WO2015012176A1 - 容器用鋼板 - Google Patents
容器用鋼板 Download PDFInfo
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- WO2015012176A1 WO2015012176A1 PCT/JP2014/068941 JP2014068941W WO2015012176A1 WO 2015012176 A1 WO2015012176 A1 WO 2015012176A1 JP 2014068941 W JP2014068941 W JP 2014068941W WO 2015012176 A1 WO2015012176 A1 WO 2015012176A1
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- steel plate
- layer
- steel sheet
- film
- plated steel
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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
- C23C22/05—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
- C23C22/50—Treatment of iron or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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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
- 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
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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
- 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
- C23C28/027—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 matrix material comprising a mixture of at least two metals or metal phases or metal matrix composites, e.g. metal matrix with embedded inorganic hard particles, CERMET, MMC.
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- 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
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- 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
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
- C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
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- 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
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- 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
Definitions
- the present invention relates to a steel plate for containers.
- an Sn-plated steel plate conventionally referred to as “blink” As a steel plate for containers (surface-treated steel plate for cans), an Sn-plated steel plate conventionally referred to as “blink” has been widely used.
- the Sn-plated surface is usually obtained by immersing the steel sheet in an aqueous solution containing a hexavalent chromium compound such as dichromic acid, or by performing a chromate treatment such as performing an electrolytic treatment in this solution.
- a chromate film is formed on the surface.
- movements for restricting the use of Cr have progressed in various fields, and several treatment techniques for replacing chromate treatment have been proposed for steel plates for containers.
- Patent Document 1 states that “without using Cr and has excellent resin adhesion” ([0013]), “having a film containing Zr and O on at least one surface of a metal plate, There is disclosed a “surface-treated metal sheet” characterized in that the F amount is less than 0.1 mg / m 2 per side ([Claim 1]). ([Claim 3]).
- the present invention has been made in view of the above points, and an object thereof is to provide a steel plate for containers that is excellent in resin adhesion and corrosion resistance.
- the inventors of the present invention have good resin adhesion and corrosion resistance because the coating of the steel plate for containers contains a specific component in a specific amount. As a result, the present invention has been completed.
- the present invention provides the following (1) to (4).
- the coating contains Zr, Ti, and silica, and the coating has a Zr equivalent adhesion amount on one side of the plated steel sheet of 1 to 40 mg / m 2 , and the Ti equivalent adhesion on one side of the plated steel sheet.
- the amount is less than 0.5 mg / m 2 ultra 10 mg / m 2
- the adhesion amount of Si in terms of per one surface of the plated steel sheet is 1 ⁇ 40mg / m 2, the container for the steel sheet.
- the above coating, the deposition amount of Ti in terms of per side of the plated steel sheet is less than 3 mg / m 2 Ultra 10 mg / m 2, the container for steel sheet according to (1).
- the atomic ratio of Ti and Zr (Ti / Zr) on the outermost surface opposite to the plated steel sheet side of the coating is 0.05 to 2.0, and the atomic ratio of Si and Zr (Si / Zr)
- the plating layer further comprises at least one layer selected from the group consisting of a Ni layer, a Ni—Fe alloy layer, a Fe—Sn alloy layer, and a Fe—Sn—Ni alloy layer.
- the plating layer further comprises at least one layer selected from the group consisting of a Ni layer, a Ni—Fe alloy layer, a Fe—Sn alloy layer, and a Fe—Sn—Ni alloy layer.
- the steel plate for containers of the present invention has a plated steel plate and a film disposed on the surface of the plated steel plate on the plating layer side. And this film
- membrane contains Zr and Ti by specific amount, and also resin is excellent in resin adhesiveness and corrosion resistance because it contains silica by specific amount.
- the plated steel sheet includes a steel sheet and a plating layer that covers at least a part of the surface of the steel sheet, and the plating layer includes at least a Sn layer.
- steel sheet The kind in particular of steel plate is not restrict
- the steel plate (For example, a low carbon steel plate, a very low carbon steel plate) normally used as a container material can be used.
- the manufacturing method and material of the steel plate are not particularly restricted, and the steel plate is manufactured through processes such as hot rolling, pickling, cold rolling, annealing, and temper rolling from a normal steel slab manufacturing process.
- a steel sheet having a nickel (Ni) -containing layer formed on the surface thereof may be used, and a plating layer including an Sn layer described later may be formed on the Ni-containing layer.
- a plating layer containing island-shaped Sn can be formed, and weldability is improved.
- the Ni-containing layer only needs to contain nickel, and examples thereof include a Ni plating layer and a Ni—Fe alloy layer.
- the method for applying the Ni-containing layer to the steel plate is not particularly limited, and examples thereof include known methods such as electroplating.
- the Ni diffusion layer is coordinated to form a Ni—Fe alloy layer by annealing after applying Ni on the steel sheet surface by electroplating or the like. Can do.
- the amount of Ni in the Ni-containing layer is not particularly limited, and is preferably 50 to 2000 mg / m 2 as the Ni conversion amount per side. If it is in the said range, it will become advantageous also in terms of cost.
- the plated steel sheet has a plating layer including a Sn layer on at least a part of the surface of the steel sheet.
- the plating layer only needs to be provided on at least one side of the steel plate, and may be provided on both sides.
