EP4116457A1 - Heissgepresstes bauteil, verfahren zu seiner herstellung und plattiertes stahlblech für heisspressen - Google Patents

Heissgepresstes bauteil, verfahren zu seiner herstellung und plattiertes stahlblech für heisspressen Download PDF

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Publication number
EP4116457A1
EP4116457A1 EP20923408.7A EP20923408A EP4116457A1 EP 4116457 A1 EP4116457 A1 EP 4116457A1 EP 20923408 A EP20923408 A EP 20923408A EP 4116457 A1 EP4116457 A1 EP 4116457A1
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Prior art keywords
steel sheet
based alloy
pressed member
phase
layer
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EP20923408.7A
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English (en)
French (fr)
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EP4116457B1 (de
EP4116457A4 (de
Inventor
Rinta Sato
Minoru Tanaka
Daisuke Mizuno
Satoru Ando
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JFE Steel Corp
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JFE Steel Corp
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • 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
    • C21D8/0242—Flattening; Dressing; Flexing
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D22/00—Shaping without cutting, by stamping, spinning, or deep-drawing
    • B21D22/20—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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C18/00—Alloys based on zinc
    • C22C18/04—Alloys based on zinc with aluminium as the next major constituent
    • 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
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • 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
    • C23C2/12—Aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/261—After-treatment in a gas atmosphere, e.g. inert or reducing atmosphere
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
    • C23C2/36—Elongated material
    • C23C2/40—Plates; Strips
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C23C28/3225—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only with at least one zinc-based layer
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • 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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C21D1/673—Quenching devices for die quenching
    • 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
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/13—Modifying the physical properties of iron or steel by deformation by hot working
    • 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
    • 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
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur

Definitions

  • This disclosure relates to a hot pressed member and a method of producing the same, and a coated steel sheet for hot press forming.
  • Hot press forming uses a press mold having a die and a punch to process a heated steel sheet while quenching it simultaneously, to achieve both easier working and higher strength.
  • Zn alloy-coated steel sheets have attracted attention as steel sheets for hot press forming having high rust resistance since their coated layers, which are electrochemically more basic (with a lower potential) than the base steel sheets, remain after heating. Accordingly, hot pressed members using such Zn alloy-coated steel sheets and manufacturing methods thereof have been proposed in the art.
  • JP 2006-265706 A (PTL 1) describes a coated steel sheet for hot press forming having a coated layer in which an Al concentration ⁇ Al ⁇ is in the range of 0.2 g/m 2 to 1.0 g/m 2 and a Mg concentration ⁇ Mg ⁇ in mass % satisfies a relation with the Al concentration of 0.10 ⁇ ⁇ Mg ⁇ / ⁇ Al ⁇ ⁇ 5, and a hot pressed member obtained by heating the coated steel sheet for hot press forming and then subjecting it to hot press forming.
  • PTL 1 describes that the hot pressed member has good post-painting corrosion resistance when subjected to electrodeposition painting (also called electrodeposition coating) after zinc phosphate-based chemical conversion treatment.
  • electrodeposition painting also called electrodeposition coating
  • zirconium-based chemical conversion treatment has begun to replace the conventional zinc phosphate-based chemical conversion treatment.
  • hot pressed members are also increasingly required to have proper painting layer adhesion and post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the hot pressed member according to the present disclosure has excellent painting layer adhesion and post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the method of producing a hot pressed member according to the present disclosure enables the production of a hot pressed member with excellent painting layer adhesion and post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the coated steel sheet for hot press forming according to the present disclosure is suitably used as a raw material for producing a hot pressed member with excellent painting layer adhesion and post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • a hot pressed member comprises: a base steel sheet; an Fe-Zn-Al-Mg-based alloy coated layer formed on at least one surface of the base steel sheet; and an oxide layer formed on the Fe-Zn-Al-Mg-based alloy coated layer.
  • the base steel sheet of the hot pressed member in this embodiment is not limited to a particular steel sheet, it is preferable to use a steel sheet having the chemical composition as described in the section "(Coated Steel Sheet for Hot Press Forming)" below, in order for the resulting hot pressed member to have a tensile strength TS of 1470 MPa or more.
