WO2023181390A1 - Procédé de fabrication de tôle d'acier recuite après galvanisation par immersion à chaud - Google Patents

Procédé de fabrication de tôle d'acier recuite après galvanisation par immersion à chaud Download PDF

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WO2023181390A1
WO2023181390A1 PCT/JP2022/014582 JP2022014582W WO2023181390A1 WO 2023181390 A1 WO2023181390 A1 WO 2023181390A1 JP 2022014582 W JP2022014582 W JP 2022014582W WO 2023181390 A1 WO2023181390 A1 WO 2023181390A1
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steel sheet
dip galvanized
hot
cooling
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PCT/JP2022/014582
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English (en)
Japanese (ja)
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聖太郎 寺嶋
達也 中垣内
裕美 吉冨
克弥 星野
友輔 奥村
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Ｊｆｅスチール株式会社
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Priority to PCT/JP2022/014582 priority Critical patent/WO2023181390A1/fr
Priority to JP2024507842A priority patent/JP7480928B2/ja
Publication of WO2023181390A1 publication Critical patent/WO2023181390A1/fr

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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
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02—Extraction of non-metals
    • C21D3/06—Extraction of hydrogen
    • 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
    • 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
    • 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
    • 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 disclosure relates to a method for manufacturing an alloyed hot-dip galvanized steel sheet.
  • alloyed hot-dip galvanized steel sheets use a thin steel sheet obtained by hot-rolling or cold-rolling a slab as a base steel sheet, and the base steel sheet is processed using a continuous hot-dip galvanizing line (CGL). It is manufactured by annealing in an annealing furnace, followed by hot-dip galvanizing and alloying.
  • CGL continuous hot-dip galvanizing line
  • the easily oxidizable elements in the base steel sheet are oxidized during annealing.
  • plating properties will be used to refer to both plating appearance and plating adhesion.
  • Patent Document 1 discloses a technique in which reduction annealing is performed after forming an oxide film on the surface of the steel sheet.
  • Patent Document 2 discloses a technique for promoting dehydrogenation in a hot rolled steel sheet at a temperature of 450° C. or higher and 550° C. or lower and an H 2 concentration of 9% or higher.
  • Patent Document 3 discloses a technique for reducing the amount of hydrogen in a hot rolled steel sheet by controlling the annealing temperature and hydrogen concentration in an annealing furnace.
  • Patent Document 4 discloses a technique for changing the ratio of water vapor partial pressure to hydrogen partial pressure in a heating zone and a soaking zone.
  • Patent Document 5 discloses that a steel plate after annealing and plating is subjected to post-heating under predetermined conditions to reduce hydrogen in the steel, and high-strength molten zinc with excellent plating properties and hydrogen embrittlement resistance is used. A method of manufacturing a plated steel sheet is disclosed.
  • JP2016-53211A Japanese Patent Application Laid-Open No. 54-130443 Patent No. 3266008 specification Patent No. 5811841 specification JP2020-45568A
  • Patent Document 1 In the method described in Patent Document 1, there is room for improvement in plating properties when the amount of Mn relative to the amount of Si added to the steel is more than a predetermined amount. Further, in Patent Document 1, in order to reduce the oxidized steel plate, the steel plate is maintained at a high temperature in a reducing atmosphere containing hydrogen, and at this time, hydrogen in the furnace atmosphere penetrates into the steel. Afterwards, the steel is plated with hydrogen penetrating it, but since the diffusion of hydrogen in the plating layer is significantly slower than in the steel, there is a risk that diffusible hydrogen may remain in the steel and cause hydrogen embrittlement. There is.
  • Patent Documents 2 and 3 are both techniques for suppressing blistering (plating blistering) of hot rolled steel sheets, and are insufficient to improve the delayed fracture resistance of high strength cold rolled steel sheets. Further, in the method of Patent Document 3, when the steel plate is oxidized and reduced to ensure plating properties, the reduction is insufficient. Further, although the dew point is not specified in Patent Document 3, there is a risk that the steel plate may be oxidized depending on the balance between the dew point and the hydrogen concentration.
  • Patent Document 5 the only regulation regarding the atmosphere in the annealing process is the hydrogen concentration, and there is no mention of moisture in the furnace such as dew point. Since the method described in Patent Document 5 does not include an oxidation-reduction step, plating properties may be impaired depending on the amounts of Si and Mn contained in the steel. For example, in Example 1 of Patent Document 5, a cold-rolled steel sheet having 1.25% by mass of Si and 2.67% by mass of Mn as steel components has a dew point of -30°C without going through a pre-process such as an oxidation-reduction process. Annealed in an atmosphere and hot-dip galvanized. In this method, there is a risk that defects such as non-plating occur and the surface appearance is impaired, and as in the present invention described later, an appropriate balance between hydrogen embrittlement resistance and surface appearance is not sufficiently considered.
  • an object of the present disclosure is to provide an alloyed hot-dip galvanized steel sheet that has a beautiful surface appearance free from defects such as unplatedness, excellent plating adhesion, and also has excellent hydrogen embrittlement resistance.
  • the present disclosure has been made based on the above findings. That is, the gist of the present disclosure is as follows.
