WO2017163299A1 - 化成処理鋼板及び化成処理鋼板の製造方法 - Google Patents

化成処理鋼板及び化成処理鋼板の製造方法 Download PDF

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WO2017163299A1
WO2017163299A1 PCT/JP2016/058905 JP2016058905W WO2017163299A1 WO 2017163299 A1 WO2017163299 A1 WO 2017163299A1 JP 2016058905 W JP2016058905 W JP 2016058905W WO 2017163299 A1 WO2017163299 A1 WO 2017163299A1
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chemical conversion
layer
steel plate
metal
amount
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PCT/JP2016/058905
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English (en)
French (fr)
Japanese (ja)
Inventor
賢明 谷
平野　茂
光 立木
偉男 柳原
誠 河端
横矢　博一
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新日鐵住金株式会社
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Priority to PCT/JP2016/058905 priority Critical patent/WO2017163299A1/ja
Priority to EP16895337.0A priority patent/EP3434811A4/en
Priority to JP2018506647A priority patent/JP6583539B2/ja
Priority to US16/086,152 priority patent/US20200123661A1/en
Priority to KR1020187026675A priority patent/KR20180113583A/ko
Priority to CN201680083793.5A priority patent/CN108779561A/zh
Publication of WO2017163299A1 publication Critical patent/WO2017163299A1/ja

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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
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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
    • C23C2/04—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
    • C23C2/08—Tin 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
    • 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
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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
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    • 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
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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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    • 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
    • C23C22/34—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 fluorides or complex fluorides
    • C23C22/36—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 fluorides or complex fluorides containing also phosphates
    • C23C22/361—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 fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds
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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
    • 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
    • C23C28/021—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 including at least one metal alloy 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
    • C23C28/32—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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/36—Phosphatising
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/30—Electroplating: Baths therefor from solutions of tin
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C25D9/10—Electrolytic coating other than with metals with inorganic materials by cathodic processes on iron or steel
    • 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
    • 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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/20—Orthophosphates containing aluminium cations

Definitions

  • the present invention relates to a chemical conversion treated steel sheet and a method for producing a chemical conversion treated steel sheet.
  • ⁇ Corrosion may occur due to continuous use of metal.
  • various techniques have been proposed to prevent corrosion generated in metal. Proposed techniques include a technique for plating a metal plate and a technique for performing various surface treatments on the surface of the metal plate or plating.
  • Patent Document 1 At least one of a vanadium compound, phosphoric acid and a phosphoric acid compound, or at least one of an epoxy group and an amino group is formed on the surface of an Al—Zn alloy-plated steel sheet used for building materials and home appliances.
  • a technique for forming an organic resin film containing as a main component an organic resin composed of at least one of a silane compound and a water-soluble organic resin and a water-dispersible organic resin is disclosed.
  • Ni-plated steel sheets, Sn-plated steel sheets, Sn-based alloy-plated steel sheets, and the like are used for manufacturing metal containers for the purpose of preserving beverages and foods.
  • the Al—Zn alloy-plated steel sheet disclosed in the following Patent Document 1 is a so-called sacrificial anti-corrosion plated steel sheet, whereas the Ni-plated steel sheet, Sn-plated steel sheet or Sn-based alloy plated steel sheet is a so-called barrier type. This is a plated steel sheet.
  • container steel sheets Sn-plated steel sheets or Sn-based alloy-plated steel sheets as steel sheets for metal containers (hereinafter referred to as container steel sheets) for the purpose of preserving beverages and foods, the adhesion between the steel sheet and the coating or film And in order to ensure corrosion resistance, the surface of a plated steel plate is often subjected to chemical conversion treatment with hexavalent chromium. Chemical conversion treatment using a solution containing hexavalent chromium is called chromate treatment.
  • Patent Document 2 discloses a steel plate for containers having a chemical conversion coating containing Zr, phosphoric acid, a phenol resin, and the like.
  • meat, vegetables, etc. are contained as a foodstuff preserve
  • Meat and vegetables contain various proteins, but these proteins may contain amino acids containing S (sulfur-containing amino acids represented by L-cysteine, L-methionine, L-(-)-cystine). .
  • S sulfur-containing amino acids represented by L-cysteine, L-methionine, L-(-)-cystine.
  • Patent Document 3 includes at least one reaction promoting component selected from the group consisting of Al ions, borate ions, Cu ions, Ca ions, metal Al, and metal Cu, Zr ions, and F ions.
  • a method for producing a steel plate for containers is disclosed in which a steel plate is immersed or electrolytically treated in a solution to form a Zr-containing film on the surface of the steel plate.