  • the Fe-Zn-Al-Mg-based alloy coated layer in the hot pressed member in this embodiment contains, preferably consists of, an ⁇ -Fe phase and a ⁇ phase.
  • the ⁇ -Fe phase is a solid solution phase that is mainly composed of Fe and contains Zn, Al, and Mg.
  • Zn, Al, and Mg in the coated layer diffuse into the base steel sheet and, in this diffusion region, a solid solution phase ( ⁇ -Fe phase) mainly composed of Fe and containing Zn, Al, and Mg is formed.
  • the ⁇ -Fe phase is formed so as to erode the surface layer of the base steel sheet of the coated steel sheet.
  • the ⁇ -Fe phase is generally interpreted to be part of the Fe-Zn-Al-Mg-based alloy coated layer located on the base steel sheet.
  • the ⁇ phase is a phase formed from an intermetallic compound that is mainly composed of Zn and contains Al, Mg, and Fe. Primarily, the ⁇ phase is composed of Fe3Zn10 phase. In this respect, ⁇ 1 phase has a crystal structure similar to that of ⁇ phase and is difficult to distinguish by X-ray diffraction. Thus, as used herein, " ⁇ phase" is intended to include ⁇ 1 phase.
  • Other compositional intermetallic compounds that make up the ⁇ phase include, for example, Fe4Zn9, FeZn4, and Fe5Zn21.
  • the Zn-Al-Mg-based alloy coated layer that remains without contributing to diffusion into the base steel sheet incorporates Fe diffused from the base steel sheet, forming a ⁇ phase composed of an intermetallic compound and forming a part of the Fe-Zn-Al-Mg-based alloy coated layer in the hot pressed member.
  • the ⁇ -Fe and ⁇ phases can be distinguished from each other by their distinctly different contrasts in the cross-sectional SEM images of the Fe-Zn-Al-Mg-based alloy coated layer of the hot pressed member. Referring to FIGS. 1 and 2 , regions that appear relatively bright in the surface layer of the hot pressed member are the ⁇ phase, and regions that appear relatively dark are the ⁇ -Fe phase.
  • the ⁇ -Fe and ⁇ phases can also be identified using a Co-K ⁇ (wavelength: 1.79021 ⁇ ) radiation source at an incident angle of 25°.
  • the ⁇ phase in the Fe-Zn-Al-Mg-based alloy coated layer has a significantly lower potential than the base steel sheet and the ⁇ -Fe phase, and is therefore preferentially corroded when exposed to a corrosion environment.
  • the ⁇ phase provides sacrificial protection against the base steel sheet and the ⁇ -Fe phase.
  • a zinc phosphate-based chemical conversion treatment layer functions as an excellent corrosion inhibitor against Zn-based alloys. Therefore, when a hot pressed member obtained by subjecting a Zn-Al-Mg-based alloy-coated steel sheet to hot press forming is subjected to electrodeposition painting after zinc phosphate-based chemical conversion treatment, the resulting member has a low corrosion rate in the ⁇ phase and a sufficiently low corrosion rate under the painting layer such that post-painting corrosion resistance is not an issue in actual use environments even in a sacrificial protection state due to flaws that penetrate the painting layer, the chemical conversion treatment layer, and the coated layer to reach the base steel sheet.
  • a zirconium oxide-based chemical conversion treatment layer does not have a corrosion inhibitor function against Zn-based alloys. Therefore, in a sacrificial protection state, the corrosion rate of the ⁇ phase becomes higher, resulting in a higher corrosion rate under the painting layer. Then, if a large amount of ⁇ phase is present contiguously in the Fe-Zn-Al-Mg-based alloy coated layer, corrosion in the ⁇ phase propagates in-plane under the painting layer in a sacrificial protection state, resulting in problems in lowered esthetics such as poor appearance including swelling in the painting layer. Therefore, when applying a zirconium-based chemical conversion treatment, it is important to limit the amount of ⁇ phase to ensure post-painting corrosion resistance.
