EP2732062B1 - Procédé de fabrication d'un produit plat en acier muni par immersion à chaud d'une couche de protection métallique - Google Patents

Procédé de fabrication d'un produit plat en acier muni par immersion à chaud d'une couche de protection métallique Download PDF

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Publication number
EP2732062B1
EP2732062B1 EP12735114.6A EP12735114A EP2732062B1 EP 2732062 B1 EP2732062 B1 EP 2732062B1 EP 12735114 A EP12735114 A EP 12735114A EP 2732062 B1 EP2732062 B1 EP 2732062B1
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Prior art keywords
flat steel
steel product
atmosphere
annealing
vol
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German (de)
English (en)
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EP2732062A2 (fr
Inventor
Marc Blumenau
Oliver Brehm
Michael Peters
Rudolf Schönenberg
Andreas WESTERFELD
Martin Norden
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ThyssenKrupp Steel Europe AG
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ThyssenKrupp Steel Europe AG
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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
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/005—Heat treatment of ferrous alloys containing Mn
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C21D8/0263—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment following hot rolling
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
    • 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
    • C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C23C2/024—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by cleaning or etching
    • 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
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226—Hot rolling
    • 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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236—Cold rolling

Definitions

  • the invention relates to a process for producing a flat steel product provided by hot dip coating with a metallic protective layer, in particular a high-strength steel flat product having a tensile strength of at least 500 MPa or a high-strength steel flat product having a tensile strength of at least 1000 MPa.
  • High- and high-strength flat steel products are in demand due to their advantageous combination of strength and formability in increasing quantities. This applies in particular to sheet metal applications in automotive body construction.
  • the outstanding mechanical properties of such flat steel products are based on a multiphase microstructure of the material. supported by induced plasticity of austenitic phase components (TRIP, TWIP or SIP effect).
  • TRIP austenitic phase components
  • the flat steel products in question usually have appreciable contents of certain alloying elements, which typically include manganese (Mn), aluminum (Al), silicon (Si) or chromium (Cr).
  • a surface finish in the form of a metallic protective layer not only increases the resistance of the steel flat products to corrosion and, consequently, their product lifetime, but also improves their visual appearance.
  • Various methods of applying a metallic protective layer are known. These include electrolytic deposition and hot dip coating. In addition to an electrolytically produced processing, the hot dipping refinement has established itself as an economically and ecologically particularly favorable process. In hot-dip coating, the flat steel product to be coated is immersed in a molten metal bath.
  • Hot dipping finishing is particularly cost-effective when a flat-rolled steel semi-finished product, delivered in the hard-rolled state, is subjected to the steps purification, recrystallization annealing, hot dip coating, cooling, optional thermal, mechanical or chemical aftertreatment and coiling.
  • the annealing treatment carried out in this way can be used to activate the steel surface.
  • an N 2 -H 2 -Glühgasatmospreheat typically with unavoidable traces of H 2 O and O 2 is usually maintained in the continuous flow in the annealing furnace.
  • a first method of this kind is from the DE 10 2006 039 307 B3 known.
  • the hot-dip coated steel flat product is bright annealed under particularly reductive atmosphere conditions (low H 2 O / H 2 ratio of the annealing atmosphere and high annealing temperature).
  • a glow annealing furnace within a direct fired furnace ("DFF") pre-heating zone.
  • DFF furnace flames emitted by gas burners act directly on the flat steel product to be treated.
  • O 2 -super titanium oxide
  • the oxidation potential of the atmosphere surrounding the steel flat product is adjusted in such a way that a covering FeO layer is deliberately formed on the surfaces of the flat steel product. This FeO layer inhibits the selective oxidation of the oxygen-affine alloying elements of the flat steel product.
  • a second annealing step which is subsequently carried out in a holding zone, the FeO layer is again completely reduced back to metallic iron.
  • a method approach of this kind has long been from the DE 25 22 485 A1 known.
  • the advantage of preheating the flat steel product in a preheating furnace designed in DFF design consists in addition to the above-mentioned effects that can be achieved particularly high heating rates of the steel strip, which significantly reduces the duration of the annealing cycle and thus coupled with the output of a corresponding continuous furnace Can significantly increase hot dip coating plant.
