EP3219826A1 - Procédé permettant la fabrication de tôle d'acier galvanisée - Google Patents

Procédé permettant la fabrication de tôle d'acier galvanisée Download PDF

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Publication number
EP3219826A1
EP3219826A1 EP15858294.0A EP15858294A EP3219826A1 EP 3219826 A1 EP3219826 A1 EP 3219826A1 EP 15858294 A EP15858294 A EP 15858294A EP 3219826 A1 EP3219826 A1 EP 3219826A1
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EP
European Patent Office
Prior art keywords
steel sheet
zinc
aqueous solution
alkaline aqueous
based coating
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EP15858294.0A
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German (de)
English (en)
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EP3219826A4 (fr
Inventor
Katsuya Hoshino
Shoichiro Taira
Shinichi Furuya
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JFE Steel Corp
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JFE Steel Corp
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Publication of EP3219826A1 publication Critical patent/EP3219826A1/fr
Publication of EP3219826A4 publication Critical patent/EP3219826A4/fr
Withdrawn legal-status Critical Current

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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
    • 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
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/53—Treatment of zinc 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
    • 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
    • C23C22/60—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 alkaline aqueous solutions with pH greater than 8
    • 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
    • C23C22/78—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C23C28/3225—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only with at least one zinc-based layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals

Definitions

  • the present invention relates to a method for manufacturing a steel sheet coated with a zinc-based coating layer having a reaction layer.
  • a steel sheet coated with a zinc-based coating layer has been used in a wide range of applications mainly in automobile bodies, domestic electrical appliances, and building materials.
  • properties such as press formability, corrosion resistance, and surface appearance quality of a steel sheet coated with a zinc-based coating layer used in such applications are improved by forming a reaction layer on the surface of the steel sheet.
  • a steel sheet coated with a zinc-based coating layer before a reaction layer is formed thereon has an unnecessary layer having a thickness of less than 10 nm composed of oxides of, for example, Zn and Al, which are impurity chemical elements, in the outermost surface layer thereof. Since such an unnecessary oxide layer decreases the reactivity of a chemical conversion treatment such as a zinc phosphate treatment or a chromate treatment, it is necessary to set a long reaction time in order to form a sufficient amount of the reaction layer.
  • An increase in reaction time is accompanied by an increase in equipment cost, line length, and running cost for, for example, electricity and gas.
  • Patent Literature 1 describes a technique in which a galvanized steel sheet is treated by using a SiO 2 -containing chromate solution after the steel sheet has been brought into contact with an alkaline aqueous solution.
  • Patent Literature 2 and Patent Literature 3 describe techniques in which an oxide layer is formed after the surface of a galvanized steel sheet has been brought into contact with an alkaline aqueous solution.
  • Patent Literature 4 describes a technique in which an oxide layer is formed after the surface of a galvannealed steel sheet has been brought into contact with an alkaline aqueous solution.
  • Patent Literature 5 describes a technique in which an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O is formed after the surface of a galvanized steel sheet has been brought into contact with an alkaline aqueous solution.
  • Patent Literature 1 through Patent Literature 5 it is possible to decrease the reaction time required to form a reaction layer through contact with an alkaline aqueous solution.
  • an alkaline aqueous solution since pressing flaws occur on the surface of a steel sheet due to precipitates of Zn and Al generated in the alkaline aqueous solution adhering to deflecting rolls and supporting rolls, there is a case where problems related to surface appearance such as an irregularity in surface appearance occurs after a reaction layer has been formed.
  • An object of the present invention is to provide a method for manufacturing a steel sheet coated with a zinc-based coating layer in which it is possible to remove an unnecessary oxide layer on the surface of the zinc-based coating layer through contact with an alkaline aqueous solution and in which it is possible to prevent a problem related to surface appearance due to precipitates generated in an alkaline aqueous solution.
  • the present inventors diligently conducted investigations in order to solve the problems described above, and, as a result, found that it is possible to solve the problems described above by adding a specific chelating agent to an alkaline aqueous solution which is used before a reaction layer is formed, resulting in the completion of the present invention. More specifically, the present invention provides the following.
  • the method for manufacturing a steel sheet coated with a zinc-based coating layer of the first invention in order to solve the problems described above is a method for manufacturing a steel sheet coated with a zinc-based coating layer having a reaction layer on the surface of the steel sheet, the method including:
  • the method for manufacturing a steel sheet coated with a zinc-based coating layer of the second invention in order to solve the problems described above is the method for manufacturing a steel sheet coated with a zinc-based coating layer according to the first invention, wherein pH of the alkaline aqueous solution is 12.6 or more.
  • the present invention it is possible to effectively remove oxides on the surface of a zinc-based coating layer through contact with an alkaline aqueous solution.
  • an alkaline treatment which is performed in order to decrease the time required to form a reaction layer, since it is possible to decrease the amount of, for example, precipitates of Al and Zn, it is possible to obtain a steel sheet coated with a zinc-based coating layer having a reaction layer and having good surface appearance.
  • Fig. 1 is a schematic diagram illustrating evaluation criteria for an irregularity in surface appearance.
  • a steel sheet coated with a zinc-based coating layer refers to a steel sheet having a coating film containing mainly zinc on the surface thereof regardless of its manufacturing method, and the meaning of the term includes a zinc-coated steel sheet, a zinc-alloy-coated steel sheet, a steel sheet coated with a coating layer containing particles dispersed in zinc, and so forth. That is, the meaning of the term "a zinc-based coating layer” includes a zinc coating layer, a zinc-alloy coating layer, a coating layer containing particles dispersed in zinc, and so forth.
  • the present invention is a method for manufacturing a steel sheet coated with a zinc-based coating layer, the steel sheet having a reaction layer, that is, an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4)1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O, with which it is possible to effectively remove an unnecessary oxide layer existing on the surface of the zinc-based coating layer.
  • the present invention includes, for example, a process in which zinc-based coating is performed, a process in which the steel sheet is brought into contact with an alkaline aqueous solution, and a process in which an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O is formed.