  • a ratio of I ⁇ /I ⁇ is 0.5 or less when measured by X-ray diffraction using a Co-K ⁇ (wavelength: 1.79021 ⁇ ) radiation source at an incident angle of 25°, where I ⁇ is an intensity of a diffraction peak of (411) plane of the ⁇ phase present in an angular range of 41.5° ⁇ 2 ⁇ ⁇ 43.0° and I ⁇ is an intensity of a diffraction peak of (110) plane of the ⁇ -Fe phase present in an angular range of 51.0° ⁇ 2 ⁇ ⁇ 52.0°.
  • I ⁇ /I ⁇ is greater than 0.5, the post-painting corrosion resistance is insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment. If I ⁇ /I ⁇ is 0.5 or less, the ⁇ phase is sufficiently broken up by the ⁇ -Fe phase in the Fe-Zn-Al-Mg-based alloy layer, and excellent post-painting corrosion resistance can be obtained when the hot pressed member is subjected to electrodeposition painting after zirconium chemical conversion treatment.
  • the lower limit is not limited.
  • the value of I ⁇ /I ⁇ that is detected by measurement using X-ray diffraction as described above is usually 0.01 or more.
  • Coating Weight Per Surface 40 g/m 2 to 400 g/m 2
  • the coating weight of the Fe-Zn-Al-Mg-based alloy coated layer of the hot pressed member is preferably 50 g/m 2 or more, and more preferably 60 g/m 2 or more.
  • the coating weight of the coated layer of the hot pressed member is preferably 350 g/m 2 or less, and more preferably 300 g/m 2 or less.
  • the "coating weight per surface of the Fe-Zn-Al-Mg-based alloy coated layer" of the hot pressed member is determined as follows. From each hot pressed member to be evaluated, three 48 mm ⁇ samples are taken by punching. Then, in each sample, a non-evaluated surface opposite the one surface where the coating weight is evaluated is masked. First, the oxide layer is dissolved by immersing each sample in a 20 % chromium oxide (VI) solution at room temperature for 10 minutes. Then, each sample is weighed. Next, 500 mL of a 35 % hydrochloric acid solution to which 3.5 g of hexamethylenetetetramine has been added is mixed up to 1 L.
  • VI chromium oxide
  • each sample is immersed in the resultant solution for 120 minutes to dissolve the Fe-Zn-Al-Mg-based alloy coated layer. Then, each sample is weighed again. The coating weight per unit area in each sample is calculated from the mass difference before and after the dissolution of the Fe-Zn-Al-Mg-based alloy coated layer. The average of the three samples is then used as the coating weight per surface.
  • the oxide layer of the hot pressed member in this embodiment is formed on the Fe-Zn-Al-Mg-based alloy coated layer and contains Zn, Al, and Mg.
  • Zn, Al, and Mg in the coated layer combine with oxygen present in the heating atmosphere to form an oxide layer containing Zn, Al, and Mg.
  • the oxide layer is mainly composed of an Al oxide. However, it may also contain Zn and Mg contained in the coated layer, as well as elements constituting the base steel sheet, such as Fe, Mn, and Cr.
  • the sum of the Al and Mg concentrations in the oxide layer be 28 atomic% or more. If the sum of the Al and Mg concentrations in the oxide layer is less than 28 atomic%, even with the ratio of I ⁇ /I ⁇ being 0.5 or less, the post-painting corrosion resistance is insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the hot pressed member may have excellent post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the oxide layer becomes brittle, resulting in insufficient painting layer adhesion when the hot pressed member is subjected to electrodeposition painting after the zirconium-based chemical conversion treatment.
  • the oxide layer has sufficient strength, and the hot pressed member has good painting layer adhesion when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the upper limit of the sum of the Al and Mg concentrations in the oxide layer is not particularly limited.
  • an oxide layer containing excessively high concentrations of Al and Mg is chemically stable in acidic environments, such as in a chemical conversion treatment liquid for coating base treatment, and may prevent the formation of a chemical conversion treatment layer. Therefore, the sum of the Al and Mg concentrations in the oxide layer is preferably 50 atomic% or less.
  • the oxide layer is formed very thinly on the Fe-Zn-Al-Mg-based alloy coated layer, and thus may not be visible in the cross-sectional SEM image as illustrated in FIG. 1 .
  • elemental mapping can be performed to identify the oxide layer as a region where oxygen is detected.