- the Sn adhesion amount per one side of the plated steel sheet of the plating layer is preferably 0.1 to 15.0 g / m 2 . If the Sn adhesion amount is within the above range, the corrosion resistance of the steel plate for containers is more excellent, among which 0.2 to 15.0 g / m 2 is preferable, and 1.0 to 15.0 g in terms of excellent workability. / M 2 is more preferable.
- the Sn adhesion amount can be measured by surface analysis by a coulometric method or fluorescent X-ray.
- fluorescent X-rays a calibration curve relating to the Sn amount is specified in advance using a Sn adhesion amount sample with a known Sn amount, and the Sn amount is relatively specified using the calibration curve.
- the plating layer is a layer covering at least a part on the surface of the steel sheet, and may be a continuous layer or a discontinuous island shape.
- a plating layer in addition to a plating layer composed of an Sn layer obtained by plating Sn, the lowermost layer (Sn layer / steel plate interface) of the Sn layer obtained by heating and melting Sn by energization heating after Sn plating, etc. A plating layer in which a part of the Fe—Sn alloy layer is formed is also included.
- Sn plating is performed on a steel sheet having a Ni-containing layer on the surface, and tin is further heated and melted by electric heating or the like, and Fe—Sn is formed in the lowest layer of the Sn layer (Sn layer / steel sheet interface).
- Ni-containing layer Ni layer, Ni—Fe alloy layer
- Examples of the method for producing the plating layer include a known method (for example, an electroplating method or a method of plating by immersing in molten Sn).
- a known method for example, an electroplating method or a method of plating by immersing in molten Sn.
- a phenol sulfonic acid Sn plating bath, a methane sulfonic acid Sn plating bath, or a halogen-based Sn plating bath is used, and Sn is applied to the surface of the steel sheet so that the adhesion amount per side becomes a predetermined amount (for example, 2.8 g / m 2 ).
- a heat melting treatment is performed at a temperature equal to or higher than the melting point of Sn (231.9 ° C.), and the Fe—Sn alloy is formed on the lowermost layer (Sn layer / steel plate interface) of the Sn single layer.
- a plating layer on which the layer is formed can be manufactured.
- the lowermost layer (Sn layer / steel sheet interface) of the plating layer (Sn layer) of Sn alone is obtained by performing a heat melting treatment after Sn plating on the Ni-containing layer.
- An Fe—Sn—Ni alloy layer, an Fe—Sn alloy layer, and the like are formed.
- membrane is arrange
- the coating contains Zr, Ti and silica as its components. First, each component will be described in detail below, and then the method for forming the film will be described in detail.
- the coating contains Zr (zirconium element) and has a Zr equivalent adhesion amount (hereinafter also referred to as “Zr adhesion amount”) of 1 to 40 g / m 2 per one side of the plated steel sheet. If the amount of Zr adhesion is within the above range, the resin adhesion and corrosion resistance of the steel plate for containers are excellent. Of these, 1 to 25 mg / m 2 is preferable because of its excellent cost performance. If the Zr adhesion amount is less than 1 mg / m 2 , the resin adhesion and the corrosion resistance are inferior. Note that there is no problem in performance even if the Zr adhesion amount exceeds 40.0 mg / m 2 , but this leads to an increase in the cost of the treatment liquid for securing the adhesion amount and an increase in current density.
- the adhesion amount of Ti in terms of per side of the plated steel sheet (hereinafter, also referred to as "Ti deposition amount") is less than 0.5 mg / m 2 Ultra 10 mg / m 2. If the amount of Ti adhesion is within the above range, the resin adhesion of the steel plate for containers is excellent. Furthermore, in that the resin adhesion is more excellent than 3 mg / m 2 Ultra 10 mg / m 2 is preferred. When the adhesion amount of Ti is 0.5 mg / m 2 or less, the resin adhesion is inferior. Note that there is no problem in performance even if the Ti adhesion amount is 10 mg / m 2 or more, but this leads to an increase in the cost of the treatment liquid for securing the adhesion amount and an increase in current density.
- the coating contains silica.
- the silica represented by the composition formula SiO 2 includes amorphous and spherical ones, and the silica contained in the coating is preferably spherical silica.
- colloidal silica in which spherical silica is dispersed as a Si component in the treatment liquid described later it is considered that this spherical silica is contained in the film while maintaining its shape.
- the fact that the silica contained in the film is spherical can be confirmed, for example, by exposing the cross section of the film by focused ion beam (FIB) processing and observing it with a transmission electron microscope (TEM).
- FIB focused ion beam
- TEM transmission electron microscope
- the coating has a Si (silicon element) conversion amount of silica per side of the plated steel sheet (hereinafter also referred to as “Si adhesion amount”) of 1 to 40 mg / m 2 .
- Si adhesion amount is within the above range, the resin adhesion is excellent.
- the Si adhesion amount is preferably 1 to 25 mg / m 2 for the reason that cost performance is excellent.
- the Si adhesion amount is less than 1 mg / m 2 , the resin adhesion is inferior.
- the Zr adhesion amount, Ti adhesion amount, and Si adhesion amount described above can be measured by surface analysis using fluorescent X-rays.
