EP3186401B1 - Procédé de fabrication d'un acier d'emballage nitruré - Google Patents

Procédé de fabrication d'un acier d'emballage nitruré Download PDF

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EP3186401B1
EP3186401B1 EP15732735.4A EP15732735A EP3186401B1 EP 3186401 B1 EP3186401 B1 EP 3186401B1 EP 15732735 A EP15732735 A EP 15732735A EP 3186401 B1 EP3186401 B1 EP 3186401B1
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Prior art keywords
nitrogen
steel
ppm
annealing furnace
gas
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German (de)
English (en)
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EP3186401A1 (fr
Inventor
Burkhard KAUP
Blaise Massicot
Dirk Matusch
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ThyssenKrupp AG
ThyssenKrupp Rasselstein GmbH
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ThyssenKrupp AG
ThyssenKrupp Rasselstein GmbH
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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
    • 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
    • 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
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • 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
    • C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
    • 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
    • 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
    • C21D8/0257—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
    • 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
    • C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
    • 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
    • C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
    • C21D8/0405—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing of ferrous alloys
    • 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
    • C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
    • C21D8/0421—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing characterised by the working steps
    • C21D8/0436—Cold 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
    • C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
    • C21D8/0447—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing characterised by the heat treatment
    • C21D8/0457—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
    • 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
    • C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
    • C21D8/0447—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing characterised by the heat treatment
    • C21D8/0473—Final recrystallisation annealing
    • 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
    • C21D9/48—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals deep-drawing sheets
    • 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
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • 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
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
    • 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
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • 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
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25

Definitions

  • the invention relates to a method for producing an embroidered packaging steel having the features of claim 1.
  • packaging steel flat steel products such as steel sheets or steel strips, which are intended for the production of packaging (hereinafter referred to as packaging steel), is known from the prior art.
  • packaging steel flat steel products
  • EP 0 216 399 B1 a steel sheet for packaging and a method for its production is described, which was prepared from an aluminum-killed, continuously cast carbon-manganese steel and obtained by picking up a lot of unbound, dissolved nitrogen, the minimum amount of unbound nitrogen depending on a desired hardness category of the steel sheet is defined and (for example for the hardness category T61 of the European standard 145-78) has an amount of unbound nitrogen of at least 5 ppm.
  • the chemical composition of the steel sheet disclosed therein corresponds to the usual soft steels in terms of carbon and manganese content and has, for example, a carbon content in the range of 0.03 to 0.1 wt .-% and a manganese content of 0.15 to 0.5 wt. -% on.
  • the steel sheet is characterized by a high yield strength in the range of 350-550 N / mm 2 .
  • a maximum value of 100 ppm is given, stating that the steel sheet at a higher content of unbound nitrogen due to the associated increase in strength no longer cold-rollable and thus not for the intended use as cold-rolled packaging steel suitable is.
  • a steel is first cast continuously, then hot rolled, cold rolled, recrystallized annealed and finally re-rolled. After re-rolling takes place a thermal Aftertreatment in which free dislocations formed in the steel by the temper rolling are fixed by the unbonded nitrogen introduced by the sticking to increase the hardness and yield strength over the post-rolling values.
  • the thermal aftertreatment can be suitably combined with another thermal treatment of the post-rolled steel, which is to be carried out anyway in the context of the production of a packaging steel, such as, for example, melting a layer of tin electrolytically applied to the surface of the steel sheet or baking a paint layer applied to the steel sheet surface ,
  • a low aluminum steel strip for the manufacture of containers which produce a hot rolled steel strip containing between 0.050% and 0.080% by weight of carbon, between 0.25% and 0.40% by weight of manganese, less than 0.020 %
  • the nitrogen content of the Stahlabnds is ensured by the addition of calcium cyanamide in the ladle during steel extraction or by blowing gaseous nitrogen into the steel bath.