  • the film formed by the chromate treatment (hereinafter referred to as the chromate film) is dense even if the amount of coating is small, so the steel plate for containers with a chromate film formed on the surface has excellent corrosion resistance and resistance to sulfur blackening. Have. However, as described above, since hexavalent chromium is harmful to the environment, it is preferable that the steel plate for containers does not contain hexavalent chromium as much as possible. On the other hand, since the organic resin film described in Patent Document 1 and the chemical conversion film described in Patent Document 2 do not contain hexavalent chromium, they are environmentally suitable.
  • the present invention has been made in view of the above circumstances, and even when the amount of the chemical conversion coating layer is small, the chemical conversion processed steel sheet and the chemical conversion processed steel sheet have excellent corrosion resistance and sulfur blackening resistance.
  • An object is to provide a manufacturing method.
  • the present invention adopts the following means in order to solve the above problems and achieve the object.
  • a chemical conversion treated steel sheet is formed on a steel sheet, an Fe—Sn alloy layer formed on at least one surface of the steel sheet, and the Fe—Sn alloy layer.
  • a chemical conversion coating layer comprising: 2 Zr compound; a phosphoric acid compound having a P content of 1.0 to 100 mg / m 2 ; and an Al compound having a metal Al content of 0.10 to 30.0 mg / m 2 ; .
  • the chemical conversion coated film layer may contain 0.10 to 30.0 mg / m 2 of Al 2 O 3 in terms of metal Al content.
  • the chemical conversion coating layer has a metal Zr content of 1.0 to 120 mg / m 2 of the Zr compound and a P content of 2.0. It said phosphoric acid compound of ⁇ 70.0 mg / m 2, and the Al compound in 0.20 ⁇ 20.0mg / m 2 of metal Al content may contain.
  • the total Sn content of the Fe—Sn alloy layer and the Sn layer is 0 in terms of metal Sn amount. It may be 30 to 20.0 g / m 2 .
  • the surface of the chemical conversion treated film layer may not be coated with a film or paint.
  • plating is performed by forming a Sn plating layer containing Sn in an amount of 0.10 to 30.0 g / m 2 on the surface of the steel sheet.
  • the chemical conversion treatment solution includes a total of 200 to 17000 ppm of Zr ions, 200 to 17000 ppm of F ions, and 100 to 2000 ppm of phosphate ions. May contain 1000 to 23000 ppm of nitrate ions and sulfate ions, and 500 to 3000 ppm of Al ions.
  • 1 is a schematic view showing a chemical conversion treated steel sheet in which a Fe—Sn alloy layer, a Sn layer and a chemical conversion film layer are formed on one surface of a steel sheet.
  • 1 is a schematic view showing a chemical conversion treated steel sheet in which a Fe—Sn alloy layer, a Sn layer and a chemical conversion film layer are formed on both surfaces of a steel sheet. It is the flowchart which showed an example of the flow of the manufacturing method of a chemical conversion treatment steel plate.
  • 3 is a graph showing the results of Example 1.
  • FIGS. 1A and 1B are explanatory views schematically showing a layer structure of a chemical conversion treated steel sheet according to the present embodiment.
  • the chemical conversion treated steel sheet 10 includes a steel sheet 103, a Fe—Sn alloy layer 105a, a Sn layer 105b, and a chemical conversion film layer 107 as shown in FIGS. 1A and 1B.
  • the steel plate 103 is used as a base material of the chemical conversion treated steel plate 10 according to the present embodiment. It does not specifically limit about the steel plate 103 used by this embodiment, It is possible to use the well-known steel plate 103 used as a steel plate for containers.
  • the manufacturing method and material of the steel plate 103 are not particularly limited, and the steel plate 103 is manufactured from a normal steel slab manufacturing process through known processes such as hot rolling, pickling, cold rolling, annealing, and temper rolling. Can be used.
  • the thickness of the steel plate 103 is preferably 0.05 to 1 mm in view of practicality and economy when used as a steel plate for containers.
  • Fe-Sn alloy layer 105a and Sn layer 105b On the surface of the steel plate 103, an Fe—Sn alloy layer 105a and an Sn layer 105b containing Sn are formed.
  • the Fe—Sn alloy layer 105a and the Sn layer 105b are barrier-type plating layers.
  • the barrier-type plating layer is formed by forming Sn metal film on the surface of the steel plate 103 using Sn that is electrochemically noble than Fe constituting the base material steel plate 103. It is a plating layer that prevents corrosion of the steel sheet 103 by preventing the corrosion factor from acting on the base material.
  • the sacrificial anticorrosion type plating layer has a function opposite to that of the barrier type plating layer.
  • a metal film is formed on the surface of the steel plate 103 using a metal that is electrochemically lower than Fe constituting the steel plate 103 as a base material (for example, Zn as in Patent Document 1).
  • the corrosion of the steel sheet 103 is suppressed by forming the plated steel layer and the metal such as Zn corroded earlier than the Fe forming the steel sheet 103.