  • a process in which zinc-based coating is performed a process in which the steel sheet is brought into contact with an alkaline aqueous solution
  • an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O is formed.
  • the grade of steel sheet on which zinc coating is performed there is no particular limitation on the grade of steel sheet on which zinc coating is performed, and a steel sheet of any steel grade such as low-carbon steel, ultralow-carbon steel, IF steel, or a high-strength steel sheet, in which various alloy chemical elements are added, may be used.
  • the steel sheet may be any of a hot-rolled steel sheet and a cold-rolled steel sheet.
  • the thickness of the steel sheet it is preferable that the thickness be 0.4 mm to 5.0 mm from the viewpoint of applications such as automobile bodies, domestic electrical appliances, and building materials.
  • a galvannealed steel sheet may be manufactured by performing an alloying treatment.
  • the conditions for performing an alloying treatment there is no particular limitation on the conditions for performing an alloying treatment, and preferable conditions may be used appropriately.
  • a contact treatment is performed by using an alkaline aqueous solution.
  • the alkaline aqueous solution which is used in this contact treatment has a pH of 10.0 or more. In the case where the pH is less than 10.0, an insufficient amount of oxide layer is removed. It is preferable that the pH be 12.6 or more, because it is possible to effectively decrease the contact time with the alkaline aqueous solution.
  • the pH be 14.0 or less from the viewpoint of preventing the dissolution of the zinc-based coating layer and the blackening of surface appearance.
  • Specific chelating agents are contained in the alkaline aqueous solution in a total amount of 0.050 mass% or more. In the case where there is an increase in the amount of, for example, precipitates of Al and Zn in the alkaline aqueous solution, the solution has a suspension-like appearance. In the present invention, 0.050 mass% or more of chelating agents are added to the alkaline aqueous solution in order to decrease the amounts of, for example, the precipitates of Al and Zn.
  • the chelating agents described above are one or more selected from among sodium gluconate, sodium glucoheptonate, sodium citrate, tartaric acid, arabonic acid, galactonic acid, sorbit, mannite, glycerin, EDTA, and sodium tripolyphosphate. It is preferable to use sodium gluconate as the chelating agent described above, because it is capable of chelating Al and Zn and inexpensive.
  • the total content of chelating agents in the alkaline aqueous solution is less than 0.050 mass%, there is an insufficient increase in the solubility of Al and Zn in the alkaline aqueous solution. It is preferable that the content of chelating agents in the alkaline aqueous solution be 0.100 mass% or more from the viewpoint of decreasing the amount of precipitates in the alkaline aqueous solution. On the other hand, it is preferable that the content of chelating agents in the alkaline aqueous solution be 10.0 mass% or less from the viewpoint of chemical cost.
  • the temperature of the alkaline aqueous solution be in the range of 20°C to 70°C, or more preferably 40°C to 70°C, in order to decrease the contact time between the alkaline aqueous solution and a steel sheet.
  • an alkaline builder there is no limitation on the kind of an alkaline builder.
  • a chemical such as NaOH from the viewpoint of cost.
  • the amount of the alkaline builder is appropriately controlled.
  • the alkaline aqueous solution may contain substances and chemical components other than chemical elements such as Zn, Al, and Fe, which are contained in a zinc-based coating solution.
  • the method used for bringing the alkaline aqueous solution into contact with a steel sheet coated with a zinc-based coating layer in particular, an oxide layer on the surface thereof
  • examples of the method include one in which the steel sheet coated with a zinc-based coating layer is dipped in the alkaline aqueous solution and one in which the steel sheet coated with a zinc-based coating layer is sprayed with the alkaline aqueous solution.
  • a time during which the steel sheet coated with a zinc-based coating layer is brought into contact with the alkaline aqueous solution is 1.0 second or more. In the case where the contact time is less than 1.0 second, since an insufficient amount of oxides is removed from the surface of the zinc-based coating layer, there is an insufficient decrease in reaction time during which a reaction layer is formed. It is preferable that the time during which the steel sheet coated with a zinc-based coating layer is brought into contact with the alkaline aqueous solution be 10.0 seconds or less from the viewpoint of equipment cost and productivity.
  • a skin pass rolling may be performed after the process in which zinc-based coating is performed and before or after the treatment is performed by using an alkaline aqueous solution.
  • a treatment is performed in order to form a reaction layer, that is, an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O.
  • an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O refers to the layer of a reaction product which is formed on the surface of a steel sheet through a chemical reaction which occurs as a result of contact between a zinc-based coating layer and a chemical treatment solution.
  • An example of a treatment for forming an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O includes an oxide-layer-forming process in which a steel sheet coated with a zinc-based coating layer is brought into contact with an acid solution containing sulfate ions, then held for 1 second to 60 seconds, and then washed with water and a neutralizing treatment process in which the surface of the oxide layer formed in the oxide-layer-forming process described above is kept in contact with an alkaline aqueous solution for 0.5 seconds or more, then washed with water, and then dried.
  • the alkaline aqueous solution may contain P ions in an amount of 0.01 g/L or more in terms of P concentration and carbonate ions in an amount of 0.1 g/L or more in terms of carbonate ion concentration.
