WO2019009003A1 - 表面外観に優れた溶融Zn-Al-Mg系めっき鋼板およびその製造方法 - Google Patents
表面外観に優れた溶融Zn-Al-Mg系めっき鋼板およびその製造方法 Download PDFInfo
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- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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- C22C18/04—Alloys based on zinc with aluminium as the next major constituent
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- 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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- 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
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- 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
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- 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
- C23C2/29—Cooling or quenching
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- 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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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/42—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also phosphates
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- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- 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
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- 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
- C23C28/02—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 only coatings only including layers of metallic material
- C23C28/023—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 only coatings only including layers of metallic material only coatings of metal elements only
- C23C28/025—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 only coatings only including layers of metallic material only coatings of metal elements only with at least one zinc-based layer
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- 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
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
Definitions
- the present invention relates to a hot-dip Zn—Al—Mg-based plated steel sheet excellent in surface appearance and a method of manufacturing the same.
- Surface-treated steel sheets such as hot-dip galvanized steel sheets are excellent in corrosion resistance and are applied to a wide range of fields such as automobiles, electric machines, building materials and the like. Furthermore, in recent years, there has been an increasing demand for the application of surface-treated steel sheets to the harsh outdoor corrosive environment, so that molten Zn- obtained by adding aluminum (Al) and magnesium (Mg) to zinc (Zn) further improves corrosion resistance.
- An Al-Mg-based plated steel sheet has been proposed (for example, Patent Document 1).
- Patent Document 1 proposes a technique for controlling the cooling rate to suppress crystallization of the Mg 2 Zn 11 phase.
- Patent Document 2 proposes a technique for suppressing the crystallization of the Mg 2 Zn 11 phase by adding Ti, B or the like to a plating bath.
- the present invention has been made in view of such circumstances, and provides a hot-dip Zn—Al—Mg-based plated steel sheet excellent in surface appearance and a method for producing the same.
- MgZn 2 / Mg / Zn compound phase in a plating film composed of Zn phase, Al phase and Mg-Zn compound phase By controlling the plating phase structure so that the X-ray intensity ratio of Mg 2 Zn 11 is 0.2 or less, it is possible to produce a hot-dip Zn-Al-Mg-based plated steel sheet excellent in surface appearance without black spots. I found out.
- the present invention is based on the above findings, and the features thereof are as follows.
- It has a plating film containing 1 to 22% by mass of Al, 0.1 to 10% by mass of Mg on the surface of a steel plate,
- the X-ray diffraction peak intensity ratio of MgZn compound phases in the plating film: Zn-Al-Mg-based plated steel sheet MgZn 2 / Mg 2 Zn 11 is 0.2 or less.
- the base steel plate is immersed in a plating bath containing 1 to 22 mass% of Al, 0.1 to 10 mass% of Mg to carry out a hot-dip Zn—Al—Mg-based plating treatment, Next, primary cooling is performed to cool the steel sheet after the hot-dip Zn-Al-Mg-based plating treatment to a primary cooling stop temperature: less than 300 ° C., Subsequently, heating temperature: It heats to 280 degreeC or more and 340 degrees C or less, Then, the manufacturing method of the hot dip Zn-Al-Mg type
- the primary cooling stop temperature is set to 200 ° C.
- examples of the hot-dip Zn-Al-Mg-based plated steel sheet include Zn-Al-Mg-plated steel plate, Zn-Al-Mg-Ni-plated steel plate, Zn-Al-Mg-Si-plated steel plate, and the like.
- the present invention is not limited to these and all known hot-dip Zn-Al-Mg-based platings including Zn, Al and Mg are applicable.
- % indicating the composition of steel and% indicating the composition of plating are all mass%.
- the plating film of the present invention is a plating film containing 1 to 22% by mass of Al and 0.1 to 10% by mass of Mg.
- Al 1 to 22% by mass Al is added for the purpose of improving the corrosion resistance.
- the Al content in the plated film is less than 1%, sufficient corrosion resistance can not be obtained.
