WO2024090569A1 - 表面処理鋼板および電池容器 - Google Patents

表面処理鋼板および電池容器 Download PDF

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Publication number
WO2024090569A1
WO2024090569A1 PCT/JP2023/038957 JP2023038957W WO2024090569A1 WO 2024090569 A1 WO2024090569 A1 WO 2024090569A1 JP 2023038957 W JP2023038957 W JP 2023038957W WO 2024090569 A1 WO2024090569 A1 WO 2024090569A1
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Prior art keywords
steel sheet
diffusion layer
intensity
treated steel
diffraction
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English (en)
French (fr)
Japanese (ja)
Inventor
貴弘 渡邉
香織 上原
裕介 橋本
悦郎 堤
慎一郎 堀江
大輔 松重
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Toyo Kohan Co Ltd
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Toyo Kohan Co Ltd
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Priority to KR1020257016160A priority Critical patent/KR20250097855A/ko
Priority to EP23882771.1A priority patent/EP4610408A1/en
Priority to JP2024553260A priority patent/JPWO2024090569A1/ja
Priority to CN202380088772.2A priority patent/CN120418482A/zh
Publication of WO2024090569A1 publication Critical patent/WO2024090569A1/ja
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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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/131—Primary casings; Jackets or wrappings characterised by physical properties, e.g. gas permeability, size or heat resistance
    • H01M50/133—Thickness
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
    • 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
    • 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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/117—Inorganic material
    • H01M50/119—Metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
    • H01M50/1245—Primary casings; Jackets or wrappings characterised by the material having a layered structure characterised by the external coating on the casing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
    • H01M50/126—Primary casings; Jackets or wrappings characterised by the material having a layered structure comprising three or more layers
    • H01M50/128—Primary casings; Jackets or wrappings characterised by the material having a layered structure comprising three or more layers with two or more layers of only inorganic material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a surface-treated steel sheet and a battery container.
  • Patent Document 1 discloses a surface-treated steel sheet for battery containers that has an iron-nickel diffusion layer formed by forming a nickel plating layer on the steel sheet and then carrying out a thermal diffusion process to prevent pitting corrosion and leakage, and in which the ratio of Ni to Fe in the outermost layer is controlled.
  • the object of the present invention is to provide a surface-treated steel sheet with an Fe-Ni diffusion layer that exhibits excellent electrolyte resistance during overdischarge.
  • the above-mentioned objective can be achieved by appropriately controlling the ratio of maximum diffraction intensities in a specified range of diffraction angles obtained from thin-film X-ray diffraction measurements in a surface-treated steel sheet having an Fe-Ni diffusion layer formed on the outermost surface of at least one side of the steel sheet, and thus completed the present invention.
  • a surface-treated steel sheet comprising a steel sheet and an Fe—Ni diffusion layer formed on at least one surface of the steel sheet, wherein a ratio I B /I A of a maximum diffraction intensity I A at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less, obtained from a thin-film X-ray diffraction measurement of a surface of the Fe—Ni diffusion layer, to a maximum diffraction intensity I B at a diffraction angle 2 ⁇ of 44.51° or more and 45.00° or less, satisfies 0.01 ⁇ I B / I A ⁇ 0.37.
  • a half-value width B of a maximum diffraction intensity I A at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less obtained from a thin film X-ray diffraction measurement of a surface of the Fe—Ni diffusion layer is 0.35 or more.
  • a surface-treated steel sheet according to aspect 1 or 2 in which the thickness of the Fe-Ni diffusion layer is 0.5 to 4 ⁇ m.
  • the surface-treated steel sheet according to any one of the first to third aspects, wherein the amount of Ni deposited on the steel sheet is 1.78 to 8.9 g/ m2 .
  • a battery container which is formed by molding the surface-treated steel sheet according to any one of aspects 1 to 5 so that the surface on which the Fe-Ni diffusion layer is formed is the inner surface of the battery container.
  • the present invention makes it possible to suppress the dissolution of iron into the electrolyte during overdischarge, and to provide a surface-treated steel sheet with excellent electrolyte resistance.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a surface-treated steel sheet according to an embodiment of the present invention.
  • FIG. 2 is a graph showing diffraction peaks obtained by subjecting the surface-treated steel sheet of Example 1 to thin-film X-ray diffraction measurement.
  • FIG. 3 is a graph showing diffraction peaks obtained by subjecting the surface-treated steel sheet in Example 3 to thin-film X-ray diffraction measurement.
  • FIG. 4 is a chart obtained by high-frequency glow discharge optical emission spectrometry of a standard sample.
  • FIG. 5 is another example of a chart obtained by high-frequency glow discharge optical emission spectrometry of a standard sample.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a surface-treated steel sheet according to an embodiment of the present invention.
  • FIG. 2 is a graph showing diffraction peaks obtained by subjecting the surface-treated steel sheet of Example 1 to thin-film X-ray diffraction measurement.