  • the setting of an optimal FeO layer thickness of 20-200 nm in a homogeneous, uniform distribution over the bandwidth is difficult to control only by trimming the DFF burner flames. Both too low and too thick a FeO layer can lead to wetting and adhesion defects.
  • the respectively provided flat steel product is heat-treated in a continuous processing process on a hot-dip coating installation with DFF preheater and a holding zone, immediately afterwards cooled and surface-finished in-line.
  • a zinc, zinc / aluminum, zinc / magnesium, aluminum or Aluminum / silicon hot dip coating can be applied. Coatings of this type are also referred to in the art as, for example, the abbreviations "Z”, “ZF”, “ZM”, "ZA”, “AZ”, "AS”.
  • a particular combination of particularly homogeneous pre-oxidation in the DFF preheater and targeted humidification of the annealing atmosphere in the holding zone prepares the respective flat steel product in a manner such that the surface of the flat steel product is largely free of interfering oxides when it enters the respective hot-dip bath.
  • the flat steel product thus provided is, if necessary, subjected to a conventionally performed cleaning.
  • the steel flat product is heated within a heating time of 5 - 60 s, in particular 5 - 30 s, in a preheating furnace of the DFF type to a 600 - 1100 ° C, in particular 750 - 850 ° C, holding temperature.
  • a heating time of at least 5 s is required to heat the flat steel product to the required minimum temperature of 600 ° C.
  • a heating time of max. 60 s should not be exceeded in order to set an optimum starting structure for the annealing process. Further heating-up times carry the risk and the necessary mechanical properties of the final product can not be achieved.
  • a shortening of the heating time to a maximum of 30 s contributes to the improvement of the plant output and the economic efficiency of the process.
  • a reducing or neutral atmosphere which consists essentially of N 2 and additionally 5 to 15% by volume CO 2 , 0.1 to 2.0% by volume CO, and in total, is maintained relative to the steel surface at most 10 vol .-% H 2 , O 2 and H 2 O consists. Even with a total of up to 10 vol .-% of H 2 + O 2 + H 2 O, the proportion of oxygen in the atmosphere is so low that the atmosphere is neutral or reducing compared to the iron of the steel substrate.
  • the flat steel product is exposed to a preoxidation atmosphere during the heating phase for 1-15 s, which amounts to 0.01-3.0% by volume. Contains O 2 .
  • the pre-oxidation should be carried out at temperatures of at least 550 ° C, because only from this temperature begins to prevent the pre-oxidation to prevent selective oxidation of the alloying elements.
  • the pre-oxidation is carried out at temperatures up to 850 ° C, because at higher temperatures, the oxide layer is too thick. Experiments have shown that a pre-oxidation in the temperature range of 600 - 700 ° C provides optimal coating results.
  • a 20-300 nm forms on each processed flat steel product, optimally 20 to 200 nm thick FeO layer, which covers the steel surface covering.
  • Temperatures of at least 600 ° C are required to achieve sufficient recrystallization of the base material.
  • temperatures of a maximum of 1100 ° C should not be exceeded in order to avoid coarse grain formation.
  • the holding temperature is preferably 750-850 ° C, because this represents the optimum production range in terms of plant utilization and cost-effectiveness of the process.
  • the relevant process window within the heating phase can be realized by operating at least one of the burners associated with the pre-oxidation zone with O 2 excess ( ⁇ > 1).
  • the aim is to produce a very homogeneous FeO layer of uniform thickness on the flat steel product.
  • a significant O 2 - or air stream can be injected separately by means of a so-called "jet pipe" in the combustion flame.
  • Jet pipes allow a highly concentrated gas flow with high flow velocity and correspondingly high kinetic energy.
  • the inventively directed into the burner flame, discharged from the jet pipe gas flow causes a strong turbulence of the burner flame.
  • the distribution of the gas components, in particular in the Vormérmöfen blown in oxygen over the furnace cross-section substantially uniformed. This results in an optimal effect when the injection rate of the gas flow is set to 60-180 m / s.
  • the temperature of the injected gas can be up to 100 ° C above the pre-oxidation temperature.