- a Zn—Fe alloy phase grows at the plating / base material interface, and the workability is significantly reduced.
- the Al content exceeds 22%, the corrosion resistance improving effect is saturated. Therefore, the range of the Al content is 1 to 22%. Preferably, it is 4 to 15%.
- Mg 0.1 to 10% by mass Like Al, Mg is also added for the purpose of improving the corrosion resistance.
- Mg content in the plating film is less than 0.1%, sufficient corrosion resistance can not be obtained.
- Mg content exceeds 10% the corrosion resistance improving effect is saturated.
- Mg oxide dross tends to occur. Therefore, the range of the Mg content is 0.1 to 10%.
- MgZn 2 may locally crystallize out as primary crystals in the plating film after primary cooling.
- MgZn 2 crystallized as primary crystals tends to be relatively large, and it is necessary to prolong the heat treatment for solid phase transformation from the MgZn 2 phase main component to the Mg 2 Zn 11 phase main component described later. Therefore, it is preferable to be 5% or less. Furthermore, it is more preferable to be 3% or less.
- the plating film can contain Ni, Si, and the like.
- Ni 0.005 to 0.25 mass% When Ni is contained, 0.005 to 0.25% is preferably contained. If the hot-dip Zn-Al-Mg-based plated steel sheet is stored for a long time in a severe corrosive environment such as high temperature and humidity, the plating surface may be oxidized to cause "blackening" that changes to gray to black. The blackening resistance can be improved by containing. If the Ni content is 0.005% or more, more excellent blackening resistance can be obtained. If it exceeds 0.25%, dross may occur in the plating bath, which may cause appearance defects due to the adhesion of dross.
- the Mg—Zn compound phase during plating is changed from the main body of MgZn 2 to the structure of the main body of Mg 2 Zn 11 by heating as described later.
- the present invention by adding Ni during plating, it is possible to suppress the decrease in blackening resistance due to the change of the Mg—Zn compound in the plating film.
- Si When Si is contained, it is preferable to contain 0.01 to 0.5%. Si is added for the purpose of corrosion resistance improvement, and if less than 0.01%, the corrosion resistance improvement effect can not be obtained. If it exceeds 0.5%, dross may occur in the plating bath, resulting in poor appearance.
- phase structure (hereinafter, also referred to as a plating phase structure or simply as a phase structure) of the plated film of the hot-dip Zn—Al—Mg-based plated steel sheet of the present invention
- the plated film of the hot-dip Zn-Al-Mg-based plated steel sheet is mainly composed of a Zn phase, an Al phase, and a Mg-Zn compound phase.
- the Mg-Zn compound phase of the hot-dip Zn-Al-Mg-based plated steel sheet which has been proposed up to this point is mainly composed of the MgZn 2 phase.
- the Mg—Zn compound phase is characterized mainly in the Mg 2 Zn 11 phase.
- the present inventors can produce a hot-dip Zn-Al-Mg-based plated steel sheet free of black spots. I found it possible.
- the ratio between the MgZn 2 phase and the Mg 2 Zn 11 phase can be determined using X-ray diffraction.
- the X-ray intensity ratio of MgZn 2 / Mg 2 Zn 11 that is, the X-ray diffraction peak intensity ratio: MgZn 2 / Mg 2 Zn 11 to 0.2 or less, the surface appearance without black spots was excellent.
- a hot-dip Zn-Al-Mg-based plated steel sheet can be obtained.
- the X-ray diffraction peak intensity ratio: MgZn 2 / Mg 2 Zn 11 is 0.1 or less.
- the base steel plate is immersed in a plating bath containing 1 to 22 mass% of Al, 0.1 to 10 mass% of Mg to carry out a hot-dip Zn-Al-Mg-based plating treatment, and then the hot-dip Zn-Al-Mg.
- Primary cooling stop temperature The primary cooling is performed to cool the steel plate after the system plating treatment to less than 300 ° C. Then, the heating temperature: 280 ° C. or more and 340 ° C. or less and secondary cooling.