  • JP 11315343-A is a steel strip with a carbon content of ⁇ 0.06%, a silicon content of ⁇ 0.03%, a manganese content of 0.05% to 0.5%, a phosphorus content of ⁇ 0.02%, a sulfur content of ⁇ 0, 02%, an aluminum content of 0.02% to 0.10% and a nitrogen content of 0.005% to 0.015% for the Production of cans known in the production of a hot steel rolled slab to a hot strip and the hot strip is first cold rolled, then annealed and finally re-rolled.
  • WO 2013/183274 A1 is a three-piece can and a process for its manufacture from a steel sheet having a carbon content of at least 0.02 and up to 0.10%, a silicon content of ⁇ 0.10%, a manganese content of 0.1% to 0.8% , a phosphorus content of 0.001% to 0.10%, a sulfur content of 0.001% to 0.02%, an aluminum content of 0.005 to 0.10% and a nitrogen content of 0.013 to 0.020%.
  • the steel strip has tensile strengths of 440 MPa or more and an elongation at break of 12% or more.
  • the embroidering of a steel can be introduced in the manufacturing process of the steel by introducing nitrogen into the molten steel, for example by blowing nitrogen gas N 2 .
  • a method of embossing steel melts in steelmaking in the oxygen inflation method is, for example, in US Pat DE 2 237 498 described.
  • Flat steel products, in particular steel strips, can be embroidered by a surface conditioning, for example by diffusion of nitrogen into the steel sheet surface, which can be done for example by gas nitriding in an ammonia atmosphere with slight overpressure, by bath nitriding in nitrogen-containing salt baths or by plasma nitriding.
  • By diffusion of nitrogen forms on the steel sheet surface while a hard, superficial bonding layer and an underlying diffusion zone in which the nitrogen is embedded to a certain depth in the (ferritic) steel matrix.
  • the object of the invention is to show a flat steel product (sheet steel or steel strip) for the production of packaging, which has the highest possible strength combined with good elongation at break and good forming properties.
  • a packaging steel with strengths of at least 600 MPa with an elongation at break of at least 5% should be made available.
  • the higher-strength packaging steel must at the same time have sufficient formability for the intended use as packaging steel, for example in deep-drawing or ironing process, so that from the flat steel product intended packaging, such. Canned or beverage cans can be produced.
  • the present as flat steel product packaging steel should have the usual thicknesses in the fine and Feinstblech Scheme, which are regularly produced by cold rolling.
  • the process of the present invention can produce an embroidered packaging steel having a carbon content of 10 to 1000 ppm and an amount of unbound steel dissolved nitrogen of greater than 100 ppm and preferably greater than 150 ppm, with the steel being upset in two stages ,
  • a molten steel is nitrided to a maximum nitrogen content of 160 ppm by feeding nitrogen to the molten steel, for example in the form of a nitrogen-containing gas and / or a nitrogen-containing solid.
  • a slab is poured and hot rolled into a hot strip.
  • the hot strip is subsequently pickled (after cooling to ambient temperature), if necessary, and cold rolled to a flat steel product (steel sheet or steel strip).
  • the cold-rolled steel flat product is then recrystallized in an annealing furnace.
  • the second step of the nitrogenizing step is carried out by introducing a nitrogen-containing gas into the annealing furnace and directing it to the flat steel product to increase the amount of unbound nitrogen in the steel beyond the amount of nitrogen introduced into the molten steel in the first stage of the nitrogenizing step continue to increase.
  • the two-stage embroidering of the packaging steel ensures that the hot-rolled strip is used with those commonly used for the production of packaging steels Cold rolling devices (rolling mills) easily to a flat steel product, in particular to a steel strip, can be cold rolled. This is made possible by the fact that in the first stage of the Aufstickens a content of unbound nitrogen of at most 160 ppm is introduced into the molten steel.
  • the hot strip produced from the embroidered molten steel by hot rolling remains cold-rolled at these nitrogen contents, so that a fine or very fine sheet can be produced in the standard thickness for packaging purposes from the hot strip by cold rolling. Higher nitrogen contents in the molten steel also lead to undesirable defects in the slab cast from the molten steel.