  • the Al and Mg concentrations in the oxide layer are the values measured by the following methods. Specifically, a test specimen for cross-sectional observation is taken from a flat part of the hot pressed member.
  • a cross-section of the test specimen including the Fe-Zn-Al-Mg-based alloy coated layer and the oxide layer is observed under SEM at 10000 ⁇ magnification and accelerating voltage of 15 kV, and the composition of the oxide layer is measured at freely-selected three locations using EDX.
  • the arithmetic means of the Al concentrations and Mg concentrations at the three locations are respectively used as the "Al concentration in the oxide layer" and "Mg concentration in the oxide layer".
  • a method of producing the hot pressed member according to one of the embodiments of the present disclosure comprises: heating a coated steel sheet for hot press forming according to one of the embodiments of the present disclosure as described below to a temperature range of Ac 3 transformation point to 1000 °C; and then subjecting the coated steel sheet to hot press forming.
  • the heating temperature of the steel sheet for hot press forming before hot press forming to the temperature range of Ac 3 transformation point to 1000 °C, it is possible to obtain an Fe-Zn-Al-Mg-based alloy coated layer with ⁇ -Fe and ⁇ phases as well as an oxide layer with predetermined Al and Mg concentrations, as described above.
  • the heating temperature is lower than the Ac 3 transformation point, the I ⁇ /I ⁇ of the Fe-Zn-Al-Mg-based alloy coated layer exceeds 0.5 after hot press forming. Consequently, the post-painting corrosion resistance becomes insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the heating temperature refers to the maximum arrival temperature of the steel sheet.
  • the holding time after the temperature is raised to the heating temperature is desirably 30 seconds or longer from the viewpoint of eliminating the ⁇ phase and avoiding liquid metal embrittlement cracking during hot press forming. From the perspective of avoiding hydrogen ingress due to the inclusion of water vapor present in the furnace during the holding time, the holding time is preferably within 5 minutes, more preferably within 3 minutes, and even more preferably within 2 minutes.
  • the method of heating the steel sheet for hot press forming is not limited in any way, and exemplary methods include furnace heating such as heating in an electric or gas furnace, electrical resistance heating, induction heating, high-frequency heating, and flame heating.
  • hot press forming the coated steel sheet for hot press forming heated as described above is simultaneously subjected to press forming and quenching using a press forming tool to obtain a hot pressed member of a predetermined shape.
  • the conditions for hot press forming are not limited, and conventional methods may be followed.
  • the coated steel sheet for hot press forming comprises: a base steel sheet; and a Zn-Al-Mg-based alloy coated layer formed on at least one surface of the base steel sheet at a coating weight per surface of 30 g/m 2 to 180 g/m 2 , having a chemical composition containing, in mass%, Al: 3 % to 10 % and Mg: 0.2 % to 0.8 %, with the balance being Zn and inevitable impurities, and having a liquidus temperature in an air atmosphere of 400 °C or lower.
  • the base steel sheet have a chemical composition containing, in mass%, C: 0.20 % to 0.35 %, Si: 0.1 % to 0.5 %, Mn: 1.0 % to 3.0 %, P: 0.1 % or less, S: 0.05 % or less, Al: 0.1 % or less, N: 0.01 % or less, with the balance being Fe and inevitable impurities.
  • the base steel sheet may be a cold-rolled steel sheet or a hot-rolled steel sheet. The reasons for the limitation of each component will be explained below.
  • the C content increases strength by forming a steel microstructure such as martensite.
  • the C content needs to be 0.20 % or more.
  • the toughness deteriorates at a spot welded portion. Therefore, the C content is preferably 0.20 % to 0.35 %.
  • the Si is an effective element in increasing the strength of steel to obtain good material properties.
  • the Si content needs to be 0.1 % or more.
  • the Si content is preferably 0.1 % to 0.5 %.
  • Mn is an effective element for increasing the strength of steel. To ensure proper mechanical properties and strength, the Mn content needs to be 1.0 % or more. However, if the Mn content exceeds 3.0 %, surface enrichment during annealing becomes more pronounced, making it difficult to ensure proper coating adhesion. Therefore, the Mn content is preferably 1.0 % to 3.0 %.