  • the barrier type plating layer and the sacrificial anticorrosion type plating layer have different interactions with the chemical conversion coating layer 107.
  • the Fe—Sn alloy layer 105a and the Sn layer 105b according to the present embodiment will be specifically described with reference to FIGS. 1A and 1B.
  • the Fe—Sn alloy layer 105a, the Sn layer 105b, and the chemical conversion coating layer 107 may be formed on one surface of the steel plate 103, or as shown in FIG. Further, the Fe—Sn alloy layer 105a, the Sn layer 105b, and the chemical conversion treatment film layer 107 may be formed.
  • the Fe—Sn alloy layer 105a is formed on the surface of the steel plate 103, and the Sn layer 105b is formed on the Fe—Sn alloy layer 105a.
  • the Fe—Sn alloy layer 105 a and the Sn layer 105 b are formed by forming a Sn plating layer (not shown) on the surface of the steel plate 103 and then performing a molten tin treatment (reflow treatment). .
  • the Sn plating layer (not shown) is formed in order to ensure the corrosion resistance and weldability of the chemical conversion treated steel sheet 10.
  • Sn—Fe—Sn alloy contained in the Fe—Sn alloy layer 105a also has excellent corrosion resistance and weldability.
  • the Fe—Sn alloy layer 105a and the Sn layer 105b according to the present embodiment both contain Sn, but the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b is 0. 0 per metal surface. 10 to 30.0 g / m 2 .
  • Sn has excellent workability, weldability, and corrosion resistance. By performing molten tin treatment after Sn plating, the corrosion resistance of the chemical conversion steel sheet 10 is further improved, and the surface appearance (mirror appearance) of the chemical conversion steel sheet 10 is improved. ) Can be made more preferable.
  • the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b needs to be 0.10 g / m 2 or more per side in terms of the amount of metal Sn. Further, the workability, weldability, and corrosion resistance of the chemical conversion treated steel sheet 10 improve as the Sn content increases, but the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b is one side with the amount of metal Sn. Exceeding 30.0 g / m 2 per saturates the effect described above with Sn.
  • the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b exceeds 30 g / m 2 per side in terms of the amount of metal Sn.
  • the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b is 30.0 g / m 2 or less per side in terms of the amount of metal Sn.
  • Sn total content of Fe-Sn alloy layer 105a and the Sn layer 105b is more preferably a per side 0.30g / m 2 ⁇ 20.0g / m 2 of metal Sn amount. Since the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b is 0.30 g / m 2 or more per one surface in terms of metal Sn, the above-described effects of Sn can be more reliably exhibited. It is. In addition, since the total Sn content of the Fe—Sn alloy layer 105a and the Sn layer 105b is 20.0 g / m 2 or less per side in terms of the metal Sn amount, the manufacturing cost can be further reduced.
  • the Fe—Sn alloy layer 105a contains 0.0010 to 100 g / m 2 of Fe in terms of the amount of metallic Fe. In addition to Sn and Fe, the Fe—Sn alloy layer 105a may contain inevitable impurities that are mixed in in trace elements or manufacturing processes. In the Fe—Sn alloy layer 105a, the total amount of Fe metal Fe and Sn metal Sn contained is 50 mass% or more. Preferably, in the Fe—Sn alloy layer 105a, the total amount of Fe metal Fe and Sn metal Sn contained is 70% by mass or more.
  • the Sn layer 105b may be composed only of Sn, and may contain 0.0010 to 6.0 g / m 2 of Fe in terms of metal Fe in addition to Sn. In addition, the Sn layer 105b may contain inevitable impurities that are mixed in in trace elements or manufacturing processes.
  • the proportion of Sn in the Sn layer 105b is 50% by mass or more in terms of the amount of metal Sn. Preferably, the proportion of Sn in the Sn layer 105b is 70% by mass or more in terms of the amount of metallic Sn.
  • the ratio of the thicknesses of the Fe—Sn alloy layer 105a and the Sn layer 105b is not particularly limited as long as the amount of metal Sn is ensured.
  • Fe—Sn alloy layer 105a and the Sn layer 105b are not densely formed, a part of the steel plate 103 as a base material is exposed.
  • Fe contained in the steel plate 103 and S contained in the beverage or food may be combined to form black FeS, Fe 2 S 3 , or Fe 2 S.
  • a chromate film has been mainly applied to the surfaces of the Fe—Sn alloy layer 105 a and the Sn layer 105 b so far. Was formed.
  • the chemical conversion treated steel sheet 10 has a Zr compound, a phosphoric acid compound, and an Al layer as an alternative to the conventional chromate film on the Fe-Sn alloy layer 105a and the Sn layer 105b.
  • a chemical conversion film layer 107 containing a compound is formed.