- the hot-dip Zn-Al-Mg-based plated steel sheet of the present invention can also be subjected to heating after primary cooling and secondary cooling by batch processing, but is preferably produced using a continuous hot-dip galvanizing line (CGL) .
- CGL continuous hot-dip galvanizing line
- Plating Treatment Plating bath contains 1 to 22% Al, 0.1 to 10% Mg.
- the plating bath composition is as described above.
- 0.005 to 0.25% of Ni can also be contained.
- 0.01 to 0.5% of Si can also be contained.
- Al content and Mg content in a plating bath, and Al content and Mg content in a plating film become substantially the same. Therefore, the bath composition is adjusted to achieve the desired plating film composition.
- the remainder of the plating bath is Zn and unavoidable impurities.
- the temperature of the plating bath is not particularly limited, but is preferably less than 470 ° C. When the temperature is 470 ° C. or more, the formation of the interfacial alloy phase is promoted, and the processability may be reduced.
- the primary cooling stop temperature cooling to less than 300 ° C.
- the MgZn 2 phase is transformed to the Mg 2 Zn 11 phase.
- the freezing point of the hot-dip Zn—Al—Mg-based plating is approximately 340 ° C.
- primary cooling stop temperature shall be less than 300 ° C. Preferably it is 250 degrees C or less, More preferably, it is 200 degrees C or less.
- the cooling rate of the primary cooling is not particularly limited. It is preferable that it is 10 degrees C / s or more from a viewpoint of productivity.
- the plated film may be in a supercooled state, and the plated film may be in a molten state even below the freezing point (about 340 ° C.).
- load may be applied in consideration of the performance of a manufacturing facility. From these points, the cooling rate is preferably 150 ° C./s or less.
- the heating temperature is heated to 280 ° C. or more and 340 ° C. or less.
- the present inventors heat-treated a Zn-Al-Mg-based plated steel sheet containing a MgZn 2 phase in a specific temperature range. It was found that the MgZn 2 phase transformed to the Mg 2 Zn 11 phase.
- the mechanism of the phase transformation from the MgZn 2 phase to the Mg 2 Zn 11 phase by heat treatment is not clear, but Mg diffuses from the MgZn 2 phase to the adjacent Zn phase to make Mg the thermodynamically most stable phase. It is inferred that solid phase transformation to the 2 Zn 11 phase has occurred.
- the heating temperature needs to be 280 ° C. or more.
- the heating temperature is less than 280 ° C., it takes time to transform the MgZn 2 phase to the Mg 2 Zn 11 phase, and the Mg 2 Zn 11 phase is not sufficiently formed.
- the higher the heating temperature the more phase transformation is promoted, but if it exceeds 340 ° C, the ternary eutectic of the Zn / Al / Mg-Zn compound in the plating melts and the MgZn 2 phase becomes secondary in secondary cooling Crystallize.
- the MgZn 2 phase crystallizes, local crystallization of the Mg 2 Zn 11 phase occurs in the subsequent manufacturing steps, resulting in black spots, which is not preferable in appearance.
- the heating temperature is in the range of 280 ° C. or more and 340 ° C. or less.
- the temperature is preferably in the range of 300 to 340 ° C. or less, more preferably 320 ° C. or more and 340 ° C. or less.
- the secondary cooling stop temperature is not particularly limited, and may be room temperature, for example.
- the secondary cooling rate is not particularly limited, but is preferably 10 ° C./s or more from the viewpoint of productivity. In consideration of the performance of the manufacturing facility, etc., 150 ° C./s or less is preferable.
- the primary cooling stop temperature and the heating temperature are both surface temperatures of the steel plate. Moreover, a heating rate, a primary cooling rate, and a secondary cooling rate are determined based on the surface temperature of a steel plate.
- the heating temperature after primary cooling is A (° C.)
- the process from heating after secondary cooling to secondary cooling the time for the steel plate to become 250 ° C. or higher is t (seconds)
- t the time for the steel plate to become 250 ° C. or higher.