  • the P content is preferably 0.1 % or less. From the viewpoint of steelmaking cost, the P content is preferably 0.01 % or more.
  • S forms as inclusions such as MnS, which cause degradation of impact resistance and cracking along the metal flow in welded portions. Therefore, a lower S content is desirable, and the S content is preferably 0.05 % or less. To ensure good stretch flangeability, the S content is more preferably 0.01 % or less. From the viewpoint of steelmaking cost, the S content is preferably 0.002 % or more.
  • the Al content is preferably 0.1 % or less. From the viewpoint of ensuring its effectiveness as a deoxidizing material, the Al content is preferably 0.01 % or more.
  • the N content is preferably 0.01 % or less. From the viewpoint of steelmaking cost, the N content is preferably 0.001 % or more.
  • the chemical composition may optionally contain at least one selected from the group consisting of Nb: 0.05 % or less, Ti: 0.05 % or less, B: 0.0002 % to 0.005 %, Cr: 0.1 % to 0.3 %, Sb: 0.003 % to 0.03 %, for the reasons given below.
  • Nb is an effective component for increasing the strength of steel. However, excessive addition of Nb reduces shape fixability. Therefore, when Nb is contained, the Nb content is 0.05 % or less.
  • Ti is also effective in increasing the strength of steel.
  • excessive addition of Ti reduces shape fixability. Therefore, when Ti is contained, the Ti content is 0.05 % or less.
  • the B content is preferably 0.0002 % or more.
  • excessive addition of B greatly impairs formability. Therefore, when B is contained, the B content is 0.005 % or less.
  • the Cr content is preferably 0.1 % or more.
  • the Cr content is 0.3 % or less.
  • the Sb has an effect of deterring decarburization of the surface layer of the steel sheet during hot pressing.
  • the Sb content is preferably 0.003 % or more.
  • the Sb content exceeds 0.03 %, the rolling load increases, resulting in lower productivity. Therefore, when Sb is contained, the Sb content is 0.03 % or less.
  • the Zn-Al-Mg-based alloy coated layer of the coated steel sheet for hot press forming has a chemical composition containing, in mass%, Al: 3 % to 10 % and Mg: 0.2 % to 0.8 %, with the balance being Zn and inevitable impurities, and has a liquidus temperature in an air atmosphere of 400 °C or lower.
  • the Al content is less than 3 %, the I ⁇ /I ⁇ of the Fe-Zn-Al-Mg-based alloy coated layer exceeds 0.5 after hot press forming, and the sum of the Al and Mg concentrations in the oxide layer is less than 28 atomic%. As a result, the painting layer adhesion and post-painting corrosion resistance are insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment. If the Al content is less than 3 %, depending on the Mg content, the liquidus temperature to be described later cannot be lowered to 400 °C or lower.
  • the Al content exceeds 10 %, the liquidus temperature to be described later cannot be lowered to 400 °C or lower, with the result that the I ⁇ /I ⁇ of the Fe-Zn-Al-Mg-based alloy coated layer exceeds 0.5 after hot press forming. Consequently, the post-painting corrosion resistance becomes insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment. Therefore, the Al content is 3 % to 10 %.
  • the Mg content is 0.2 % or more, preferably 0.3 % or more, and more preferably 0.4 % or more. However, if the Mg content exceeds 0.8 %, the sum of the Al and Mg concentrations in the oxide layer is less than 28 atomic% after hot press forming.
  • the Mg content is 0.8 % or less, preferably 0.7 % or less, and more preferably 0.6 % or less.
  • Liquidus Temperature in Air Atmosphere 400 °C or lower
  • the liquidus temperature of the Zn-Al-Mg-based alloy coated layer in an air atmosphere is kept at or below 400°C by controlling the Al and Mg contents as appropriate. If the liquidus temperature is above 400 °C, the I ⁇ /I ⁇ of the Fe-Zn-Al-Mg-based alloy coated layer exceeds 0.5 after hot press forming. Consequently, the post-painting corrosion resistance becomes insufficient when the hot pressed member is subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the lower limit of the liquidus temperature is not particularly limited, yet in the range of Al and Mg contents specified above, the liquidus temperature is generally 380 °C or higher.