  • the chemical conversion film layer 107 is formed on the Sn layer 105b.
  • the chemical conversion coating layer 107 is a composite coating layer mainly composed of a Zr compound.
  • the amount of metal Zr is 1.0 to 150 mg / m 2 per side and the amount of P is 1.0 to 100 mg / m per side. 2 phosphoric acid compound and 0.10-30.0 mg / m 2 of Al compound per side in terms of metal Al content.
  • the composite coating layer refers to a coating layer in which the Zr compound, the phosphate compound and the Al compound are not completely mixed but are partially mixed.
  • the Zr compound contained in the chemical conversion coating layer 107 according to the present embodiment has a function of improving corrosion resistance, adhesion, and processing adhesion.
  • Examples of the Zr compound according to this embodiment include oxidized Zr, phosphoric acid Zr, hydroxylated Zr, and fluorided Zr.
  • the chemical conversion film layer 107 contains a plurality of the above-described Zr compounds.
  • a preferred combination of Zr compounds is Zr oxide, Zr phosphate and Zr fluoride.
  • the content of the Zr compound contained in the chemical conversion coating layer 107 is 1.0 mg / m 2 or more per side in terms of metal Zr, practically suitable corrosion resistance, adhesion and work adhesion are ensured.
  • the corrosion resistance, adhesion, and processing adhesion are improved.
  • the content of the Zr compound exceeds 150 mg / m 2 per side in terms of the amount of metal Zr, the chemical conversion coating layer 107 becomes too thick, mainly due to cohesive failure, and the Sn layer of the chemical conversion coating layer 107 While the adhesiveness with respect to 105b falls, an electrical resistance rises and weldability falls.
  • the content of Zr compound of the chemical conversion coating layer 107 is a per side 1.0mg / m 2 ⁇ 150mg / m 2 by metal Zr content.
  • the content of the Zr compound is more preferably 1.0 to 120 mg / m 2 per side in terms of the amount of metal Zr.
  • the chemical conversion treatment film layer 107 further includes one or more phosphate compounds in addition to the Zr compound described above.
  • the phosphoric acid compound according to this embodiment has a function of improving corrosion resistance, adhesion, and processing adhesion.
  • Examples of the phosphoric acid compound according to the present embodiment include phosphoric acid formed by a reaction between a phosphoric acid ion and a compound contained in the steel plate 103, the Fe—Sn alloy layer 105a, the Sn layer 105b, and the chemical conversion coating layer 107. Fe, phosphoric acid Ni, phosphoric acid Sn, phosphoric acid Zr, phosphoric acid Al, etc. are mentioned.
  • the chemical conversion film layer 107 may contain one or more of the above phosphoric acid compounds.
  • the corrosion resistance, adhesion and work adhesion of the chemical conversion treatment steel sheet 10 are improved. Specifically, when the content of the phosphoric acid compound in the chemical conversion coating layer 107 is 1.0 mg / m 2 or more in terms of the amount of P, practically suitable corrosion resistance, adhesion and work adhesion are ensured. Is done. On the other hand, as the content of the phosphoric acid compound increases, the corrosion resistance, adhesion and processing adhesion also improve.
  • the content of the phosphoric acid compound exceeds 100 mg / m 2 per side in terms of P amount, The treatment film layer 107 becomes too thick, mainly due to cohesive failure, and the adhesion of the chemical conversion treatment film layer 107 to the Sn layer 105b is lowered, and the electrical resistance is increased and the weldability is lowered.
  • the content of the phosphoric acid compound exceeds 100 mg / m 2 per side in terms of the P amount, the appearance may be non-uniform due to non-uniform adhesion of the chemical conversion coating layer 107. .
  • the content of the phosphoric acid compound in the chemical conversion coating layer 107 is 1.0 to 100 mg / m 2 per side in terms of the P amount.
  • the content of the phosphate compound in the chemical conversion coating layer 107 is more preferably 2.0 to 70.0 mg / m 2 per side in terms of P amount.
  • the chemical conversion film layer 107 further includes an Al compound in addition to the Zr compound and the phosphate compound described above.
  • the Al compound in the chemical conversion coating layer 107 exists mainly as an Al oxide in the chemical conversion coating layer 107. Since the Al oxide reinforces the film defect of the chemical conversion coating layer 107 containing Zr as a main component, the chemical conversion steel plate 10 can obtain excellent resistance to sulfur blackening. Since the chemical conversion treatment film layer 107 containing Zr as a main component is originally a very uniform film, the amount of Al compound added to the chemical conversion treatment film layer 107 to reinforce the film defects is the amount of metal Al per side. it may be at 0.10 mg / m 2 or more.
  • the content of the Al compound is 0.10 mg / m 2 or more per side in terms of the amount of metal Al, it is possible to suitably improve the sulfurization blackening resistance of the chemical conversion treated steel sheet 10.