- Desired X-ray diffraction peak intensity ratio In order to stably obtain 0.2 or less of MgZn 2 / Mg 2 Zn 11, it is preferable to set 1/2 ⁇ (A ⁇ 250) ⁇ t to 18 or more. More preferably, 1 ⁇ 2 ⁇ (A ⁇ 250) ⁇ t is 100 or more. On the other hand, 1 ⁇ 2 ⁇ (A ⁇ 250) ⁇ t is preferably 13500 or less. When 1/2 ⁇ (A ⁇ 250) ⁇ t exceeds 13500, Mg 2 Zn 11 grows into grains and becomes coarse due to excessive heat treatment, so that the blackening resistance deteriorates. Therefore, 1/2 ⁇ (A ⁇ 250) ⁇ t is preferably 13500 or less. More preferably, it is 8000 or less.
- the hot-dip Zn—Al—Mg-based plated steel sheet of the present invention is obtained.
- the plating adhesion amount there is no particular limitation on the plating adhesion amount. From the viewpoint of corrosion resistance, 10 g / m 2 or more per side is preferable. From the viewpoint of processability, 500 g / m 2 or less per side is preferable.
- the base steel plate to be subjected to the hot-dip Zn-Al-Mg-based plating treatment is not particularly limited. It is applicable to both a hot rolled steel sheet and a cold rolled steel sheet.
- the molten Zn—Al—Mg-based plated steel sheet may be further subjected to a chemical conversion treatment to form a chemical conversion treatment film on the plating film.
- a chemical conversion treatment to form a chemical conversion treatment film on the plating film.
- An inorganic compound film, an organic resin film, an inorganic compound-organic resin composite film or the like can be applied to the chemical conversion film.
- the inorganic compound include titanium, metal oxides mainly composed of vanadium, and metal phosphate compounds.
- ethylene, an epoxy, the resin of a urethane type etc. are mentioned as an organic resin.
- the chemical conversion treatment film may be formed by applying and drying a treatment liquid containing an inorganic compound, a treatment liquid containing an organic resin, or a treatment liquid in which an inorganic compound and an organic resin are mixed.
- Adhesion amount of chemical conversion film is preferably 0.1 g / m 2 or more 10 g / m 2 or less. If it is less than 0.1 g / m 2 , a sufficient corrosion resistance improvement effect may not be obtained. If it exceeds 10 g / m 2 , the effect of improving the corrosion resistance is saturated.
- the surface of the plating layer is not subjected to chromate treatment.
- a cold-rolled steel plate having a thickness of 1.6 mm was used as a base steel plate, and a hot-dip Zn—Al—Mg-based plated steel plate was manufactured under the conditions shown in Table 1 using a continuous hot dip galvanization facility (CGL).
- the plating adhesion amount was 100 g / m 2 per one side.
- the X-ray intensity ratio of MgZn 2 / Mg 2 Zn 11 was measured on the hot-dip Zn—Al—Mg-based plated steel sheet obtained as described above, and the surface appearance, corrosion resistance, and blackening resistance were evaluated. The detailed measurement method is shown below.
- X-ray diffraction peak intensity ratio MgZn 2 / Mg 2 Zn 11
- X-ray diffraction measurement conditions X-ray source: CuK ⁇ ray (tube voltage: 40 kV, tube current: 50 mA) Evaluation of surface appearance 10 samples of width 1000 mm ⁇ length 500 mm are collected every 100 m from the coil of length 1000 m of the galvanized Zn-Al-Mg-based plated steel sheet manufactured above, and black spots are present under the following conditions I made an observation. A: There are no black spots visually confirmed B: There are black spots visually confirmed (one or more) The case of A was regarded as pass, and the case of B as rejection.
- a test piece of 70 mm x 150 mm in size is cut out from the hot-dip Zn-Al-Mg-based plated steel sheet manufactured above, and the back and end of this test piece are sealed with a vinyl tape to obtain SST (salt spray test; It evaluated by the weight change (corrosion loss) before and behind the test of the steel plate after 1000 h implementation of JIS Z 2371). Evaluation criteria are as follows. A: Corrosion weight loss less than 20 g / m 2 B: Corrosion weight loss 20 g / m 2 or more but less than 40 g / m 2 C: Corrosion weight loss 40 g / m 2 or more A or B is regarded as pass, and C case is rejected .