  • At least two burners are used in the preheating furnace, one of which is assigned to one of the upper side and the other of the lower side of the respectively processed flat steel product.
  • the DFF preheating oven can be preceded by an additional DFI booster, which heats the steel strip evenly and quickly without pre-oxidizing and improves belt cleaning. This can additionally increase plant output.
  • the inventively preoxidized flat steel product passes through 30-120 s, in particular 30-60 s, an annealing furnace connected to the preheating furnace, in which it is subjected to a recrystallizing annealing at the respective holding temperature.
  • the annealing furnace in which holding at the holding temperature is carried out, is typically designed in RTF-type.
  • the minimum throughput time of 30 s is required to fully recrystallize the material.
  • the maximum cycle time of 120 s should not be exceeded in order to prevent coarse grain formation.
  • a turnaround time of 30-60 seconds proves to be advantageous not only in terms of optimum furnace throughput and equally optimal plant application for economic reasons, but also after dissolution of the FeO layer to which it acts due to the reducing Fe Atmosphere comes to avoid external oxidation of the alloying elements (Mn, Si, Al, Cr, ...) of the steel substrate.
  • the annealing gas atmosphere prevailing in the annealing furnace consists of 0.01-85.0% by volume of H 2 , up to 5% by volume of H 2 O, less than 0.01% by volume of O 2 and the remainder N 2 .
  • the preferred range for the hydrogen content is 3.0-10.0 vol%. From 3 vol .-% hydrogen in the atmosphere, it is possible to set a sufficient reduction potential compared to FeO even with short annealing times. It is preferable to set levels of less than or equal to 10.0% by volume of hydrogen for resource saving and to reduce H 2 consumption.
  • the dew point "TP" of the annealing atmosphere is kept at -40 ° C to +25 ° C.
  • the dew point is -40 ° C. or more in order to minimize the driving force of the external oxidation of the alloying elements (eg, Mn, Al, Si, Cr).
  • a dew point of at most +25 ° C avoids unwanted oxidation of iron. It could be shown experimentally that at a dew point of at least -30 ° C particularly good surface results are obtained.
  • the dew point is preferably at most 0 ° C in order to minimize the risk of surface decarburization.
  • the annealing parameters of the recrystallizing annealing are to be adjusted overall so that during the annealing a reduction of the FeO is produced, which has been formed on the surfaces of the flat steel product in the course of the preceding preoxidation (step c).
  • the flat steel product annealed according to the invention has a surface consisting essentially of metallic iron.
  • this effect is prevented by the reduction, carried out according to the invention, of the FeO present on the pre-oxidized flat steel product in combination with a targeted moistening of the annealing furnace section.
  • the FeO layer which is still present completely on the pre-oxidized flat steel product as it enters the annealing furnace is converted to metallic iron by the onset of reduction by the H 2 contained in the annealing atmosphere to form gaseous H 2 O.
  • At least one moistening device is provided, with which the annealing atmosphere can be selectively supplied with moisture to compensate for moisture loss or irregularities.
  • annealing furnaces used for the recrystallizing annealing of a flat steel product are flowed through by a gas flow directed from its exit in the direction of its entrance against the conveying direction of the steel flat product to be treated. It is therefore particularly appropriate for the targeted Moisture supply provided to arrange at least one humidifier adjacent to the output of the annealing furnace.
  • This arrangement not only results in a uniform distribution of moisture supported by the gas flow, but also takes into account the fact that the amount of water vapor resulting from the reduction of the FeO deposit of the flat steel product steadily decreases in the direction of the exit of the annealing furnace and, accordingly, without the supply of additional moisture the dew point could fall below the critical value.
  • an atmosphere is thus ensured by the targeted introduction of moisture into the annealing atmosphere over the entire length of the conveying path through the annealing furnace, whose dew point is always above the critical threshold value.
  • the inventively provided moistening device may consist of a slotted or perforated tube, wherein optimally each such tube is arranged transversely to the conveying direction of the flat steel product above and below the conveying path.
  • the individual design of the system may require the installation of additional humidifiers distributed over the holding zone length in order to ensure the desired homogeneity of the annealing atmosphere with respect to the dew point.
