WO2019163466A1 - Corps multicouche en aluminium et son procédé de production - Google Patents

Corps multicouche en aluminium et son procédé de production Download PDF

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Publication number
WO2019163466A1
WO2019163466A1 PCT/JP2019/003392 JP2019003392W WO2019163466A1 WO 2019163466 A1 WO2019163466 A1 WO 2019163466A1 JP 2019003392 W JP2019003392 W JP 2019003392W WO 2019163466 A1 WO2019163466 A1 WO 2019163466A1
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Prior art keywords
aluminum
anodic oxide
oxide film
less
thickness
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PCT/JP2019/003392
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English (en)
Japanese (ja)
Inventor
享 新宮
光成 大八木
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東洋アルミニウム株式会社
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Application filed by 東洋アルミニウム株式会社 filed Critical 東洋アルミニウム株式会社
Priority to KR1020207021339A priority Critical patent/KR20200127156A/ko
Priority to CN201980013622.9A priority patent/CN111727277A/zh
Publication of WO2019163466A1 publication Critical patent/WO2019163466A1/fr

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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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing

Definitions

  • the present invention relates to an aluminum laminate and a method for producing the same.
  • thinning, lightening, and flexibility have been studied for a substrate constituting an electronic device while realizing high gas barrier properties.
  • a method for realizing a reduction in thickness, weight, and flexibility of a substrate it has been studied to use a material constituting the substrate as a resin.
  • a substrate made of a resin such as a plastic film is relatively easily permeable to gas such as water vapor and oxygen supplied from the outside.
  • gas such as water vapor and oxygen supplied from the outside.
  • the substrate of the electronic device itself is made of a material having low gas permeability and has a gas barrier property.
  • a substrate that exhibits a high reflectance with respect to visible light is suitable for the substrate constituting the electronic device.
  • aluminum has a high gas barrier property and high reflectivity, and can be made thin, light, and flexible, and can be manufactured by roll-to-roll processing. (Al).
  • Aluminum has higher gas barrier properties and higher reflectivity for visible light than plastic films. Furthermore, by making aluminum into a foil shape, it becomes possible to reduce the thickness, weight, and flexibility.
  • the aluminum foil can be roll-to-roll processed.
  • an insulating layer for ensuring electrical insulation between the substrate and the electrode laminated on the substrate is disposed on the substrate of the electronic device for the above-mentioned use.
  • the dielectric breakdown voltage of such an insulating layer is generally 0.2 kV or more.
  • An anodized film having an insulating property can be easily formed on the surface of aluminum by anodizing treatment.
  • a laminate of aluminum and an anodized film laminated on the aluminum is suitable for the substrate of the electronic device for the above-mentioned use.
  • Patent Document 1 contains Fe: 0.05 mass% to 0.40 mass%, Si: 0.02 mass% to 0.20 mass%, with the balance being aluminum and After continuously casting and rolling an aluminum alloy composed of inevitable impurities, the maximum height roughness Rz in the surface roughness curve is 0.50 ⁇ m or less by performing cold rolling, and the equivalent circle diameter existing on the surface is 1 ⁇ m or more.
  • An aluminum substrate with an anodized film characterized in that an aluminum rolled material having an intermetallic compound of 1000 pieces / mm 2 or less is produced, and the aluminum rolled material is further subjected to an anodizing treatment in a sulfuric acid aqueous solution having a liquid temperature of 15 ° C. or lower. The manufacturing method of this is proposed.
  • Patent Document 1 discloses a laminate of an aluminum base material and an anodized film formed with a thickness of 0.1 ⁇ m to 20 ⁇ m on the surface of the aluminum base material.
  • an aluminum laminate in which an anodized film is laminated on an aluminum plate having a thickness of 0.3 mm described as an example in Patent Document 1 has sufficient flexibility. It was confirmed that they do not have. Specifically, cracks were confirmed in the anodized film layer of the aluminum laminate produced by roll-to-roll processing using a guide roll having a minimum diameter of 50 mm.
  • an object of the present invention is to provide an anodized film having a dielectric breakdown voltage of 0.2 kV or more, and no cracks are generated in the anodized film layer even in a roll-to-roll process using a guide roll having a minimum diameter of 50 mm. It is to provide an aluminum laminate.
  • the present inventors have found that the composition of the aluminum base material, the surface smoothness and thickness of the anodized film, and the aluminum laminate satisfy the specific conditions, the anode It has been found that an aluminum laminate can be obtained in which the oxide breakdown voltage of the oxide film is 0.2 kV or more and the crack of the anodized film layer does not occur even when passing through a guide roll having a minimum diameter of 50 mm.
  • the bending process with a minimum diameter of 50 mm or less means that the aluminum laminate can be held for at least 10 seconds along the outer peripheral surface of a cylinder with a diameter of 50 mm, and then the anodized film surface is visually observed. In a bending process test (hereinafter simply referred to as a bending process test), it means that no cracks are confirmed on the surface of the anodized film.
