume ratio of austenite grows too much, and external selective oxidation occurs on the steel surface. But when T2 is below 770°C, the time required to form a sufficient volume ratio of austenite is too high.
  • sufficient austenite must be formed during the soaking step, so that sufficient residual austenite is maintained during the cooling step.
  • the soaking is performed for a time t2, which is preferably between 20 and 180s. If the time t2 is longer than 180s, the austenite grains coarsen and the yield strength R e of the steel after forming will be limited. Furthermore, the hardenability of the steel is low. However, if the steel sheet is soaked for a time t2 less than 20s, the proportion of austenite formed will be insufficient and sufficient residual austenite and bainite will not form when cooling.
  • the reduced steel sheet is finally cooled at a cooling temperature T3 near the temperature of the bath of molten zinc, in order to avoid the cooling or the re-heating of said bath.
  • T3 is thus preferably between 460 and 510°C. Therefore, a zinc-based coating having a homogenous microstructure can be obtained.
  • the steel sheet When the steel sheet is cooled, it is hot dipped in the bath of molten zinc whose temperature is preferably between 450 and 500°C.
  • This bath can contain 0.08 to 0.135% by weight of dissolved aluminium, the balance being zinc and unavoidable impurities. Aluminium is added in the bath in order to deoxidize the molten zinc, and to make it easier to control the thickness of the zinc-based coating. In that condition, precipitation of delta phase (FeZn 7 ) is induced at the interface of the steel and of the zinc-based coating.
  • the steel sheet When leaving the bath, the steel sheet is wiped by projection of a gas, in order to adjust the thickness of the zinc-based coating.
  • This thickness which is generally between 3 and 10 ⁇ m, is determined according to the required resistance to corrosion.
  • the hot-dip galvanized steel sheet is finally heat-treated so that a coating made of a zinc-iron alloy is obtained, by diffusion of the iron from steel to the zinc of the coating.
  • This alloying treatment can be performed by maintaining said steel sheet at a temperature T4 between 460 and 510°C for a soaking time t4 between 10 and 30s. Thanks to the absence of external selective oxidation of silicon, manganese and aluminium, this temperature T4 is lower than the conventional alloying temperatures. For that reason, large quantities of molybdenum to the steel are not required, and the content of molybdenum in the steel can be limited to less than 0.01 % by weight. If the temperature T4 is below 460°C, the alloying of iron and zinc is not possible.
  • the time t4 is adjusted so that the average iron content in the alloy is between 8 and 12% by weight, which is a good compromise for improving the weldability of the coating and limiting the powdering while shaping.
  • Samples A and B are pre-heated from ambient temperature (20°C) to 750°C, in a direct flame furnace. They are subsequently and continuously annealed in a radiant tube furnace, where they are heated from 750° to 800°C, then they are soaked at 800°C for 60 s, and finally they are cooled to 460 °C.
  • the atmosphere in the radiant tube furnace comprises 30% by volume of hydrogen, the balance being nitrogen and unavoidable impurities.
  • samples A and B are hot dip galvanized in a molten zinc-based bath comprising 0.12% by weight of aluminium, the balance being zinc and unavoidable impurities.
  • the temperature of said bath is 460 °C.
  • the thickness of the zinc-based coating is 7 ⁇ m.
  • the aim is to compare the wettablilty and the adherence of these samples, when the air-to-fuel ratio in the direct flame furnace fluctuates.
  • the air-to-fuel ratio is 0.90 for sample A, and 1.05 according to the invention for sample B.
  • the results are shown in table II.
  • the wettability is visually controlled by an operator.
  • the adherence of the coating is also visually controlled after a 180° bending test of samples.
  • Table I chemical composition of the steel of samples A and B, in % by weight, the balance of the composition being iron and unavoidable impurities (sample A and B).