  • Regulation of the dew point as well as the dew point distribution in the annealing furnace can additionally be effected by regulating the respectively injected carrier gas volume flow or the velocity of the gas flow within the annealing furnace.
  • the speed of the gas flow flowing through the annealing furnace can be manipulated by changing the pressure gradient between the exit region of the annealing furnace and an exhaust, which is typically positioned at the beginning of the preheating furnace. This change can be done by controlling the suction or the injected Glühgasmenge in the oven room.
  • the pressure gradient is usually set to values of 2 - 10 mmWs.
  • the preheating furnace should be removed from the Annealing furnace are divided so that the possibly discharged from the annealing furnace, flowing in the direction of the preheating H 2 volume fractions are set before reaching the pre-oxidation zone.
  • an O 2 -containing, for example, pure O 2 gas flow or air flow present gas flow are introduced to vent from the annealing furnace in this area penetrating H 2 to H 2 O.
  • the amount of O 2 injected in each case is regulated in such a way that it is usually tunnel-like formed transition region between preheating and annealing furnace metrologically largely H 2 is not detectable.
  • the targeted Abresure of reaching into the preheating furnace hydrogen can also be done by at least one arranged in the vicinity of the output of the preheating furnace last burner of the preheating furnace is operated with such a high excess of O 2 , that in consequence of this excess of there excess O 2 content of the pre-oxidation atmosphere, in turn, sets the hydrogen, which may enter the preheating furnace, into water vapor.
  • the flat steel product which now has an active surface consisting essentially of metallic iron, is cooled to the required bath inlet temperature.
  • the bath inlet temperature is varied between 430 and 800 ° C.
  • the bath inlet temperature is typically 430-650 ° C and the temperature of the molten bath is in the range of 420-600 ° C.
  • bath inlet temperatures will typically occur of the flat steel product of 650 - 800 ° C at melt bath temperatures of 650 - 780 ° C chosen.
  • an overaging treatment extending for 5 to 60 seconds may be added at the bath inlet temperature.
  • Such overaging treatment is useful in some steels to adjust the microstructures necessary to achieve the required material properties. This is z. This is the case, for example, with TRIP steels in which the time and temperature for the diffusion of the carbon are made available by the overaging treatment.
  • the cooled to the Badein SharePointstemperatur steel flat product is passed while avoiding contact with an oxygen-containing atmosphere, in particular with the ambient atmosphere, in the metallic molten bath.
  • a so-called proboscis is usually used, which is connected to the end of the cooling zone or the optional existing overaging zone of the annealing furnace and dipped with its free end in the melt bath.
  • the optionally existing overaging zone and in the trunk there is a protective gas atmosphere of 100% N 2 , N 2 with up to 50.0% by volume, in particular up to 10.0% by volume H 2 , or 100 % H 2 which is non-reactive or reducing in relation to the steel strip.
  • An addition of hydrogen to the inert gas atmosphere in the trunk is not required in principle. However, it turns out to be advantageous depending on tape speed and tape dimensions to coating errors To avoid upper slag. A hydrogen addition of up to 10 vol .-% has proven to be particularly favorable in this context.
  • the dew point should be between -80 - -25 ° C, especially -50 ° C to -25 ° C.
  • the dew point of the inert gas atmosphere in the trunk should not be below -80 ° C, because the atmosphere is too dry underneath. This could lead to the formation of dust, which in turn would negatively affect the coating result.
  • the dew point of the inert gas atmosphere in the trunk should not be above -25 ° C, because otherwise the atmosphere would be too wet, which in turn would bring an increased slag formation with it.
  • a minimized risk of dust formation and simultaneously high process stability arise when the dew point in the trunk is between -50 ° C to -25 ° C.
  • the steel flat product thus conducted into the melt bath passes through the melt bath within a residence time of 1 to 10 s, in particular 2 to 5 s.
  • the passage time is at least 1 s, it is ensured that in the molten bath, a reactive wetting between the steel surface and the coating bath takes place.
  • the cycle time should not exceed 10 s to avoid unwanted coating sagging.