  • FIG. 6 is a chart obtained by high-frequency glow discharge optical emission spectrometry of the surface-treated steel sheet of Example 4.
  • FIG. 7 is a diagram showing a method for calculating a thermal history Y in a thermal diffusion treatment of a steel sheet having a Ni plating layer formed thereon in an embodiment of the present invention.
  • FIG. 8 is a schematic diagram of a measuring jig used for evaluating the electrolyte resistance of a surface-treated steel sheet by the LSV method.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a surface-treated steel sheet in this embodiment.
  • the surface-treated steel sheet in this embodiment comprises a steel sheet and an Fe-Ni diffusion layer formed on at least one surface of the steel sheet.
  • the steel sheet of this embodiment is not particularly limited as long as it has excellent formability, but for example, low carbon aluminum killed steel (carbon content 0.01 to 0.15 wt%), ultra-low carbon steel with a carbon content of less than 0.01 wt%, or non-aging ultra-low carbon steel obtained by adding Ti, Nb, or the like to ultra-low carbon steel can be used.
  • hot rolled sheets of these steels are pickled to remove surface scale (oxide film), then cold rolled, electrolytically cleaned, annealed, and temper rolled, or those that are cold rolled, electrolytically cleaned, and then temper rolled without annealing can also be used.
  • the thickness of the steel plate may be appropriately selected depending on the application of the surface-treated steel plate, and is not particularly limited. From the viewpoint of reducing manufacturing costs, the thickness of the steel plate is preferably 1.5 mm or less, more preferably 1.25 mm or less, and even more preferably 0.9 mm or less. From the viewpoint of improving the mechanical properties of the surface-treated steel plate, the thickness of the steel plate is preferably 0.03 mm or more, more preferably 0.1 mm or more, even more preferably 0.15 mm or more, and particularly preferably 0.2 mm or more. A micrometer is preferably used to measure the thickness of the steel plate. The thickness of the steel plate may also be measured by cross-sectional observation using an optical microscope or a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • the surface-treated steel sheet of this embodiment includes an Fe—Ni diffusion layer on the steel sheet.
  • the Fe—Ni diffusion layer is formed by forming a Ni plating layer on the steel sheet, and then performing a thermal diffusion treatment on the steel sheet on which the Ni plating layer has been formed, thereby thermally diffusing iron (Fe) constituting the steel sheet and nickel (Ni) constituting the Ni plating layer.
  • the diffraction intensity at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less includes peaks of Fe 0.64 Ni 0.36 , FeNi, and FeNi 3.
  • the diffraction intensity at a diffraction angle 2 ⁇ of 44.51° or more and 45.00° or less includes peaks of Fe 0.95 Ni 0.05 .
  • the ratio I B /I A of the maximum diffraction intensity I A to the maximum diffraction intensity I B is the ratio of the diffraction intensity originating from Fe 0.64 Ni 0.36 , FeNi, and FeNi 3 in the Fe-Ni diffusion layer to the diffraction intensity originating from Fe 0.95 Ni 0.05 in the Fe-Ni diffusion layer, and is an index of the relative abundance ratio.
  • the respective crystal structures and diffraction peaks are based on the following database.
  • the ratio of maximum diffraction intensities IB / IA is 0.01 ⁇ IB / IA ⁇ 0.37, preferably 0.01 ⁇ IB / IA ⁇ 0.3, more preferably 0.02 ⁇ IB / IA ⁇ 0.15, even more preferably 0.036 ⁇ IB / IA ⁇ 0.15, and particularly preferably 0.036 ⁇ IB / IA ⁇ 0.094.
  • the penetration depth of X-rays into the sample is theoretically 0.11 ⁇ m or less, and compared with X-ray diffraction by the focusing method, in which the penetration depth is several ⁇ m to several tens of ⁇ m, the crystalline state of the portion closer to the surface of the sample can be measured.
  • the ratio I B /I A of the maximum diffraction intensity is 0.01 ⁇ I B /I A ⁇ 0.37, so that the state of the Fe-Ni alloy on the outermost surface is appropriately controlled, and the electrolyte resistance during overdischarge is high, and the occurrence of corrosion due to the elution of iron can be suppressed.
  • the reason why the electrolyte resistance during overdischarge is high is not clear, but the present inventors speculate as follows. In the course of developing nickel-plated steel sheets for batteries, the present inventors have found a problem that while there is no problem with electrolyte resistance at the potential during normal charging and discharging of lithium-ion batteries, the electrolyte resistance during overdischarge may decrease.
  • the maximum diffraction intensity I A and the maximum diffraction intensity I B can be obtained by the following method.
  • a diffraction pattern is obtained by thin-film X-ray diffraction method using an X-ray diffractometer for the surface of the Fe-Ni diffusion layer of the surface-treated steel sheet.
  • the half-width B is preferably 0.35 or more, more preferably 0.40 or more, and even more preferably 0.43 or more.
  • the upper limit of the half-width B is not particularly limited, but is 1.3 or less.