- membrane is contained as zirconium compounds, such as a zirconium oxide, a zirconium hydroxide, a zirconium fluoride, a zirconium phosphate, or these composite compounds, for example.
- the Zr adhesion amount means a Zr equivalent amount of these zirconium compounds.
- Ti in the film is contained as a titanium compound such as titanium phosphate, titanium hydrated oxide, or a composite compound thereof.
- the Ti adhesion amount means the Ti equivalent amount of these titanium compounds.
- the atomic ratio (Ti / Zr) of Ti and Zr on the outermost surface of the coating is 0.05 to 2.0, and Si and Zr And an atomic ratio (Si / Zr) of 0.1 to 3.0. If it is this aspect, the resin adhesiveness of the steel plate for containers will be more excellent.
- the atomic ratio is obtained by analyzing peaks of Zr3d, Ti2p, and Si2p by XPS (X-ray Photoelectron Spectroscopy) analysis.
- XPS X-ray Photoelectron Spectroscopy
- Equipment Shimadzu / Kraitos AXIS-HS
- Measurement area Hybrid mode 250 ⁇ 500 ( ⁇ m)
- the method comprises at least a film forming step for forming the above-described film by subjecting the plated steel sheet immersed in the treatment liquid to cathodic electrolysis (hereinafter also referred to as “production method of the present invention”).
- production method of the present invention the production method of the present invention will be described, and in this description, the treatment liquid of the present invention will also be described.
- the film forming step is a step of forming the above-described film on the surface of the plated steel sheet on the plating layer side, and immersing the plated steel sheet in the treatment liquid of the present invention described later (immersion process) or dipping.
- the steel sheet is subjected to cathodic electrolysis.
- Cathodic electrolytic treatment is preferable because a uniform film can be obtained at a higher speed than immersion treatment.
- the treatment liquid of the present invention used, conditions for the cathodic electrolysis, and the like will be described in detail.
- the treatment liquid of the present invention contains a Zr component (Zr compound) as a Zr supply source for supplying Zr (zirconium element) to the coating.
- Zr component Zr compound
- Zr compound contained in the treatment liquid of the present invention include hexafluorozirconic acid and / or a salt thereof (for example, potassium, ammonium, etc.), zirconium oxyacetate, zirconium oxynitrate, and the like.
- hexafluorozirconic acid is also called zircon hydrofluoric acid.
- Zirconium oxyacetate [ZrO (CH 3 COO) 2 ] is also called zirconyl acetate.
- Zirconium oxynitrate [ZrO (NO 3 ) 2 ] is also called zirconyl nitrate.
- the content of the Zr compound in the treatment liquid of the present invention is preferably from 0.3 to 10.0 g / L, more preferably from 0.5 to 4.0 g / L.
- the treatment liquid of the present invention contains a Ti component (Ti compound) as a Ti supply source for supplying Ti (titanium element) to the film.
- Ti compound contained in the treatment liquid of the present invention include titanium lactate, hexafluorotitanic acid and / or a salt thereof (for example, potassium, ammonium, etc.), titanium alkoxide, titanyl ammonium oxalate, potassium titanyl oxalate 2 Examples thereof include hydrates and titanium sulfate. Titanium lactate [Ti (OH) 2 [OCH (CH 3 ) COOH] 2 ] is also called dihydroxybis (lactato) titanium.
- ammonium salt (monoammonium salt or diammonium salt) is also used. Shall be included. Hexafluorotitanic acid is also called titanium hydrofluoric acid.
- the content of the Ti compound in the treatment liquid of the present invention is preferably 0.1 to 10 g / L, and more preferably 0.2 to 1.0 g / L.
- the treatment liquid of the present invention further contains silica as a Si supply source for supplying Si (silicon element) to the coating.
- silica is used as the silica. It is preferable to contain.
- colloidal silica is a dispersion system in which spherical silica having SiO 2 as a basic unit is dispersed in a dispersion medium such as water.
- the amount of the dispersion medium is not particularly limited, but usually the solid content in the colloidal silica is, for example, 20 to 30% by mass.
- the average particle size of the colloidal silica used in the present invention is preferably 40 nm or less. When the average particle diameter of the colloidal silica is within this range, the specific surface area of the Si compound precipitated in the film becomes larger and the resin adhesion is more excellent.
- the lower limit of the average particle diameter of colloidal silica is not particularly limited, and is preferably 5 nm or more, which is generally distributed, for example.
- the average particle size can be measured by the BET method (converted from the specific surface area by the adsorption method). It is also possible to substitute an average value actually measured from an electron micrograph.
- the content of the Si compound in the treatment liquid of the present invention is preferably 0.01 to 5.0 g / L, more preferably 0.1 to 4.0 g / L in the case of colloidal silica.
- the treatment liquid of the present invention preferably contains a conductive aid.
- the conductive aid is selected from the group consisting of anions which are nitrate ions, potassium ions, ammonium ions and sodium ions. And at least one cation.
- the line speed at which the film can be formed can be increased. That is, it is excellent in high-speed operability. This is presumably because the electrical conductivity of the treatment liquid, that is, the liquid resistance is reduced and improved by including the conductive auxiliary agent, and it becomes easy to pass a high current accompanying the increase in speed.