  • the desired strength of the packaging steel preferably greater than 600 MPa, is achieved during cold rolling and in the second stage of the nitrogen blanketing of the flat steel product during its recrystallizing annealing.
  • flat steel products, in particular steel strips, with thicknesses in the fine and Feinstblech Scheme for use as packaging steel with very high tensile strengths at the same time high elongation at break of preferably at least 5% can be produced without suffering a restriction in the forming properties.
  • the steel melt is embossed in the first stage by introducing nitrogen gas (N 2 ) and / or lime nitrogen (CaCN 2 ) and / or manganese nitrogen (MnN) into the molten steel.
  • the embroidering of the flat steel product in the second stage is preferably carried out by introducing ammonia gas (NH 3 ) into the annealing furnace, in which the steel flat product is annealed in a recrystallizing manner.
  • the ammonia gas is thereby gassed by means of spray nozzles on the surface of the flat steel product.
  • the amount of ammonia gas introduced into the annealing furnace is preferably adjusted so that an ammonia equilibrium with an ammonia concentration in the range of 0.05 to 1.5% is established in the annealing furnace.
  • the ammonia concentration in the annealing furnace is preferably detected by means of an ammonia sensor, and the detected value of the ammonia equilibrium concentration is used for controlling the amount of ammonia gas introduced into the annealing furnace per unit time.
  • an inert gas is preferably introduced into the annealing furnace during the recrystallizing annealing in the annealing furnace in the second stage of the addition of nitrogen, for example nitrogen gas and / or hydrogen gas or a mixture thereof, for example in a composition of 95% by weight. Nitrogen gas and 5% by weight of hydrogen gas.
  • the total amounts of unbound nitrogen introduced by the two-stage embroidering of the packaging steel are between 100 and 500 ppm, preferably above 150 ppm and more preferably in the range between 200 and 350 ppm.
  • a maximum nitrogen content of 160 ppm is introduced into the molten steel. Maintaining an upper limit of about 160 ppm for the content of unbound nitrogen in the molten steel ensures that no defects occur on the slab produced from the molten steel, for example in the form of pores and cracks, which can oxidise by ambient oxygen.
  • the hot strip produced from the slab remains cold-rolled at a nitrogen content of at most 160 ppm.
  • the amount of unbound nitrogen which can additionally be introduced in the second stage when the steel flat product is being embroidered is preferably in the range from 180 to 350 ppm.
  • a total amount of unbound nitrogen in the packaging steel according to the invention of up to 500 ppm can be introduced by the two stages of the embroidering.
  • tensile strengths of more than 650 MPa and up to 1000 Mpa can be achieved, whereby a linear relationship has been established between the content of unbound nitrogen and the tensile strength and, for example for tensile strengths of about 650 MPa, a content of unbound nitrogen of approx 200 ppm is required.
  • the cold-rolled steel flat product For recrystallizing annealing of the cold-rolled steel flat product, it is preferably heated in the annealing furnace to temperatures of more than 600 ° C. and in particular of more than 620 ° C.
  • the recrystallizing annealing restores the formability of the cold-rolled steel flat product.
  • heating of the flat steel product to a temperature of 620 ° C. to 660 ° C. and more preferably of approximately 640 ° C. has proven to be preferred.
  • a plurality of spray nozzles is preferably used, with which a nitrogen-containing gas, such. Ammonia gas can be uniformly applied to the surface of the flat steel product.
  • the plurality of spray nozzles for example transversely to the strip running direction, are preferably arranged equidistant from each other. As a result, a homogeneous nitriding of the flat steel product over the entire surface is possible.
  • an embroidered molten steel is initially produced in a converter and / or in a subsequent ladle treatment, which has a content of free, unbound (ie dissolved in steel) nitrogen of up to 160 ppm.
  • the carbon content of the steel produced is preferably in the range from 10 to 1000 ppm and more preferably between 100 and 900 ppm and usually between 400 and 900 ppm.
  • the converter is filled with scrap and pig iron and the melt is blown with oxygen gas and nitrogen gas, whereby the oxygen gas (O2) from above and nitrogen gas (N2) is injected from below into the converter by means of bottom nozzles.
