WO2014157155A1 - めっき密着性に優れた溶融亜鉛系めっき鋼板およびその製造方法 - Google Patents
めっき密着性に優れた溶融亜鉛系めっき鋼板およびその製造方法 Download PDFInfo
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- WO2014157155A1 WO2014157155A1 PCT/JP2014/058208 JP2014058208W WO2014157155A1 WO 2014157155 A1 WO2014157155 A1 WO 2014157155A1 JP 2014058208 W JP2014058208 W JP 2014058208W WO 2014157155 A1 WO2014157155 A1 WO 2014157155A1
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- 229910001335 Galvanized steel Inorganic materials 0.000 title claims abstract description 17
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- 229910006639 Si—Mn Inorganic materials 0.000 claims abstract description 7
- 229910008458 Si—Cr Inorganic materials 0.000 claims abstract description 3
- 239000011247 coating layer Substances 0.000 claims abstract 3
- 238000007747 plating Methods 0.000 claims description 107
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- 230000009467 reduction Effects 0.000 claims description 48
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
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- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0226—Hot rolling
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- 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
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- C21D8/0263—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment following hot rolling
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- C—CHEMISTRY; METALLURGY
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- 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
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/04—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing
- C21D8/0478—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips to produce plates or strips for deep-drawing involving a particular surface treatment
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- C—CHEMISTRY; METALLURGY
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- 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
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- C22C18/04—Alloys based on zinc with aluminium as the next major constituent
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- C22C—ALLOYS
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- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- 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
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C—CHEMISTRY; METALLURGY
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
- C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
- C23C2/0222—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating in a reactive atmosphere, e.g. oxidising or reducing atmosphere
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
- C23C2/024—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by cleaning or etching
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- 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
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- 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
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/004—Dispersions; Precipitations
Definitions
- the present invention is a steel plate containing B as a plating base plate and further containing one or more of Si, Mn, and Cr and subjected to hot-dip Zn-Al-Mg plating,
- the present invention relates to a hot dip galvanized steel sheet having improved metal embrittlement cracking and plating adhesion and a method for producing the same.
- Hot-dip galvanized steel sheets are widely used in various applications. However, when galvanized steel sheets are welded, cracks may occur in the weld heat affected zone, which may be a problem. This phenomenon is generally called “molten metal embrittlement cracking”, and it is considered that the molten plating component acts on the grain boundaries of the steel sheet to cause brittle fracture (grain boundary fracture).
- hot-dip Zn-Al-Mg-based steel sheets are excellent in corrosion resistance and are used in various corrosion resistance applications including building materials. Recently, a hot-dip Zn—Al—Mg-based steel sheet has been increasingly applied as a substitute for a conventional general galvanized steel sheet. However, the hot-dip Zn—Al—Mg-based plated steel sheet tends to cause molten metal embrittlement cracking more easily than the conventional hot-dip galvanized steel sheet.
- Patent Document 1 it is known that it is effective to apply a plating original plate containing B as a technique for improving resistance to molten metal embrittlement cracking.
- Patent Document 2 discloses a technique for producing a molten Zn—Al—Mg based steel sheet using a steel type for a high-strength steel sheet containing a relatively large amount (around 2% by mass) of Mn as a plating base sheet.
- molten metal embrittlement cracking no special consideration is given to the resistance to molten metal embrittlement cracking, and when this is used for welding, molten metal embrittlement cracking may become a problem.
- Patent Document 3 also discloses a technique for manufacturing a hot-dip Zn—Al—Mg based steel sheet using a high strength steel sheet containing a relatively large amount (1% by mass or more) of Mn as a plating base sheet.
- the plating original plate targeted by this technique contains B in order to improve the resistance to molten metal embrittlement cracking.
- the use of a relatively high Mn-based high-strength steel type containing B for the plating original plate causes a new problem that the adhesion of the molten Zn—Al—Mg-based plating layer tends to be lowered. .
- Patent Document 4 discloses a technique for manufacturing a hot-dip Zn—Al—Mg-based plated steel sheet on a high-strength steel sheet containing a large amount of Mn (1.5% by mass or more). Although the original plating plate targeted by this technique does not contain B, this document discloses that hot-dip Zn-Al-Mg-based plating causes problems such as non-plating and poor plating adhesion. ing. In this technique, the problem of non-plating and plating adhesion is solved by controlling the reducing atmosphere in the reduction heat treatment to bring SiO 2 in the surface layer portion of the steel sheet into an internal oxidation state.
- the external oxidation of Si is suppressed while reducing Fe, and one kind selected from FeSiO 3 , Fe 2 SiO 4 , MnSiO 3 , Mn 2 SiO 4 on the steel sheet surface or surface side.