  • the alloy is formed from only one of these alloys, or when one of the alloys is dominant, the diffraction peak becomes sharp and the half-width B becomes narrow (see FIG. 2).
  • FIG. 2 is a graph showing diffraction peaks obtained by subjecting the surface-treated steel sheet in Example 1 to thin-film X-ray diffraction measurement
  • FIG. 3 is a graph showing diffraction peaks obtained by subjecting the surface-treated steel sheet in Example 3 to thin-film X-ray diffraction measurement.
  • the thickness of the Fe-Ni diffusion layer is preferably 4 ⁇ m or less, more preferably 3 ⁇ m or less, even more preferably 2.5 ⁇ m or less, and particularly preferably 2.0 ⁇ m or less. Furthermore, from the viewpoint of improving the electrolyte resistance of the surface-treated steel sheet during overdischarge, the thickness of the Fe-Ni diffusion layer is preferably 0.5 ⁇ m or more, more preferably 1 ⁇ m or more, and even more preferably 1.2 ⁇ m or more.
  • the thickness of the Fe-Ni diffusion layer can be determined by continuously measuring the changes in Fe intensity and Ni intensity in the depth direction from the outermost surface of the surface-treated steel sheet using a high-frequency glow discharge optical emission spectroscopy (GDS) device.
  • GDS glow discharge optical emission spectroscopy
  • the Fe ratio on the surface of the Fe-Ni diffusion layer can also be determined using a high-frequency glow discharge optical emission spectroscopy device.
  • the thickness of the Fe--Ni diffusion layer and the Fe ratio on the surface of the Fe--Ni diffusion layer can be determined by the following steps.
  • Measurement step 1 A high-frequency glow discharge optical emission spectroscopy is performed on the standard sample to obtain intensity data for each etching time, and the saturation value of the Fe intensity, the maximum value of the Ni intensity, and the etching rate of Ni are confirmed. If the saturation value of the Fe intensity and the maximum value of the Ni intensity are not the same value in the measurement data of the standard sample obtained in this manner, correction coefficients are obtained for Fe and Ni such that the saturation value of the Fe intensity and the maximum value of the Ni intensity become the same value (for example, 10), and all the intensity data are corrected.
  • Measurement step 2 Analyze the target test piece of the surface-treated steel sheet under the same analytical conditions as in measurement step 1 to obtain strength data for each etching time. If a correction coefficient was applied in measurement step 1, the target test piece data is also similarly multiplied by the correction coefficient, and the strength data obtained is used to proceed to the subsequent steps.
  • Ni ratio Ni strength / (Fe strength + Ni strength)
  • Measurement step 4 In the chart obtained from the data obtained in measurement step 3, the point where the Ni ratio first reaches a minimum value is determined as the outermost surface.
  • Measurement step 5 The outermost surface determined in measurement step 4 is taken as the starting point, and the point where the Ni intensity in the data is 10% of the maximum Ni intensity is taken as the interface point, the difference in etching time between the starting point and the interface point is calculated, and the etching depth calculated by multiplying the difference in etching time by the etching rate is the thickness of the Fe-Ni diffusion layer.
  • the interface point refers to the interface between the Fe-Ni diffusion layer and the steel sheet.
  • Measurement step 6 The Fe ratio at the outermost surface determined in measurement step 4 is the Fe ratio at the surface of the Fe--Ni diffusion layer.
  • the measurement step 1 will be explained.
  • high-frequency glow discharge optical emission spectroscopy is performed on the standard sample to obtain intensity data for each etching time, and the saturation value of the Fe intensity, the maximum value of the Ni intensity, and the etching rate of Ni are confirmed.
  • a standard sample is prepared consisting of a Ni-plated steel sheet that has not been subjected to heat treatment and whose plating layer thickness (or deposition amount) is known.
  • a Ni-plated steel sheet is prepared by applying a non-glossy Ni plating of 1.1 ⁇ m to a low-carbon steel sheet of 0.3 mm thickness.
  • the Fe intensity and Ni intensity in the Ni-plated steel sheet are measured using a high-frequency glow discharge optical emission spectroscopy analyzer until the Fe intensity is saturated.
  • a chart like that shown in Figure 4 can be obtained.
  • Figure 4 is a chart obtained by high-frequency glow discharge optical emission spectroscopy of the standard sample.
  • the vertical axis indicates the Fe intensity and Ni intensity
  • the horizontal axis indicates the measurement time when the measurement is performed in the depth direction from the surface of the Ni-plated steel sheet (the surface on which the Ni plating is formed) using a high-frequency glow discharge optical emission spectroscopy analyzer.
  • the saturation value of Fe strength is determined from the resulting chart.
  • the saturation value of Fe strength can be determined from the change in Fe strength per second, that is, the time rate of change of Fe strength (Fe strength change/second).
  • the time rate of change of Fe strength increases rapidly when Fe is detected after measurement begins, and decreases after passing the maximum value, stabilizing at approximately zero.
  • the value of Fe strength when the time rate of change of Fe strength stabilizes at approximately zero is the saturation value of Fe strength.