  • a cooling step of cooling the steel plate after the soaking step A plating step in which the cooled steel sheet is immersed in a hot-dip galvanizing bath to obtain a hot-dip galvanized steel sheet; an alloying step of performing an alloying treatment on the hot-dip galvanized steel sheet to obtain an alloyed hot-dip galvanized steel sheet; After cooling the alloyed hot-dip galvanized steel sheet to a cooling stop temperature below the Ms point, it is heated for 30 seconds at a temperature above the cooling stop temperature and above 100°C and below 450°C in a reheating atmosphere with a hydrogen concentration of 0.2% by volume or below. A cooling-reheating step of holding the above, A method for producing an alloyed hot-dip galvanized steel sheet.
  • the component composition satisfies [Si]/[Mn] of 0.23 or more,
  • the atmosphere in the soaking step has a dew point of -20°C or more and +20°C or less,
  • [Si] and [Mn] respectively indicate the content (mass %) of Si and Mn in the above component composition.
  • the component composition satisfies [Si]/[Mn] less than 0.23,
  • the atmosphere in the reduction step has a dew point of less than -20°C,
  • the atmosphere in the soaking step has a dew point of less than -20°C,
  • [Si] and [Mn] respectively indicate the content (mass %) of Si and Mn in the above component composition.
  • the steel plate after the soaking step is cooled at an average cooling rate of 10 from 600°C to 900°C in an atmosphere with a hydrogen concentration of 0.5% by volume to 30% by volume and a dew point of 0°C or less.
  • the component composition further comprises, in mass%, B: 0.0100% or less, Ti: 0.200% or less, Nb: 0.200% or less, Sb: 0.200% or less, Sn: 0.200% or less, V: 0.100% or less, Cu: 1.00% or less, Cr: 1.00% or less, Ni: 1.00% or less, Mo: 0.50% or less, Ta: 0.100% or less, W: 0.500% or less, Zr: 0.020% or less, Ca: 0.0200% or less, Mg: 0.0200% or less, Zn: 0.020% or less, Co: 0.020% or less, Ce: 0.0200% or less, Se: 0.0200% or less, Te: 0.0200% or less, Ge: 0.0200% or less, As: 0.0200% or less, Sr: 0.0200% or less, Cs: 0.0200% or less, Hf: 0.0200% or less, Pb: 0.0200% or less, The method for producing an alloyed hot-dip gal:
  • the alloyed hot-dip galvanized steel sheet according to any one of [1] to [7], wherein the cooling stop temperature is (Ms point -50 ° C.) or lower. Production method.
  • an alloyed hot-dip galvanized steel sheet that has a beautiful surface appearance free from defects such as unplatedness, excellent plating adhesion, and also has excellent hydrogen embrittlement resistance.
  • FIG. 3 is a diagram showing an example of atmospheric dew point measurement positions in a split annealing furnace.
  • Oxidation-reduction of steel sheets is effective for improving the plating properties of Si and Mn-containing steels.
  • annealing in a high hydrogen concentration atmosphere is essential, and a large amount of hydrogen inevitably enters the steel.
  • the hydrogen concentration during annealing is low, Fe reduction is not completed, and Fe oxide remaining on the steel sheet surface causes deterioration of plating properties.
  • annealing is divided into a reduction process and a soaking process, and after completing the reduction at a high hydrogen concentration, the hydrogen concentration in the soaking process is reduced as necessary to the minimum level that does not re-oxidize Fe. This makes it possible to reduce hydrogen that has once penetrated into the steel.
  • the unit of the content of each element in the steel composition and the content of each element in the plating layer composition is “mass %”, and unless otherwise specified, it is simply expressed as “%”.
  • the unit of hydrogen concentration is “volume %”, and unless otherwise specified, it is simply expressed as “%”.
  • a numerical range expressed using “ ⁇ ” means a range that includes the numerical values written before and after " ⁇ " as lower and upper limits.
  • the expression "high strength" of the steel plate means that the tensile strength of the steel plate is 340 MPa or more.
  • Si 0.10% or more and 2.00% or less
  • Si is a solid solution strengthening element and contributes to increasing the strength of the steel plate. Furthermore, since it also has the effect of suppressing carbide formation and making it easier to obtain retained austenite, it is effective in achieving both strength and ductility of steel sheets. In order to obtain such an effect, the Si content needs to be 0.10% or more. On the other hand, if the Si content exceeds 2.00%, hot rollability and cold rollability will be greatly reduced, which may adversely affect productivity or even reduce the ductility of the steel sheet itself. . Furthermore, the formation of Si oxide on the surface of the steel sheet becomes significant, and good plating properties may not be obtained. Therefore, the amount of Si is 0.10% or more and 2.00% or less. The amount of Si is preferably 0.25% or more. Moreover, the amount of Si is preferably 1.70% or less.