  • Table I C Mn Si Al Mo Cr P Ti V Ni Nb 0.20 1.73 1.73 0.01 0.005 0.02 0.01 0.005 0.005 0.01 0.005
  • Table II Wettabilty Adherence Aspect of the surface Sample A** Bad Bad Bad Sample B* Good Good Good Good * according to the invention ** according to the conventional process
  • Figure 1 is a photography of sample A after the pre-heating step and before the annealing step
  • figure 2 is a photography of sample B after the pre-heating step and before the annealing step.
  • the aim is to show the effect of the internal selective oxidation of silicon and manganese on the temperature of alloying.
  • the temperature of alloying treatment applied to sample B in order to obtain a galvannealed steel sheet according to the invention is compared with the temperature of alloying of sample A.
  • Sample B which has been hot dip galvanized is then subjected to an alloying treatment by heating it to 480°C, and by maintaining it at this temperature for 19 s .
  • the inventors have checked that the TRIP microstructure of the obtained hot dip galvannealed steel sheet according to the invention was not lost by this alloying treatment.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

L'invention porte sur un procédé de fabrication d'une tôle d'acier recuite par galvanisation par immersion à chaud, ayant une microstructure TRIP, et comprenant, en pourcentage en poids, 0,01 ≤ C ≤ 0,22%, 0,50 ≤ Mn ≤ 2,0%, 0,5 < Si ≤ 2,0%, 0,005 ≤ Al ≤ 2,0%, Mo < 0,01 %, Cr ≤1,0%, P < 0,02%, Ti ≤ 0,20%, V ≤ 0,40%, Ni ≤ 1,0%, Nb ≤ 0,20 %, le reste de la composition étant du fer et des impuretés inévitables résultant de la fusion, ledit procédé comprenant les étapes consistant à : oxyder ladite tôle d'acier afin de former une couche d'oxyde de fer sur la surface de la tôle d'acier, et de former un oxyde interne d'au moins un type d'oxyde choisi dans le groupe constitué par l'oxyde de Si, l'oxyde de Mn, l'oxyde d'Al, un oxyde complexe comprenant Si et Mn, un oxyde complexe comprenant Si et Al, un oxyde complexe comprenant Al et Mn, et un complexe comprenant Si, Mn et Al, réduire ladite tôle d'acier oxydée afin de réduire la couche d'oxyde de fer, galvaniser par immersion à chaud ladite tôle d'acier réduite pour former une tôle d'acier revêtue à base de zinc, et soumettre ladite tôle d'acier revêtue à base de zinc à un traitement d'alliage pour former une tôle d'acier recuite par galvanisation.

Claims (11)

  1. Procédé pour fabriquer une tôle d'acier galvanisé-allié ayant une microstructure à plasticité induite par transformation (TRIP) comprenant de la ferrite, de l'austénite résiduelle et éventuellement de la martensite et/ou de la bainite, ledit procédé comprenant les étapes consistant à :
    - approvisionner une tôle d'acier dont la composition comprend, en poids :
    0,01 ≤ Cl 0,22 %
    0,50 ≤ Mn ≤ 2,0 %
    0,5 < Si ≤ 2,0 %
    0,005 ≤ A1 ≤ 2,0 %
    Mo < 0,01 %
    Cr ≤ 1,0 %
    P < 0,02 %
    Ti ≤ 0,20 %
    V ≤ 0,40 %
    N ≤ 1,0 %
    Nb ≤ 0,20 %
    le solde de la composition étant du fer et les inévitables impuretés résultant de la fusion,
    - oxyder ladite tôle d'acier en la chauffant de la température ambiante à une température T1 comprise entre 680 et 800 °C, dans un four à flamme directe où l'atmosphère comprend de l'air et un combustible avec un rapport air sur combustible compris entre 1,0 et 1,2 afin de former une couche d'oxyde de fer sur la surface de la tôle d'acier, et de former un oxyde interne d'au moins un type d'oxyde choisi dans le groupe constitué par un oxyde de Si, un oxyde de Mn, un oxyde d'Al, un oxyde complexe comprenant Si et Mn, un oxyde complexe comprenant Si et Al, un oxyde complexe comprenant Al et Mn, et un oxyde complexe comprenant Si, Mn et Al,
    - réduire ladite tôle d'acier oxydé afin de réduire la couche d'oxyde de fer,
    - galvaniser à chaud au trempé ladite tôle d'acier réduit pour former une tôle d'acier avec revêtement à base de zinc, et
    - soumettre ladite tôle d'acier avec revêtement à base de zinc à un traitement d'alliation pour former une tôle d'acier galvanisé-allié.