  • the liquidus temperatures of the Zn-Al-Mg-based alloy coated layer in an air atmosphere are calculated by Thermo Calc, a thermodynamic calculation software, using a database.
  • the inevitable impurities contained in the Zn-Al-Mg-based alloy coated layer include components of the base steel sheet that are incorporated into the coated layer by the reaction between the coating bath and the base steel sheet during the coating treatment, inevitable impurities in the coating bath, and so on.
  • the components of the base steel sheet that are incorporated into the coated layer include Fe in an amount of 0.01 % to several percent.
  • the inevitable impurities in the coating bath include, for example, Fe, Cr, Cu, Mo, Ni, and Zr.
  • Fe in the coated layer it is not possible to quantify the amount of Fe incorporated from the base steel sheet and the amount of Fe incorporated from the coating bath separately.
  • the total content of inevitable impurities is not limited, from the viewpoint of uniform melting of the coated layer during the process of hot press forming, the total amount of inevitable impurities, excluding Fe, is preferably 1 mass% or less.
  • the chemical composition of the Zn-Al-Mg-based alloy coated layer may further contain at least one selected from the group consisting of Ca, Sr, Mn, V, Cr, Mo, Ti, Ni, Co, Sb, Zr, and B in a total amount of 1 mass% or less.
  • the coating weight of the Zn-Al-Mg-based alloy coated layer in the range of 30 g/m 2 to 180 g/m 2 , it is possible to obtain a hot pressed member that is excellent in corrosion resistance and resistance to liquid metal embrittlement cracking during hot press forming. If the coating weight is less than 30 g/m 2 , it is not possible to obtain a hot pressed member with the desired corrosion resistance. If the coating weight exceeds 180 g/m 2 , alloying is not completed in the heating process before hot press forming, and the liquid phase remains. This may cause liquid metal embrittlement cracking.
  • the coating weight of the Zn-Al-Mg-based alloy coated layer is preferably 45 g/m 2 or more, and more preferably 55 g/m 2 or more.
  • the coating weight of the Zn-Al-Mg-based alloy coated layer is preferably 120 g/m 2 or less, and more preferably 100 g/m 2 or less.
  • the "coating weight per surface of the Zn-Al-Mg-based alloy coated layer" is determined as follows. From each of the Zn-Al-Mg alloy-coated steel sheets to be evaluated, three 48 mm ⁇ samples are taken by punching. Then, each sample is weighed. Subsequently, in each sample, a non-evaluated surface opposite the one surface where the coating weight is evaluated is masked. Then, 500 mL of a 35 % hydrochloric acid solution to which 3.5 g of hexamethylenetetetramine has been added is mixed up to 1 L. Then, each sample is immersed in the resultant solution for 10 minutes to dissolve the Zn-Al-Mg-based alloy coated layer. Then, each sample is weighed again. The coating weight per unit area in each sample is calculated from the mass difference before and after the dissolution of the Zn-Al-Mg-based alloy coated layer. The average of the three samples is then used as the coating weight per surface.
  • an additional layer may be provided according to the purpose without deteriorating the actions and effects of the present disclosure.
  • the lower layer include a nickel pre-coated layer.
  • the upper layer include a chemical conversion treatment layer containing, for example, a zirconium oxide or a zirconium-titanium oxide.
  • the cold-rolled steel sheets were immersed in a hot-dip Zn-Al-Mg-based coating bath with a predetermined chemical composition at a predetermined bath temperature in a galvanizing line, and then subjected to N 2 gas wiping, to produce coated steel sheets for hot press forming, which are labeled No. 1 to No. 14 in Table 1.
  • Table 1 lists the Al content, the Mg content, and the content of other elements, as well as the liquidus temperature in an air atmosphere for each Zn-Al-Mg-based alloy coated layer. The content of each element and the liquidus temperature were controlled by adjusting the chemical composition of the coating bath.
  • the content of each element in the coated layer was determined by quantitative analysis of each component of the coated layer contained in the hydrochloric acid exfoliation solution using ICP-AES.
  • the liquidus temperature of the coated layer was determined by the above-mentioned method.