  • Mn 1.0% or more and 5.0% or less Mn has the effect of solid solution strengthening the steel to increase its strength, increasing hardenability, and promoting the formation of retained austenite, bainite, and martensite. It is an element. Such an effect is produced by adding 1.0% or more of Mn. On the other hand, if the Mn content exceeds 5.0%, not only will the cost increase, but even if the manufacturing method according to the present embodiment is used, the formation of Mn oxides on the surface of the steel sheet during plating will be insufficiently suppressed. , good plating properties may not be obtained. Therefore, the amount of Mn is set to 1.0% or more and 5.0% or less. The amount of Mn is more preferably 1.5% or more, and even more preferably 2.0% or more. Moreover, the amount of Mn is more preferably 4.0% or less, and even more preferably 3.5% or less.
  • the component composition of the base steel plate according to the present embodiment requires that it contain Si and Mn in a predetermined amount and ratio range. Others may be freely selected according to the design of mechanical properties and are not particularly limited. However, in order to obtain a steel plate with a tensile strength of 340 MPa or more, it is preferable to have the following composition.
  • C 0.05% or more and 0.40% or less
  • C is an effective element for increasing the strength of a steel plate, and contributes to increasing the strength by forming martensite, which is one of the hard phases of the steel structure.
  • the amount of C is preferably 0.40% or less.
  • the amount of C is more preferably 0.07% or more. Further, the amount of C is preferably 0.35% or less.
  • the amount of P is preferably 0.100% or less.
  • the amount of P is more preferably 0.050% or less.
  • the lower limit of P is not particularly limited. Due to production technology constraints, the P amount may be more than 0%, and may be 0.001% or more.
  • the amount of S is preferably 0.0200% or less (not including 0%)
  • the amount of S is preferably 0.0200% or less, more preferably 0.0150% or less.
  • the amount of S is preferably 0.0200% or less.
  • the amount of S is more preferably 0.0100% or less.
  • the lower limit of S is not particularly limited, and may be more than 0% due to production technology constraints, and may be 0.0001% or more.
  • Al 0.003% or more and 2.000% or less
  • Al is the most easily oxidized thermodynamically, so it oxidizes before Si and Mn, suppresses the oxidation of Si and Mn in the outermost layer of the steel sheet, and suppresses the oxidation of Si and Mn. It has the effect of promoting oxidation inside the steel plate. This effect is obtained when the Al amount is 0.003 or more.
  • the amount of Al is preferably 2.000% or less. Therefore, when added, the amount of Al is preferably 0.003% or more and 2.000% or less.
  • the amount of Al is more preferably 0.010% or more.
  • N 0.0100% or less (not including 0%)
  • the amount of N is preferably 0.0100% or less.
  • the amount of N is preferably 0.0100% or less.
  • the amount of N is preferably 0.0100% or less, more preferably 0.0050% or less.
  • the lower limit of the N content is not particularly limited, and may be more than 0% due to production technology constraints, and may be 0.0005% or more.
  • the component composition may further optionally contain a predetermined amount of at least one selected from the following element groups.
  • B 0.0100% or less B is an effective element for improving the hardenability of steel.
  • the amount of B is preferably 0.0001% or more, more preferably 0.0005% or more.
  • the amount of B is preferably 0.0100% or less, more preferably 0.0050% or less.
  • Ti 0.200% or less Ti is effective for precipitation strengthening of steel.
  • the lower limit of Ti is not particularly limited, but in order to obtain the effect of adjusting strength, it is preferably 0.001% or more.
  • the amount of Ti is preferably 0.200% or less, more preferably 0.060% or less.
  • Nb 0.200% or less
  • the amount of Nb is preferably 0.001% or more, more preferably 0.005% or more. Further, by setting the content to 0.200% or less, cost increases can be prevented. Therefore, the amount of Nb is preferably 0.200% or less, more preferably 0.060% or less.
  • Sb 0.200% or less Sb can be added for the purpose of suppressing excessive decarburization on the surface of the steel sheet, preventing a decrease in the amount of martensite generated, and improving the fatigue characteristics and surface quality of the steel sheet. .
  • the amount of Sb is preferably 0.001% or more.
  • the amount of Sb is preferably 0.200% or less. More preferably, the amount of Sb is 0.060% or less.
  • Sn 0.200% or less
  • Sn is an effective element for suppressing decarburization, denitrification, etc., and suppressing a decrease in strength of steel.
  • the amount of Sn is 0.002% or more.
  • the amount of Sn is preferably 0.200% or less.
  • the amount of Sn is more preferably 0.060% or less.
  • V 0.100% or less
  • the V amount is preferably 0.001% or more, more preferably 0.005% or more. Further, by setting the content to 0.100% or less, an increase in cost can be prevented. Therefore, the V amount is preferably 0.100% or less, more preferably 0.060% or less.
  • the amount of Cu is an element that increases hardenability, and is an effective element for setting the area ratio of the hard phase within a more suitable range and tensile strength within a more suitable range. .
  • the Cu content is preferably 0.005% or more, more preferably 0.020% or more.
  • the Cu amount is preferably 1.00% or less, more preferably 0.20% or less.
  • the Cr content is 0.001% or more.
  • the amount of Cr is preferably 1.00% or less, more preferably 0.80% or less, from the viewpoint of preventing cost increases.
  • Ni 1.00% or less
  • the amount of Ni is preferably 1.00% or less, more preferably 0.80% or less, from the viewpoint of preventing cost increases.