  • the aluminum laminate according to one embodiment of the present invention has the following characteristics.
  • An aluminum laminate according to an embodiment is formed in contact with an aluminum base material having a first surface and the first surface, and is located away from the first surface in a direction intersecting the first surface.
  • the surface layer including the first surface of the aluminum substrate contains aluminum having a purity of 99.9% by mass or more and iron having a purity of 0.001% by mass or more and 0.02% by mass or less.
  • the surface roughness Ra of the second surface of the first anodic oxide film is 15 nm or less.
  • the thickness of the intersecting direction of the first anodized film is 3 ⁇ m or more and 20 ⁇ m or less.
  • the total thickness value T1 (unit: ⁇ m) in the intersecting direction of the aluminum laminate and the thickness value T2 (unit: ⁇ m) in the intersecting direction of the first anodized film are expressed by the relation X + 10 ⁇ Y. ⁇ 230 is satisfied.
  • the sealing degree admittance Y value of the anodized film is preferably less than 100 ⁇ S.
  • the aluminum laminate according to another embodiment of the present invention has the following characteristics.
  • An aluminum laminate according to another embodiment is formed in contact with an aluminum substrate having a first surface, and is separated from the first surface in a direction intersecting the first surface.
  • the surface layer including the first surface of the aluminum substrate contains aluminum having a purity of 99.9% by mass or more and iron having a purity of 0.001% by mass or more and 0.02% by mass or less.
  • the surface roughness Ra of the second surface of the first anodic oxide film is 15 nm or less.
  • the thickness of the first anodized film in the intersecting direction is 2 ⁇ m or more and 20 ⁇ m or less.
  • the total thickness value T1 (unit: ⁇ m) in the intersecting direction of the aluminum laminate and the thickness value T2 (unit: ⁇ m) in the intersecting direction of the first anodized film are expressed by the relation X + 10 ⁇ Y. ⁇ 230 is satisfied. Furthermore, the sealing degree admittance Y value of the anodized film is less than 100 ⁇ S.
  • the present inventors have confirmed that the dielectric breakdown voltage of the anodized film of the aluminum laminate according to the above two embodiments is 0.2 kV or more. Furthermore, the present inventors have confirmed that the aluminum laminates according to the above two embodiments have high reflection characteristics with respect to visible light.
  • the anodized film is preferably a sulfuric acid anodized film.
  • the method for producing the aluminum laminate includes a step of preparing an aluminum substrate having a surface roughness Ra of 15 nm or less on the first surface, and an electrolytic solution containing sulfuric acid on the first surface of the aluminum substrate. And a step of forming a first anodized film having a thickness in the intersecting direction of 2 ⁇ m or more and 20 ⁇ m or less.
  • an aluminum laminate is provided with an anodized film having a dielectric breakdown voltage of 0.2 kV or higher, and in which the anodized film layer does not crack even in roll-to-roll processing using a guide roll having a minimum diameter of 50 mm.
  • the body can be provided.
  • an aluminum laminate 10 As shown in FIG. 1, an aluminum laminate 10 according to the present embodiment includes an aluminum substrate 1 and a first anodic oxide film 2.
  • the aluminum substrate 1 has a first surface 1A and a third surface 1B located on the opposite side of the first surface 1A.
  • the material which comprises the aluminum base material 1 contains aluminum (Al).
  • the aluminum substrate 1 is, for example, an aluminum foil.
  • the surface layer including the first surface 1A of the aluminum base 1 has an aluminum purity of 99.9% by mass or more.
  • the surface layer including the first surface 1A of the aluminum substrate 1 contains 0.001 mass% or more and 0.02 mass% or less of iron (Fe).
  • strength of the aluminum base material 1 falls that content of iron is less than 0.001 mass%.
  • intermetallic compounds such as FeAl 3 are easily crystallized at the time of casting of aluminum. These crystallized substances have a lower reflectance in the visible light region than the aluminum base, and cause a decrease in glossiness and visible light reflectance as an aluminum substrate.
  • the anodic oxide film becomes non-uniform, the transparency of the anodic oxide film is remarkably deteriorated and the reflectance is reduced, and the hardness of the anodic oxide film is also reduced.
  • the dielectric breakdown voltage of the anodized film also decreases. For this reason, it is necessary to make iron content into 0.02 mass% or less.
  • the surface layer including the first surface 1A of the aluminum substrate 1 may contain, for example, 0.001 mass% or more and 0.09 mass% or less of silicon (Si). Since silicon has a high solid solubility in aluminum and hardly forms a crystallized substance, the reflectivity in the visible light region is not lowered if the content is such that no crystallized substance is generated. Further, the mechanical strength of the aluminum base material 1 in which 0.001% by mass or more of silicon is dissolved is improved by solid solution strengthening compared to the mechanical strength of the aluminum base material 1 in which silicon is not dissolved. Yes.