- FeSiO 3 , Fe 2 SiO 4 , MnSiO 3 , Mn 2 SiO 4 on the steel sheet surface or surface side.
- the reduction heat treatment is also a treatment for adjusting the metal structure so that the mechanical properties of the plated steel plate have a predetermined performance by subjecting the steel plate to a high temperature. If the metal structure of a steel sheet containing B simultaneously with Si, Mn and Cr is adjusted according to the combination of the reduction heat treatment temperature and the holding time with good plating adhesion disclosed in Patent Document 3, the holding time cannot be increased. There was also a problem. In production equipment that continuously performs reduction heat treatment and hot dipping, the sheet passing speed of the steel sheet may be reduced for operational reasons. Even in such a case, it is advantageous that the plating adhesion can be secured even if the holding time is increased.
- the present invention uses a steel plate to which B is added and imparted resistance to molten metal embrittlement cracking as a plating base plate, and a molten Zn—Al—Mg based alloy plating excellent in plating adhesion
- the object is to produce a steel plate.
- the above-mentioned object is intended for a plating original sheet containing B, and by defining the conditions of the coiling temperature when hot rolling the steel sheet and the conditions of the reduction heat treatment performed when introduced into the hot dip galvanizing bath This is achieved by suppressing the steel sheet surface from being covered with a Si—Mn—B-based oxide during the reduction heat treatment to ensure plating adhesion.
- C 0.01 to 0.20%, P: 0.030% or less, S: 0.010% or less, Ti: 0.010 to 0.150%, sol.Al. : 0.100% or less, N: less than 0.010%, B: 0.0003 to 0.0100%, Si: 0.01 to 1.00%, Mn: 0.10 to 2.50%, Cr: A steel plate containing at least one selected from the group of 0.05 to 1.00%, the balance being Fe and unavoidable impurities, Winding a hot-rolled steel sheet in the range of 550 to 700 ° C; Subsequent to the reduction heat treatment, by hot dip galvanizing containing Al: 1.0 to 22.0%, Mg: 0.1 to 10.0% in mass%, the balance being Zn and inevitable impurities is applied.
- the time during which the steel sheet surface temperature is maintained at 750 ° C. or higher in the reductive heat treatment furnace is defined as “holding time”, and the maximum temperature reached on the steel sheet surface in the furnace is defined as “reducing heat treatment temperature”.
- the reduction heat treatment temperature is 750 to 860 ° C.
- Concentration (mass%) of Si and Mn within 4 ⁇ m from the steel sheet surface before the reduction heat treatment A; Si: 0.15% or less, and Mn: 0.8% or less, B; Si: 0.6% or less and Mn: 1.5% or less, provided that A is not satisfied, C: Si: more than 0.6%, or Mn: more than 1.5%.
- the hot dip galvanizing further contains at least one selected from the group consisting of Ti: 0.10% or less, B: 0.05% or less, Si: 2.0% or less by mass%. It does not matter.
- the surface of the steel plate within 10 ⁇ m of the surface of the plating original plate when hot rolling is taken up, the Si single oxide, the Mn single oxide, the Cr single oxide, the Si—Mn composite oxide, At least one of a Si—Cr composite oxide, a Mn—Cr composite oxide, and a Si—Mn—Cr composite oxide is formed.
- Such internal oxides are generated when the plating original plate has a chemical composition of mass%, Si: 0.01 to 1.00%, Mn: 0.10 to 2.50%, Cr: 0.00. This is because it contains one or more selected from the group of 05 to 1.00%.
- the inventors delay the diffusion of B to the surface layer even if a Si—Mn-based oxide is generated on the steel sheet surface in a reducing atmosphere.
- the concentration of Si and Mn is lower than the content of Si and Mn in the steel sheet within 4 ⁇ m from the surface of the steel sheet where the internal oxide is formed by winding under the above conditions during hot rolling. I also found. That is, a deficient layer of Si and Mn exists on the steel plate surface.
- a material having improved both “melting metal embrittlement cracking resistance” and “plating adhesion” in a steel sheet subjected to hot-dip Zn—Al—Mg plating having high corrosion resistance is realized.
- Production of a hot-dip Zn-Al-Mg alloy-plated steel sheet that simultaneously achieves these characteristics has been difficult, but the present invention is intended for use in hot-dip Zn-based steel sheets used for bending and welding. This contributes to the spread of hot-dip Zn—Al—Mg-based steel sheets.
- the schematic diagram which shows the boss-welding test performed in order to evaluate a melt-proof embrittlement countermeasure cracking property.
- % in the chemical composition of the plating original plate and the hot dipping means “% by mass” unless otherwise specified.