  • Mo 0.50% or less
  • the amount of Mo is preferably 0.005% or more, more preferably 0.01% or more.
  • the content is preferably 0.50% or less, more preferably 0.45% or less, from the viewpoint of preventing cost increases.
  • Ta 0.100% or less
  • the amount of Ta is preferably 0.100% or less from the viewpoint of preventing cost increases.
  • the amount of Ta is more preferably 0.050% or less.
  • W 0.500% or less
  • the amount of W is preferably 0.001% or more, more preferably 0.003% or more.
  • the amount of W is preferably 0.500% or less, more preferably 0.450% or less, from the viewpoint of preventing cost increases.
  • the Zr amount is preferably 0.0005% or more, more preferably 0.0010% or more. Furthermore, when containing Zr, the amount of Zr is preferably 0.020% or less from the viewpoint of preventing cost increases. The amount of Zr is more preferably 0.010% or less.
  • Ca 0.0200% or less
  • the amount of Ca is preferably 0.0200% or less. More preferably, the amount of Ca is 0.0100% or less.
  • Mg 0.0200% or less
  • Mg 0.0200% or less
  • the Mg amount is preferably 0.0200% or less.
  • the amount of Mg is more preferably 0.0100% or less.
  • the amount of Zn 0.020% or less
  • the amount of Zn is 0.001% or more.
  • the amount of Zn is preferably 0.020% or less from the viewpoint of preventing cost increases.
  • the amount of Zn is more preferably 0.010% or less.
  • Co 0.020% or less
  • the amount of Co is 0.001% or more.
  • the amount of Co is preferably 0.020% or less from the viewpoint of preventing cost increases.
  • the amount of Co is more preferably 0.010% or less.
  • the remainder of the composition of the base steel plate according to this embodiment other than the above-mentioned components consists of Fe and inevitable impurities.
  • the thickness of the base steel plate according to this embodiment is not particularly limited, but may generally be 0.5 mm or more and 3.2 mm or less.
  • a steel plate having the above-mentioned composition is manufactured according to a standard method.
  • a steel slab having the above-mentioned composition is hot-rolled and cold-rolled to produce a cold-rolled steel plate.
  • the steel plate having the above-mentioned composition is immersed in a hot-dip galvanizing bath, the steel plate is subjected to recrystallization annealing including an oxidation process, a reduction process, and a soaking process.
  • cold rolled steel sheet is fed to a CGL.
  • the configuration of the CGL is not particularly limited, in one example, the CGL includes a continuous annealing furnace in which a heating zone, a soaking zone, and a cooling zone are arranged in this order, hot-dip galvanizing equipment provided downstream of the cooling zone, and It has an alloying furnace installed downstream of the hot-dip galvanizing equipment.
  • a steel plate is transported inside a continuous annealing furnace through a heating zone, a soaking zone, and a cooling zone in order, recrystallization annealing is performed on the steel sheet, and hot-dip galvanizing equipment is used to discharge the steel sheet from the cooling zone.
  • the hot-dip galvanized steel sheet is subjected to hot-dip galvanizing to obtain a hot-dip galvanized steel sheet, and then, using an alloying furnace, the hot-dip galvanized steel sheet is subjected to alloying treatment to obtain an alloyed hot-dip galvanized steel sheet.
  • the oxidation step is performed in the heating zone of the CGL.
  • Oxidizing atmosphere containing 1000 volume ppm or more and 30000 volume ppm or less of O 2 By setting the O 2 concentration of the oxidizing atmosphere in the oxidation step to 1000 volume ppm or more, oxidation of the steel sheet is promoted. If the O 2 concentration in the oxidizing atmosphere is less than 1000 ppm by volume, the steel sheet will not be oxidized sufficiently, and the above effects will not be obtained. On the other hand, if the O 2 concentration in the oxidizing atmosphere exceeds 30,000 ppm by volume, the steel sheet will be excessively oxidized, and unreduced iron oxide will remain in the subsequent reduction step, causing deterioration in plating properties.
  • the remainder of the oxidizing atmosphere is not particularly limited, in one example, it consists of N 2 , CO, CO 2 , H 2 O, and inevitable impurities, and the ratio thereof is not particularly limited.
  • the steel plate temperature in the oxidation step is preferably 650°C or higher.
  • the upper limit of the steel plate temperature in the oxidation step is not particularly limited, it is preferably 900° C. or lower.
  • Steel plate temperature 700°C or higher If the steel plate temperature in the reduction step is less than 700°C, the reduction rate is slow and unreduced iron oxide may remain.
  • the steel plate temperature in the reduction step is preferably 750°C or higher.
  • the upper limit of the steel plate temperature in the reduction process is not particularly limited, but in order to better prevent the deterioration of the furnace body, the steel plate temperature in the reduction process is preferably 950°C or less.
  • Hydrogen concentration more than 8% by volume and not more than 30% by volume
  • the hydrogen concentration in the reducing atmosphere is 8% by volume or less, the rate of reduction of iron oxide will be insufficient.
  • the hydrogen concentration in the reducing atmosphere exceeds 30% by volume, the reduction rate becomes saturated and it becomes difficult to sufficiently reduce the amount of hydrogen in the steel in the next soaking step. Therefore, the hydrogen concentration of the reducing atmosphere is set to 8% by volume or more and 30% by volume or less.