  • the Al compound content of the chemical conversion coating layer 107 increases, the resistance to sulfur blackening also improves, but the Al compound content exceeds 30.0 mg / m 2 per side in terms of the amount of metal Al. As a result, the resistance to sulfur blackening is saturated and economically undesirable. Therefore, the content of the Al compound contained in the chemical conversion coating layer 107 is 30.0 mg / m 2 or less per side in terms of the amount of metal Al.
  • the content of the Al compound in the chemical conversion coating layer 107 is more preferably 0.20 to 20.0 mg / m 2 per side in terms of the amount of metallic Al.
  • the content of the Al compound in the chemical conversion coating layer 107 is more preferably 0.20 to 20.0 mg / m 2 per side in terms of the amount of metallic Al.
  • the content of Al oxide (Al 2 O 3 ) in the chemical conversion coating layer 107 is preferably 0.10 to 30.0 mg / m 2 in terms of metal Al.
  • the coating defects of the chemical conversion coating layer 107 can be suitably reinforced and excellent sulfurization resistance can be obtained.
  • the content of the phosphoric acid compound that improves the sulfur blackening resistance can be reduced in the same manner as Al.
  • the phosphoric acid compound contained in the chemical conversion treatment film layer 107 a large amount of phosphoric acid Zr produced by reaction of phosphate ions with Zr ions is contained in the chemical conversion treatment solution for forming the chemical conversion treatment coating layer 107. In the presence of water, it precipitates and the chemical conversion solution becomes cloudy.
  • the Al compound contributes to improvement of resistance to sulfur blackening as compared with the phosphoric acid compound.
  • the chemical conversion treatment film layer 107 contains an Al compound
  • the content of the phosphoric acid compound that causes white turbidity of the chemical conversion treatment liquid can be reduced while suitably improving the resistance to sulfur blackening.
  • the amount of F ions that inhibit the binding between Zr and phosphoric acid and the binding between Al and phosphoric acid can be reduced.
  • Zr can be deposited more easily, so that the electrolytic efficiency for forming the chemical conversion treatment film layer 107 can be improved.
  • the chemical conversion treatment film layer 107 may contain inevitable impurities that are mixed in during the manufacturing process. Moreover, when the chemical conversion treatment film layer 107 contains Cr, the upper limit of the Cr content is 2 mg / m 2 .
  • the chemical conversion treated steel sheet 10 according to the present embodiment exhibits excellent resistance to sulfur blackening even when the adhesion amount of the chemical conversion film 107 is reduced.
  • a coating material is made to adhere to the surface of the chemical conversion treatment steel plate 10, and is baked, and a coating film is formed.
  • a chemical conversion treated steel sheet 10 with a coating film formed on the surface is placed and fixed as a lid on the mouth of a heat-resistant bottle holding a 0.6 mass% L-cysteine liquid boiled for 1 hour, using a soaking furnace or the like. Heat treatment at 110 ° C. for 30 minutes.
  • the chemical conversion treated steel sheet 10 according to this embodiment has excellent corrosion resistance and sulfide blackening resistance. Therefore, even when the surface of the chemical conversion treatment film layer 107 is not covered with a film or paint, the chemical conversion treatment steel plate 10 can be used as a steel plate for containers.
  • the chemical conversion steel sheet 10 has the Fe—Sn alloy layer 105a, the Sn layer 105b, and the chemical conversion film layer 107 on the steel sheet 103. That is, in the chemical conversion treated steel sheet 10, the steel sheet 103 and the Fe—Sn alloy layer 105a are in contact with each other, and no other layer is provided between the steel sheet 103 and the Fe—Sn alloy layer 105a. Similarly, the Fe—Sn alloy layer 105a and the Sn layer 105b are in contact with each other, and no other layer is provided between the Fe—Sn alloy layer 105a and the Sn layer 105b. Further, the Sn layer 105 b and the chemical conversion treatment film layer 107 are in contact with each other, and no other layer is provided between the Sn layer 105 b and the chemical conversion treatment film layer 107.
  • the amount of metallic Sn and the amount of metallic Fe in the Fe—Sn alloy layer 105a and the Sn layer 105b can be measured by, for example, a fluorescent X-ray method.
  • a calibration curve relating to the amount of metal Sn or metal Fe is created in advance, and the amount of metal Sn or metal Fe is relatively determined using the created calibration curve. Identify.