- C 0.01 to 0.20%
- C is a basic element responsible for the strength of the steel sheet, and in the present invention, a steel type having a C content level of 0.01% or more is targeted. You may manage to use the thing of C content of 0.10% or more. However, since excessive C content reduces ductility and weldability, the C content is limited to 0.20% or less.
- Si 0.01 to 1.00% Si in the steel sheet causes a Si oxide film harmful to the plating property to be generated on the steel sheet surface.
- the Si content needs to be 1.00% or less.
- Si is also one of the main elements that generate internal oxides on the inner surface of the steel sheet surface, so a content of 0.01% or more is required. More preferably, it is 0.20% or more.
- Mn in the steel sheet has the effect of strengthening the steel material by solid solution strengthening, and has the action of stabilizing the austenite and promoting the generation of transformation phases such as martensite.
- the Mn content needs to be 0.10% or more.
- the addition of a large amount of Mn causes a decrease in workability and plating properties, so the Mn content should be limited to 2.50% or less.
- Mn is one of the main elements that generate an internal oxide on the inner side of the steel sheet surface, and for that purpose, a content of 0.10% or more is required. More preferably, it is 0.20% or more.
- Cr 0.05 to 1.00% Cr in the steel sheet also has an effect of strengthening the steel material by solid solution strengthening, and is effective in suppressing molten metal embrittlement cracking. It is also one of the elements. For this reason, a content of 0.05% or more is required. More preferably, it is 0.20% or more. However, if added in a large amount, it causes a decrease in workability, so it should be limited to 1.00% or less. More preferably, it is 0.50% or less.
- P 0.030% or less P has an effect of strengthening a steel material by solid solution strengthening, but if contained in a large amount, it causes a decrease in workability. Therefore, in the present invention, the target is 0.030% or less. And It is more preferable that it is 0.020% or less.
- S 0.010% or less Since S forms a sulfide that causes a decrease in workability, it is desirable to reduce it as much as possible. As a result of various studies, the S content is allowed to be 0.010%, but is more preferably 0.005% or less particularly in applications where workability is important.
- Ti 0.010 to 0.150%
- Ti is a strong nitride-forming element and is an important element for fixing N in the plating original plate as TiN.
- N the amount of free B is secured, and the effect of improving the resistance to molten metal embrittlement cracking by free B is exhibited.
- the content is 0.020% or more.
- Ti content is restrict
- sol.Al 0.100% or less Al is added as a deoxidizing agent.
- sol.Al acid-soluble Al
- the content is limited to 0.100% or less. More preferably, it is 0.060% or less. In deoxidation, it is more effective to add Al in a range where the sol.Al content is 0.005% or more, and addition in a range where it is 0.010% or more is more effective. .
- N Less than 0.010% N reacts with B to form a boride, which causes a reduction in the amount of free B effective in improving the resistance to molten metal embrittlement cracking. As a result of various studies, the N content is limited to a range of less than 0.010%.
- B 0.0003-0.0100%
- B is an element effective for suppressing molten metal embrittlement. The effect is considered to be brought about by the fact that B is segregated as free B to the grain boundary and the interatomic bonding force increases. For that purpose, it is necessary to secure a B content of at least 0.0003% or more. More preferably, the B content is 0.0005% or more. However, excessive addition of B causes formation of borides and deterioration of workability, so the upper limit of B content is limited to 0.0100%.
- Nb 0.10% or less
- Nb is an element effective in securing free B having an effect of improving resistance to molten metal embrittlement cracking because Nb has an action of fixing N.
- the steel plate of this invention can contain Nb as needed. When Nb is contained, it is more effective to set the content to 0.001% or more. However, since a large amount of addition causes a decrease in workability, Nb is 0.10% or less, preferably 0.05% or less.
- Mo 0.50% or less
- Mo is also an element having an effect of improving the resistance to molten metal embrittlement cracking, and the steel sheet of the present invention can contain Mo if necessary. When Mo is contained, it is more effective to set the content to 0.01% or more. However, since a large amount of addition causes a decrease in workability, Mo should be added to 0.50% or less, preferably 0.20% or less.
- the slab to be subjected to hot rolling and the finishing temperature are not particularly limited, and may be as usual.
- the coiling temperature is in the range of 550 to 700 ° C. By winding at this temperature, within a range of 10 ⁇ m or less from the surface layer of the steel plate covered with oxide scale, a single oxide or complex oxide of Si, Mn, and Cr is generated as an internal oxide, and Si and Mn A depletion layer is formed.
- a hot-rolled steel plate or a cold-rolled steel plate having the above chemical composition can be used as the plating base plate.
- cold rolling is performed in accordance with a conventional method, and finished to a predetermined thickness.
- the surface oxide scale needs to be sufficiently removed.
- the plate thickness may be selected in the range of 0.6 to 4.5 mm, for example, depending on the application.