  • the hydrogen concentration of the reducing atmosphere is preferably 20% by volume or less, more preferably 18% by volume or less. Further, the hydrogen concentration of the reducing atmosphere is preferably 12% by volume or more.
  • Holding time 20 seconds or more
  • the holding time under the reducing atmosphere is preferably 25 seconds or more.
  • the upper limit of the retention time in a reducing atmosphere is not particularly limited. From the viewpoint of productivity, the holding time in a reducing atmosphere is preferably 150 seconds or less.
  • Hydrogen concentration 0.2% by volume or more and 8% by volume or less Since the reduction of the steel plate has been completed in this process, it is maintained in a soaked atmosphere with a lower hydrogen concentration than in the reduction process to reduce hydrogen solidly dissolved inside the steel plate. can do. In order to obtain this effect, the hydrogen concentration needs to be 8% by volume or less. Further, the hydrogen concentration is preferably 5% by volume or less. On the other hand, if the hydrogen concentration is less than 0.2% by volume, it is difficult to uniformly control the inside of the furnace, and there is a risk that the reduced iron will be reoxidized. Therefore, the hydrogen concentration in the soaking atmosphere is preferably 0.2% by volume or more, more preferably 0.5% or more.
  • the steel plate temperature in the heating step is preferably 780°C or higher.
  • the upper limit of the steel plate temperature in the soaking step is not particularly limited, it is preferably 950° C. or lower from the viewpoint of production equipment.
  • the steel plate temperature in the soaking step is more preferably 900° C. or lower.
  • Holding time 20 seconds or more and 300 seconds or less If the holding time in the soaking step is less than 20 seconds, hydrogen in the steel may not be sufficiently reduced. On the other hand, if the holding time exceeds 300 seconds, a large amount of Si and Mn oxides will be formed on the outermost surface of the steel sheet, which may lead to deterioration of plating properties. Therefore, the holding time is set to 20 seconds or more and 300 seconds or less. The holding time is preferably 50 seconds or more. Further, the holding time is preferably 200 seconds or less.
  • the dew point of the atmosphere in the reduction process and soaking process is not particularly limited, but from the viewpoint of industrial ease of handling, it is preferably -50°C or higher, and should be +20°C or lower. is preferred.
  • the dew point By setting the dew point to ⁇ 50° C. or higher, the equipment cost for maintaining the atmosphere can be further reduced.
  • the dew point By setting the dew point to +20° C. or lower, the dew point inside the furnace can be more easily controlled and adverse effects on the furnace body can be suitably avoided.
  • the dew point in the soaking step is preferably -20°C or higher, more preferably -15°C or higher.
  • ⁇ [Si]/[Mn] ⁇ 0.23 ⁇ Ambient dew point in the reduction process is less than -20°C ⁇ Ambient dew point in the soaking process is less than -20°C If [Si]/[Mn] is less than 0.23, the amount of Mn is higher than the amount of Si in the steel.
  • the oxides formed in the surface layer of the steel sheet are mainly Mn oxides. In this case, by setting the dew point of the reducing atmosphere and the atmospheric dew point of the soaking process within the above range, it is possible to suppress the formation of a single Mn oxide on the outermost surface of the steel sheet after the reduction of iron oxide is completed. This further improves plating wettability and provides a more excellent surface appearance.
  • the dew point of the reduction step is preferably lower than -20°C, more preferably lower than -25°C. Further, the dew point of the soaking step is preferably less than -20°C, more preferably less than -25°C.
  • the hydrogen concentrations of the atmospheres used are different from each other.
  • the dew points used in the reduction step and the soaking step may also be different.
  • the method of varying the hydrogen concentration and dew point of the atmosphere is not particularly limited.
  • a method is to divide the furnace that performs both processes, use the furnaces connected via seal rolls, and separately inject gas controlled to the desired hydrogen concentration and dew point into each divided furnace. be.
  • the method of controlling the dew point in the gas is not particularly limited, but for example, there is a method of humidifying at least one of N 2 gas or H 2 gas by bubbling or the like before inputting it into the furnace.
  • the above-mentioned reduction step and soaking step are performed using a furnace in which the soaking zone of the CGL is divided into a first stage and a second stage, which are connected via a seal roll. That is, as an example of a CGL that can be suitably applied to the method for manufacturing an alloyed hot-dip galvanized steel sheet according to the present disclosure, a continuous annealing furnace in which a heating zone, a soaking zone, and a cooling zone are arranged in this order, and a continuous annealing furnace in which a heating zone, a soaking zone, and a cooling zone are arranged in this order, and a continuous hot-dip galvanizing facility, the soaking zone having a first soaking zone and a second soaking zone, the first soaking zone and the second soaking zone being connected via a seal roll; Examples include plating equipment.
  • the movement of the atmosphere is blocked between the first soaking zone and the second soaking zone, thereby reducing the reduction.
  • the method for monitoring the hydrogen concentration and dew point in the atmosphere inside the furnace is not particularly limited.
  • measurement can be performed by providing an atmosphere measurement port that can guide the gas inside the furnace to the outside at a necessary position in each furnace and connecting it to a hydrogen concentration meter and a dew point meter.