- the conductive aid is substantially contained in the treatment liquid of the present invention as a salt (for example, ammonium nitrate, potassium nitrate, sodium nitrate, etc.) in which the anion and the cation are ion-bonded.
- a salt for example, ammonium nitrate, potassium nitrate, sodium nitrate, etc.
- water is usually used as the solvent in the treatment liquid of the present invention, but an organic solvent may be used in combination.
- the pH of the treatment liquid of the present invention is not particularly limited, but is preferably pH 2.0 to 5.0. Within this range, the treatment time can be shortened and the stability of the treatment liquid is excellent.
- a known acid component for example, phosphoric acid, sulfuric acid
- alkali component for example, sodium hydroxide, aqueous ammonia
- the treatment liquid of the present invention may contain a surfactant such as sodium lauryl sulfate or acetylene glycol as necessary. Further, from the viewpoint of the stability of the adhesion behavior over time, the treatment liquid may contain a condensed phosphate such as pyrophosphate.
- the liquid temperature of the treatment liquid when performing the treatment is preferably 20 to 80 ° C., and preferably 40 to 60 ° C. from the viewpoints of film formation efficiency and tissue uniformity and low cost. More preferred.
- the electrolysis current density when performing the cathodic electrolysis treatment is preferably a low current density because the resin adhesion and corrosion resistance of the film to be formed are more excellent, and more specifically, 0.05 to 7.0 A / dm 2 is preferable, and 1.0 to 4.0 A / dm 2 is more preferable.
- a film can be formed at a low current density.
- the energization time of the cathodic electrolysis treatment is 0.1 to 5 seconds from the viewpoint that a decrease in the adhesion amount is further suppressed and a film can be stably formed, and a decrease in the characteristics of the formed film is further suppressed.
- 0.3 to 2 seconds are more preferable.
- the electric charge density during the cathodic electrolysis treatment is preferably 0.20 ⁇ 15C / dm 2, more preferably 0.40 ⁇ 10C / dm 2.
- the steel sheet obtained may be washed with water and / or dried to remove unreacted materials as necessary.
- the temperature and method for drying are not particularly limited, and for example, a normal dryer or an electric furnace drying method can be applied.
- the temperature during the drying treatment is preferably 100 ° C. or lower.
- the lower limit is not particularly limited, but is usually about room temperature.
- the steel plate for containers of the present invention obtained by the manufacturing method of the present invention is used for manufacturing various containers such as DI cans, food cans and beverage cans.
- Plated steel sheets were produced by the following two methods [(K-1) and (K-2)].
- K-1 Electrolytic degreasing and pickling were performed on a steel plate (T4 original plate) having a thickness of 0.22 mm, and then Sn plating was performed. Subsequently, a heat melting treatment was performed at a temperature equal to or higher than the melting point of tin, and a plating layer having an Sn adhesion amount per one side shown in Table 2 was formed on both sides of the T4 original plate. In this way, a plating layer composed of Fe—Sn alloy layer / Sn layer was formed in order from the lower layer side.
- K-2 A steel plate (T4 original plate) having a thickness of 0.22 mm was electrolytically degreased, and a nickel plating layer was formed on both sides with a Ni adhesion amount per one side shown in Table 2 using a Watt bath, and then 10 vol.% H 2 +90 vol.% An Ni—Fe alloy layer (Ni-containing layer) (showing Ni adhesion amount in Table 2) was formed on both sides by annealing at 700 ° C. in an N 2 atmosphere to diffuse and infiltrate nickel plating.
- the steel sheet having the Ni-containing layer as the surface layer was formed on both surfaces using an Sn plating bath with the Sn adhesion amount per one side shown in Table 2, and then subjected to heat melting treatment at a melting point of Sn or higher.
- the plating layer was formed on both sides of the T4 original plate. In this way, a plating layer of Ni—Fe alloy layer / Fe—Sn—Ni alloy layer / Sn layer was formed in order from the lower layer side.
- the colloidal silica shown in Table 1 includes SNOWTEX OXS (average particle size: 6 nm), SNOWTEX OS (average particle size: 10 nm), SNOWTEX O (average particle size: 15 nm) manufactured by Nissan Chemical Industries, Ltd. Snowtex O-40 (average particle size: 25 nm) and Snowtex OL (average particle size: 45 nm) were used. Further, as orthophosphoric acid shown in Table 1, phosphoric acid having a concentration of 85% by mass was used.
- the produced steel sheet was evaluated for resin adhesion and corrosion resistance by the following methods.
- the amount of each component and the evaluation results are summarized in Table 2.
- the Ti adhesion amount, Zr adhesion amount, Si adhesion amount, and atomic ratio of the film were measured by the above-described methods.
- a laminated steel plate was prepared by laminating an isophthalic acid copolymerized polyethylene terephthalate film having a thickness of 25 ⁇ m and a copolymerization ratio of 12 mol% on both surfaces of the produced steel plate for containers. Lamination was performed by sandwiching a steel plate and a film heated to 210 ° C. between a pair of rubber rolls, fusing the film to the steel plate, and cooling with water within 1 sec after passing through the rubber roll. At this time, the feeding speed of the steel plate was 40 m / min, and the nip length of the rubber roll was 17 mm.