  • the amount of metal Zr, the amount of P, and the amount of metal Al in the chemical conversion coating layer 107 can be measured by a quantitative analysis method such as fluorescent X-ray analysis, for example. Further, what kind of compound is present in the chemical conversion coating layer 107 can be specified by performing an analysis by X-ray photoelectron spectroscopy (XPS). . In addition, the content of Al 2 O 3 in the chemical conversion coating layer 107 is determined based on the peak intensity ratio of Al 2 O 3 , metal Al, and other Al compounds by X-ray photoelectron spectroscopy (XPS). Ask for. Then, the content of Al 2 O 3 in the chemical conversion coating layer 107 is calculated from the total metal Al amount obtained by the quantitative analysis method such as fluorescent X-ray analysis and the peak intensity ratio obtained by XPS as described above. calculate.
  • XPS X-ray photoelectron spectroscopy
  • the measuring method of each component is not limited to said method, It is possible to apply a well-known measuring method.
  • FIG. 2 is a flowchart for explaining an example of the flow of the manufacturing method of the chemical conversion treated steel sheet 10 according to the present embodiment.
  • Pretreatment process In the method for manufacturing the chemical conversion treated steel sheet 10 according to the present embodiment, first, a known pretreatment is performed on the steel sheet 103 as necessary (step S101).
  • an Sn plating layer (not shown) is formed on the surface of the steel plate 103 (step S103).
  • the formation method of Sn plating layer (not shown) is not specifically limited, The well-known electroplating method, the method of immersing the steel plate 103 in molten Sn, etc. can be used.
  • a molten tin treatment (reflow treatment process) is performed (step S104).
  • the Fe—Sn alloy layer 105 a and the Sn layer 105 b are formed on the surface of the steel plate 103.
  • the molten tin treatment is performed by forming an Sn plating layer (not shown) on the steel sheet 103, heating to 200 ° C. or higher, once melting the Sn plating layer (not shown), and then rapidly cooling.
  • Sn in the Sn plating layer (not shown) located on the steel plate 103 side is alloyed with Fe in the steel plate 103 to form the Fe—Sn alloy layer 105a, and the remaining Sn is Sn layer. 105b is formed.
  • the chemical conversion treatment film layer 107 is formed by cathodic electrolysis (step S105).
  • the chemical conversion treatment film layer 107 is formed by electrolytic treatment (for example, cathodic electrolytic treatment).
  • the chemical conversion treatment solution used to form the chemical conversion coating layer 107 by electrolytic treatment is 10 ppm or more and 20000 ppm or less of Zr ions, 10 ppm or more and 20000 ppm or less of F ions, and 10 ppm or more and 3000 ppm or less of phosphate ions. This includes nitrate ions and sulfate ions of 30000 ppm or less and Al ions of 500 ppm or more and 5000 ppm or less.
  • (NH 4 ) 3 AlF 6 is used as a supply source of Al ions.
  • the nitrate ion and the sulfate ion only need to be contained in the chemical conversion treatment liquid in a total of 10 ppm to 3000 ppm, and both the nitrate ion and the sulfate ion may be contained in the chemical conversion treatment liquid. Only one of nitrate ion and sulfate ion may be contained in the chemical conversion treatment liquid.
  • the chemical conversion treatment liquid is preferably 200 ppm or more and 17000 ppm or less of Zr ions, 200 ppm or more and 17000 ppm or less of F ions, 100 ppm or more and 2000 ppm or less of phosphate ions, and a total of 1000 ppm or more and 23000 ppm or less of nitrate ions and sulfate ions, It is preferable to contain 500 ppm or more and 3000 or less Al ions.
  • concentration of Zr ions By setting the concentration of Zr ions to 200 ppm or more, it is possible to more reliably prevent a decrease in the amount of Zr adhesion.
  • the cloudiness of the chemical conversion treatment film layer 107 accompanying precipitation of phosphate can be more reliably prevented by setting the concentration of F ions to 200 ppm or more.
  • the concentration of phosphate ions to 100 ppm or more, it is possible to more reliably prevent the clouding of the chemical conversion treatment film layer 107 accompanying the precipitation of phosphate. Moreover, the fall of the adhesion efficiency of the chemical conversion treatment film layer 107 can be prevented more reliably by setting the concentration of at least one of nitrate ions and sulfate ions to 1000 ppm or more. In addition, when the Al ion concentration is 500 ppm or more, the effect of improving sulfurization resistance can be more reliably realized. In addition, the manufacturing cost of the chemical conversion treatment film layer 107 can be reduced more reliably by setting the upper limit value of each component of the chemical conversion treatment liquid to the above values.
  • the temperature of a chemical conversion liquid is 5 degreeC or more and less than 90 degreeC.
  • the temperature of the chemical conversion treatment liquid is less than 5 ° C.
  • the formation efficiency of the chemical conversion treatment film layer 107 is poor and not economical, which is not preferable.
  • the temperature of the chemical conversion treatment liquid is 90 ° C. or higher, the structure of the chemical conversion treatment film layer 107 to be formed is non-uniform, and defects such as cracks and microcracks are generated. Since it is the starting point, it is not preferable.