  • the saturation value of Fe strength is the value when the time rate of change of Fe strength is 0.02 or less.
  • the maximum Ni intensity is found.
  • the Ni intensity of 10 at a measurement time of 9.9 seconds is the maximum Ni intensity.
  • the saturation value of Fe intensity and the maximum Ni intensity may not be the same value as in Figure 5, depending on the GDS measurement conditions.
  • a correction coefficient is found to be multiplied by the Fe intensity or Ni intensity so that the saturation value of Fe intensity and the maximum Ni intensity are the same value, and the subsequent steps are carried out.
  • the saturation value of Fe intensity of 10 is used as the standard, and a correction coefficient is found to be multiplied by the Ni intensity so that the maximum Ni intensity after correction is 10.
  • Figure 5 is another example of a chart obtained by radio frequency glow discharge optical emission spectroscopy analysis of a standard sample.
  • the etching rate of Ni is calculated.
  • the etching rate can be calculated based on the thickness of the Ni plating and the etching time.
  • the etching time since in GDS analysis Ni is considered to be present up to the point where the Ni intensity is 10% of the maximum Ni intensity, the etching time is set to the time from the start of measurement to the point where the Ni intensity is 10% of the maximum Ni intensity in the standard sample.
  • the etching rate can be calculated by dividing the Ni plating thickness of 1.1 ⁇ m by the time from the start of measurement to the time where the Ni intensity is 10% of the maximum Ni intensity.
  • the etching rates of Ni and Fe are approximately the same, so in the present invention, the thickness of the Fe-Ni diffusion layer is determined using the Ni etching rate calculated as described above.
  • the measurement step 2 will be described.
  • the surface-treated steel sheet of this embodiment is subjected to GDS analysis.
  • the surface-treated steel sheet of this embodiment is used as the target test piece, and is measured under the same conditions as in step 1 above using GDS to obtain the Fe intensity and Ni intensity in the surface-treated steel sheet.
  • a correction coefficient is applied in the measurement step 1
  • the data of the target test piece is also corrected with the same correction coefficient used in the standard sample, and the subsequent steps are performed using the obtained intensity data.
  • the intensity data obtained does not have a zero Fe intensity on the surface, as shown in FIG. 6.
  • FIG. 6 is a chart obtained by high-frequency glow discharge optical emission spectroscopy of the surface-treated steel sheet of Example 4. In FIG.
  • the vertical axis indicates Fe intensity and Ni intensity
  • the horizontal axis indicates the measurement time when the surface of the surface-treated steel sheet (the surface on which the Fe-Ni diffusion layer is formed) is measured in the depth direction using a high-frequency glow discharge optical emission spectroscopy analyzer.
  • whether the surface of the surface-treated steel sheet is an Fe-Ni diffusion layer can be determined by whether the Fe intensity of the surface in the surface-treated steel sheet exceeds 10% of the saturation value of the Fe intensity. If the Fe intensity of the outermost surface exceeds 10%, the surface can be determined to be an Fe-Ni diffusion layer, and conversely, if it does not exceed 10%, it is determined that a Ni layer exists on the Fe-Ni diffusion layer.
  • Measurement step 3 the Fe ratio and Ni ratio at each depth position of the Fe-Ni diffusion layer are obtained.
  • the Fe ratio at each time i.e., at each depth position, can be obtained by calculating the percentage of the Fe and Ni intensity values (corrected intensity values if a correction factor is used) at each time. That is, the Fe ratio and Ni ratio can be obtained by the following formula.
  • Fe ratio Fe strength / (Fe strength + Ni strength) x 100
  • Ni ratio Ni strength / (Fe strength + Ni strength) x 100
  • Measurement step 4 the depth position of the outermost surface of the Fe-Ni diffusion layer is defined.
  • the point (depth position) where the Fe ratio is at its minimum is defined as the outermost surface of the Fe-Ni diffusion layer. Under normal measurement conditions, this minimum value of the Fe ratio appears between 0 and 5 seconds into the measurement time.
  • Measurement step 5 the thickness of the Fe-Ni diffusion layer is found by determining the etching depth from the outermost surface to the boundary between the Fe-Ni diffusion layer and the steel plate.
  • the position of the outermost surface is the position defined in measurement step 4.
  • the boundary between the Fe-Ni diffusion layer and the steel plate is the point (depth position) where the Ni intensity of the target sample is 10% of the maximum Ni intensity of the standard sample. In other words, if the maximum Ni intensity of the standard sample in step 1 is 10, the point where the Ni intensity of the target sample found in step 2 is 1 is the boundary between the Fe-Ni diffusion layer and the steel plate.
  • the point where the Ni intensity is 1 is naturally located deeper than the outermost surface, and so the point where the Ni intensity is 1 at the start of measurement (a depth position smaller than the depth position at the maximum Ni intensity) is excluded.