  • the aluminum substrate 1 in which 0.001% by mass or more of silicon is solid-dissolved is rolled with a thinner foil while maintaining the same mechanical strength as the aluminum substrate 1 in which silicon is not dissolved. Can also be made easier.
  • the aluminum substrate 1 contains more than 0.09% by mass of silicon, increasing the thickness of the first anodic oxide film 2 decreases the transparency of the first anodic oxide film 2 and decreases the reflectance. Furthermore, the hardness of the 2nd surface 2A of the 1st anodic oxide film 2 also falls. Therefore, the silicon content needs to be 0.09% by mass or less.
  • the impurity is, for example, an unavoidable impurity, but may contain a trace amount of impurity that does not greatly affect the glossiness and the total reflectance of visible light in addition to the unavoidable impurity.
  • the impurities include, for example, copper (Cu), manganese (Mn), magnesium (Mg), zinc (Zn), titanium (Ti), vanadium (V), nickel (Ni), chromium (Cr), zirconium (Zr), It contains at least one element selected from the group consisting of boron (B), gallium (Ga), bismuth (Bi), and the like. Each impurity element has an individual content of 0.01% by mass or less.
  • the surface layer including the first surface 1A of the aluminum base 1 is a region from the first surface 1A to 5 ⁇ m in the direction (depth direction) intersecting the first surface 1A.
  • the surface roughness Ra of the first surface 1A is 15 nm or less.
  • a polishing roll such as physical polishing, electrolytic polishing, chemical polishing, or a roll whose surface is in a mirror surface state is used. There is cold rolling used.
  • composition of the other part of the aluminum substrate 1 other than the surface layer is not particularly limited, and the aluminum substrate 1 may be configured as, for example, a clad material.
  • the first anodic oxide film 2 is formed in contact with the first surface 1A.
  • the first anodic oxide film 2 has a surface that is in contact with the first surface 1A and a second surface 2A that is located away from the first surface 1A in the direction intersecting the first surface 1A.
  • the first anodic oxide film 2 is formed by an anodic oxidation treatment on the first surface 1A of the aluminum base 1.
  • the anodizing treatment may be any known anodizing treatment method.
  • the anodizing treatment is an anodizing treatment using an electrolytic solution containing at least one of sulfuric acid, boric acid, oxalic acid, and phosphoric acid.
  • the first anodic oxide film 2 is formed by an anodic oxidation treatment using an electrolytic solution containing sulfuric acid. That is, preferably, the first anodized film 2 is a sulfuric acid anodized film.
  • the first anodic oxide film 2 is sealed.
  • the first anodic oxide film 2 is transparent.
  • the thickness of the first anodized film 2 in the intersecting direction is 2 ⁇ m or more and 20 ⁇ m or less.
  • the thickness of the first anodic oxide film 2 in the intersecting direction is the distance between the surface of the first anodic oxide film 2 that is in contact with the first surface 1A and the second surface 2A.
  • the thickness of the first anodic oxide film 2 in the intersecting direction is smaller than 2 ⁇ m, it is difficult to set the dielectric breakdown voltage of the anodic oxide film to 0.2 kV or more.
  • the thickness of the first anodic oxide film 2 in the intersecting direction is larger than 20 ⁇ m, cracks are likely to occur on the surface of the first anodic oxide film 2 in the bending test.
  • the present inventors show that the first anodic oxide film 2 having a thickness in the intersecting direction of 3 ⁇ m or more and 20 ⁇ m or less has a high insulating property regardless of its sealing degree, as shown in Examples described later. In addition, it was confirmed that the generation of cracks was also suppressed in the bending test.
  • the present inventors have found that the dielectric breakdown voltage of the first anodic oxide film 2 changes according to the sealing degree admittance Y value of the first anodic oxide film 2, and in particular, the first anodic oxide film 2 intersects.
  • the sealing degree admittance Y value should be less than a certain value in order to make the dielectric breakdown voltage 0.2 kV or more.
  • the dielectric breakdown voltage of the first anodic oxide film 2 having a thickness in the intersecting direction of 2 ⁇ m or more and 3 ⁇ m or less and a sealing degree admittance Y value of less than 100 ⁇ S was 0.2 kV or more.
  • the dielectric breakdown voltage of the first anodic oxide film 2 having a thickness in the intersecting direction of 2 ⁇ m or more and 3 ⁇ m or less and a sealing degree admittance Y value of 100 ⁇ S or more was less than 0.2 kV.
  • the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 is 20 nm or less. A part of the light incident on the aluminum laminate 10 is reflected by the second surface 2A of the first anodic oxide film 2, and the remaining part is refracted by the second surface 2A and reaches the first surface 1A of the aluminum substrate 1. When the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 exceeds 15 nm, the light reflected by the second surface 2A or the light refracted by the second surface 2A diffuses to cause the second surface 2A to diffuse. The glossiness and total reflectance of 2A are reduced.