- the steel plate sample was subjected to reduction heat treatment under various conditions, and the surface was observed. According to this, in the steel type without addition of B, which provides good plating adhesion, the surface is dotted with Si-Mn-based oxides, and even if the reductive heat treatment conditions are changed, this surface state changes greatly. Was not seen.
- the same Si—Mn-based oxide as described above becomes a surface state scattered on the surface of the plating base plate, but as the heating proceeds, It was found that the B diffused from the silicon was added to the Si—Mn oxide, and the scattered oxide became an Si—Mn—B oxide. As the diffusion of B from the steel further progresses, the Si—Mn—B-based oxide on the surface of the steel sheet increases the B concentration and lowers the melting point. As a result, it is considered that the Si—Mn—B-based oxide partially melts during the reduction heat treatment, and the resulting melt covers the flat portion of the steel sheet surface.
- the time during which the steel sheet surface temperature is maintained at 750 ° C. or higher in a reducing atmosphere furnace is defined as “holding time”, and the maximum temperature reached on the steel sheet surface in the furnace is defined as “reducing heat treatment temperature”
- holding time the time during which the steel sheet surface temperature is maintained at 750 ° C. or higher in a reducing atmosphere furnace
- reducing heat treatment temperature the maximum temperature reached on the steel sheet surface in the furnace
- the concentration of Si and Mn within 4 ⁇ m of the steel sheet surface is determined by a preliminary experiment according to the combination of the steel type to be passed through the production line and the coiling temperature, and the combination of the Si concentration and the Mn concentration is the following A
- the holding time of the reduction heat treatment is controlled depending on which of the following conditions is met.
- the reduction heat treatment temperature is 750 to 860 ° C.
- the holding time is within 250 seconds
- the condition B is satisfied
- the holding time is within 200 seconds
- the condition C is satisfied
- the reduction heat treatment may be performed under the condition that the holding time is within 150 seconds.
- the recrystallization annealing is also performed by the reduction heat treatment
- a condition in which the recrystallization temperature is reached or higher up to the inside of the steel sheet may be employed in each of the above condition ranges.
- the reduction treatment temperature maximum surface temperature
- an atmosphere conventionally used as a pretreatment for hot dipping can be applied.
- a 5 to 50 volume% H 2 —N 2 atmosphere can be exemplified.
- Al in the plating bath is effective in improving the corrosion resistance of the plated steel sheet, and suppresses the generation of Mg oxide-based dross in the plating bath.
- the effect is recognized when the Al content of the hot dipping bath is 4.0% or more.
- Al is also effective in improving the plating adhesion.
- the Al content of the hot dipping bath needs to be 1.0% or more.
- the Al content exceeds 22.0%, a brittle Fe—Al alloy layer grows excessively at the interface between the plating layer and the steel substrate, which causes a decrease in plating adhesion.
- the Al content is preferably 15.0% or less, and may be controlled to 10.0% or less.
- Mg in the plating bath exhibits the effect of significantly increasing the corrosion resistance of the plated steel sheet by generating a uniform corrosion product on the surface of the plating layer. It is also effective in improving plating adhesion. These effects are manifested when the Mg content of the hot dipping bath is in the range of 0.10% or more, and in order to obtain a particularly remarkable effect, it is more preferable to secure a Mg content of 1.0% or more. On the other hand, when the Mg content exceeds 10.0%, Mg oxide-based dross tends to occur. In order to obtain a higher quality plating layer, the Mg content is preferably 5.0% or less, and may be controlled to 4.0% or less.
- Si When Si is contained in the hot dip plating bath, excessive growth of the Fe—Al alloy layer formed at the interface between the steel substrate and the plating layer is suppressed, and the workability of the hot dip Zn—Al—Mg plated steel sheet is improved. Is advantageous. Moreover, Si is effective in preventing the black change of the plating layer and maintaining the glossiness of the surface. Therefore, Si can be contained as necessary. When Si is contained, it is more effective to set the Si content of the hot dipping bath to 0.005% or more. However, since excessive Si content increases the amount of dross in the hot dipping bath, the Si content in the plating bath is limited to 2.0% or less.
- Fe is mixed in the hot dipping bath because of the immersion and passage of the steel sheet.
- the Fe content in the Zn—Al—Mg plating bath is generally allowed to be about 2.0%.
- the plating bath for example, one or more of Ca, Sr, Na, rare earth elements, Ni, Co, Sn, Cu, Cr and Mn may be mixed, but the total content thereof is 1 It is desirable to manage to 0.0% or less.
- the amount of plating adhesion is desirably adjusted in the range of 20 to 300 g / m 2 per one side of the steel sheet.
- the steel having the chemical composition shown in Table 1 is melted, the slab is heated to 1250 ° C., extracted, and hot rolled at a finish rolling temperature of 880 ° C. and a winding temperature of 520 to 700 ° C., A hot-rolled steel strip having a thickness of 2.4 mm was obtained.