  • the difference between the etching time from depth position 0 (i.e., measurement time 0) to the outermost surface and the etching time from depth position 0 to the boundary between the Fe-Ni diffusion layer and the steel plate is calculated, and the thickness of the Fe-Ni diffusion layer is calculated by multiplying this difference by the etching rate calculated in measurement step 1.
  • a Ni-plated steel sheet that has not been subjected to thermal diffusion treatment and has a known Ni plating thickness can be measured using a high-frequency glow discharge optical emission spectrometer to measure the depth time (measurement time using a high-frequency glow discharge optical emission spectrometer) and the actual thickness, and the measured value can be used to convert the thickness of the Fe-Ni diffusion layer of the surface-treated steel sheet of this embodiment and the thickness of the Ni plating before heat treatment.
  • the actual Ni plating thickness before heat treatment can be determined by converting the Ni adhesion amount determined by cross-sectional observation of the surface-treated steel sheet using an SEM or fluorescent X-ray analysis into a thickness using the specific gravity of Ni.
  • the measurement step 6 will now be described.
  • the Fe percentage at the outermost surface of the Fe-Ni diffusion layer is determined.
  • the Fe percentage at the outermost surface of the Fe-Ni diffusion layer can be determined as the Fe percentage at the depth position of the outermost surface determined in measurement step 4.
  • the percentage of Fe (atomic %) at the outermost surface of the Fe-Ni diffusion layer is preferably 10% or more, more preferably 20% or more, even more preferably 25% or more, and particularly preferably 30% or more, from the viewpoint of improving weldability. Also, the percentage of Fe at the outermost surface of the Fe-Ni diffusion layer is preferably 70% or less, more preferably 60% or less, and even more preferably 55% or less, from the viewpoint of rust resistance during storage before assembling a battery using the surface-treated steel sheet.
  • the Ni adhesion amount in the Fe-Ni diffusion layer is preferably 8.90 g / m 2 or less, more preferably 6.23 g / m 2 or less, and even more preferably 5.00 g / m 2 or less.
  • the Ni adhesion amount in the Fe-Ni diffusion layer is preferably 1.78 g / m 2 or more, more preferably 2.67 g / m 2 or more.
  • the Ni adhesion amount can be determined by fluorescent X-ray measurement. In fluorescent X-ray measurement, it is possible to quantitatively determine the metal elements contained in the surface treatment layer of the surface-treated steel sheet by a calibration curve method.
  • the Fe-Ni diffusion layer is formed only on one side of the steel plate, but the configuration of the surface-treated steel plate is not particularly limited thereto, and the Fe-Ni diffusion layer may be formed on at least one outermost surface of the surface-treated steel plate.
  • the Fe-Ni diffusion layer may be formed on the outermost surface of both sides of the steel plate.
  • the Fe-Ni diffusion layer may be formed on both sides of the steel plate, and a Ni layer may be formed on the Fe-Ni diffusion layer on one of the surfaces.
  • the Fe-Ni diffusion layer is formed as the outermost surface of the surface that will become the inner surface of the battery container, while the Fe-Ni diffusion layer is formed on the surface that will become the outer surface of the battery container, and the Ni layer is formed on the Fe-Ni diffusion layer.
  • the total Ni deposition amount contained in the Fe-Ni diffusion layer and the Ni layer is preferably 9.0 to 90 g/m 2 .
  • the surface-treated steel sheet in this embodiment can be manufactured as follows.
  • a Ni plating layer is formed on a steel sheet.
  • the Ni plating bath used to form the Ni plating layer may be a commonly used plating bath, i.e., a Watts bath, a sulfamic acid bath, a boron fluoride bath, a chloride bath, or the like.
  • the Ni plating layer may be formed using a Watts bath having a bath composition of 200 to 350 g/L of nickel sulfate hexahydrate, 20 to 60 g/L of nickel chloride hexahydrate, and 10 to 50 g/L of boric acid, under conditions of pH 3.0 to 5.0, bath temperature 40 to 70° C., and current density 10 to 40 A/dm 2.
  • the Ni plating layer may be formed on at least one side of the steel sheet.
  • the amount W of Ni attached to the steel sheet by forming the Ni plating layer is not particularly limited as long as an Fe-Ni diffusion layer can be formed as the outermost surface of the surface-treated steel sheet and its configuration can be controlled, but if the amount is too large, it becomes difficult to diffuse Fe to the outermost surface, and it becomes necessary to increase the heat treatment temperature or lengthen the heat treatment time in order to sufficiently diffuse Fe, which may make it difficult to set I B /I A in an appropriate range, so the amount W of Ni is preferably 8.9 g / m 2 or less, more preferably 6.23 g / m 2 or less, and even more preferably 4.45 g / m 2 or less.
  • the amount W of Ni attached is preferably 1.78 g / m 2 or more, more preferably 2.67 g / m 2 or more.
  • the Fe-Ni diffusion layer is formed on both sides of the steel sheet, it is preferable to set the amount W of Ni attached on each side within the above range.