- the evaluation criteria were as follows: A to D were judged to pass and E to be disqualified.
- the X-ray diffraction peak intensity ratio of the Mg-Zn compound constituting the plating film MgZn 2 / Mg 2 Zn 11 It is understood that a hot-dip Zn-Al-Mg-based plated steel sheet excellent in corrosion resistance and surface appearance without black spots is obtained.
- any of the manufacturing conditions is out of the scope of the present invention, and at least one of the surface appearance and the corrosion resistance is inferior.
- the hot-dip Zn-Al-Mg-based plated steel sheet of the present invention is excellent in surface appearance and can be applied to a wide range of fields such as automobiles, electrical machines, and building materials.
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Abstract
Description
[1] 鋼板表面に、1~22質量%のAl、0.1~10質量%のMgを含むめっき皮膜を有し、
前記めっき皮膜中のMg-Zn化合物相のX線回折ピーク強度比:MgZn2/Mg2Zn11が0.2以下である溶融Zn-Al-Mg系めっき鋼板。
[2] 前記めっき皮膜は、さらに、0.005~0.25質量%のNiを含む[1]に記載の溶融Zn-Al-Mg系めっき鋼板。
[3] 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の無機化合物系皮膜を有する[1]または[2]に記載の溶融Zn-Al-Mg系めっき鋼板。
[4] 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の有機樹脂系皮膜を有する[1]または[2]に記載の溶融Zn-Al-Mg系めっき鋼板。
[5] 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の無機化合物-有機樹脂複合皮膜を有する
[1]または[2]に記載の溶融Zn-Al-Mg系めっき鋼板。
[6] 下地鋼板を、1~22質量%のAl、0.1~10質量%のMgを含むめっき浴に浸漬して溶融Zn-Al-Mg系めっき処理を行い、
次いで、前記溶融Zn-Al-Mg系めっき処理後の鋼板を一次冷却停止温度:300℃未満まで冷却する一次冷却を行い、
次いで、加熱温度:280℃以上340℃以下まで加熱し
次いで、二次冷却する溶融Zn-Al-Mg系めっき鋼板の製造方法。
[7] 前記一次冷却停止温度を200℃以下とし、
前記加熱温度を300~340℃以下とする[6]に記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
[8] 一次冷却後の前記加熱および前記二次冷却の条件が、以下の式(1)を満足する[6]または[7]に記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
18≦1/2×(A-250)×t≦13500 (1)
ここで、A:一次冷却後の加熱温度(℃)
t:一次冷却後の加熱から二次冷却までの工程において、鋼板が250℃以上となる時間(秒)
[9] 前記めっき浴が、さらに、0.005~0.25質量%のNiを含む[6]~[8]のいずれかに記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
[10] さらに、前記二次冷却後、化成処理を行い、めっき皮膜の表面に無機化合物系皮膜、有機樹脂系皮膜、無機化合物-有機樹脂複合皮膜のいずれか1種を形成する[6]~[9]のいずれかに記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