  • the temperature of the chemical conversion treatment liquid is preferably higher than the surface temperature of the steel sheet 103 on which the Fe—Sn alloy layer 105a and the Sn layer 105b are formed.
  • the current density during the electrolytic treatment is preferably 1.0 A / dm 2 or more and 100 A / dm 2 or less.
  • the current density is less than 1.0 A / dm 2
  • the current density exceeds 100 A / dm 2
  • the amount of the chemical conversion treatment film layer 107 is excessive, and the chemical conversion treatment film layer 107 having insufficient adhesion among the formed chemical conversion treatment film layers 107.
  • the time for the electrolytic treatment is preferably 0.20 seconds or more and 150 seconds or less.
  • the electrolytic treatment time is less than 0.20 seconds, the amount of adhesion of the chemical conversion treatment film layer 107 decreases, and the desired performance cannot be obtained, which is not preferable.
  • the electrolytic treatment time exceeds 150 seconds, the amount of the chemical conversion treatment film layer 107 is excessive, and among the formed chemical conversion treatment film layers 107, the chemical conversion treatment film layer 107 with insufficient adhesion is formed. Since it may be washed away (peeled off) in a washing step such as washing with water after the electrolytic treatment, it is not preferable.
  • the pH of the chemical conversion solution is preferably in the range of 3.1 to 3.7, more preferably around 3.5.
  • nitric acid or ammonia may be added as necessary.
  • tannic acid may be further added to the chemical conversion treatment solution used for the electrolytic treatment.
  • the tannic acid reacts with Fe in the steel sheet 103 to form a film of Fe tannic acid on the surface of the steel sheet 103.
  • a film of Fe tannate is preferable because it improves rust resistance and adhesion.
  • the solvent for the chemical conversion treatment liquid for example, deionized water, distilled water or the like can be used.
  • the electrical conductivity of the chemical conversion solution solvent is preferably 10 ⁇ S / cm or less, more preferably 5 ⁇ S / cm or less, and further preferably 3 ⁇ S / cm or less.
  • the solvent of the said chemical conversion liquid is not limited to this, It is possible to select suitably according to the material to melt
  • a Zr source for example, a Zr complex such as H 2 ZrF 6 can be used.
  • Zr in the Zr complex as described above is present in the chemical conversion solution as Zr 4+ due to a hydrolysis reaction accompanying an increase in pH at the cathode electrode interface.
  • Such Zr ions form a compound such as ZrO 2 or Zr 3 (PO 4 ) 4 by a dehydration condensation reaction with a hydroxyl group (—OH) present on the metal surface in the chemical conversion solution.
  • (NH 4 ) 3 AlF 6 is used as an Al supply source.
  • AlF complex a state where it is complexed with F
  • Al in the AlF complex is precipitated together with Zr in the electrolytic treatment process to form the chemical conversion coating layer 107, thereby contributing to the resistance to sulfur blackening resistance as described above.
  • Al is present as a cation in the chemical conversion treatment liquid, like Zr. Therefore, by using (NH 4 ) 3 AlF 6 as the supply source of Al, it becomes possible to supply Al into the chemical conversion treatment liquid without increasing the concentration of phosphate ions in the chemical conversion treatment liquid.
  • step S107 a known post-treatment is performed on the steel sheet 103 on which the Fe—Sn alloy layer 105a, the Sn layer 105b, and the chemical conversion treatment film layer 107 are formed.
  • the chemical conversion treatment film layer 107 is formed by the electrolytic treatment. However, when it is allowed to take a sufficient time for the formation of the chemical conversion treatment coating, the immersion treatment is not performed.
  • the chemical conversion treatment film layer 107 may be formed by the treatment.
  • the chemical conversion treatment steel plate and the method for manufacturing the chemical conversion treatment steel plate according to the embodiment of the present invention will be specifically described with reference to examples.
  • the Example shown below is an example of the manufacturing method of the chemical conversion treatment steel plate and chemical conversion treatment steel plate which concern on embodiment of this invention, Comprising: The manufacturing method of the chemical conversion treatment steel plate and chemical conversion treatment steel plate which concern on embodiment of this invention is shown.
  • the present invention is not limited to the following examples.
  • Example 1 In Example 1, the content of the Zr compound and the phosphate compound in the chemical conversion coating layer was not changed, but the content of the Al compound was changed to verify how the sulfurization blackening resistance changed. .
  • Example 1 a steel plate generally used as a steel plate for containers was used as a base material.
  • An Fe—Sn alloy layer and an Sn layer were formed on the steel sheet by performing molten tin treatment in the state where the Sn plating layer was formed on the steel sheet.
  • the total Sn content of the Fe—Sn alloy layer and the Sn layer was 2.8 g / m 2 per side in terms of the amount of metallic Sn in all samples.