  • the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 is 15 nm or less, the diffusion of the light reflected by the second surface 2A or the light refracted by the second surface 2A can be suppressed, and the second surface 2A.
  • the surface roughness Ra of the second surface 2A of the first anodic oxide coating 2 can be applied to the surface with the arithmetic average roughness Ra defined in JIS B0601 (2001 version) and ISO 4287 (1997 version). It is a value calculated by extending to three dimensions.
  • the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 is made small.
  • the surface roughness Ra of the first surface 1A of the aluminum base 1 is 15 nm or less.
  • the present inventors have found that an aluminum laminate that does not satisfy the above relational expression and X + 10 ⁇ Y exceeds 230 has a crack in the anodized film when subjected to the bending test with a minimum diameter of 50 mm or less. It was confirmed.
  • the present inventors have found that the aluminum laminate having the above-described features and satisfying the above relational expression is suppressed from cracking even when the bending test is performed. .
  • the present inventors have intensively studied an aluminum laminate having high electrical insulation, high total reflectance, and high bending workability.
  • the surface layer including the first surface 1A of the aluminum substrate 1 contains aluminum having a purity of 99.9% by mass or more and iron having a purity of 0.001% by mass or more and 0.02% by mass or less, and the first anode
  • the aluminum laminate in which the surface roughness Ra of the second surface 2A of the oxide film 2 is 15 nm or less and the thickness of the first anodic oxide film 2 in the intersecting direction is 2 ⁇ m or more and 20 ⁇ m or less has high electrical insulation and It was confirmed to have a high total reflectance.
  • the present inventors have found that the bending property of such an aluminum laminate, that is, the difficulty of cracking when the bending is performed, is the value of the total thickness T1 of the aluminum laminate and the first anode. It was found to correlate with the thickness value T2 of the oxide film 2 (details will be described later in Examples).
  • the T1 and T2 of the aluminum laminate 10 can be arbitrarily set as long as the thickness of the first anodic oxide film 2 is 2 ⁇ m or more and 20 ⁇ m or less and the relational expression T1 + 10 ⁇ T2 ⁇ 230 is satisfied.
  • the aluminum laminate 10 preferably satisfies T1 + 10 ⁇ T2 ⁇ 200, more preferably satisfies T1 + 10 ⁇ T2 ⁇ 150, and more preferably satisfies T1 + 10 ⁇ T2 ⁇ 100. To do.
  • the lower limit value of T1 + 10 ⁇ T2 of the aluminum laminate 10 may be set so that at least the thickness T2 in the intersecting direction of the first anodic oxide film 2 can be 2 ⁇ m or more.
  • the lower limit value of T1 + 10 ⁇ T2 may be 50, for example.
  • the said value T1 will be the value T3 of the thickness of the aluminum base material 1.
  • the aluminum laminate 10 shown in FIG. 1 satisfies the relational expression T3 + 11 ⁇ T2 ⁇ 230.
  • the method for manufacturing an aluminum laminate according to the present embodiment includes a step of preparing an ingot (S10), a step of homogenizing the ingot (S20), The step of rolling (S30), the step of cold rolling the hot-rolled material obtained by hot rolling (S40), and cold rolling (hereinafter referred to as final finishing cold)
  • an ingot is prepared (step (S10)). Specifically, an aluminum ingot having a predetermined composition is prepared, and the ingot is cast (for example, semi-continuous casting) by solidifying the aluminum melt.
  • the content of metal elements such as Fe, Mn, and Si in the molten metal is controlled so that the aluminum purity in the surface layer of the aluminum base 1 is 99.9% by mass or more.
  • the Fe content in the molten metal is controlled so that the Fe content in the surface layer of the aluminum base 1 is 0.001% by mass or more and 0.02% by mass or less.
  • the content of Fe in the molten metal is controlled so that the content of Fe in the surface layer of the aluminum base 1 is 0.001% by mass or more and 0.02% by mass or less.
  • homogenization heat treatment is performed on the obtained ingot (step (S20)).
  • the homogenization heat treatment may be performed within the range of general operating conditions.
  • the homogenization heat treatment is performed under conditions where the heating temperature is 400 ° C. or more and 630 ° C. or less and the heating time is 1 hour or more and 20 hours or less.
  • step (S30) the ingot is hot-rolled (step (S30)).
  • a hot rolled material having a predetermined thickness W1 is obtained. Hot rolling may be performed once or a plurality of times.
  • the thin plate ingot may be cold-rolled without going through this step.
  • the hot-rolled material obtained by hot rolling is cold-rolled (step (S40)).
  • a cold-rolled material (the material to be rolled in the final finish cold rolling step (S50)) having a predetermined thickness W2 is obtained.
  • cold rolling is performed a plurality of times, for example, with an intermediate annealing step.