  • the time span of 2 to 5 s for the throughput time has proven to be particularly suitable in order to ensure a surface texture optimized with regard to the coating and adhesion results.
  • the thickness of the metallic protective layer present on the steel flat product exiting the melt bath is adjusted in a conventional manner.
  • known devices such as wiping nozzles or the like can be used.
  • the hot dip coated steel flat product may be thermally post-treated inline on the hot dip coating to produce a Fe-Zn alloy coating ("ZF coating").
  • ZF coating Fe-Zn alloy coating
  • a molten bath has been found to contain, in addition to zinc and unavoidable impurities including traces of Si, Mn and Pb, 0.1-0.15 wt% Al and up to 0.5 wt% Fe.
  • the hot-dip coating installation A has, in a horizontally oriented conveying direction F of the steel flat product S to be coated, to be coated, a DFI booster 1 optionally provided for preheating the flat steel product S, a preheating furnace 3 connected to its input 2 to the DFI booster, in which a Voroxidationsabites 4 is formed, an annealing furnace 6, which is connected to a transition region 7 to the output 8 of the preheating furnace 3, connected to the output 9 of the annealing furnace 6 cooling zone 10, connected to the cooling zone 10 proboscis 11, the the outlet 12 of the cooling zone 10 is connected and immersed with its free end in a melt bath 13, a arranged in the melt bath 13 first deflecting means 14, a means 15 for adjusting the thickness of the applied on the Stahlflach GmbH S in the melt bath 13 metallic coating and a second deflection 16 on.
  • a DFI booster 1 optionally provided for preheating the flat steel product S
  • a preheating furnace 3 connected to its input 2 to the DFI
  • the preheating furnace 3 is of the DFF type. In it are distributed over the conveyor line of the preheating furnace 3 in Fig. 1 arranged for the sake of clarity not shown burner. One group of these burners is assigned to the underside and another group of the upper side of the flat steel product S to be coated. Outside the pre-oxidation section 4, the burners are designed in a conventional manner and are supplied in a known manner with the required fuel gas and oxygen.
  • the burners each form a jet / jet-tube combination 17 of the in Fig. 2
  • the burners 18 of the burner / jet-tube combinations 17 are each connected via a fuel gas line 19 to a fuel gas supply, not shown here, and via an oxygen supply line 20 to an oxygen supply, also not shown here.
  • a respective oxygen branch line 22 is connected to the oxygen supply line 20 via a control valve 21.
  • the oxygen branch line 22 leads to each one of the type in the DE 10 2004 047 985 A1 explained prior art jet pipe 23, which directs the emerging from it with high flow energy and concentration of oxygen gas jet in the burner flame. In this way, a strong turbulence of the burner flame and thus an intense Contact the burner flame and prevailing in the pre-oxidation zone Voroxidationsatmospreheat with the coated steel flat product S causes.
  • a device for selectively feeding oxygen or air into the transition region 7.
  • the purpose of this feed is the setting of hydrogen, which possibly passes in the transition region 7 as a result of flowing in the annealing furnace 6 from the outlet 9 in the direction of its inlet gas flow G.
  • a suction device 24 is arranged in the region of the entrance of the annealing furnace 6, which sucks the reaching to the entrance of the annealing gas flow G.
  • two humidifiers 25,26 Adjacent to the outlet 9 of the annealing furnace 6 two humidifiers 25,26 are arranged, one of which is assigned to the top and the other of the underside of the flat steel product S to be coated.
  • the moistening devices 25, 26 are designed as slotted or perforated tubes oriented transversely to the conveying direction F of the flat steel product S and connected to a supply line 27, via which the moistening devices 25, 26 are supplied with steam or a moistened carrier gas, such as N 2 or N 2 /. H 2 , to be supplied.
  • the cooling zone 10 can be designed so that the cooled to the respective bath inlet temperature flat steel product S before it enters the trunk 11 still in the cooling zone 10 undergoes an overaging treatment at the bath inlet temperature.
  • the flat steel product S is deflected at the first deflection device 14 in the vertical direction and passes through the device 15 for adjusting the thickness of the metallic protective layer. Subsequently, the steel flat product S provided with the metallic protective layer is deflected again in the horizontal conveying direction F at the second deflection device 16 and, if appropriate, subjected to further treatment steps in plant parts not shown here.