  • the reduction process and soaking process are carried out in separate furnaces as described above, it is possible to install independent atmosphere measurement ports at three locations in the upper, middle, and lower parts of each furnace. It is possible to know the distribution state of hydrogen concentration in the height direction inside the reactor.
  • FIG. 1 shows an example of atmospheric dew point measurement positions in a split annealing furnace. In one example, an example of a CGL soaking area is schematically shown. As shown in FIG.
  • the steel strip 6 is supplied to a split annealing furnace in which a first stage soaking zone 1 and a second stage soaking zone 2 are connected via an atmosphere sealing zone 3, and the above-mentioned reduction process and soaking process are performed.
  • the dew point measurement positions 6 can be independently provided at three locations in each furnace: an upper part, a middle part, and a lower part.
  • the steel plate after the soaking process is cooled.
  • the cooling conditions are not particularly limited, but preferably, the steel plate after the soaking step is cooled from 600°C to 950°C in a cooling atmosphere with a hydrogen concentration of 0.5% by volume to 30% by volume and a dew point of 0°C or less. Cool to 300°C or more and 500°C or less at a cooling rate of 10°C/s or more. In one example, the cooling step is performed in a cooling zone of the CGL.
  • the hydrogen concentration of the cooling atmosphere is more preferably 5% by volume or more. Further, the hydrogen concentration of the cooling atmosphere is more preferably 20% by volume or less.
  • the dew point of the cooling atmosphere is more preferably ⁇ 30° C. or lower.
  • the steel sheet in order to better prevent the amount of hydrogen in the steel from increasing during cooling, it is preferable to cool the steel sheet from a temperature of 600° C. or higher and 950° C. or lower at an average cooling rate of 10° C./s or higher.
  • the cooling start temperature is more preferably 700°C or higher.
  • the average cooling rate is 15° C./s or more.
  • the cooling stop temperature is preferably 500°C or less. Further, by setting the cooling stop temperature to 300° C. or higher, excessive martensitic transformation can be prevented and the strength of the steel plate can be further improved. Therefore, it is preferable to cool to 300°C or more and 500°C or less at the above average cooling rate.
  • the steel plate after the cooling process is immersed in a hot-dip galvanizing bath to obtain a hot-dip galvanized steel plate.
  • the plating process is performed using CGL's hot dip galvanizing equipment.
  • the conditions for immersion in the hot-dip galvanizing bath are not particularly limited, and a general method may be used.
  • the hot-dip galvanizing bath consists of Al, Zn, and inevitable impurities, and its composition is not particularly specified, but in one example, the Al concentration in the bath may be 0.05% by mass or more and 0.190% by mass or less. could be. If the Al concentration in the bath is 0.05% by mass or more, the generation of bottom dross can be more suitably prevented. Moreover, if the Al concentration in the bath is 0.190% by mass or less, the generation of top dross can be more suitably prevented. Also from the viewpoint of cost, it is preferable that the Al concentration in the bath is 0.190% by mass or less.
  • the plating bath temperature is also not particularly specified, but may be 440°C or higher and 500°C or lower.
  • the amount of plating deposited per side is not particularly limited, but in one example, it is 25 g/m 2 or more and 80 g/m 2 or less. If the amount of plating deposited per side is 25 g/m 2 or more, corrosion resistance is particularly good, and control of the amount of plating deposited is particularly easy. Further, if the amount of plating deposited per side is 80 g/m 2 or less, the plating adhesion is particularly good.
  • the method of adjusting the coating amount is not particularly limited, but it can be adjusted by using gas wiping and adjusting the gas pressure and the distance between the wiping nozzle and the steel plate.
  • the hot-dip galvanized steel sheet is subjected to alloying treatment to obtain an alloyed hot-dip galvanized steel sheet.
  • the hydrogen diffusion rate in the hot-dip galvanized layer mainly consisting of the ⁇ phase before alloying treatment is significantly slower than that in the steel, which prevents the release of hydrogen in the steel during the subsequent cooling-reheating process. If the hot-dip galvanized layer is an alloyed hot-dip galvanized layer, the hydrogen diffusion rate in the alloyed hot-dip galvanized layer is much faster than that in the hot-dip galvanized layer, so the release of hydrogen in the steel is promoted. Therefore, in order to significantly reduce hydrogen in the steel in the subsequent cooling-reheating and holding process, it is important to perform an alloying process prior to the cooling-reheating and holding process.
  • the conditions for the alloying treatment are not particularly limited.
  • the alloying treatment may be performed by maintaining the steel sheet temperature at a temperature of 440° C. or higher. Further, the alloying treatment may be performed while maintaining the steel sheet temperature at a temperature of 600° C. or lower.
  • the alloying treatment may be performed by holding the hot-dip galvanized steel sheet at the above temperature for 5 seconds or more and 60 seconds or less.
  • the alloyed hot-dip galvanized layer after alloying preferably has an alloying degree (Fe content in the hot-dip galvanized layer) of 7% by mass or more. Moreover, it is preferable that the alloyed hot-dip galvanized layer after alloying has an alloying degree of 15% by mass or less.