  2. Procédé selon la revendication 1, dans lequel ladite tôle d'acier comprend, en % en poids, P < 0,010 %.
  3. Procédé selon la revendication 1 ou 2, dans lequel ladite tôle d'acier comprend, en % en poids, Mo ≤ 0,006 %.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel la réduction de ladite tôle d'acier oxydé consiste en un traitement thermique effectué dans une atmosphère comprenant plus de 15 % en volume d'hydrogène, le solde étant de l'azote et les inévitables impuretés, ledit traitement thermique comprenant une phase de chauffage de la température T1 à une température d'égalisation T2, une phase d'égalisation à ladite température d'égalisation T2 pendant un temps d'égalisation t2, et une phase de refroidissement de ladite température d'égalisation T2 à une température de refroidissement T3.
  5. Procédé selon la revendication 4, dans lequel ladite température d'égalisation T2 se situe entre 770 et 850 °C.
  6. Procédé selon la revendication 4 ou 5, dans lequel ledit temps d'égalisation t2 se situe entre 20 et 180 s.
  7. Procédé selon l'une quelconque des revendications 4 à 6, dans lequel ladite température de refroidissement T3 se situe entre 460 et 510 °C.
  8. Procédé selon l'une quelconque des revendications 3 à 7, dans lequel ladite réduction est effectuée dans un four à tubes radiants ou dans un four à résistance.
  9. Procédé selon l'une quelconque des revendications 1 à 8, dans lequel la galvanisation à chaud est effectuée en trempant ladite tôle d'acier réduit dans un bain fondu comprenant 0,08 à 0,135 % en poids d'aluminium, le solde étant du zinc et les inévitables impuretés.
  10. Procédé selon la revendication 9, dans lequel la température dudit bain fondu se situe entre 450 et 500 °C.
  11. Procédé selon l'une quelconque des revendications 1 à 10, dans lequel ledit traitement d'alliage est réalisé en chauffant ladite tôle d'acier avec revêtement à base de zinc à une température T4 comprise entre 460 et 510 °C pendant un temps d'égalisation t4 compris entre 10 et 30 s.
EP08762800A 2007-06-29 2008-06-06 Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff Active EP2171116B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PL08762800T PL2171116T3 (pl) 2007-06-29 2008-06-06 Proces produkcji blachy stalowej cynkowanej zanurzeniowo z krótkotrwałym wyżarzaniem przez regulację DFF
EP08762800A EP2171116B1 (fr) 2007-06-29 2008-06-06 Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff

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EP07290816A EP2009129A1 (fr) 2007-06-29 2007-06-29 Processus de fabrication d'une plaque d'acier galvanisée par régulation DFF
EP08762800A EP2171116B1 (fr) 2007-06-29 2008-06-06 Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff
PCT/IB2008/001462 WO2009004425A1 (fr) 2007-06-29 2008-06-06 Procédé de fabrication d'une tôle d'acier recuite par galvanisation par régulation dff

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JP (2) JP5713673B2 (fr)
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BR (1) BRPI0813687B1 (fr)
CA (1) CA2701091C (fr)