  • the first cold rolling step (S40A) is first performed on the hot-rolled material to form a rolled material that is thinner than the hot-rolled material thickness W1 and thicker than the cold-rolled material thickness W2.
  • an intermediate annealing step (S40B) is performed on the obtained rolled material.
  • the intermediate annealing may be performed within the range of general operating conditions.
  • the annealing is performed under conditions where the annealing temperature is 50 ° C. or more and 500 ° C. or less and the annealing time is 1 second or more and 20 hours or less.
  • a 2nd cold rolling process (S40C) is implemented with respect to the rolled material after annealing, and the cold-rolled material of thickness W2 is formed.
  • the cold rolled material is subjected to final finish cold rolling (step (S50)).
  • the material to be rolled is subjected to final finish cold rolling using a rolling roll.
  • the rolling roll has a roll surface that rolls in contact with the material to be rolled. It is preferable that the surface roughness Ra of the roll surface of at least one of the rolling rolls among the pair of rolling rolls arranged with the material to be rolled is 50 nm or less.
  • the resulting aluminum base material has a surface roughness Ra of the first surface of 20 nm or more.
  • the surface roughness Ra of the rolling roll used in this step is preferably as small as possible, and more preferably 40 nm or less. In this way, the aluminum substrate 1 is prepared.
  • step (S60) the first anodic oxide film 2 is formed on the first surface 1A of the obtained aluminum substrate 1 (step (S60)).
  • This step (S60) can be performed by a generally known anodizing method.
  • the anodizing treatment for example, at least one selected from the group consisting of a sulfuric acid bath, a boric acid bath, an oxalic acid bath, and a phosphoric acid bath is used as an electrolytic solution, and the aluminum substrate 1 is immersed in the electrolytic solution to form an anode.
  • the other electrode immersed in the electrolytic solution is used as a cathode, and electricity is passed between them.
  • Each condition of the anodizing method is appropriately selected so that the thickness of the first anodized film 2 is 2 ⁇ m or more and 20 ⁇ m or less, and the surface roughness Ra of the second surface 2A is 15 nm or less.
  • a sulfuric acid bath is used for the electrolyte.
  • the surface layer including the first surface 1A of the aluminum substrate 1 may not contain Si.
  • Si contributes to the improvement of the mechanical strength of the aluminum substrate 1, but when the mechanical strength required by other parameters such as thickness can be secured, the aluminum substrate 1 contains Si. You don't have to.
  • the total content of the impurities constituting the balance other than Al and Fe in the surface layer including the first surface 1A of the aluminum substrate 1 may be 0.10% by mass or less.
  • the aluminum laminate 11 may further include a second anodized film 3 provided so as to be in contact with the third surface 1 ⁇ / b> B of the aluminum base 1.
  • the 2nd anodic oxide film 3 has the 4th surface 3B in the position away from the 3rd surface 1B in the said crossing direction. That is, the aluminum laminate 11 includes the aluminum base 1 and the first anodic oxide film 2 and the second anodic oxide film 3 provided so as to sandwich the aluminum base 1.
  • the total thickness value T1 is the thickness value T3 (unit: ⁇ m) of the aluminum base 1 and the thickness value T2 of the first anodic oxide film 2 (unit: ⁇ m). ) And the value T4 (unit: ⁇ m) of the thickness of the second anodic oxide film 3 in the intersecting direction.
  • the thickness of the second anodized film 3 is equal to or less than the thickness of the first anodized film 2.
  • the thickness of the second anodic oxide film 3 is not less than 2 ⁇ m and not more than 20 ⁇ m.
  • the aluminum laminate 11 satisfies the relational expression T1 + 10 ⁇ T2 ⁇ 230. That is, the aluminum laminate 11 satisfies the relational expression T1 + 10 ⁇ T4 ⁇ T1 + 10 ⁇ T2 ⁇ 230.
  • the aluminum laminate 11 that satisfies the above relational expression can achieve the same effects as the aluminum laminate 10 according to Embodiment 1, and has high bending workability.
  • the aluminum laminate 11 satisfies the relational expression T1 + 10 ⁇ (T2 + T4) ⁇ 230.
  • the surface layer including the third surface 1B of the aluminum substrate 1 has an aluminum purity of 99.9% by mass or more, and 0.001% by mass or more 0 similarly to the surface layer including the first surface 1A. 0.02 mass% or less of iron is included.
  • Such an aluminum substrate 1 can be prepared by a method similar to the above-described steps (S10) to (S50) of the method for manufacturing the aluminum laminate 10 described above.
  • the second anodic oxide film 3 has a surface roughness Ra of the fourth surface 3B of 15 nm or less, like the first anodic oxide film 2.
  • Such a second anodic oxide film 3 can be formed by a method similar to the above-described step (S60) of the method for manufacturing the aluminum laminate 10 described above.
  • the second surface 2A of the first anodic oxide coating 2 and the fourth surface 3B of the second anodic oxide coating 3 have high gloss and high total reflectance.