  • the degree of alloying of the alloyed hot-dip galvanized layer is set to 15% by mass or less, the formation of ⁇ phase at the interface between the alloyed hot-dip galvanized layer and the base steel sheet can be more effectively prevented. Good plating adhesion can be obtained.
  • Cooling stop temperature Below Ms point Austenite has a larger amount of hydrogen in solid solution than ferrite, but the diffusion rate of hydrogen is higher in ferrite with BCC structure and martensite with BCT structure than in austenite with FCC structure. . Therefore, by performing reheating after transforming austenite containing more dissolved hydrogen into martensite, it is possible to more efficiently reduce hydrogen in steel. Therefore, the cooling stop temperature in the cooling-reheating process is set to be below the Ms point at which martensitic transformation begins. Furthermore, the greater the degree of supercooling relative to the Ms point, the more the martensitic transformation is promoted, and the reheating can be performed with less untransformed austenite, which is advantageous for reducing hydrogen in the steel.
  • the cooling stop temperature in the cooling-reheating step is more preferably (Ms point -50°C) or lower, and even more preferably (Ms point -100°C or lower).
  • the lower limit of the cooling stop temperature is not particularly limited, it is preferably set to 20°C or higher because a cooling stop temperature of less than 20°C requires a high heat extraction ability in the cooling zone, leading to an increase in cost.
  • Atmospheric hydrogen concentration during reheating 0.2% by volume or less
  • the lower limit of the hydrogen concentration is not particularly limited, but since hydrogen gas is inevitably included in the atmosphere, it may be, for example, 0.00001% by volume or more.
  • Reheating temperature Cooling stop temperature or higher and 100°C or higher and 450°C or lower After cooling is stopped, reheating is performed to a reheating temperature higher than the cooling stop temperature in order to promote release of hydrogen in the steel. In order to sufficiently obtain the effect of reducing hydrogen in steel, it is necessary to set the reheating temperature to 100° C. or higher. On the other hand, if the reheating temperature exceeds 450° C., there is a risk that the plating properties will deteriorate. Therefore, the reheating temperature is set to 100°C or more and 450°C or less. The reheating temperature is preferably 200°C or higher. The reheating temperature is preferably 400°C or lower.
  • Holding time 30 seconds or more If the holding time at the reheating temperature is less than 30 seconds, the effect of reducing hydrogen in steel will be insufficient. Therefore, the holding time at the reheating temperature is set to 30 seconds or more.
  • the holding time at the heating temperature is preferably 50 seconds or more.
  • the upper limit of the holding time at the reheating temperature is not particularly limited, but from the viewpoint of productivity, the holding time at the reheating temperature is preferably 300 seconds or less.
  • an alloyed hot-dip galvanized steel sheet having a tensile strength of preferably 340 MPa or more.
  • the tensile strength of the alloyed hot-dip galvanized steel sheet is more preferably 500 MPa or more, and still more preferably 980 MPa or more.
  • the tensile strength (TS) is measured in accordance with JIS Z 2241 as follows. A JIS No. 5 test piece is taken from an alloyed hot-dip galvanized steel sheet so that the longitudinal direction is perpendicular to the rolling direction of the steel sheet. Using the test piece, a tensile test is performed under the condition that the crosshead displacement speed Vc is 1.67 ⁇ 10 ⁇ 1 mm/s, and TS is measured.
  • the amount of diffusible hydrogen in the alloyed hot-dip galvanized steel sheet produced by this production method is preferably 0.30 wt. ppm or less, more preferably 0.20wt. ppm or less.
  • the upper limit of the amount of diffusible hydrogen in the alloyed hot-dip galvanized steel sheet is not particularly limited, but is, for example, 0.01 wt. It can be more than ppm.
  • the amount of diffusible hydrogen is measured as follows. A 5 ⁇ 30 mm test piece is cut out from an alloyed hot-dip galvanized steel sheet, and the alloyed hot-dip galvanized layer on the surface of the test piece is removed using a router (precision grinder). Immediately, hydrogen analysis is performed using a temperature programmed desorption analyzer at an analysis start temperature of 25°C, an analysis end temperature of 300°C, and a heating rate of 200°C/hr, and the amount of released hydrogen at each temperature is measured. Among these, the cumulative value of the amount of released hydrogen in the range of 210° C. from the analysis start temperature is determined as the amount of diffusible hydrogen in the steel.
  • ⁇ Plating bath composition 0.13wt.% Al-added Zn bath ⁇ Plating bath temperature: 460°C ⁇ Plating coverage range: 40-60gm -2 ⁇ Alloying degree range: 8.0 to 14.0% by mass ⁇ Hydrogen concentration during reheating and holding: 0.1% by volume
  • the tensile strength (TS) was measured by the method described above.
  • Amount of diffusible hydrogen in steel sheet was determined according to the method described above, and evaluated based on the following criteria. Those with ranks 1 and 2 were set as the preferred range of the present invention.
  • Amount of diffusible hydrogen in steel (wt.ppm) Rank 0.20 or less: 1 More than 0.20 and less than 0.30: 2 More than 0.30: 3
  • the welding current value was set to form a nugget diameter corresponding to the tensile strength of each steel plate.