- the hot-rolled steel strip was pickled and cold-rolled to prepare a cold-rolled steel plate having a thickness of 1.4 mm.
- a part of the cold-rolled steel sheet is sampled and embedded in the resin, a cross section parallel to the thickness direction is observed with a scanning transmission electron microscope (STEM), and energy dispersive X-ray spectroscopy (EDX) is used.
- STEM scanning transmission electron microscope
- the Si concentration and Mn concentration in the vicinity of the steel sheet surface layer (within a depth of 4 ⁇ m from the rolled surface) were quantified.
- the internal oxide was confirmed by performing etching with a nital solution on the embedded cross section and using an optical microscope or a scanning electron microscope (SEM). Displayed in Tables 2 and 3 as “O” for the formation of oxide in the region within 10 ⁇ m depth from the vicinity of the steel plate surface of the cross section (within 10 ⁇ m depth from the rolling surface), and “X” for those not confirmed. did.
- each cold-rolled steel sheet is subjected to reduction heat treatment at various holding times and reduction heat treatment temperatures, and then immersed in a hot dip galvanizing bath without being exposed to the atmosphere, pulled up from the bath, and the amount of plating deposited per side Of about 90 g / m 2 was obtained.
- the experimental conditions are described in Tables 2 and 3 and are as follows.
- the welding conditions were a welding current: 217 A, a welding voltage of 25 V, a welding speed of 0.2 m / min, a shielding gas: CO 2 , and a shielding gas flow rate: 20 L / min.
- YGW12 was used for the welding wire. After the welding start point made one round around the boss and after the welding start point was passed, welding was continued further to make a portion 4 where the weld beads 3 overlapped.
- the test piece 1 and the boss 2 were cut as indicated by a broken line so as to include the bead overlap portion 4, embedded in a resin so that the cut surface 5 could be observed, and the bead overlap portion was observed with an optical microscope. .
- the length of the crack was measured.
- the longest crack length was defined as the “maximum crack length”. This crack occurs along the prior austenite grain boundary of the weld heat affected zone, and it is determined that this crack is a molten metal embrittlement crack.
- the evaluation of the resistance to molten metal embrittlement cracking was a pass ( ⁇ ) when the maximum crack length was 0.1 mm or less, and a reject (x) when the maximum crack length exceeded 0.1 mm.
- the evaluation results are shown in Table 4. Steels A to J and O passed, but steels K to N failed.