本発明のめっき皮膜は、1~22質量%のAl、0.1~10質量%のMgを含むめっき皮膜である。
Alは耐食性向上を目的に添加される。めっき皮膜中のAl含有量が1%未満の場合、耐食性が十分に得られない。これに加えて、めっき/母材界面にZn-Fe合金相が成長し、加工性が著しく低下する。一方、Al含有量が22%を超えると耐食性向上効果が飽和する。したがって、Al含有量の範囲は1~22%とする。好ましくは4~15%である。
MgもAl同様、耐食性の向上を目的に添加される。めっき皮膜中のMg含有量が0.1%未満の場合は、耐食性が十分に得られない。一方、Mg含有量が10%を超えると耐食性向上効果が飽和する。また、Mg酸化物系のドロスが発生しやすくなる。したがって、Mg含有量の範囲は0.1~10%とする。また、めっき皮膜中のMg量が上記の上限値範囲内であっても5%を超えると、一次冷却後のめっき皮膜中にMgZn2が初晶として局所的に晶出する場合がある。初晶として晶出したMgZn2は比較的サイズが大きくなり易く、後述するMgZn2相主体からMg2Zn11相主体への固相変態のための加熱処理を長くする必要がある。したがって、5%以下とすることが好ましい。さらに、3%以下とすることがより好ましい。
Niを含む場合、0.005~0.25%を含有させることが好ましい。溶融Zn-Al-Mg系めっき鋼板を、高温多湿など厳しい腐食環境中に長時間保管すると、めっき表面が酸化されることで灰色~黒色に変色する「黒変」が生じる場合があるが、Niを含有させることで、耐黒変性を改善できる。Ni含有量が0.005%以上であれば、より優れた耐黒変性を得ることができる。0.25%を超えると、めっき浴中にドロスが発生し、ドロスの付着に起因する外観不良を招く場合がある。さらに本発明では、めっき中のMg-Zn化合物相を後述する加熱によりMgZn2主体からMg2Zn11主体の構造へと変化させるが、その際、耐黒変性が低下する場合がある。本発明では、めっき中にNiを添加することでめっき皮膜中のMg-Zn化合物の変化による耐黒変性の低下を抑制することが可能となる。
溶融Zn-Al-Mg系めっき鋼板のめっき皮膜は、おもにZn相、Al相、Mg-Zn化合物相から構成される。しかし、これまでに提案されてきた溶融Zn-Al-Mg系めっき鋼板のMg-Zn化合物相はMgZn2相が主体であった。
本発明の溶融Zn-Al-Mg系めっき鋼板は、一次冷却後の加熱、二次冷却をバッチ処理で行うこともできるが、連続式溶融亜鉛めっきライン(CGL)を用いて製造することが好ましい。
めっき浴には、1~22%のAl、0.1~10%のMgが含有される。本発明の1~22%のAl、0.1~10%のMgを含むめっき皮膜を有する溶融Zn-Al-Mg系めっき鋼板を得るために、めっき浴組成は上記とする。さらにNiを0.005~0.25%含有させることもできる。また、Siを0.01~0.5%を含有させることもできる。
なお、めっき浴中のAl含有量およびMg含有量と、めっき皮膜中のAl含有量およびMg含有量は、ほぼ同じとなる。したがって、所望のめっき皮膜の組成になるように、浴組成を調整する。また、めっき浴の残部はZnおよび不可避的不純物とする。
溶融Zn-Al-Mg系めっき処理後に、一次冷却停止温度:300℃未満まで冷却する。本発明では次工程である加熱処理において、後述するように、MgZn2相をMg2Zn11相に相変態させる。この相変態が起こるためには、加熱処理前にめっき皮膜が完全に凝固し、MgZn2相が晶出している必要がある。溶融Zn-Al-Mg系めっきの凝固点は、およそ340℃である。めっき処理後の一次冷却の冷却速度が大きい場合には過冷却状態となり、凝固点以下でもめっき皮膜が溶融状態になっている可能性がある。そのため、加熱処理前にめっき鋼板を凝固点よりも低い温度に冷却しておく必要がある。そのため、加熱処理前にめっき鋼板を冷却停止温度:300℃未満まで冷却し、めっき皮膜を完全に凝固させることが必要である。以上より、一次冷却停止温度は、300℃未満とする。好ましくは250℃以下、より好ましくは200℃以下とする。一次冷却の冷却速度は特に限定しない。生産性の観点から10℃/s以上であることが好ましい。一次冷却の冷却速度が大きすぎる場合、めっき皮膜が過冷却状態となり、凝固点(約340℃)以下でもめっき皮膜が溶融状態になっている可能性がある。また、製造設備の性能などを考慮すると負荷がかかる場合がある。これらの点から、冷却速度は150℃/s以下が好ましい。
一次冷却後に、加熱温度:280℃以上340℃以下まで加熱する。