  • the present invention is not limited to such a treatment method as long as a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O exists on the surface of a steel sheet.
  • a skin pass rolling was performed on steel sheets which had been prepared by performing a galvanizing treatment on cold-rolled steel sheets having a thickness of 0.7 mm and a width of 1100 mm. Subsequently, the steel sheets were subjected to a treatment for removing an oxide layer in which the steel sheets were kept in contact with the alkaline aqueous solutions prepared under the conditions given in Tables 1-1 and 1-2 over the specified times, then washed with water, and then dried.
  • steel sheets which had been prepared by performing a galvanizing treatment followed by an alloying treatment and skin pass rolling on a cold-rolled steel sheets having a thickness of 0.7 mm and a width of 1100 mm and steel sheets which had been prepared by performing an electro-galvanizing treatment on cold-rolled steel sheets having a thickness of 0.7 mm and a width of 1100 mm were kept in contact with the alkaline aqueous solutions in the same procedures as those described above, then washed with water, and then dried.
  • a treatment for forming an oxide layer containing a crystal-structured substance expressed by Zn 4 (SO 4 ) 1-x (CO 3 ) x (OH) 6 ⁇ nH 2 O was performed by dipping the steel sheets in a sulfuric acid solution containing 30 g/L of sodium acetate trihydrate and having a pH of 1.5, then squeezing the steel sheets by using rolls, and then holding the steel sheets for 10 seconds. Then, after having performed washing with water, drying was performed. Subsequently, a neutralizing treatment was performed by using a treatment solution containing 9.8 g/L of sodium pyrophosphate and 0.48 g/L of sodium carbonate decahydrate.
  • an X-ray fluorescence spectrometer was used for determining the thickness of an unnecessary oxide layer formed on the surface of the steel sheet coated with a zinc-based coating layer. It is judged that a case where the thickness of the oxide layer (thickness of an oxide film) is 4 nm or less as a case where there is a decrease in reaction time required to form a reaction layer. It is judged that a case where the thickness of an oxide film is 2 nm or less as a case where there is a further decrease in reaction time.
  • an O-K ⁇ ray was detected.
  • intensity was determined at a peak position and a background position in order to calculate the net intensity of an O-K ⁇ ray.
  • the integration time at each of the peak position and the background position was 20 seconds.
  • silicon wafers which were cleaved into an appropriate size and whose surface were respectively covered with silicon oxide films having a film thickness of 96 nm, 54 nm, and 24 nm were set on the sample stage with these series of samples so that it was possible to calculate the intensity of an O-K ⁇ ray of each of such silicon oxide films.
  • a calibration curve is prepared to determine the relationship between the thickness of an oxide layer and the intensity of an O-K ⁇ ray by using such data.
  • the thickness of the oxide layer of the sample is calculated as the thickness of the oxide layer in terms of the thickness of a silicon oxide film.
  • the alkaline aqueous solution which had been used for the treatment of 100 tons or more of a steel sheet coated with a zinc-based coating layer was collected and subjected to suction filtration by using a membrane filter having a pore size of 1 ⁇ m. After having dried the material retained on the filter at a temperature of 110°C, the weight of the dried material was determined, and the weight was expressed in units of mg/L. The amount of production for which the determined value was more than 10 mg/L was recorded. A case where the amount of steel sheets treated for which the determined value was more than 10 mg/L was 3000 tons or more was judged as satisfactory from the viewpoint of productivity.
  • Nos. 24 and 28 through 33 are the examples of the present invention in which the effect of pH was clarified by performing a contact treatment with a contact time of 1.0 second.
  • pH was 12.6 or more, since it was possible to decrease the thickness of an oxide film to 2 nm or less even with a contact time of 1.0 second, it was possible to decrease a reaction time required to form a reaction layer to a higher degree.
  • the composition of the gas was analyzed.
  • the column temperature at the time of GC/MS analysis was set to be 300°C.
  • X-ray-absorption fine-structure spectrometer By using an X-ray-absorption fine-structure spectrometer, the existence form of P was analyzed. By using beam line BL27A of Photon Factory, High Energy Accelerator Research Organization, the observation of an X-ray absorption fine structure (ZAFS) was performed at room temperature. By irradiating the surface of a degreased sample with a monochrome radiation beam, the spectrum of an X-ray absorption near-edge structure (XANES) of P-K shell was observed by using a total electron yield method (TEY) by performing sample absorption current measurement.
  • ZAFS X-ray absorption fine structure
  • TEY total electron yield method
  • the amount of decrease in weight at a temperature of 100°C or lower was determined. About 15 mg of powder sample was used for the determination. After having charging the sample into the analyzer, by increasing the temperature from room temperature (about 25°C) to 1000°C at an increasing rate of 10°C/min, a change in weight while the temperature was being increased was recorded.
  • the crystal structure was presumed. The determination was performed with Cu being used as the target under the conditions of an acceleration voltage of 40 kV, a tube current of 50 mA, a scanning speed of 4 deg/min, and a scanning range of 2° to 90°.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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EP15858294.0A 2014-11-12 2015-11-09 Procédé permettant la fabrication de tôle d'acier galvanisée Withdrawn EP3219826A4 (fr)