  • the composition of the surface layer including the third surface 1B of the aluminum substrate 1 may be different from the composition of the surface layer including the first surface 1A, but is preferably the same.
  • the aluminum base material 1 may have different compositions of the surface layer including the first surface 1A and the surface layer including the third surface 1B, and the composition of the intermediate layer sandwiched between them, like a clad material, for example. .
  • the aluminum substrate obtained by final finish cold rolling is polished after the step (S50) and before the step (S60).
  • the process (S70) to process may be implemented.
  • the surface of the aluminum base material to be the first surface 1A is polished to form the aluminum base material 1 having the first surface 1A.
  • the surface to be the first surface 1A and the surface to be the third surface 1B are polished to form the aluminum substrate 1 having the first surface 1A and the third surface 1B. Is done.
  • the polishing method can be selected from physical polishing, electrolytic polishing, chemical polishing, and the like, but is not limited thereto.
  • a step of forming an aluminum substrate obtained by final finish cold rolling into a predetermined shape is performed after the step (S50) and before the step (S60). May be.
  • molding the said aluminum laminated bodies 10 and 11 obtained by the process (S60) may be implemented after the said process (S60).
  • membrane on the 3rd surface 1B of the aluminum base material 1 may be implemented after the said process (S60) on the at least 1 surface of the aluminum laminated body 10, for example.
  • the material constituting the film is at least one selected from the group consisting of resin, metal, ceramics and the like.
  • the film is, for example, an adhesive layer, and after the step of forming the film, a step of bonding the aluminum laminates 10 and 11 to another member or a wall or the like through the film may be performed. Further, after the step (S60), at least one of the porous portions of the first anodic oxide film 2 and the second anodic oxide film 3 of the aluminum laminates 10, 11 obtained by the step (S60) is colored. Further, the sealing process may be performed or only the sealing process may be performed.
  • the coloring process may be any method, but may be, for example, a method of adsorbing a dye or pigment, or a secondary electrolytic coloring method.
  • samples of the aluminum laminates of the examples of the present embodiment and comparative examples were prepared, and their glossiness, total reflectance, bending workability, and dielectric breakdown voltage were evaluated.
  • the aluminum ingot obtained by DC casting was subjected to homogenization heat treatment in a heating furnace. Thereafter, hot rolling was performed until the thickness became about 6.5 mm.
  • the obtained hot-rolled material was cold-rolled a plurality of times until the thickness reached a predetermined value. A plurality of cold rolling operations were performed with intermediate annealing in between, and aluminum substrates having thicknesses shown in Tables 1 and 2 were produced.
  • Examples 1 to 10 and Comparative Examples 1 to 9 and 12 to 18 were rolled using a rolling roll having a surface roughness Ra of 40 nm in the final finish cold rolling.
  • rolling was performed using a rolling roll having a surface roughness Ra of 50 nm in the final finish cold rolling.
  • rolling was performed in the final finish cold rolling using a rolling roll having a surface roughness Ra of 150 nm.
  • the homogenization heat treatment was performed under the conditions of a heating temperature of 400 ° C. to 630 ° C. and a heating time of 1 hour to 20 hours.
  • the intermediate annealing was performed, for example, under conditions where the annealing temperature was 50 ° C. or higher and 500 ° C. or lower, and the annealing time was 1 second or longer and 20 hours or shorter.
  • Surface roughness Ra of the 1st surface of the aluminum base material of each Example was 15 nm or less.
  • the aluminum base material obtained as described above was anodized.
  • the electrolyte was an aqueous solution containing 15% by volume sulfuric acid and having a bath temperature of 21 ° C.
  • Each sample was immersed in the electrolytic solution to form an anode, and a current having a current density of 130 mA / m 2 was passed between the cathode and the cathode for a predetermined time to perform anodization.
  • the anodizing time for each sample was set to a time for obtaining an anodized coating layer having a predetermined thickness. That is, the anodizing conditions for each sample were the same except for the anodizing time.
  • Example 2 to 10 and Comparative Examples 2 and 4 to 21 were carried out by using each sample on which an anodized film was formed, containing nickel acetate at a concentration of 5 g / L and boric acid at a concentration of 5 g / L. It was immersed in an aqueous solution having a temperature of 90 ° C. for 20 minutes and then immersed in pure water having a temperature of 98 ° C. for 20 minutes.
  • the sealing treatment of Example 1 and Comparative Examples 1 and 3 was performed by immersing in pure water at a temperature of 66 ° C. for 5 minutes.
  • the thickness of the obtained anodic oxide film was measured by the following measuring method using Vimetrics F20 manufactured by Vitec Co., Ltd. From the reflected light obtained when the third surface of the aluminum laminate was irradiated with visible light, a reflectance spectrum in a wavelength range from 400 nm to 1100 nm was obtained. Fitting was performed so that the obtained reflectance spectrum and the valley or peak of the interference part had the same wavelength as the theoretical spectrum, and the film thickness was derived.