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Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104388870B (zh) 2009-12-29 2017-04-12 Posco公司 一种热压模塑部件
KR20120075260A (ko) * 2010-12-28 2012-07-06 주식회사 포스코 도금밀착성이 우수한 용융도금강판 및 그 제조방법
KR101608605B1 (ko) * 2011-09-30 2016-04-01 신닛테츠스미킨 카부시키카이샤 고강도 용융 아연 도금 강판 및 그 제조 방법
KR20130076589A (ko) * 2011-12-28 2013-07-08 주식회사 포스코 도금표면 품질 및 도금밀착성이 우수한 고강도 용융아연도금강판 및 그 제조방법
EP2840161B1 (fr) * 2012-04-17 2018-09-12 JFE Steel Corporation Procédé de production d'une tôle d'acier galvanisée alliée par immersion à chaud, présentant une excellente adhérence au placage et d'excellentes propriétés de glissement
WO2014037627A1 (fr) 2012-09-06 2014-03-13 Arcelormittal Investigación Y Desarrollo Sl Procede de fabrication de pieces d'acier revêtues et durcies a la presse, et tôles prerevêtues permettant la fabrication de ces pieces
CN103805840B (zh) 2012-11-15 2016-12-21 宝山钢铁股份有限公司 一种高成形性热镀锌超高强度钢板及其制造方法
JP5920249B2 (ja) * 2013-03-05 2016-05-18 Ｊｆｅスチール株式会社 めっき密着性に優れた高強度溶融亜鉛めっき鋼板およびその製造方法
WO2014135753A1 (fr) 2013-03-06 2014-09-12 Arcelormittal Investigacion Y Desarrollo, S.L. Procédé de réalisation d'une tôle à revêtement znal avec un essorage optimisé, tôle, pièce et véhicule correspondants
CA2910703C (fr) 2013-05-17 2018-07-03 Ak Steel Properties, Inc. Acier recouvert de zinc pour application de durcissement par presse et procede de production associe
WO2015001367A1 (fr) 2013-07-04 2015-01-08 Arcelormittal Investigación Y Desarrollo Sl Feuille d'acier laminée à froid, procédé de fabrication et véhicule
JP5799996B2 (ja) 2013-09-12 2015-10-28 Ｊｆｅスチール株式会社 外観性とめっき密着性に優れる溶融亜鉛めっき鋼板および合金化溶融亜鉛めっき鋼板ならびにそれらの製造方法
RU2647419C2 (ru) 2013-12-10 2018-03-15 Арселормиттал Способ отжига листовой стали
WO2017006144A1 (fr) 2015-07-09 2017-01-12 Arcelormittal Acier pour trempe à la presse et pièce trempée à la presse fabriquée à partir d'un tel acier
US11572610B2 (en) * 2017-01-25 2023-02-07 Nippon Steel Corporation Steel sheet
WO2018234839A1 (fr) * 2017-06-20 2018-12-27 Arcelormittal Tôle d'acier revêtue de zinc présentant une soudabilité par points de haute résistance
WO2019092467A1 (fr) 2017-11-08 2019-05-16 Arcelormittal Tôle d'acier recuite après galvanisation
CN108165892A (zh) * 2017-11-23 2018-06-15 南阳汉冶特钢有限公司 一种低温压力容器用35-50mm厚Q420R高强钢及其生产方法
CN113969336B (zh) 2020-07-23 2023-03-28 宝山钢铁股份有限公司 一种热镀锌钢板的制造方法、钢板及车用构件

Family Cites Families (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3925579A (en) * 1974-05-24 1975-12-09 Armco Steel Corp Method of coating low alloy steels
US3936543A (en) * 1974-08-22 1976-02-03 Armco Steel Corporation Method of coating carbon steel
JP2619550B2 (ja) * 1990-03-20 1997-06-11 川崎製鉄株式会社 合金化溶融亜鉛めっき鋼板の製造方法
JP2970445B2 (ja) * 1994-12-14 1999-11-02 住友金属工業株式会社 Ｓｉ添加高張力鋼材の溶融亜鉛めっき方法
RU2128719C1 (ru) * 1997-03-05 1999-04-10 Научно-производственный институт АО "Новолипецкий металлургический комбинат" Способ производства горячеоцинкованного металла высших категорий вытяжки с тончайшим цинковым покрытием с превосходной штампуемостью
BE1014997A3 (fr) * 2001-03-28 2004-08-03 Ct Rech Metallurgiques Asbl Procede de recuit en continu de bandes en acier en vue de leur galvanisation au trempe et four pour sa mise en oeuvre.