  • O2 oxygen gas
  • N2 nitrogen gas
  • a nitrogen content in the molten steel of 70 to 120 ppm sets, whereby it comes to a saturation.
  • the composition and esp. The nitrogen content of the melt is detected. If the given analysis has not been made (for example, if the level of phosphorus is too high) oxygen gas is bubbled through an oxygen lance and argon gas (Ar) through the bottom nozzles. Since hardly any more carbon (C) is present in the steel, no overpressure arises and the nitrogen of the air is pulled in with, whereby it can come to an additional nitriding.
  • lime-nitrogen calcium cyanamide, CaCN2
  • the lime nitrogen is added, for example, in the form of granules (5-20 mm).
  • the pan comes to the first Argon capitae, where with a refractory immersed lance with argon for about 3 minutes is rinsed. After a control analysis, if necessary, rinse a second time in a second argon rinse for about 3 minutes. The pan then comes to a third argon sink. This represents the last stage before casting.
  • manganese nitride for example in the form of a wire of MnN powder in a steel sheath, may be added to the third argon sink.
  • the amount of possibly missing nitrogen is converted into a required amount of MnN (for example, into a required length of the MnN wire), which is added to the melt.
  • the MnN is added until the predetermined target nitrogen content or Mn upper limit of the steel is reached.
  • the melt is placed in a distributor trough to pour a slab from the molten steel. Due to leaks and diffusion of atmospheric nitrogen, the nitrogen content may rise by about 10 ppm. An upper limit of the amount of dissolved nitrogen in the cast steel slab of about 160 ppm should not be exceeded, because at higher nitrogen contents, defects can form on the slab such as cracks or pores, which lead to undesired oxidation.
  • the slab cast from the molten steel is then hot rolled and cooled to room temperature.
  • the hot strip produced has thicknesses in the range of 1 to 4 mm and is possibly wound up into a roll (coil).
  • the hot strip must be cold rolled, with a reduction in thickness ranging from 50 to more than 90%.
  • Thin sheet is understood to mean a sheet with a thickness of less than 3 mm and a fine sheet has a thickness of less than 0.5 mm.
  • the hot strip which may have been wound up as a roll, is unwound from the roll, pickled and introduced into a cold rolling device, for example a cold rolling mill.
  • the cold-rolled steel strip In order to restore the crystal structure of the steel, which has been destroyed during cold rolling, the cold-rolled steel strip must be recrystallized. This is done by passing the cold-rolled steel strip through a continuous annealing furnace in which the steel strip is heated to temperatures above the recrystallization point of the steel and in particular to temperatures above 600 ° C. In the process according to the invention, a further embroidering of the steel strip in a second stage takes place simultaneously with the recrystallization annealing. This is carried out in the annealing furnace by introducing into the annealing furnace a nitrogen-containing gas, preferably ammonia (NH 3 ).
  • a nitrogen-containing gas preferably ammonia (NH 3 ).
  • FIG. 1 schematically a continuous annealing furnace for carrying out the recrystallization and the second stage of the Aufstickens is shown.
  • different zones are formed, which are in the direction of passage (tape running direction V, in FIG. 1 from right to left) of the guided through the continuous annealing furnace steel strip are arranged one behind the other.
  • a heating zone 1 arranged on the input side of the continuous annealing furnace, the steel strip S is heated to temperatures in the range from 600 ° C. to 750 ° C.
  • a temperature range of 620 ° C to 700 ° C and has proven to be particularly preferred from 620 ° C to 660 ° C. The best results were achieved at temperatures of about 640 ° C. These temperatures are above the recrystallization temperature of the steel, which is why in the heating zone 1, the steel strip S is annealed recrystallizing.
  • the heating zone 1 is followed by a holding zone 2, in which the temperature of the steel strip S is maintained in the above-mentioned temperature range.
  • a plurality of cascades 3a, 3b, 3c of spray nozzles in the strip running direction are arranged one behind the other.
  • Each cascade 3a, 3b, 3c comprises a plurality of nozzles 3, which are arranged transversely to the strip running direction at a distance from each other.