  • Ni-plated steel sheet the steel sheet with the Ni-plated layer (hereinafter referred to as Ni-plated steel sheet) is subjected to a thermal diffusion treatment to form an Fe-Ni diffusion layer.
  • the thermal diffusion treatment may be either a continuous annealing method or a box annealing method, and is not particularly limited, but it is preferable that the heat treatment atmosphere is a non-oxidizing atmosphere or a reducing protective gas atmosphere, and when a reducing protective gas atmosphere is used, it is preferable to use a mixed gas of H2 and N2 , for example, called HNX gas.
  • the thermal diffusion treatment includes a first heating step, a second heating step, and a cooling step.
  • the first heating step is a step of heating the Ni-plated steel sheet from room temperature to the starting temperature of the second heating step (second heating start temperature) described below.
  • the heating rate in the first heating step is not particularly limited, but it is preferable to set the heating rate to be higher than the heating rate in the second heating step described below.
  • the second heating step is a step of heating from the second heating start temperature to the maximum temperature in the heating step (hereinafter referred to as the reached temperature).
  • the second heating start temperature is preferably 550°C or higher, at which the Ni in the Ni plating layer and the Fe in the steel sheet begin to diffuse actively, more preferably 600°C or higher, at which they begin to diffuse more actively, even more preferably 650°C or higher, and particularly preferably 700°C or higher.
  • the reached temperature is preferably less than 900°C, more preferably 850°C or lower, and even more preferably 820°C or lower.
  • the heating rate in the second heating step (hereinafter also referred to as the second heating rate) is preferably 4° C./sec or less, more preferably 3° C./sec or less, and further preferably 1° C./sec or less.
  • the heating rate in the second heating step is preferably 0.1° C./sec or more, and more preferably 0.2° C./sec or more.
  • the temperature difference between the final temperature and the second heating start temperature may be 10°C or more, but is preferably 30°C or more, more preferably 40°C or more. If the temperature difference is too small, the heating time (second heating time) in the second heating step may be insufficient, and the desired alloy state of the surface of the Fe-Ni diffusion layer may not be obtained.
  • the Ni deposition amount is 3.5 g/ m2 or more
  • a temperature difference of 30°C or more is preferable, more preferably 40°C or more, and even more preferably 60°C or more is preferable, so that the desired alloy state of the surface can be obtained, and a higher electrolyte resistance during overdischarge can be stably obtained.
  • the upper limit of the temperature difference is preferably 150°C or less, more preferably 120°C or less, and even more preferably 100°C or less.
  • the Ni-plated steel sheet that has been heated to the target temperature is cooled to 120°C or less.
  • the cooling rate There are no particular restrictions on the cooling rate, but from the viewpoint of preventing defects in shape and wrinkles, a rate of 1°C/sec to 20°C/sec is preferable, and a rate of 1°C/sec to 10°C/sec is more preferable.
  • FIG. 7 shows a method for calculating the thermal history Y during thermal diffusion treatment of a steel sheet on which a Ni plating layer is formed in this embodiment.
  • the thermal history Y of the Ni-plated steel sheet through the first heating step, the second heating step, and the cooling step in the thermal diffusion treatment is preferably 150,000°C ⁇ sec or less, more preferably 120,000°C ⁇ sec or less, and even more preferably 100,000°C ⁇ sec or less.
  • the total thermal history Y is preferably 15,000°C ⁇ sec or more, more preferably 35,000°C ⁇ sec or more, and even more preferably 45,000°C ⁇ sec or more.
  • the thermal history Y can be calculated by integrating the amount of change in the heating temperature and cooling temperature over time at 450°C or more. That is, the area of the shaded portion in FIG. 7 corresponds to the thermal history Y in the thermal diffusion treatment.
  • the heating rate and heating time in the first heating step, the second heating step, and the cooling step may be appropriately adjusted.
  • thermal history Y in the thermal diffusion treatment is too large, I B /I A is likely to become large and electrolyte resistance during overdischarge tends to deteriorate.
  • the thermal history Y in the thermal diffusion treatment is too small, Fe diffusion becomes insufficient and the thickness of the Fe-Ni diffusion layer becomes too thin, which may deteriorate electrolyte resistance during overdischarge, or a layer of Ni alone may remain on the outermost surface of the surface-treated steel sheet, which may deteriorate weldability when welding the battery container to an electrode lead or the like.
  • the ratio W/Y ⁇ 10 5 of the Ni deposition amount W (g/m 2 ) to the thermal history Y is preferably 20.0 or less, more preferably 10.0 or less.
  • W/Y ⁇ 10 5 exceeds 20.0, there is a possibility that Fe diffusion is insufficient and the surface cannot become an Fe—Ni diffusion layer.
  • W/Y ⁇ 10 5 is 4.5 to 10, and the ultimate temperature is less than 850° C. or the thermal history Y is less than 100,000.
  • Ni in the Ni-plated layer and Fe in the steel sheet are mutually diffused, and an Fe-Ni diffusion layer can be formed in which the crystal state of the outermost surface is appropriately controlled so that 0.01 ⁇ I B /I A ⁇ 0.37 is satisfied.