- the nip length is the length in the transport direction of the portion where the rubber roll and the steel plate are in contact.
- the following resin adhesiveness evaluation was performed. Evaluation of resin adhesion was performed by a 180 degree peel test in a retort atmosphere at a temperature of 150 ° C. and a relative humidity of 100%.
- the 180 degree peel test uses a test piece (size: 30 mm ⁇ 100 mm) obtained by cutting a part 3 of the steel plate 1 while leaving the film 2 as shown in FIG. 1A, as shown in FIG.
- it is a film peeling test performed by attaching a weight 4 (150 g) to one end of the test piece, turning it 180 degrees toward the film 2 and leaving it for 30 minutes.
- peeling length 5 shown in FIG.1 (c) was measured, resin adhesiveness was evaluated as follows, and if it was (double-circle) or (circle), it was considered that resin adhesiveness was favorable.
Abstract
Description
しかしながら、昨今の環境問題を踏まえて、Crの使用を規制する動きが各分野で進行しており、容器用鋼板においてもクロメート処理に替わる処理技術がいくつか提案されている。
例えば、特許文献1には、「Crを用いず、樹脂密着性に優れ」るものとして([0013])、「金属板の少なくとも片面に、ZrおよびOを含む皮膜を有し、該皮膜のF量が片面あたり0.1mg/m2未満であることを特徴とする表面処理金属板」が開示されており([請求項1])、ここでいう「金属板」は「電気Snめっき鋼板」である([請求項3])。
本発明者らは、特許文献1に開示された容器用鋼板(表面処理金属板)について、さらに検討を行なった。その結果、PETフィルム等の樹脂をラミネートした後にレトルト処理を行なった際に、樹脂であるフィルムに対する密着性(以下「樹脂密着性」ともいう)が不十分となる場合があることが分かった。
また、本発明者らは、容器用鋼板にエポキシフェノール系塗料による塗膜を形成した後、所定条件下でトマトジュースに浸漬すると、塗膜が剥離したり錆が発生したりする等、耐食性に劣る場合があることが分かった。
(1)鋼板の表面の少なくとも一部を覆うSn層を含むめっき層を有するめっき鋼板と、上記めっき鋼板の上記めっき層側の表面上に配置された皮膜とを有する容器用鋼板であって、上記皮膜が、Zr、Tiおよびシリカを含有し、上記皮膜は、上記めっき鋼板の片面あたりのZr換算の付着量が1~40mg/m2であり、上記めっき鋼板の片面あたりのTi換算の付着量が0.5mg/m2超10mg/m2未満であり、上記めっき鋼板の片面あたりのSi換算の付着量が1~40mg/m2である、容器用鋼板。
(2)上記皮膜は、上記めっき鋼板の片面あたりのTi換算の付着量が3mg/m2超10mg/m2未満である、上記(1)に記載の容器用鋼板。
(3)上記皮膜の上記めっき鋼板側とは反対の最表面におけるTiとZrとの原子比(Ti/Zr)が0.05~2.0であり、SiとZrとの原子比(Si/Zr)が0.1~3.0である、上記(1)または(2)に記載の容器用鋼板。
(4)上記めっき層が、さらに、Ni層、Ni-Fe合金層、Fe-Sn合金層およびFe-Sn-Ni合金層からなる群から選ばれる少なくとも1層を含む、上記(1)~(3)のいずれかに記載の容器用鋼板。
本発明の容器用鋼板は、めっき鋼板と、めっき鋼板のめっき層側の表面上に配置された皮膜とを有する。そして、この皮膜が、ZrおよびTiを特定量で含有し、さらに、シリカを特定量で含有することで、樹脂密着性および耐食性が優れる。
めっき鋼板は、鋼板と、鋼板の表面の少なくとも一部を覆うめっき層とを有し、めっき層は、少なくともSn層を含む。以下に、鋼板およびめっき層の態様について詳述する。
鋼板の種類は特に制限されるものではなく、通常、容器材料として使用される鋼板(例えば、低炭素鋼板、極低炭素鋼板)を用いることができる。この鋼板の製造方法、材質なども特に規制されるものではなく、通常の鋼片製造工程から熱間圧延、酸洗、冷間圧延、焼鈍、調質圧延等の工程を経て製造される。
Ni含有層としてはニッケルが含まれていればよく、例えば、Niめっき層、Ni-Fe合金層などが挙げられる。
鋼板にNi含有層を付与する方法は特に制限されず、例えば、公知の電気めっきなどの方法が挙げられる。また、Ni含有層としてNi-Fe合金層を付与する場合、電気めっきなどにより鋼板表面上にNi付与後、焼鈍することにより、Ni拡散層を配位させ、Ni-Fe合金層を形成することができる。