- Test piece 2 Boss 3 Weld bead 4 Bead overlap part 5 Cut surface
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Abstract
Description
しかし、還元熱処理を行う還元帯において、Feを還元しながらSiの外部酸化を抑制し、鋼板表面または表面側にFeSiO3,Fe2SiO4,MnSiO3,Mn2SiO4から選ばれた1種以上のSi酸化物を生成させる目的で、還元帯の雰囲気中の酸素分圧PO2が所定の範囲となるように管理しなければならず煩雑である。
熱延鋼板を550~700℃の範囲で巻き取ることと、
還元熱処理に引き続いて、質量%で、Al:1.0~22.0%、Mg:0.1~10.0%を含有し、残部がZnおよび不可避的不純物からなる溶融亜鉛系めっきを施すにあたり、
還元熱処理工程において、還元熱処理の炉内で鋼板表面温度が750℃以上に保持される時間を「保持時間」、当該炉内での鋼板表面の最高到達温度を「還元熱処理温度」と定義するとき、
還元熱処理温度を750~860℃とし、
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度が下記の条件Aを満たす場合は保持時間を250秒以内、条件Bを満たす場合は保持時間を200秒以内、条件Cを満たす場合は保持時間を150秒以内として還元熱処理を行うことにより、めっき密着性に優れた溶融亜鉛系めっき鋼板を得る。
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度(質量%):
A; Si:0.15%以下、かつMn:0.8%以下、
B; Si:0.6%以下、かつMn:1.5%以下、ただしAを満たさない、
C; Si:0.6%超え、またはMn:1.5%超え。
また、発明者らは、熱間圧延時に前記の条件で巻き取って内部酸化物が生成した鋼板表面から4μm以内では、SiとMnの濃度が鋼板のSiとMnの含有量よりも低下することも見出した。すなわち、鋼板表面には、SiとMnの欠乏層が存在する。この濃度に応じて還元熱処理の保持時間を設定することにより、めっき密着性に優れた溶融Zn-Al-Mg系めっき鋼板が得られるのである。
本発明の対象となる鋼板の化学組成は以下のとおりである。
C:0.01~0.20%
Cは、鋼板の強度を担う基本的な元素であり、本発明では0.01%以上のC含有量レベルの鋼種を対象とする。0.10%以上のC含有量のものを使用するように管理してもよい。ただし、過剰のC含有は延性、溶接性を低下させるので、C含有量は0.20%以下に制限される。
鋼板中のSiは、めっき性に有害なSi酸化膜を鋼板表面に生じさせる要因となる。種々検討の結果、Si含有量は1.00%以下とする必要がある。ただし、本発明では、Siは鋼板表面の内側に内部酸化物を生成させる主要な元素のひとつでもあるため、0.01%以上の含有量が必要となる。0.20%以上とすることがより好ましい。
鋼板中のMnは、固溶強化によって鋼材を強化する作用を有すると共に、オーステナイトを安定化させマルテンサイト等の変態相の生成を促進させる作用を有するので、鋼板の強度の確保と機械的特性の安定化のために、Mn含有量は0.10%以上とする必要がある。ただし、多量のMn添加は加工性およびめっき性を低下させる要因となるので、Mn含有量は2.50%以下に制限するのがよい。
一方、本発明では、Mnは鋼板表面の内側に内部酸化物を生成させる主要な元素のひとつであり、そのためにも0.10%以上の含有量が必要となる。0.20%以上とすることがより好ましい。
鋼板中のCrも、固溶強化によって鋼材を強化する作用を有するとともに、耐溶融金属脆化割れの抑制にも有効であり、しかも本発明では、鋼板表面の内側に内部酸化物を生成させる主要な元素のひとつでもある。そのため、0.05%以上の含有量が必要となる。0.20%以上とすることがより好ましい。ただし、多量に添加すると加工性を低下させる要因となるので、1.00%以下に制限するのがよい。0.50%以下とすることがより好ましい。
Pは、固溶強化によって鋼材を強化する作用を有するが、多量に含有すると加工性を低下させる要因となるので、本発明では、0.030%以下のものを対象とする。0.020%以下であることがより好ましい。
Sは、加工性低下の要因となる硫化物を形成するので、できるだけ低減することが望ましい。種々検討の結果、S含有量は0.010%まで許容されるが、特に加工性を重視する用途では0.005%以下とすることがより好ましい。
Tiは、強力な窒化物形成元素であり、めっき原板中のNをTiNとして固定する上で重要な元素である。Nを固定することによりフリーBの量が確保され、フリーBによる耐溶融金属脆化割れ性の向上作用が発揮される。検討の結果、上記作用を十分に発揮させるためには0.010%以上のTi含有量を確保する必要がある。0.020%以上とすることがより好ましい。ただし、過剰にTiを添加しても上記効果は飽和し、またTiの多量添加は鋼材の加工性を劣化させる要因になる。このためTi含有量は0.150%以下の範囲に制限される。
Alは、脱酸剤として添加されるが、過剰のAl添加はプレス成形性の低下を招く等の弊害を生じるので、sol.Al(酸可溶Al)として0.100%以下の含有量に制限される。0.060%以下であることがより好ましい。なお、脱酸においてはsol.Al含有量が0.005%以上となる範囲でAlを添加することがより効果的であり、0.010%以上となる範囲での添加が一層効果的である。
Nは、Bと反応して硼化物を形成し、耐溶融金属脆化割れ性の改善に有効なフリーBの量を低減させる要因となる。種々検討の結果、N含有量は0.010%未満の範囲に制限される。
Bは、溶融金属脆化の抑制に有効な元素である。その作用はBがフリーBとして結晶粒界に偏析して原子間結合力が増大することによってもたらされるものと考えられる。そのためには少なくとも0.0003%以上のB含有量を確保する必要がある。0.0005%以上のB含有量とすることがより好ましい。ただし、過剰のB添加は硼化物の生成、加工性劣化の要因となるため、B含有量の上限は0.0100%に制限される。