  • the reason why the formation of the Fe 0.95 Ni 0.05 alloy phase can be suppressed by heating under the above conditions is not clear, but it is considered that it is possible to suppress the movement of Fe to the outermost surface and suppress the formation of excessive Fe 0.95 Ni 0.05 by setting the thermal history Y in the temperature range of 450° C. or higher to an appropriate range for the Ni deposition amount W.
  • the I B /I A in the Fe-Ni diffusion layer can be controlled within an appropriate range.
  • the steel sheet is subjected to soaking at the highest temperature for a predetermined time, and then cooled, and in the soaking step, iron is diffused to the outermost surface by mutual diffusion.
  • the thermal diffusion treatment method of the present embodiment after the first heating, the steel sheet is not heated to the highest temperature in the first heating, and in the second heating step, heating is continued at a relatively slow heating rate, and soaking at the same temperature is not performed, and then cooling is performed.
  • the thermal diffusion treatment method of the present embodiment can more appropriately control the alloy state of the outermost surface of the Fe-Ni diffusion layer, compared to a thermal diffusion treatment method in which soaking is performed.
  • the battery container in this embodiment is obtained by forming the surface-treated steel sheet so that the surface on which the Fe-Ni diffusion layer is formed faces the inside of the battery container.
  • the surface-treated steel sheet is formed into the shape of the battery container by drawing, ironing, DI (Drawing and Ironing) or DTR (Draw and Thin Redraw) forming.
  • the battery container in this embodiment is equipped with the above-mentioned surface-treated steel plate, so it has high electrolyte resistance during overdischarge and can suppress the occurrence of corrosion due to the elution of Fe.
  • ⁇ Thickness of steel plate> The thickness of the steel plate used in each of the examples and comparative examples was measured using a micrometer.
  • Ni adhesion amount, Ni plating layer thickness The surface-treated steel sheets obtained in each of the Examples and Comparative Examples were measured with an X-ray fluorescence device to determine the Ni deposition amount in the Fe-Ni diffusion layer.
  • the ZSX100e manufactured by Rigaku Corporation was used as the X-ray fluorescence device. It was confirmed that the metal elements contained in the surface treatment layer of the surface-treated steel sheets could be quantified by the calibration curve method in the X-ray fluorescence measurement.
  • the Ni deposition amount was converted to thickness using the density of Ni (8.9 g/cm 3 ) to determine the thickness of the Ni plating layer before heat treatment.
  • ⁇ Thickness and Fe ratio of Fe-Ni diffusion layer The thickness and Fe content of the Fe--Ni diffusion layer were determined using a high-frequency glow discharge optical emission spectrometer (manufactured by Horiba, Ltd., model number: GD-PROFILER2). The thickness and Fe ratio of the Fe-Ni diffusion layer can be determined using a high-frequency glow discharge optical emission spectrometer in the above-mentioned procedure of measurement steps 1 to 5.
  • the specific measurement conditions for the high-frequency glow discharge optical emission spectrometer were as follows: Measurement mode: HDD mode Excitation mode: RF (normal) Output: 35W Pressure: 600 Pa Module: 7V Fuse: 7V Anode diameter: 4 mm Gas replacement time: 30 seconds Pre-sputtering time: 30 seconds Background measurement time: 10 seconds Measurement time: 80 seconds Capture interval: 0.1 seconds
  • An X-ray diffraction apparatus (a fully automated multipurpose X-ray diffraction apparatus, Smart Lab, manufactured by Rigaku Corporation) was used to measure the surface of the surface-treated steel sheet on which the Fe—Ni diffusion layer was formed.
  • the diffraction pattern obtained as a result of the X-ray diffraction measurement was subjected to background removal of the diffraction pattern by the Sonneveld-Visser method using thin film data processing software (manufactured by Rigaku Corporation).
  • the maximum diffraction intensity I A at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less and the maximum diffraction intensity I B at a diffraction angle 2 ⁇ of 44.51° or more and 45.00° or less were then obtained, and the ratio I B /I A was calculated.
  • the half-width B of the diffraction peak at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less was obtained for the obtained diffraction pattern.
  • the difference between the values of two diffraction angles 2 ⁇ that are half the value of the maximum diffraction intensity I A in the diffraction peak at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less is the half-width B.
  • FIG. 8 is a schematic diagram of a measurement jig used for evaluating the electrolyte resistance of the surface-treated steel sheet by the LSV method. As shown in FIG.
  • a surface-treated steel sheet sample was attached to the bottom of the measurement jig, an electrolyte (1 mol/L LiPF 6 , EC:DEC (1:1 v/v%), manufactured by Kishida Chemical Co., Ltd.) was added to the jig, and metallic lithium (manufactured by Honjo Metals Co., Ltd.) was attached to the upper electrode of the jig as a counter electrode and a reference electrode.
  • the surface areas of the counter electrode and the reference electrode were 1 cm 2 or more.