  • the concentration of the Al compound in the chemical conversion coating layer was changed for each sample to form a chemical conversion coating layer, and a plurality of samples were manufactured.
  • the Zr compound content was 8 mg / m 2 per side in terms of metal Zr
  • the phosphate compound content was 3 mg / m 2 per side in terms of P amount.
  • the evaluation of the resistance to sulfurization blackening was performed as follows. First, a 0.6 mass% L-cysteine solution boiled for 1 hour was placed in a heat-resistant bottle, and the sample ( ⁇ 40 mm) was placed and fixed as a lid on the mouth of the heat-resistant bottle. Next, the heat-resistant bottle covered as described above was subjected to heat treatment (retort treatment) at 110 ° C. for 15 minutes in a soaking furnace. Then, in each sample, the external appearance observation of the contact part with a heat-resistant bottle was performed, and 10 steps
  • the horizontal axis indicates the content of Al compound (amount of metal Al) in the chemical conversion coating layer in each sample
  • the vertical axis indicates the evaluation result of resistance to sulfur blackening.
  • the evaluation result of the resistance to sulfur blackening was a rating of 1.
  • the evaluation result of the resistance to sulfur blackening is a score of 7 or more, and it is clear that the resistance to sulfur blackening is extremely excellent. It became. From this result, it was shown that by containing a predetermined amount of Al compound in the chemical conversion coating layer, the sulfur blackening resistance of the chemical conversion steel plate having the chemical conversion coating was dramatically improved.
  • Example 2 Next, it verified about how sulfuration blackening resistance changes, changing the component amount of each component contained in the chemical conversion treatment film layer 107. More specifically, a chemical conversion treatment film layer was formed on the Sn layer using a steel sheet on which an Fe—Sn alloy layer and an Sn layer were formed.
  • a chemical conversion treatment film layer was formed on the Sn layer using a steel sheet on which an Fe—Sn alloy layer and an Sn layer were formed.
  • (NH 4 ) 3 AlF 6 was used as the Al ion supply source
  • Comparative Examples a5 and a6 Al 2 was used as the Al ion supply source.
  • a chemical conversion film layer was formed using (SO 4 ) 3 .
  • the amount of metal Zr, the amount of P and the amount of metal Al contained in the chemical conversion coating film layer are measured with a fluorescent X-ray adhesion meter, and the corrosion resistance and sulfide blackening resistance Evaluation was performed.
  • the content of Al 2 O 3 in the chemical conversion coating layer is determined by calculating the peak intensity ratio of Al 2 O 3 , metal Al, and other Al compounds by X-ray photoelectron spectroscopy (XPS). Asked. Then, the content of Al 2 O 3 in the chemical conversion coating layer is calculated from the total metal Al amount obtained by the quantitative analysis method such as fluorescent X-ray analysis and the peak intensity ratio obtained by XPS as described above. did.
  • ⁇ Evaluation of corrosion resistance> As the corrosion resistance test solution, 3% acetic acid was used. The chemical conversion treated steel plate of the sample was cut into ⁇ 35 mm and fixed on the mouth of a heat-resistant bottle containing a corrosion resistance test solution. After heat treatment at 121 ° C. for 60 minutes, the degree of corrosion of the sample was evaluated by observing the contact portion between the sample and the corrosion resistance test solution. Specifically, the following 10-step evaluation was performed according to the ratio of the area that did not corrode in the contact area between the sample and the corrosion resistance test solution. In addition, if a score is 5 points or more, it can be used as a steel plate for containers.
  • Corrosion resistance evaluation items are labeled “Very Good” for 10 to 9 points, “Good” for 8 to 5 points, and “Not Good” for 4 points and below.
  • Examples A1 to A18 all had excellent corrosion resistance and excellent resistance to sulfur blackening.
  • Comparative Examples a1 to a6 were inferior in either corrosion resistance or sulfurization blackening resistance.
  • the Al amount and Al 2 O 3 amount were remarkably small, and the resistance to sulfur blackening was “Not Good”.
  • Example 3 Next, it was verified how the sulfide blackening resistance changes depending on the Sn content and the content of each component included in the chemical conversion coating layer.
  • Table 2 shows the Sn content of each sample, and Table 3 shows the conditions for the chemical conversion treatment (the conditions for the chemical conversion treatment solution and the conditions for the electrolytic treatment).
  • Table 4 shows the amount of metal Zr, the amount of P, the amount of metal Al, and the amount of Al 2 O 3 contained in the chemical conversion coating layer formed on each sample. Further, each sample was evaluated for corrosion resistance and sulfur blackening resistance in the same manner as in Example 2. The results are shown in Table 4.

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JP6583539B2 (ja) 2019-10-02
KR20180113583A (ko) 2018-10-16
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