  • the nozzles 3 are coupled to a gas supply line via which they are charged with a nitrogen-containing gas.
  • a nitrogen-containing gas As the gas particularly suitable for the second stage of the gasification, ammonia gas has been found.
  • nozzles 3 of the cascades are in the German patent application DE 102014106135 from 30.4. 2014, the disclosure of which is hereby incorporated by reference.
  • a nozzle device for treating a flat steel product is described, wherein the nozzle device comprises an outer tube and an inner tube disposed therein with a primary opening for feeding a gas flowing through the nozzle device in the outer tube and the outer tube is provided with a secondary opening through which the gas escape can.
  • the primary opening of the inner tube and the secondary opening of the outer tube are offset from each other. This allows a very homogeneous flow of gas to the surface of the flat steel product.
  • a homogeneous fumigation of the surface of the steel strip in the holding zone 2 of the continuous annealing furnace with the nitrogen-containing gas (ammonia) can be achieved, whereby over the surface of the steel strip, in particular across its width, a homogeneous diffusion of nitrogen and thereby the formation of a homogeneous, nitrogen-enriched and cured surface layer can be achieved.
  • the nitrogen-containing gas ammonia
  • the method of direct loading of the steel strip (gassing) with a nitrogen-containing gas by means of nozzles has two major advantages: Firstly, only a low concentration of nitrogen (NH 3 concentration) in the protective gas is required, resulting in a low consumption of nitrogen-containing gas (eg NH 3 consumption). On the other hand, there is no formation of a nitride layer due to a very short reaction time. Following gassing with a nitrogen-containing gas (eg NH 3 treatment), the steel strip is annealed even further (expediently more than 5 seconds) at unchanged temperatures, before it is cooled. This results in a homogenization of the nitrogen distribution over the cross section of the steel strip and consequently to improved forming properties. In particular, this can be used to avoid expansion loss due to paint aging (see page 6, lines 14 - 20).
  • a nitrogen-containing atmosphere with a nitrogen equilibrium concentration which is as constant as possible must be maintained during the passage of the steel strip S through the holding zone 2 of the continuous annealing furnace.
  • a nitrogen-containing atmosphere with a nitrogen equilibrium concentration which is as constant as possible is in the range of cascades 3a, 3b, 3c with the Nozzles 3 detects the nitrogen concentration formed.
  • ammonia is used as the nitrogen-containing gas
  • the ammonia concentration formed in the holding zone 2 by gassing with ammonia is measured for this purpose.
  • a concentration sensor arranged outside the continuous annealing furnace is provided, which may, for example, be a laser spectroscopy sensor.
  • This is fed to a gas sample taken from the holding zone 2 in order to detect the ammonia concentration and from this the nitrogen concentration of the gas atmosphere in the holding zone 2.
  • the gas sample is, for example, at the in FIG. 1 taken from the point indicated by reference numeral 4.
  • the concentration of the nitrogen in the gas atmosphere of the holding zone 2 detected by the concentration sensor is supplied to and used by a controller to keep the amount of nitrogen-containing gas (ammonia) sprayed into the holding zone 2 via the nozzles 3 constant at a predetermined target value.
  • Target values for the equilibrium concentration of the ammonia in the range of 0.05 to 1.5%, and preferably of less than 1%, in particular less than 0.2%, have proven particularly expedient when ammonia is used as the nitrogen-containing gas.
  • the equilibrium concentration of the ammonia is in the range of 0.1 to 1.0%, and more preferably between 0.1 and 0.2%.
  • an inert gas is expediently introduced into the annealing furnace in the holding zone 2 in addition to the nitrogen-containing gas (ammonia).
  • This may, for example, be nitrogen gas and / or hydrogen gas.
  • a mixture of about Vol. 95% nitrogen and about Vol. 5% hydrogen gas is used.
  • a plurality of cooling zones 5, 6 adjoin the holding zone 2 in the strip running direction V, with a faster cooling of the steel strip S in a first cooling zone 5 and a slower cooling in a subsequent second cooling zone 6.