  • the distance between the reference electrode and the working electrode was 2 mm, the distance between the counter electrode and the working electrode was 2 mm, and the distance between the counter electrode and the reference electrode was 12 mm.
  • the measurement was performed in a dry room with a dew point of -40°C or less and a room temperature of 25°C.
  • the surface-treated steel sheet was polarized to +4.0 V (vs Li/Li+), which corresponds to overdischarge, at a scanning speed of 2 mV/sec from the natural potential, and the current density (nA/cm 2 ) at 4.0 V was measured to evaluate the electrolyte resistance of the surface-treated steel sheet during overdischarge. The smaller the current density, the less Fe was eluted, indicating excellent electrolyte resistance during overdischarge.
  • the prepared steel sheet was subjected to alkaline electrolytic degreasing and pickling by immersion in sulfuric acid, and then electrolytic plating (Ni plating) was performed under the following conditions using a Ni plating bath having the following bath composition, to form a Ni plating layer having a thickness of 0.5 ⁇ m and a Ni coating weight W of 4.45 g/ m2 on the surface of the steel sheet.
  • Ni plating conditions Bath composition: Nickel sulfate hexahydrate 250 g/L, nickel chloride hexahydrate 45 g/L, boric acid 30 g/L pH: 4.0-5.0 Bath temperature: 60°C Current density: 10 A/ dm2
  • the steel sheet on which the Ni plating layer was formed was subjected to thermal diffusion treatment by continuous annealing to form an Fe-Ni diffusion layer, and a surface-treated steel sheet was obtained.
  • the continuous annealing in the first heating step, the surface-treated steel sheet was heated from room temperature to the second heating start temperature (temperature range of 830-859°C).
  • the end temperature was set within a temperature range of 890-919°C so that the difference between the second heating temperature and the end temperature (second heating temperature difference) was 50°C, and the surface-treated steel sheet was heated at a heating rate of 0.53°C/sec.
  • the surface-treated steel sheet was cooled to a temperature of 120°C or less by spraying a cooling gas such as HNX gas.
  • a cooling gas such as HNX gas.
  • the thermal history Y applied to the surface-treated steel sheet through the first heating step, the second heating step, and the cooling step was 115,867°C/sec.
  • the obtained surface-treated steel sheet was subjected to various evaluations according to the methods described above. The results are shown in Table 1.
  • the thickness of the Fe-Ni diffusion layer was 2.02 ⁇ m.
  • the surface-treated steel sheet in which the ratio I B /I A of the maximum diffraction intensity I A at a diffraction angle 2 ⁇ of 43.00° or more and 44.30° or less to the maximum diffraction intensity I B at a diffraction angle 2 ⁇ of 44.51° or more and 45.00° or less obtained from thin film X-ray diffraction measurement of the surface of the Fe-Ni diffusion layer was 0.01 ⁇ I B / I A ⁇ 0.37 had a small current density caused by the dissolution of Fe at 4.0 V equivalent to overdischarge and had excellent electrolyte resistance during overdischarge (Examples 1-10).
  • Example 1 When Example 1 is compared with Comparative Example 3, although the Fe ratio is higher in Example 1, the current density was reduced by 33% to 123 nA/ cm2 in the electrolyte resistance evaluation during overdischarge by the LSV method, and the superiority of the surface-treated steel sheet in which the IB / IA ratio was controlled can be recognized.
  • the half-value width B was evaluated in Examples 1 and 2. The results are shown in Table 2.
  • the diffraction intensity ratio I B /I A was 0.01 ⁇ I B /I A ⁇ 0.37, and the electrolyte resistance during overdischarge was excellent.
  • the surface-treated steel sheets having a half-value width B of the maximum diffraction intensity I A of 0.35 or more were particularly excellent in electrolyte resistance during overdischarge (Examples 3 to 6).

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JP2012201949A (ja) * 2011-03-25 2012-10-22 Nisshin Steel Co Ltd 絶縁性の良好なステンレス鋼材およびその製造法
JP2014047359A (ja) 2012-08-29 2014-03-17 Toyo Kohan Co Ltd 電池容器用表面処理鋼板、電池容器および電池
JP2014077175A (ja) * 2012-10-10 2014-05-01 Nisshin Steel Co Ltd 表面改質ステンレス鋼板およびその製造方法
WO2016013572A1 (ja) * 2014-07-22 2016-01-28 新日鐵住金株式会社 蓄電デバイス容器用鋼箔、蓄電デバイス用容器及び蓄電デバイス、並びに蓄電デバイス容器用鋼箔の製造方法
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JP2014047359A (ja) 2012-08-29 2014-03-17 Toyo Kohan Co Ltd 電池容器用表面処理鋼板、電池容器および電池
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WO2016013572A1 (ja) * 2014-07-22 2016-01-28 新日鐵住金株式会社 蓄電デバイス容器用鋼箔、蓄電デバイス用容器及び蓄電デバイス、並びに蓄電デバイス容器用鋼箔の製造方法
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