Nbは、Nを固定する作用を有するので、耐溶融金属脆化割れ性を高める効果を有するフリーBを確保する上で有効な元素である。このため、本発明の鋼板は、必要に応じてNbを含有させることができる。Nbを含有させる場合は、0.001%以上の含有量とすることがより効果的である。ただし、多量の添加は加工性を低下させる要因となるので、Nbは0.10%以下、好ましくは0.05%以下がよい。
Moも耐溶融金属脆化割れ性を高める効果を有する元素であり、本発明の鋼板は、必要によりMoを含有させることができる。Moを含有させる場合は、0.01%以上の含有量とすることがより効果的である。ただし、多量の添加は加工性を低下させる要因となるので、Moは0.50%以下、好ましくは0.20%以下の添加に留めるべきである。
熱間圧延に供するスラブや、仕上げ温度は特に限定されず、常法のとおりでよい。巻取り温度は550~700℃の範囲とする。この温度で巻取ることによって、酸化スケールに覆われた鋼板表層から10μm以下の範囲内に、Si、MnやCrの単独酸化物あるいは複合酸化物が内部酸化物として生成するととともに、SiやMnの欠乏層が形成される。
めっき原板を溶融亜鉛系めっき浴に導入する前に、通常、鋼板表面を活性化させるために還元熱処理が行われる。大量生産現場の連続溶融めっきラインでは、還元熱処理と溶融めっきを連続的に行うようになっている。この還元熱処理工程は、単にめっき原板の表面を活性化させるだけではなく、鋼板の金属組織を最終的な組織状態に調整するための焼鈍工程を兼ねる場合が多い。したがって、目的に応じて種々のヒートパターンが採用される。また、ラインの操業状況によっては、活性化や焼鈍に支障のない範囲で熱処理炉を通過する鋼帯の速度(ライン速度)が調整されることもある。
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度が下記の条件Aを満たす場合は保持時間を250秒以内、条件Bを満たす場合は保持時間を200秒以内、条件Cを満たす場合は保持時間を150秒以内とする条件により還元熱処理を行えばよい。
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度(質量%):
A; Si:0.15%以下、かつMn:0.8%以下、
B; Si:0.6%以下、かつMn:1.5%以下、ただしAを満たさない、
C; Si:0.6%超え、またはMn:1.5%超え。
上記の還元熱処理を終えためっき原板を、大気に曝すことなく、溶融Zn-Al-Mg系めっき浴に導入する。
次に、各冷延鋼板について、種々の保持時間、還元熱処理温度にて還元熱処理を施し、その後、大気に曝すことなく溶融亜鉛系めっき浴に浸漬し、浴から引き上げ、片面当たりのめっき付着量が約90g/m2の溶融亜鉛系めっき鋼板を得た。実験条件は表2、表3に記載した他、以下のとおりである。
表2、表3には、上述の条件A、B、Cに対応する条件を次のように記号で表記した。
◎: Si:0.15%以下、かつMn:0.8%以下、
○; Si:0.6%以下、かつMn:1.5%以下、ただし◎に含まれない、
●; Si:0.6%超え、またはMn:1.5%超え。
雰囲気ガス;30%H2-N2雰囲気
熱処理温度と保持時間:表2、表3に記載
・浴組成; 表2、表3に記載
・浴温; 400℃
・浴浸漬時間; 2sec
得られためっき鋼板から幅15mmの曲げ試験片を切り出し、先端半径R=5mmのポンチを用いて90°V曲げ試験を行った。試験片の幅方向(=曲げ軸の方向)が圧延方向と一致するようにした。曲げ試験後の試験片について、曲げ加工部の外周部にJIS Z1522で定めるセロハン粘着テープを貼付した後、剥ぎ取って、テープにめっき層の付着が認められないものを○(めっき密着性;良好)、それ以外のものを×(めっき密着性;不良)と判定した。同種のめっきサンプルについてn=3で曲げ試験を行い、最も評価の悪い試験片の結果をそのサンプルの成績として採用した。結果は、表2、表3に示している。
めっき鋼板から100mm×75mmのサンプルを切り出し、これをアーク溶接による溶融金属脆化に起因する溶接最大割れ長さを評価するための試験片とした。
溶接試験は図1に示すような外観のボス溶接部材を作製する「ボス溶接」を行い、その溶接部断面を観察して割れの発生状況を調べた。すなわち、試験片1の板面中央に直径20mm×長さ25mmの軟鋼からなるボス(突起)2を垂直に立て、このボス2を試験片1にアーク溶接にて接合した。溶接条件は、溶接電流:217A、溶接電圧25V、溶接速度0.2m/min、シールドガス:CO2、シールドガス流量:20L/minとした。溶接ワイヤは、YGW12を用いた。
溶接開始点からボスの周囲を1周して溶接開始点を過ぎた後もさらに溶接を続けて溶接ビード3が重なった部分4を作った。
その評価結果を表4に示す。鋼A~JおよびOは合格であったが、鋼K~Nの4種は不合格であった。
2 ボス
3 溶接ビード
4 ビード重なり部
5 切断面
Claims (8)
- めっき原板である鋼板とその表面上に形成された溶融亜鉛系めっき層との界面から10μm以内の鋼板内部に、Si単独酸化物、Mn単独酸化物、Cr単独酸化物、Si-Mn系複合酸化物、Si-Cr系複合酸化物、Mn-Cr系複合酸化物、Si-Mn-Cr系複合酸化物の少なくとも1種以上が存在するめっき密着性に優れた溶融亜鉛系めっき鋼板。
- めっき原板である鋼板は、質量%で、Si:0.01~1.00%、Mn:0.10~2.50%、Cr:0.05~1.00%の群から選ばれる1種以上を含有する化学組成を有するものである請求項1に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板。