Ni含有層中のNi量は特に制限されず、片面当たりのNi換算量として50~2000mg/m2が好ましい。上記範囲内であれば、コスト面でも有利となる。
めっき鋼板は、鋼板表面上の少なくとも一部に、Sn層を含むめっき層を有する。該めっき層は鋼板の少なくとも片面に設けられていればよく、両面に設けられていてもよい。
めっき層のめっき鋼板片面当たりのSn付着量は、0.1~15.0g/m2が好ましい。Sn付着量が上記範囲内であれば、容器用鋼板の耐食性がより優れ、なかでも、0.2~15.0g/m2が好ましく、加工性が優れる点で、1.0~15.0g/m2がさらに好ましい。
また、めっき層としては、Ni含有層を表面に有する鋼板に対してSnめっきを行い、さらに通電加熱などにより錫を加熱溶融させ、Sn層の最下層(Sn層/鋼板界面)にFe-Sn-Ni合金層、Fe-Sn合金層などが一部形成されためっき層も含む。
なお、本発明においては、上述したNi含有層(Ni層、Ni-Fe合金層)も、めっき鋼板のめっき層に含まれるものとする。
例えば、フェノールスルフォン酸Snめっき浴、メタンスルフォン酸Snめっき浴、またはハロゲン系Snめっき浴を用い、片面あたり付着量が所定量(例えば、2.8g/m2)となるように鋼板表面にSnを電気めっきした後、Snの融点(231.9℃)以上の温度で加熱溶融処理を行って、Sn単体のめっき層(Sn層)の最下層(Sn層/鋼板界面)にFe-Sn合金層を形成しためっき層を製造できる。加熱溶融処理を省略した場合、Sn単体のめっき層(Sn層)を製造できる。
皮膜は、上述しためっき鋼板のめっき層側の表面上に配置される。
皮膜は、その成分として、Zr、Tiおよびシリカを含有する。まず、以下に各成分に関して詳述し、その後該皮膜の形成方法について詳述する。
皮膜は、Zr(ジルコニウム元素)を含有し、めっき鋼板の片面あたりのZr換算の付着量(以下、「Zr付着量」ともいう)が1~40g/m2である。Zr付着量が上記範囲内であれば、容器用鋼板の樹脂密着性および耐食性が優れる。なかでも、コストパフォーマンスが優れるという理由から、1~25mg/m2が好ましい。
Zr付着量が1mg/m2未満であると樹脂密着性および耐食性が劣る。なお、Zr付着量が40.0mg/m2を超えても性能上の問題はないが、付着量確保のための処理液コスト増加および高電流密度化によるコスト増加につながる。
Ti付着量が0.5mg/m2以下であると、樹脂密着性が劣る。なお、Ti付着量が10mg/m2以上であっても性能上の問題はないが、付着量確保のための処理液コスト増加および高電流密度化によるコスト増加につながる。
なお、組成式SiO2で表されるシリカには、不定形な形状のものと球状のものとが存在するが、皮膜に含まれるシリカとしては、球状シリカであるのが好ましい。後述する処理液中のSi成分として、球状シリカが分散したコロイダルシリカを用いることで、この球状シリカが形状を維持したまま皮膜中に含まれると考えられる。このとき、皮膜に含まれるシリカが球状であることは、例えば、皮膜の断面を収束イオンビーム(FIB)加工により露出させ、透過型電子顕微鏡(TEM)観察することにより確認できる。
Si付着量が1mg/m2未満であると、樹脂密着性が劣る。また、Si付着量が40mg/m2を超えると、皮膜内で凝集破壊が発生して樹脂密着性を低下させる。
なお、皮膜中のZrは、例えば、酸化ジルコニウム、水酸化ジルコニウム、フッ化ジルコニウム、リン酸ジルコニウム、またはこれらの複合化合物などのジルコニウム化合物として含まれる。上記Zr付着量とは、これらジルコニウム化合物のZr換算量を意味する。
皮膜中のTiは、例えば、リン酸チタン、チタン水和酸化物、またはこれらの複合化合物などのチタン化合物として含まれる。上記Ti付着量とは、これらチタン化合物のTi換算量を意味する。
皮膜の好適態様として、皮膜の最表面(めっき鋼板側とは反対側の最表面)におけるTiとZrとの原子比(Ti/Zr)が0.05~2.0であり、SiとZrとの原子比(Si/Zr)が0.1~3.0である態様が挙げられる。この態様であれば、容器用鋼板の樹脂密着性がより優れる。
XPS分析としては、例えば、以下のような条件が挙げられる。
装置: 島津/KRATOS社製 AXIS-HS
X線源: モノクロ AlKα線(hv=1486.6eV)
測定領域: Hybridモード 250×500(μm)
上述した本発明の容器用鋼板を製造する方法としては、特に限定されないが、後述する処理液(以下、「本発明の処理液」ともいう)中にめっき鋼板を浸漬する、または、本発明の処理液中に浸漬しためっき鋼板に陰極電解処理を施すことにより、上述した皮膜を形成する皮膜形成工程を少なくとも備える方法(以下、「本発明の製造方法」ともいう)であるのが好ましい。
以下、本発明の製造方法について説明を行い、この説明の中で、併せて本発明の処理液についても説明する。
皮膜形成工程は、めっき鋼板のめっき層側の表面上に、上述した皮膜を形成する工程であって、後述する本発明の処理液中にめっき鋼板を浸漬する(浸漬処理)、または、浸漬した鋼板に陰極電解処理を施す工程である。陰極電解処理は、浸漬処理よりも、より高速に、均一な皮膜を得ることができるという理由から好ましい。なお、陰極電解処理と陽極電解処理とを交互に行う交番電解を実施してもよい。