  • the dielectric breakdown voltage was measured using a dielectric breakdown tester YST-243-30RO manufactured by Yamayo Tester Co., Ltd. Electricity was applied from the 2A surface of the test piece cut to 50 mm ⁇ 50 mm, and the time when a current of 5 mA or more flowed to the 1B surface was defined as a dielectric breakdown voltage. The voltage was increased at a speed of 50 V / second.
  • the sealing degree admittance Y value was measured based on JIS H 8683 (2013 edition).
  • the sealing degree admittance Y value was measured by using ANOTESTYMP30-S manufactured by Fisher Instruments, when the measurement area was 28.26 mm 2 .
  • Observation of surface irregularities with an atomic force microscope was performed using a scanning probe microscope AFM5000II manufactured by Hitachi High-Tech Science Co., Ltd. with a dynamic force mode method (non-contact) in a rectangular field of view of 80 ⁇ m ⁇ 80 ⁇ m.
  • the inclination of the sample was corrected by third-order curved surface automatic inclination correction in which a curved surface was obtained by least square approximation and fitting was performed, and the surface roughness Ra was measured.
  • the surface roughness Ra is calculated by extending the arithmetic average roughness Ra defined in JIS B0601 (2001 edition) and ISO 4287 (1997 edition) in three dimensions so that it can be applied to the entire observed surface. Value.
  • the glossiness was measured using a gloss meter VG7000 manufactured by Nippon Denshoku Industries Co., Ltd., with a light incident angle of 60 °.
  • the glossiness was measured in two directions, ie, a rolling direction (RD) and a direction perpendicular to the rolling direction (TD), and the value in each direction was evaluated.
  • RD rolling direction
  • TD rolling direction
  • the total reflectance is measured using an ultraviolet-visible spectrophotometer V570 manufactured by JASCO Corporation, and the total reflectance of the integrating sphere in the wavelength range of 250 nm to 2000 nm with reference to the standard white plate Spectralon for integrating sphere manufactured by Labsphere. It was measured. The average value of visible light in the wavelength region of 400 nm to 800 nm was determined from the obtained total reflectance measurement value.
  • the total reflectance was measured in two directions, a rolling direction (RD) and a direction perpendicular to the rolling direction (TD), and the total reflectance was evaluated as an average value of these.
  • Bending workability was evaluated by observing the presence or absence of cracks in each anodic oxide film for each sample subjected to the bending work described above.
  • test pieces of each Example and Comparative Example were cut out in a rolling direction (RD) of 100 mm and a direction perpendicular to the rolling direction (TD) by 15 mm. Furthermore, a plurality of cylinders having different diameters were prepared in stages. Next, each piece cut out was placed along the outer peripheral surface of the cylinder with the longest diameter and held for 10 seconds. Next, the surface of the anodized film after such bending was visually observed. In the case where no crack was confirmed in the anodized film by visual observation, the surface of the anodized film after being held for 10 seconds was visually observed along the outer peripheral surface of the cylinder whose diameter was shorter than that of the previously used cylinder.
  • RD rolling direction
  • TD direction perpendicular to the rolling direction
  • the minimum diameter in Tables 3 and 4 indicates the minimum value (unit: mm) of the diameter of the cylinder used for the bending process in which no crack was confirmed in the anodized film for each test piece.
  • the aluminum purity is 99.9% by mass or more
  • the surface roughness Ra of the second surface is 15 nm.
  • an anodized film having a thickness of 2 ⁇ m or more and 20 ⁇ m or less and satisfying the above relational expression.
  • the dielectric breakdown voltages of the anodic oxide films of Examples 1 to 10 were 0.2 kV or more. In Examples 1 to 6 and 8 where the thickness of the anodized film was 2 ⁇ m or more and less than 9 ⁇ m, the dielectric breakdown voltage was 0.2 kV or more.
  • Comparative Examples 2, 6, and 7 are related to the above-mentioned five parameters, namely, the aluminum purity and iron content of the aluminum base material, the surface roughness and thickness of the anodized film, and the above relational expression, and the anodic oxidation. It differs from Examples 1 to 10 only in that the thickness of the film is less than 2 ⁇ m.
  • the dielectric breakdown voltage of the anodic oxide films of Comparative Examples 2, 6, and 7 was less than 0.2 kV.
  • Comparative Examples 14 and 15 differ from Examples 1 to 10 only in that the iron content of the aluminum base material exceeds 0.02% by mass with respect to the five parameters described above. It is an aluminum laminate.
  • the dielectric breakdown voltages of the anodic oxide films of Comparative Examples 14 and 15 were less than 0.2 kV.
  • Comparative Example 19 is different from Examples 1 to 10 only in that the surface roughness Ra of the second surface exceeds 15 nm with respect to the five parameters described above.