加熱終了後、めっき鋼板を冷却する二次冷却を行う。二次冷却停止温度には特に制限はなく、たとえば室温としてもよい。二次冷却速度は特に制限されないが、生産性の観点から、10℃/s以上が好ましい。製造設備の性能などを考慮すると、150℃/s以下が好ましい。
18≦1/2×(A-250)×t≦13500 (1)
ここで、A:一次冷却後の加熱温度(℃)
t:一次冷却後の加熱から二次冷却までの工程において、鋼板が250℃以上となる時間(秒)
所望のX線回折ピーク強度比:MgZn2/Mg2Zn11が0.2以下を安定して得るためには、1/2×(A-250)×tを18以上とすることが好ましい。より好ましくは、1/2×(A-250)×tは100以上とする。一方、1/2×(A-250)×tは13500以下が好ましい。1/2×(A-250)×tが13500を超えると、過度の加熱処理によってMg2Zn11が粒成長して粗大化するため耐黒変性が劣化する。よって、1/2×(A-250)×tは13500以下が好ましい。より好ましくは、8000以下である。
板厚1.6mmの冷延鋼板を下地鋼板とし、連続溶融亜鉛めっき設備(CGL)を用いて表1に示す条件で溶融Zn-Al-Mg系めっき鋼板を製造した。めっき付着量は片面あたり100g/m2とした。
上記で製造した溶融Zn-Al-Mg系めっき鋼板のめっき皮膜を、以下の条件でX線回折(対称反射法)で測定し、MgZn2のピーク(2θ=19.6°付近)強度をMg2Zn11のピーク(2θ=14.6°付近)強度で除した値をX線回折ピーク強度比:MgZn2/Mg2Zn11として算出した。
[X線回折測定条件]
X線源:CuKα線(管電圧:40kV、管電流:50mA)
表面外観の評価
上記で製造した溶融Zn-Al-Mg系めっき鋼板の長さ1000mのコイルから100m毎に幅1000mm×長さ500mmのサンプルを10枚採取し、以下の条件で黒色斑点の有無の観察を行った。
A:目視で確認される黒色斑点が無し
B:目視で確認される黒色斑点が有り(1個以上)
Aの場合を合格とし、Bの場合を不合格とした。
上記で製造した溶融Zn-Al-Mg系めっき鋼板から70mm×150mmのサイズの試験片を切り出し、この試験片の裏面と端部をビニールテープでシールして、SST(salt spray test;JIS Z 2371に準拠)を1000h実施した後の、鋼板の試験前後の重量変化(腐食減量)で評価した。評価基準は以下の通りである。
A:腐食減量 20g/m2未満
B:腐食減量 20g/m2以上40g/m2未満
C:腐食減量 40g/m2以上
AまたはBである場合を合格とし、Cの場合を不合格とした。
上記で製造した溶融Zn-Al-Mg系めっき鋼板から試験片(50mm×50mm)を採取し、温度40℃、湿度80%の環境に10日間晒し、分光光度計を用いて試験前後のL値(明度)を測定した。L値は、日本電色工業(株)製のSQ2000を使用し、SCIモード(正反射光含む)で測定を行い、ΔL=(試験前の鋼板のL値)-(試験後の鋼板のL値)を求めた。評価基準は下記5段階とし、A~Dを合格、Eを不合格と判断した。
A:ΔL=0以上、3未満
B:ΔL=3以上、6未満
C:ΔL=6以上、9未満
D:ΔL=9以上、12未満
E:ΔL=12以上
以上により得られた結果を製造条件と併せて、表1に示す。
Claims (10)
- 鋼板表面に、1~22質量%のAl、0.1~10質量%のMgを含むめっき皮膜を有し、
前記めっき皮膜中のMg-Zn化合物相のX線回折ピーク強度比:MgZn2/Mg2Zn11が0.2以下である溶融Zn-Al-Mg系めっき鋼板。 - 前記めっき皮膜は、さらに、0.005~0.25質量%のNiを含む請求項1に記載の溶融Zn-Al-Mg系めっき鋼板。
- 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の無機化合物系皮膜を有する
請求項1または2に記載の溶融Zn-Al-Mg系めっき鋼板。 - 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の有機樹脂系皮膜を有する
請求項1または2に記載の溶融Zn-Al-Mg系めっき鋼板。 - 前記めっき皮膜の上に、さらに、片面あたりの付着量が0.1~10g/m2の無機化合物-有機樹脂複合皮膜を有する
請求項1または2に記載の溶融Zn-Al-Mg系めっき鋼板。 - 下地鋼板を、1~22質量%のAl、0.1~10質量%のMgを含むめっき浴に浸漬して溶融Zn-Al-Mg系めっき処理を行い、
次いで、前記溶融Zn-Al-Mg系めっき処理後の鋼板を一次冷却停止温度:300℃未満まで冷却する一次冷却を行い、
次いで、加熱温度:280℃以上340℃以下まで加熱し