以下に、使用される本発明の処理液、陰極電解処理の条件などについて詳述する。
本発明の処理液は、上記皮膜にZr(ジルコニウム元素)を供給するZr供給源としてZr成分(Zr化合物)を含有する。
本発明の処理液が含有するZr化合物としては、例えば、六フッ化ジルコン酸および/またはその塩(例えば、カリウム、アンモニウム等)、オキシ酢酸ジルコニウム、オキシ硝酸ジルコニウム等が挙げられる。なお、六フッ化ジルコン酸は、ジルコンフッ化水素酸とも呼ばれる。オキシ酢酸ジルコニウム〔ZrO(CH3COO)2〕は、酢酸ジルコニルとも呼ばれる。オキシ硝酸ジルコニウム〔ZrO(NO3)2〕は、硝酸ジルコニルとも呼ばれる。
本発明の処理液におけるZr化合物の含有量は、0.3~10.0g/Lが好ましく、0.5~4.0g/Lがより好ましい。
本発明の処理液が含有するTi化合物としては、例えば、チタンラクテート、六フッ化チタン酸および/またはその塩(例えば、カリウム、アンモニウム等)、チタンアルコキシド、シュウ酸チタニルアンモニウム、シュウ酸チタニルカリウム2水和物、硫酸チタン等が挙げられる。なお、チタンラクテート〔Ti(OH)2[OCH(CH3)COOH]2〕は、ジヒドロキシビス(ラクタト)チタンとも呼ばれ、本発明では、そのアンモニウム塩(モノアンモニウム塩、ジアンモニウム塩)をも含むものとする。また、六フッ化チタン酸は、チタンフッ化水素酸とも呼ばれる。
本発明の処理液におけるTi化合物の含有量は、0.1~10g/Lが好ましく、0.2~1.0g/Lがより好ましい。
ここで、コロイダルシリカとは、SiO2を基本単位とする球状シリカが水等の分散媒に分散した分散系である。分散媒の量は特に限定されないが、通常、コロイダルシリカ中の固形分量としては、例えば20~30質量%が挙げられる。
一方、コロイダルシリカの平均粒子径の下限値は特に限定されず、例えば、一般に流通している5nm以上が好ましい。
平均粒子径はBET法(吸着法による比表面積から換算)により測定できる。また、電子顕微鏡写真から実測した平均値で代用することも可能である。
本発明の処理液におけるSi化合物の含有量としては、コロイダルシリカの場合、0.01~5.0g/Lが好ましく、0.1~4.0g/Lがより好ましい。
本発明の処理液が上記電導助剤を含むことにより、上記皮膜を形成できるラインスピードを高速化できる。すなわち、高速操業性に優れる。これは、電導助剤を含むことにより、処理液の電気伝導性すなわち液抵抗が低下・改善し、高速化に伴う高電流を通電することが容易になるためと考えられる。
上記電導助剤は、実質的には、上記陰イオンと上記陽イオンとがイオン結合した塩(例えば、硝酸アンモニウム、硝酸カリウム、硝酸ナトリウム等)として、本発明の処理液に含まれ、その含有量としては、高速操業性がより優れるという理由から、0.1~10.0g/Lが好ましく、0.5~5.0g/Lがより好ましい。
pHの調整には公知の酸成分(例えば、リン酸、硫酸)・アルカリ成分(例えば、水酸化ナトリウム、アンモニア水)を使用することができる。
また、陰極電解処理の際の電気量密度は、0.20~15C/dm2が好ましく、0.40~10C/dm2がより好ましい。
乾燥処理の際の温度としては、100℃以下が好ましい。下限は特に限定されないが、通常室温程度である。
以下の2つの方法[(K-1)および(K-2)]によって、めっき鋼板を製造した。
(K-1)
板厚0.22mmの鋼板(T4原板)について電解脱脂と酸洗を行い、その後Snめっきを施した。引き続き、錫の融点以上の温度で加熱溶融処理を施し、第2表に示す片面当たりのSn付着量のめっき層をT4原板の両面に形成した。このようにして、下層側から順に、Fe-Sn合金層/Sn層からなるめっき層を形成した。
(K-2)
板厚0.22mmの鋼板(T4原板)を電解脱脂し、ワット浴を用いて第2表に示す片面当たりのNi付着量でニッケルめっき層を両面に形成後、10vol.%H2+90vol.%N2雰囲気中にて700℃で焼鈍してニッケルめっきを拡散浸透させることによりNi-Fe合金層(Ni含有層)(第2表にNi付着量を示す)を両面に形成した。
引き続き、上記表層にNi含有層を有する鋼板を、Snめっき浴を用い、第2表中に示す片面当たりのSn付着量でSn層を両面に形成後、Snの融点以上で加熱溶融処理を施し、めっき層をT4原板の両面に形成した。このようにして、下層側から順に、Ni-Fe合金層/Fe-Sn-Ni合金層/Sn層からなるめっき層を形成した。
鋼板を、第1表に示す組成の処理液(溶媒:水)を用い、第2表に示す浴温、電解条件(電流密度、通電時間)で陰極電解処理を施した。その後、得られた鋼板を水洗して、ブロアを用いて室温で乾燥を行い、皮膜を両面に形成した。
また、第1表に示すオルトリン酸としては、リン酸濃度が85質量%のものを用いた。
なお、皮膜のTi付着量、Zr付着量およびSi付着量ならびに原子比は、上述の方法により測定した。
作製した容器用鋼板の両面に、厚さ25μm、共重合比12mol%のイソフタル酸共重合ポリエチレンテレフタラートフィルムをラミネートして、ラミネート鋼板を作製した。ラミネートは、210℃に加熱した鋼板とフィルムを一対のゴムロールで挟んでフィルムを鋼板に融着させ、ゴムロール通過後1sec以内に水冷して行った。このとき、鋼板の送り速度は40m/min、ゴムロールのニップ長は17mmであった。ここで、ニップ長とは、ゴムロールと鋼板が接する部分の搬送方向の長さのことである。そして、作製したラミネート鋼板について、次の樹脂密着性の評価を行った。