  • the hot-dip coated samples each consisted of one of the high / high strength steels S1-S7, whose composition is given in Table 1.
  • Table 1 stolen C Mn Si Cr al Not a word S1 0.23 1.60 0.12 0.05 1.00 0,004 S2 0.07 1.45 0.11 0.49 0.03 ⁇ 0.002 S3 0.12 1.75 0.10 0.50 1.30 0,100 S4 0.22 1.75 0.10 0.10 1.55 0,100 S5 0.16 1.60 1.60 0.06 0.05 0,010 S6 0.15 1.85 0.25 0.70 0.70 ⁇ 0.002 S7 0.24 1.22 0.25 0.13 0.03 ⁇ 0.002 All data in% by weight, balance iron and unavoidable impurities
  • a hot-dip coated flat steel product according to the invention is excellently suited, due to its mechanical properties and surface properties, to be further processed by means of one-, two- or multi-stage cold or hot forming to form a high-strength / high-strength sheet metal component.
  • a sheet metal component continues to be distinguished by its particular resistance to environmental influences.
  • the use of a hot-dip coated steel flat product according to the invention thus not only raises lightweight potential, but also prolongs the product life.
  • the process according to the invention achieves optimum wetting and adherence of the hot-dip coating by a pre-oxidation in a DFF preheating furnace and a humidification of the annealing atmosphere in a holding zone in a hot-dip coated flat steel product.
  • a pre-oxidation in a DFF preheating furnace and a humidification of the annealing atmosphere in a holding zone in a hot-dip coated flat steel product.
  • the steel flat product is recrystallized in such a manner heated to a holding temperature of 600 - 1100 ° C steel flat product under a FeO reducing atmosphere whose dew point is maintained by moisture addition at -40 ° C to +25 ° C, below a ⁇ 100% N2 and a dew point cooled from -80 ° C to -25 ° C atmosphere to a bath inlet temperature of 420 - 780 ° C and passed through a melt bath.

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  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Heat Treatment Of Sheet Steel (AREA)

Claims (15)

  1. Procédé de fabrication d'un produit plat en acier muni par immersion à chaud d'une couche de protection métallique, comprenant les étapes de travail suivantes :
    a) Préparation d'un produit plat en acier laminé à chaud ou à froid constitué par, outre du fer et des impuretés inévitables, (en % en masse), jusqu'à 35,0 % de Mn, jusqu'à 10,0 % de Al, jusqu'à 10,0 % de Si, jusqu'à 5,0 % de Cr, jusqu'à 2,0 % de Ni, respectivement jusqu'à 0,5 % de Ti, V, Nb, Mo, respectivement jusqu'à 0,1% de S, P et N, jusqu'à 1,0 % de C et, au choix, 0,0005 - 0,01 % de B ;
    b) Nettoyage au choix du produit plat en acier ;
    c) Réchauffement du produit plat en acier à une température de maintien allant de 600 à 1100 °C, auquel cas
    c.1) le réchauffement a lieu pendant une durée de réchauffement allant de 5 à 60 secondes,
    c.2) le réchauffement a lieu dans un four de préchauffage du type DFF (« DFF » = « Direct Fired Furnace »),
    c.3) dans lequel est formée une section de préoxydation, dans lequel le produit plat en acier présente une température de préoxydation de 550 à 850 °C et dans lequel est tout d'abord exposé, pendant 1 à 15 secondes, à une atmosphère oxydante avec une teneur en oxygène de 0,01 - 3,0 % en volume qui est introduite dans une atmosphère de préoxydation par soufflage d'un flux gazeux contenant de l'oxygène dans la flamme d'au moins un brûleur associé à la section de préoxydation afin de former sur la surface du produit plat en acier une couche de recouvrement de FeO,
    c.4) tandis qu'il règne hors de la section de préoxydation dans le four de préchauffage une atmosphère réductrice ou neutre par rapport à la surface de l'acier qui se compose de N2 et, en outre, de 5 - 15 % en volume de CO2, 0,1 - 2,0 % en volume de CO et au total au maximum 10 % en volume de H2, O2 et H2O ;