  • the nugget diameter was 3.8 mm, and when the tensile strength was 1250 MPa or more, the nugget diameter was 4.8 mm.
  • the distance between the spacers at both ends was 40 mm, and the steel plate and the spacer were secured together by welding in advance. After being left for 24 hours after welding, the spacer portion was cut off.
  • the cross section of the weld nugget was observed and evaluated based on the following criteria. Those with ranks 1 and 2 were set as the preferred range of the present invention. Crack observation results Rank: No cracks: 1 (particularly excellent in hydrogen embrittlement resistance) Only microcracks of 100 ⁇ m or less occur: 2 (excellent hydrogen embrittlement resistance) Cracks exceeding 100 ⁇ m: 3 (poor hydrogen embrittlement resistance)
  • the examples of the present invention have better plating properties than the comparative examples, and the amount of diffusible hydrogen in the steel is sufficiently reduced, resulting in excellent hydrogen embrittlement resistance. I can see that

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Abstract

La présente invention concerne une tôle d'acier recuite après galvanisation par immersion à chaud qui a un bel aspect externe sans défauts tels que des points nus, présente une excellente adhérence de placage, et possède également une excellente résistance à la fragilisation par l'hydrogène.　Un procédé de fabrication de ladite tôle d'acier recuite après galvanisation par immersion à chaud consiste à : chauffer une tôle d'acier ayant une composition contenant, en pourcentages en masse, 0,10 à 2,00 %, inclus, de Si et 1,0 à 5,0 %, inclus, de Mn à au moins 600 °C dans une atmosphère d'oxydation comprenant 1 000 à 30 000 ppm volumétriques, inclus, d'O2 ; maintenir la tôle d'acier après l'étape d'oxydation pendant au moins 20 s dans une atmosphère de réduction ayant une concentration en hydrogène qui est supérieure à 8 % en volume et est d'au maximum 30 % en volume, à 700 °C ou plus ; maintenir la tôle d'acier pendant 20 à 300 s, inclus, dans une atmosphère isotherme ayant une concentration en hydrogène de 0,2 à 8 % en volume, inclus, à 750 °C ou plus ; refroidir la tôle d'acier ; immerger la tôle d'acier dans un bain de zinc fondu pour obtenir une tôle d'acier galvanisée par immersion à chaud ; réaliser un procédé d'alliage sur la tôle d'acier galvanisée par immersion à chaud pour obtenir une tôle d'acier recuite après galvanisation par immersion à chaud ; et, après refroidissement de la tôle d'acier recuite par galvanisation par immersion à chaud à une température d'arrêt du refroidissement qui est au maximum un point Ms, maintenir la tôle d'acier pendant au moins 30 s à une température qui est au moins la température d'arrêt du refroidissement et est de 100 à 450 °C, inclus, dans une atmosphère de réchauffage ayant une concentration en hydrogène d'au plus 0,2 % en volume.
PCT/JP2022/014582 2022-03-25 2022-03-25 Procédé de fabrication de tôle d'acier recuite après galvanisation par immersion à chaud WO2023181390A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013142198A (ja) * 2012-01-13 2013-07-22 Nippon Steel & Sumitomo Metal Corp めっき濡れ性及び耐ピックアップ性に優れる溶融亜鉛めっき鋼板の製造方法
WO2015087549A1 (fr) * 2013-12-13 2015-06-18 Ｊｆｅスチール株式会社 Procédé de fabrication d'une tôle d'acier de résistance élevée galvanisée à chaud
WO2019106894A1 (fr) * 2017-11-29 2019-06-06 Ｊｆｅスチール株式会社 Tôle d'acier galvanisée à résistance élevée et son procédé de fabrication
WO2020170542A1 (fr) * 2019-02-22 2020-08-27 Ｊｆｅスチール株式会社 Tôle d'acier galvanisée par immersion à chaud à haute résistance et procédé de fabrication de ladite tôle
WO2021166350A1 (fr) * 2020-02-21 2021-08-26 Ｊｆｅスチール株式会社 Procédé pour la production de tôle d'acier galvanisée par immersion à chaud à haute résistance

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013142198A (ja) * 2012-01-13 2013-07-22 Nippon Steel & Sumitomo Metal Corp めっき濡れ性及び耐ピックアップ性に優れる溶融亜鉛めっき鋼板の製造方法
WO2015087549A1 (fr) * 2013-12-13 2015-06-18 Ｊｆｅスチール株式会社 Procédé de fabrication d'une tôle d'acier de résistance élevée galvanisée à chaud
WO2019106894A1 (fr) * 2017-11-29 2019-06-06 Ｊｆｅスチール株式会社 Tôle d'acier galvanisée à résistance élevée et son procédé de fabrication
WO2020170542A1 (fr) * 2019-02-22 2020-08-27 Ｊｆｅスチール株式会社 Tôle d'acier galvanisée par immersion à chaud à haute résistance et procédé de fabrication de ladite tôle
WO2021166350A1 (fr) * 2020-02-21 2021-08-26 Ｊｆｅスチール株式会社 Procédé pour la production de tôle d'acier galvanisée par immersion à chaud à haute résistance

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