樹脂密着性の評価は、温度150℃、相対湿度100%のレトルト雰囲気における180度ピール試験により行った。180度ピール試験とは、図1(a)に示すようなフィルム2を残して鋼板1の一部3を切り取った試験片(サイズ:30mm×100mm)を用い、図1(b)に示すように、試験片の一端に重り4(150g)を付けてフィルム2側に180度折り返して30min間放置して行うフィルム剥離試験のことである。そして、図1(c)に示す剥離長5を測定し、次のように樹脂密着性を評価し、◎または○であれば樹脂密着性が良好であるとした。
◎:剥離長が40mm未満
○:剥離長が40mm以上50mm未満
△:剥離長が50mm以上70mm未満
×:剥離長が70mm以上
作製した容器用鋼板の両面に、付着量が50mg/dm2となるようにエポキシフェノール系塗料を塗布した後、210℃で10分間の焼付を行ない塗膜を形成した。次いで、市販のトマトジュースを入れたビーカーに、50℃で10日間浸漬させて、塗膜の剥離および錆の発生の有無を目視観察して、次のように評価し、○であれば耐食性が良好であるとした。
○:塗膜剥離および錆発生なし(クロメート処理材同等)
△:塗膜剥離なし、わずかに錆発生
×:塗膜剥離あり、顕著に錆発生
これに対して、Zr付着量が1mg/m2未満である比較例1,2,8および9は、樹脂密着性および耐食性が劣っていた。
また、Ti付着量が0.5mg/m2以下である比較例3,4,10および11は、樹脂密着性が劣っていた。
また、Si付着量が1mg/m2未満または40mg/m2を超える比較例5~7および12~14は、樹脂密着性が劣っていた。
2 フィルム
3 鋼板の切り取った部位
4 重り
5 剥離長
Claims (4)
- 鋼板の表面の少なくとも一部を覆うSn層を含むめっき層を有するめっき鋼板と、前記めっき鋼板の前記めっき層側の表面上に配置された皮膜とを有する容器用鋼板であって、
前記皮膜が、Zr、Tiおよびシリカを含有し、
前記皮膜は、前記めっき鋼板の片面あたりのZr換算の付着量が1~40mg/m2であり、前記めっき鋼板の片面あたりのTi換算の付着量が0.5mg/m2超10mg/m2未満であり、前記めっき鋼板の片面あたりのSi換算の付着量が1~40mg/m2である、容器用鋼板。 - 前記皮膜は、前記めっき鋼板の片面あたりのTi換算の付着量が3mg/m2超10mg/m2未満である、請求項1に記載の容器用鋼板。
- 前記皮膜の前記めっき鋼板側とは反対の最表面におけるTiとZrとの原子比(Ti/Zr)が0.05~2.0であり、SiとZrとの原子比(Si/Zr)が0.1~3.0である、請求項1または2に記載の容器用鋼板。
- 前記めっき層が、さらに、Ni層、Ni-Fe合金層、Fe-Sn合金層およびFe-Sn-Ni合金層からなる群から選ばれる少なくとも1層を含む、請求項1~3のいずれか1項に記載の容器用鋼板。
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JP2014555639A JP5773093B2 (ja) | 2013-07-24 | 2014-07-16 | 容器用鋼板 |
CN201480041403.9A CN105408526B (zh) | 2013-07-24 | 2014-07-16 | 容器用钢板 |
KR1020167001759A KR101745978B1 (ko) | 2013-07-24 | 2014-07-16 | 용기용 강판 |
MYPI2016700222A MY182555A (en) | 2013-07-24 | 2014-07-16 | Steel sheet for container |
PH12016500160A PH12016500160B1 (en) | 2013-07-24 | 2016-01-22 | Steel sheet for container |
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US10479550B2 (en) | 2012-03-26 | 2019-11-19 | Kraft Foods R & D, Inc. | Packaging and method of opening |
US10507970B2 (en) | 2013-03-07 | 2019-12-17 | Mondelez Uk R&D Limited | Confectionery packaging and method of opening |
US10513388B2 (en) | 2013-03-07 | 2019-12-24 | Mondelez Uk R&D Limited | Packaging and method of opening |
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KR101745978B1 (ko) | 2017-06-12 |
CN105408526B (zh) | 2018-04-24 |
JPWO2015012176A1 (ja) | 2017-03-02 |
PH12016500160B1 (en) | 2016-04-25 |
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