    d) Recuit de recristallisation du produit plat en acier en maintenant le produit plat en acier pendant une durée de maintien de 30 - 120 secondes à une température de maintien dans un four de recuit qui est situé à la suite du four de préchauffage, afin d'entraîner une recristallisation du produit plat en acier, auquel cas
    d.1) il règne dans le four de recuit une atmosphère de recuit agissant de manière réductrice par rapport au FeO et étant constituée par 0,01 - 85,0 % en volume de H2, au total jusqu'à 5 % en volume de H2O, moins de 0,01 % en volume de O2, le reste étant de N2 et
    d.2) le point de rosée de l'atmosphère de recuit sur l'ensemble du parcours du produit plat en acier à travers le four de recuit est maintenu entre -40 °C et +25 °C par l'apport d'humidité à l'aide d'au moins d'un dispositif d'humidification servant à compenser les pertes ou irrégularités de la répartition de l'humidification de l'atmosphère ;
    e) Refroidissement du produit plat en acier à une température d'entrée dans le bain qui se monte à 430 - 800 °C, auquel cas le refroidissement a lieu sous une atmosphère de refroidissement étant constituée de 100 % en volume de N2, et de N2 avec jusqu'à 50,0 % en volume de H2 ou 100 % de H2, ainsi que des impuretés inévitables ;
    f) Au choix, maintien du produit plat en acier pendant 5 - 60 secondes à la température d'entrée dans le bain et sous l'atmosphère de refroidissement ;
    g) Introduction du produit plat en acier dans un bain de fusion dont la température est de 420 - 780 °C, auquel cas dans la zone de transition vers le bain de fusion l'atmosphère de refroidissement est maintenue et le point de rosée de l'atmosphère de refroidissement est réglé entre -80°C et -25°C ;
    h) Passage du produit plat en acier à travers le bain de fusion et réglage de l'épaisseur de la couche de protection métallique disponible sur le produit plat en acier sortant du bain de fusion ;
    i) Au choix, traitement à chaud du produit plat en acier pourvu de la couche de protection métallique.
  2. Procédé selon la revendication 1, caractérisé en ce que la durée de réchauffement est de 5 - 30 secondes.
  3. Procédé selon une des revendications précédentes, caractérisé en ce que la température de préoxydation est de 600 - 700 °C.
  4. Procédé selon une des revendications précédentes, caractérisé en ce que le au moins un brûleur associé à la section de préoxydation est exploité avec un excédent de O2 (facteur d'air λ > 1).
  5. Procédé selon une des revendications précédentes, caractérisé en ce que le courant de gaz contenant de l'oxygène est introduit dans la flamme du brûleur associé à la section de préoxydation par l'intermédiaire d'une buse jet qui dirige un jet gazeux concentré dirigé en direction de la flamme.
  6. Procédé selon une des revendications précédentes, caractérisé en ce qu'au moins deux brûleurs sont associés à la section de préoxydation.
  7. Procédé selon une des revendications de 1 à 4, caractérisé en ce que l'on utilise en tant que brûleur un booster DFI, lors duquel une rampe de brûleur est à chaque fois associée à la partie supérieure et partie inférieure du produit plat en acier.
  8. Procédé selon une des revendications précédentes, caractérisé en ce que la température de maintien se monte à 750 - 850 °C.
  9. Procédé selon une des revendications précédentes, caractérisé en ce que le four de recuit est du type RTF (« RTF » = « Radiant Tube Furnace »).
  10. Procédé selon une des revendications précédentes, caractérisé en ce que l'atmosphère de recuit contient, pendant la phase de maintien, 3,0 - 10,0 % en volume de H2, au total jusqu'à 5 % en volume de H2O, moins de 0,01 % en volume de O2, le reste étant de N2.
  11. Procédé selon une des revendications précédentes, caractérisé en ce que le point de rosée de l'atmosphère de recuit est maintenu sur l'ensemble du trajet du produit plat en acier à travers le four de recuit entre - 30 °C et 0 °C.