  • the steel strip S After cooling in the cooling zones 5 and 6, the steel strip S leaves the continuous annealing furnace and is dry-rolled (dressed) in order to give the strip the forming properties required for the production of packaging.
  • the degree of rolling varies between 0.4 and 2%, depending on the intended use of the packaging steel.
  • the steel strip can also be wet rolled to another Thickness reduction by up to 43% (double reduced steel strip, "double reduced DR").
  • the steel strip S is fed to a coating installation in which the surface of the steel strip, for example, is electrolytically provided with a tin or a chromium / chromium dioxide coating (ECCS) or a coating in order to increase the corrosion resistance.
  • ECCS chromium / chromium dioxide coating
  • embroidered steel strips can be produced, which are characterized by a very high strength of more than 600 MPa with simultaneously good elongation at break of more than 5% and good forming properties.
  • the increased through the two-stage Aufsticken strength and elongation at break are very homogeneous over the cross section of the steel strip both in and across the rolling direction of the cold-rolled steel strip. This results from the very homogeneous introduction of unbound nitrogen into the steel, especially in the second stage of the stitching.
  • the recrystallizing annealing and the second step of the embossing can be carried out in a continuous annealing furnace instead of in a continuous annealing furnace.
  • the cold rolled and wound as a roll steel strip S is placed in a crucible annealing furnace and annealed there under a protective gas atmosphere at the required for a recrystallizing annealing annealing temperatures of more than 520 ° C.
  • the annealing process takes place in the "open-coil" process. In this case, spacers are inserted between the layers of rolled into a roll steel strip to keep the surface of the steel strip for the diffusion of nitrogen accessible.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
  • Laminated Bodies (AREA)

Claims (15)

  1. Procédé servant à fabriquer un acier d'emballage azoté avec une teneur en carbone, rapportée au poids, allant de 10 à 1000 ppm et une teneur rapportée au poids d'un azote non lié dissous dans l'acier supérieure à 100 ppm, caractérisé par des étapes suivantes :
    a) la nitruration d'une matière fondue d'acier à une teneur d'azote rapportée au poids de 160 ppm au maximum par l'introduction d'un gaz contenant de l'azote et/ou d'une matière solide contenant de l'azote dans la matière fondue d'acier ;
    b) la coulée d'une brame composée de la matière fondue d'acier et le laminage à chaud de la brame en un feuillard à chaud ;
    c) le laminage à froid du feuillard à chaud en un produit plat en acier ;
    d) le recuit recristallisant du produit plat en acier laminé à froid dans un four de recuit, en particulier un four de recuit continu, dans lequel un gaz contenant de l'azote est introduit dans le four de recuit et est dirigé sur le produit plat en acier pour augmenter la quantité d'azote non lié dans le produit plat en acier au-dessus de la teneur en azote déjà contenue dans la matière fondue en acier.
  2. Procédé selon la revendication 1, caractérisé en ce que lors de l'étape a), la nitruration de la matière fondue en acier est effectuée par l'introduction d'azote gazeux (N2) et/ou de cyanamide calcique (CaCN2) et/ou d'azote de manganèse (MnN) dans la matière fondue d'acier.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que lors de l'étape d), du gaz ammoniac (NH3) est introduit dans le four de recuit.
  4. Procédé selon la revendication 3, caractérisé en ce que le gaz ammoniac (NH3) est dirigé sur le produit plat en acier dans le four de recuit au moyen d'une ou de plusieurs buses de pulvérisation.
  5. Procédé selon la revendication 3 ou 4, caractérisé en ce que l'ammoniac est équilibré avec une concentration dans la plage de 0,05 à 1,5 % en vol. dans le four de recuit du fait de l'introduction du gaz ammoniac (NH3).
  6. Procédé selon l'une quelconque des revendications 3 à 5, caractérisé en ce que la concentration d'ammoniac équilibrée est détectée au moyen d'un capteur d'ammoniac dans le four de recuit du fait de l'introduction du gaz ammoniac (NH3).