FR2828888B1 (fr) * 2001-08-21 2003-12-12 Stein Heurtey Procede de galvanisation a chaud de bandes metalliques d'aciers a haute resistance
JP4729850B2 (ja) * 2003-02-10 2011-07-20 Ｊｆｅスチール株式会社 めっき密着性に優れた合金化溶融亜鉛めっき鋼板およびその製造方法
JP4464720B2 (ja) * 2003-04-10 2010-05-19 新日本製鐵株式会社 高強度溶融亜鉛めっき鋼板およびその製造方法
CA2521710C (fr) * 2003-04-10 2009-09-29 Nippon Steel Corporation Feuille en acier a placage de zinc moule a resistance elevee et procede de production connexe
JP4119804B2 (ja) * 2003-08-19 2008-07-16 新日本製鐵株式会社 密着性の優れた高強度合金化溶融亜鉛めっき鋼板及びその製造方法
JP5040093B2 (ja) * 2004-10-07 2012-10-03 Ｊｆｅスチール株式会社 溶融亜鉛めっき鋼板および合金化溶融亜鉛めっき鋼板
DE102004059566B3 (de) * 2004-12-09 2006-08-03 Thyssenkrupp Steel Ag Verfahren zum Schmelztauchbeschichten eines Bandes aus höherfestem Stahl
CN102260842B (zh) * 2004-12-21 2013-12-25 株式会社神户制钢所 熔融镀锌方法及熔融镀锌设备
JP4741376B2 (ja) * 2005-01-31 2011-08-03 新日本製鐵株式会社 外観が良好な高強度合金化溶融亜鉛めっき鋼板及びその製造方法と製造設備
JP4619404B2 (ja) * 2005-03-30 2011-01-26 新日本製鐵株式会社 溶融めっき熱延鋼板の製造方法
JP4644077B2 (ja) * 2005-09-05 2011-03-02 新日本製鐵株式会社 耐食性と成形性に優れた溶融亜鉛めっき高強度鋼板および合金化溶融亜鉛めっき高強度鋼板、およびそれらの製造方法
SK288275B6 (sk) * 2005-12-01 2015-06-02 Posco Oceľová doska na tvarovanie lisovaním za horúca s tepelnou úpravou a rázovými vlastnosťami, za horúca lisovaný diel z nej vyrobený a spôsob ich výroby
EP1978113B1 (fr) * 2005-12-06 2018-08-01 Kabushiki Kaisha Kobe Seiko Sho Toles en acier recuites apres galvanisation de haute resistance excellentes en termes de resistance au farinage et leur procede de production

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EP2171116A1 (fr) 2010-04-07
US20100193081A1 (en) 2010-08-05
JP2015078438A (ja) 2015-04-23
ATE521726T1 (de) 2011-09-15
CA2701091C (fr) 2012-04-17
RU2010102924A (ru) 2011-08-10
CA2701091A1 (fr) 2009-01-08
JP5713673B2 (ja) 2015-05-07
EP2009129A1 (fr) 2008-12-31
WO2009004425A1 (fr) 2009-01-08
RU2451107C2 (ru) 2012-05-20
KR101273308B1 (ko) 2013-06-11
CN101809182B (zh) 2015-08-05
KR20100055389A (ko) 2010-05-26
ES2371985T3 (es) 2012-01-12
CN101809182A (zh) 2010-08-18
BRPI0813687B1 (pt) 2018-10-30
JP2010532820A (ja) 2010-10-14
PL2171116T3 (pl) 2012-01-31
AR067339A1 (es) 2009-10-07
BRPI0813687A2 (pt) 2014-12-30
BRPI0813687A8 (pt) 2015-12-15

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