次いで、二次冷却する溶融Zn-Al-Mg系めっき鋼板の製造方法。 - 前記一次冷却停止温度を200℃以下とし、
前記加熱温度を300~340℃以下とする請求項6に記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。 - 一次冷却後の前記加熱および前記二次冷却の条件が、以下の式(1)を満足する請求項6または7に記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
18≦1/2×(A-250)×t≦13500 (1)
ここで、A:一次冷却後の加熱温度(℃)
t:一次冷却後の加熱から二次冷却までの工程において、鋼板が250℃以上となる時間(秒) - 前記めっき浴が、さらに、0.005~0.25質量%のNiを含む請求項6~8のいずれかに記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
- さらに、前記二次冷却後、化成処理を行い、めっき皮膜の表面に無機化合物系皮膜、有機樹脂系皮膜、無機化合物-有機樹脂複合皮膜のいずれか1種を形成する
請求項6~9のいずれかに記載の溶融Zn-Al-Mg系めっき鋼板の製造方法。
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JP2020186457A (ja) * | 2019-05-16 | 2020-11-19 | Jfe鋼板株式会社 | 表面処理鋼板の製造方法 |
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JP7266459B2 (ja) | 2019-05-16 | 2023-04-28 | Jfe鋼板株式会社 | 表面処理鋼板の製造方法 |
JP7120166B2 (ja) | 2019-06-21 | 2022-08-17 | Jfeスチール株式会社 | 溶融Al-Zn系めっき鋼板の製造方法 |
JP2021001374A (ja) * | 2019-06-21 | 2021-01-07 | Jfeスチール株式会社 | 溶融Al−Zn系めっき鋼板の製造方法 |
JP2023507959A (ja) * | 2019-12-18 | 2023-02-28 | ポスコホールディングス インコーポレーティッド | 耐腐食性に優れた溶融合金めっき鋼材及びその製造方法 |
CN111074187A (zh) * | 2019-12-19 | 2020-04-28 | 河钢股份有限公司 | 包括锌铝镁镀层的钢板及其制造方法 |
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JP7040695B1 (ja) * | 2020-11-18 | 2022-03-23 | 日本製鉄株式会社 | めっき鋼材 |
US11851764B2 (en) | 2020-11-18 | 2023-12-26 | Nippon Steel Corporation | Plated steel material |
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WO2023037396A1 (ja) * | 2021-09-07 | 2023-03-16 | 日本製鉄株式会社 | 溶融めっき鋼材 |
US11814732B2 (en) | 2021-09-07 | 2023-11-14 | Nippon Steel Corporation | Hot-dip plated steel |
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AU2018297757B2 (en) | 2021-02-25 |
CN110832105A (zh) | 2020-02-21 |
JP6756370B2 (ja) | 2020-09-16 |
AU2018297757A1 (en) | 2019-12-05 |
MY192929A (en) | 2022-09-15 |
JPWO2019009003A1 (ja) | 2019-07-04 |
CN110832105B (zh) | 2021-11-02 |
US11618938B2 (en) | 2023-04-04 |
TWI697584B (zh) | 2020-07-01 |
TW201907025A (zh) | 2019-02-16 |
US20210147971A1 (en) | 2021-05-20 |
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