  12. Procédé selon une des revendications précédentes, caractérisé en ce que le au moins un dispositif d'humidification est agencé adjacent à la sortie du four de recuit et le four de recuit est traversé par un écoulement gazeux qui est dirigé en direction de l'entrée de celui-ci.
  13. Procédé selon une des revendications précédentes, caractérisé en ce que l'on utilise de la vapeur d'eau ou un gaz N2 humidifié avec au choix une teneur en H2 en tant qu'agent de support pour l'introduction d'humidité à l'aide du dispositif d'humidification.
  14. Procédé selon une des revendications précédentes, caractérisé en ce qu'un écoulement gazeux contenant du O2 est introduit dans la zone de transition allant du four de préchauffage au four de recuit afin de faire réagir le H2 entrant dans cette zone par le four de recuit en H2O.
  15. Procédé selon une des revendications précédentes, caractérisé en ce que l'atmosphère de refroidissement comporte au maximum 10,0 % en volume de H2.
EP12735114.6A 2011-07-11 2012-07-05 Procédé de fabrication d'un produit plat en acier muni par immersion à chaud d'une couche de protection métallique Not-in-force EP2732062B1 (fr)

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DE102011051731A DE102011051731B4 (de) 2011-07-11 2011-07-11 Verfahren zur Herstellung eines durch Schmelztauchbeschichten mit einer metallischen Schutzschicht versehenen Stahlflachprodukts
PCT/EP2012/063069 WO2013007578A2 (fr) 2011-07-11 2012-07-05 Procédé de fabrication d'un produit plat en acier muni par immersion à chaud d'une couche de protection métallique

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CA (1) CA2839183C (fr)
DE (1) DE102011051731B4 (fr)
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FR2920439B1 (fr) 2007-09-03 2009-11-13 Siemens Vai Metals Tech Sas Procede et dispositif d'oxydation/reduction controlee de la surface d'une bande d'acier en defilement continu dans un four a tubes radiants en vue de sa galvanisation
EP2055799A1 (fr) 2007-11-05 2009-05-06 ThyssenKrupp Steel AG Produit en tôle d'acier doté d'une coiffe métallique anti-corrosion et procédé de production d'une coiffe Zn-Mg métallique anti-corrosion sur un produit en tôle d'acier
DE102009018577B3 (de) 2009-04-23 2010-07-29 Thyssenkrupp Steel Europe Ag Verfahren zum Schmelztauchbeschichten eines 2-35 Gew.-% Mn enthaltenden Stahlflachprodukts und Stahlflachprodukt
DE102010037254B4 (de) 2010-08-31 2012-05-24 Thyssenkrupp Steel Europe Ag Verfahren zum Schmelztauchbeschichten eines Stahlflachprodukts

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3511430A1 (fr) 2018-01-12 2019-07-17 SMS Group GmbH Procédé de traitement thermique en continu d'une bande en acier et installation de revêtement par immersion en bain fondu d'une bande en acier
EP3686534A1 (fr) 2019-01-23 2020-07-29 Drever International Procédé et four pour le traitement thermique d'une bande d acier de haute résistance comprenant une chambre d homogénéisation en température
BE1026986A1 (fr) 2019-01-23 2020-08-17 Drever Int Sa Procédé et four pour le traitement thermique d’une bande d’acier de haute résistance comprenant une chambre d’homogénéisation en température

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WO2013007578A3 (fr) 2013-05-02
US9096919B2 (en) 2015-08-04
DE102011051731B4 (de) 2013-01-24
DE102011051731A1 (de) 2013-01-17
WO2013007578A2 (fr) 2013-01-17
KR20140059777A (ko) 2014-05-16
RU2573843C2 (ru) 2016-01-27
CA2839183C (fr) 2018-12-11
KR101940250B1 (ko) 2019-01-18
EP2732062A2 (fr) 2014-05-21
US20140251505A1 (en) 2014-09-11
CA2839183A1 (fr) 2013-01-17
ES2593490T3 (es) 2016-12-09
JP2014525986A (ja) 2014-10-02
RU2014104593A (ru) 2015-08-20
JP5753319B2 (ja) 2015-07-22

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