  7. Procédé selon la revendication 6, caractérisé en ce que la valeur de mesure détectée de la concentration d'ammoniac équilibrée est détectée pour une régulation de la quantité de gaz ammoniac introduite par unité de temps dans le four de recuit.
  8. Procédé selon l'une quelconque des revendications 3 à 7, caractérisé en ce qu'encore un gaz inerte, en particulier de l'azote gazeux (N2) et/ou du gaz d'hydrogène (H2), est introduit dans le four de recuit outre le gaz ammoniac (NH3), de manière préférée un mélange de 95 % en vol. d'azote gazeux (N2) et 5 % en vol. de gaz d'hydrogène (H2).
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la fraction en poids d'azote non lié est comprise, après la nitruration du produit plat en acier laminé à froid, dans le four de recuit entre 100 et 500 ppm, de manière préférée entre 200 et 350 ppm.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le recuit recristallisant du produit plat en acier laminé à froid est effectué lors de l'étape d) au moyen du passage du produit plat en acier à travers un four de recuit en continu, dans lequel le produit plat en acier est réchauffé à des températures supérieures à 600 °C et de manière préférée à une température allant de 620 °C à 660 °C.
  11. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la teneur en carbone de l'acier se situe, par rapport au poids, entre 100 et 1000 ppm et de manière préférée entre 500 et 900 ppm.
  12. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'épaisseur du produit plat en acier est inférieure à 0,5 mm et la répartition de la concentration de l'azote non lié fluctue sur l'épaisseur du produit plat en acier d'une valeur inférieure à ± 10 ppm autour de la valeur moyenne de la teneur d'azote rapportée à la masse.
  13. Procédé selon la revendication 12, caractérisé en ce que la répartition de concentration de l'azote non lié fluctue sur l'épaisseur du produit plat en acier d'une valeur inférieure à ± 5 ppm autour de la valeur moyenne de la teneur en azote rapportée à la masse.
  14. Procédé selon la revendication 12, caractérisé en ce que la résistance à la traction de l'acier d'emballage fabriqué avec le procédé présente une valeur supérieure à 600 MPa.
  15. Procédé selon la revendication 12, caractérisé en ce que la valeur moyenne de la teneur d'azote rapportée à la masse en azote non lié est supérieure à 150 ppm.
EP15732735.4A 2014-08-27 2015-07-02 Procédé de fabrication d'un acier d'emballage nitruré Active EP3186401B1 (fr)

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DE102014112286.0A DE102014112286A1 (de) 2014-08-27 2014-08-27 Verfahren zur Herstellung eines aufgestickten Verpackungsstahls
PCT/EP2015/065055 WO2016030056A1 (fr) 2014-08-27 2015-07-02 Procédé pour la fabrication d'un acier d'emballage azoté

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DE102020106164A1 (de) * 2020-03-06 2021-09-09 Thyssenkrupp Rasselstein Gmbh Kaltgewalztes Stahlflachprodukt für Verpackungen
DE102020112485B3 (de) * 2020-05-08 2021-08-12 Thyssenkrupp Rasselstein Gmbh Stahlblech und Verfahren zur Herstellung eines Stahlblechs für Verpackungen

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US10920309B2 (en) 2021-02-16
JP2017534748A (ja) 2017-11-24
JP6357274B2 (ja) 2018-07-11
AU2015309232A1 (en) 2017-02-02
US20170253957A1 (en) 2017-09-07
EP3186401A1 (fr) 2017-07-05
ES2734402T3 (es) 2019-12-05
CA2954713A1 (fr) 2016-03-03
KR102439567B1 (ko) 2022-09-02
KR20170046642A (ko) 2017-05-02
WO2016030056A1 (fr) 2016-03-03
CA2954713C (fr) 2020-05-12
BR112017002172B1 (pt) 2021-09-08
CN106661655B (zh) 2018-09-28
CN106661655A (zh) 2017-05-10
DE102014112286A1 (de) 2016-03-03
RS59266B1 (sr) 2019-10-31
AU2015309232B2 (en) 2018-06-14

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