  • Table 1 also lists the coating weight per surface of the Zn-Al-Mg-based alloy coated layer as determined by the above-described method. The coating weight was controlled by adjusting the wiping gas flow rate and the line speed.
  • each test specimen was removed from the electric furnace and immediately subjected to hot press forming at a forming start temperature of 700 °C using a hat-shaped press mold to obtain a hot pressed member.
  • the shape of each obtained hot pressed member was 100 mm in flat length on the top surface, 50 mm in flat length on the side surfaces, and 50 mm in flat length on the bottom surface.
  • the bending radius (or bending R) of the press mold was 7R for each shoulder on both the top and bottom surfaces.
  • FIG. 1 illustrates a cross-sectional SEM image of the Fe-Zn-Al-Mg-based alloy coated layer of the hot pressed member indicated by No. 2, which represents one of our examples
  • FIG. 2 illustrates a cross-sectional SEM image of the Fe-Zn-Al-Mg-based alloy coated layer of the hot pressed member indicated by No.
  • I ⁇ and I ⁇ were measured by X-ray diffraction using a Co-K ⁇ (wavelength: 1.79021 ⁇ ) radiation source at an incident angle of 25°, where Ir is an intensity of a diffraction peak of (411) plane of the ⁇ phase present in an angular range of 41.5° ⁇ 2 ⁇ ⁇ 43.0° and I ⁇ is an intensity of a diffraction peak of (110) plane of the ⁇ -Fe phase present in an angular range of 51.0° ⁇ 2 ⁇ ⁇ 52.0°.
  • Table 1 lists the ratio of I ⁇ /I ⁇ .
  • X-ray diffraction measurements were performed using a curved IP X-ray diffractometer (RINT-RAPID II-R available from Rigaku Corporation), under a set of conditions including tube voltage of 45 kV, tube current of 160 mA, integration time of 600 sec, and collimator diameter of 3 mm.
  • RINT-RAPID II-R available from Rigaku Corporation
  • the Al and Mg concentrations in the oxide layer were measured by the above-mentioned method, and the results are listed in Table 1.
  • the coating weight per surface of the Fe-Zn-Al-Mg-based alloy coated layer was measured by the above-mentioned method, and the results are listed in Table 1.
  • a test specimen of 70 mm ⁇ 150 mm was cut from a flat part on the top surface of each obtained hot pressed member, and subjected to zirconium-based chemical conversion treatment.
  • the chemical conversion treatment was performed using commercially available chemical conversion treatment liquid (zirconium-based chemical conversion treatment: Palmina 2100, available from Nihon Parkerizing Co. Ltd.) under a set of conditions including bath temperature of 35°C and treatment time of 120 seconds.
  • each test specimen was energized under the voltage condition that the voltage was raised in 30 seconds and held at a constant voltage for 150 seconds such that a painting layer having a thickness of 1.5 ⁇ m would be formed after baking with commercially available cationic electrodeposition paint, and then baked in an electric furnace at an ambient temperature of 170 °C for 20 minutes.
  • the cationic electrodeposition paint used was Electron GT-100 V-1 Gray, available from Kansai Paint Co. Ltd.
  • Test specimens were prepared in the same way as in Evaluation 1 until the step of electrodeposition painting, and the 7.5 mm edge of the evaluation surface and the non-evaluation surface (rear side) of each test specimen were sealed with tape. Then, a cross-cut scratch of 60 mm in length and 60° center angle was made in the center of the evaluation surface with a cutter knife to a depth that reached the base steel sheet. Each obtained test specimen was subjected to a corrosion test (VDA 233-102) and evaluated according to the corrosion condition after 4 weeks.
  • VDA 233-102 corrosion test
  • each of the hot pressed members in our examples has excellent painting layer adhesion and post-painting corrosion resistance when subjected to electrodeposition painting after zirconium-based chemical conversion treatment.
  • the hot pressed member according to the present disclosure is suitable for automotive undercarriage parts and automotive body structural parts.

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EP20923408.7A 2020-03-03 2020-10-29 Heissgepresstes bauteil und verfahren zu seiner herstellung, und beschichtetes stahlblech für heisspressen Active EP4116457B1 (de)

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