- めっき原板である鋼板は、質量%で、C:0.01~0.20%、P:0.030%以下、S:0.010%以下、Ti:0.010~0.150%、sol.Al:0.100%以下、N:0.010%未満、B:0.0003~0.0100%と、さらにSi:0.01~1.00%、Mn:0.10~2.50%、Cr:0.05~1.00%の群から選ばれる1種以上を含有し、残部Feおよび不可避的不純物からなる化学組成を有するものである請求項1に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板。
- めっき原板である鋼板は、質量%で、さらにNb:0.10%以下、Mo:0.50%以下を含有する化学組成を有するものである請求項3に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板。
- 溶融亜鉛系めっきの組成が、質量%でAl:1.0~22.0%、Mg:0.1~10.0%、残部がZnおよび不可避的不純物である請求項1~4のいずれか1項に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板。
- 溶融亜鉛系めっきの組成が、さらに、質量%で、Ti:0.10%以下、B:0.05%以下、Si:2.0%以下の群から選ばれる1種以上を含有するものである請求項5に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板。
- 質量%で、C:0.01~0.20%、P:0.030%以下、S:0.010%以下、Ti:0.010~0.150%、sol.Al:0.100%以下、N:0.010%未満、B:0.0003~0.0100%と、さらにSi:0.01~1.00%、Mn:0.10~2.50%、Cr:0.05~1.00%の群から選ばれる1種以上を含有し、残部Feおよび不可避的不純物からなる鋼板をめっき原板として熱間圧延し、還元熱処理に引き続いて、質量%でAl:1.0~22.0%、Mg:0.1~10.0%、残部がZnおよび不可避的不純物である組成の溶融亜鉛系めっきを施して溶融亜鉛系めっき鋼板を製造するにあたり、
めっき原板の熱間圧延工程において巻取り温度を550~700℃の範囲とし、
還元熱処理工程において、還元熱処理の炉内で鋼板表面温度が750℃以上に保持される時間を「保持時間」、当該炉内での鋼板表面の最高到達温度を「還元熱処理温度」と定義するとき、
還元熱処理温度を750~860℃とし、
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度が下記の条件Aを満たす場合は保持時間を250秒以内、条件Bを満たす場合は保持時間を200秒以内、条件Cを満たす場合は保持時間を150秒以内として還元熱処理を行うめっき密着性に優れた溶融亜鉛系めっき鋼板の製造方法。
還元熱処理前の鋼板表面から4μm以内におけるSiとMnの濃度(質量%):
A; Si:0.15%以下、かつMn:0.8%以下、
B; Si:0.6%以下、かつMn:1.5%以下、ただしAを満たさない、
C; Si:0.6%超え、またはMn:1.5%超え。 - 溶融亜鉛系めっきの組成が、さらに、質量%で、Ti:0.10%以下、B:0.05%以下、Si:2.0%以下の群から選ばれる1種以上を含有するものである請求項7に記載のめっき密着性に優れた溶融亜鉛系めっき鋼板の製造方法。
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JP2011231346A (ja) * | 2010-04-23 | 2011-11-17 | Nisshin Steel Co Ltd | 溶融亜鉛系めっき高張力鋼板の製造法 |
JP2012126994A (ja) * | 2010-11-26 | 2012-07-05 | Jfe Steel Corp | 溶融Al−Zn系めっき鋼板 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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US10975454B2 (en) * | 2015-12-15 | 2021-04-13 | Posco | Ultra-high strength steel sheet having excellent phosphatability and bendability |
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MX366702B (es) | 2019-07-22 |
US20160024632A1 (en) | 2016-01-28 |
MY172243A (en) | 2019-11-19 |
CN105051238A (zh) | 2015-11-11 |
SG10201707903VA (en) | 2017-11-29 |
EP2980259A4 (en) | 2016-11-30 |
JP5826321B2 (ja) | 2015-12-02 |
US9523142B2 (en) | 2016-12-20 |
AU2014245876A1 (en) | 2015-10-08 |
MX2015013368A (es) | 2016-01-08 |
KR20150133708A (ko) | 2015-11-30 |
SG11201507737QA (en) | 2015-10-29 |
JP2014208902A (ja) | 2014-11-06 |
CN105051238B (zh) | 2017-10-10 |
AU2014245876B2 (en) | 2018-06-14 |
CA2904131C (en) | 2019-10-22 |
CA2904131A1 (en) | 2014-10-02 |
EP2980259A1 (en) | 2016-02-03 |
BR112015024016A2 (pt) | 2017-07-18 |
KR102014062B1 (ko) | 2019-08-27 |
NZ711709A (en) | 2020-07-31 |
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