Applications Claiming Priority (2)

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JP2014229484 2014-11-12
PCT/JP2015/005583 WO2016075920A1 (fr) 2014-11-12 2015-11-09 Procédé permettant la fabrication de tôle d'acier galvanisée

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EP3219826A1 true EP3219826A1 (fr) 2017-09-20
EP3219826A4 EP3219826A4 (fr) 2017-11-22

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US (1) US20170314138A1 (fr)
EP (1) EP3219826A4 (fr)
JP (1) JPWO2016075920A1 (fr)
KR (1) KR102007103B1 (fr)
CN (1) CN107109660A (fr)
MX (1) MX2017006133A (fr)
WO (1) WO2016075920A1 (fr)

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US11661666B2 (en) 2019-10-10 2023-05-30 The Boeing Company Electrodeposited zinc and iron coatings for corrosion resistance

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JP4525252B2 (ja) 2003-08-29 2010-08-18 Ｊｆｅスチール株式会社 合金化溶融亜鉛めっき鋼板の製造方法
KR20050022264A (ko) * 2003-08-29 2005-03-07 제이에프이 스틸 가부시키가이샤 합금화용융아연도금강판의 제조방법 및합금화용융아연도금강판
JP4604712B2 (ja) 2004-12-27 2011-01-05 Ｊｆｅスチール株式会社 溶融亜鉛めっき鋼板の製造方法および溶融亜鉛めっき鋼板
JP4517887B2 (ja) 2005-02-25 2010-08-04 Ｊｆｅスチール株式会社 溶融亜鉛めっき鋼板の製造方法および溶融亜鉛めっき鋼板
JP4961743B2 (ja) * 2005-12-20 2012-06-27 株式会社デンロコーポレーション 溶融亜鉛めっき表面の着色処理方法
KR101106516B1 (ko) * 2006-10-31 2012-01-20 제이에프이 스틸 가부시키가이샤 인산염 처리 아연계 도금 강판 및 그 제조 방법
TWI394863B (zh) * 2007-12-27 2013-05-01 Kansai Paint Co Ltd 金屬表面處理用組成物及從該金屬表面處理用組成物獲得之具有金屬表面處理層的表面處理金屬材
JP5338226B2 (ja) * 2008-09-26 2013-11-13 Ｊｆｅスチール株式会社 熱間プレス用亜鉛系めっき鋼板
DE102012213089A1 (de) 2012-07-25 2014-01-30 Hamilton Bonaduz Ag Kopplungsausbildung eines Pipettierkanals einer Pipettiervorrichtung zur Ankopplung einer Pipettierspitze daran
CN106062249B (zh) * 2014-02-27 2019-07-02 杰富意钢铁株式会社 镀锌系钢板及其制造方法
MX2016011086A (es) * 2014-02-27 2016-11-25 Jfe Steel Corp Lamina de acero galvanizada y metodo para la produccion de la misma.
JP7013305B2 (ja) * 2018-03-29 2022-01-31 株式会社Lixil 水栓装置

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US20170314138A1 (en) 2017-11-02
JPWO2016075920A1 (ja) 2017-04-27
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MX2017006133A (es) 2017-07-27
CN107109660A (zh) 2017-08-29
WO2016075920A1 (fr) 2016-05-19
EP3219826A4 (fr) 2017-11-22

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