  • the dielectric breakdown voltage of the anodized film of Comparative Example 19 was less than 0.2 kV.
  • the anodized film of Example 1 has a thickness of 4.7 ⁇ m and a sealing degree admittance Y value exceeding 100 ⁇ S.
  • the anodic oxide films of Examples 2, 4, 5, and 10 have a thickness of 2 ⁇ m or more and 3 ⁇ m or less, and a sealing degree admittance Y value of less than 100 ⁇ S.
  • Comparative Examples 1 and 3 are equivalent to Examples 1 to 10 with respect to the five parameters described above, but differ from Examples 2 to 10 only in that the sealing degree admittance Y value exceeds 100 ⁇ S. Is.
  • Example 4 and Comparative Example 3 differ only in the degree of sealing of the anodized film, and Example 4 has a lower sealing degree admittance Y value than Comparative Example 3, that is, the degree of sealing is low. It is expensive.
  • the dielectric breakdown voltage of the anodic oxide films of Examples 1 to 10 was 0.2 kV or more as described above, whereas the dielectric breakdown voltage of the anodic oxide films of Comparative Examples 1, 3 and 18 was less than 0.2 kV. there were.
  • the dielectric breakdown voltage of the anodized film on the aluminum substrate depends on the thickness of the anodized film and the iron content of the aluminum substrate rather than the sealing degree of the anodized film. In order to make it 0.2 kV or more, it was confirmed that the lower limit of the thickness of the anodized film should be 2 ⁇ m and the lower limit of the iron content of the aluminum base should be 0.02 mass%.
  • the dielectric breakdown voltage of the anodic oxide film on the aluminum substrate depends on the sealing degree, and the dielectric breakdown voltage is 0.2 kV or more. In order to achieve this, it was confirmed that the upper limit value of the sealing admittance Y value should be 100 ⁇ S.
  • the inventors of the Examples 1 to 10 and Comparative Examples 1 to 21 have the shortest diameter of the cylinder used in the bending process in which no crack was confirmed in the anodized film in the bending process test.
  • the value (unit: mm) is T1 + 10 ⁇ , where T1 is the total thickness value of the aluminum substrate and the anodized film in the intersecting direction, and T2 is the thickness value of the anodized film in the intersecting direction. It was found to correlate with T2.
  • the correlation coefficient R 2 was greater than 0.92.
  • the first T6 and the eighth T8 have a diameter of 32 mm. 1 No cracks were observed in the anodized film 2. Further, in Examples 6 and 8 in which the above value T1 + 10 ⁇ T2 is 100 or less, no cracks are confirmed in the first anodic oxide film 2 even when being bent along the outer peripheral surface of a cylinder having a diameter of 16 mm. It was.
  • the anodic oxide film is formed when bent along the outer peripheral surface of a cylinder having a diameter of 50 mm or more. Cracks were confirmed.
  • the inventors of the present invention have confirmed that high bending workability is realized as long as the above relational expression is satisfied even when the anodized film thickness T2 is a relatively thick aluminum laminate of 2 ⁇ m or more.
  • the thickness of the anodized film of Example 6 is the same as that of Comparative Examples 8 and 9, but the thickness of the aluminum base material is 100 ⁇ m or more thinner than that of Comparative Examples 8 and 9.
  • Example 6 satisfying the above relational expression no cracks were observed when wound around the outer periphery of a cylinder having a minimum diameter of 25 mm in a bending test.
  • Comparative Examples 8 and 9 which did not satisfy the above relational expression cracks were confirmed when wound around the outer periphery of a cylinder having a diameter of 50 mm in a bending test.
  • the present inventors consider that the coefficients 1 and 10 of the left side T1 + 10 ⁇ T2 in the above relational expression are related to the difference in the degree of influence on the bending workability of the aluminum base material and the anodized film.
  • the anodized film has a lower ductility than the aluminum base material. Therefore, it is considered that the anodized film has a higher influence on the bending workability than the aluminum base material. For example, when the thickness of the aluminum laminate is increased or decreased by several tens of ⁇ m, and the increase or decrease is caused by the increase or decrease of the thickness of the aluminum base material, the bending workability does not change greatly depending on the increase or decrease.
  • Comparative Examples 16 and 17 in which the aluminum purity of the aluminum base material is lower than 99.9% by mass and the Fe content of the aluminum base material is higher than 0.052% by mass, the surface roughness Ra of the anodized film exceeds 15 nm.
  • the glossiness was less than 63%, the visible light total reflectance was less than 83%, and the glossiness was not high and the total reflectance was not high.
  • Comparative Example 6 in which the thickness of the anodized film was less than 1 ⁇ m had a visible light total reflectance of less than 83% and did not have a high total reflectance.
  • this embodiment can provide an aluminum laminate having high electrical insulation and high bending workability, and high glossiness and high total reflectance.
  • the aluminum laminate according to the present embodiment is particularly suitable for a substrate of an electronic device that constitutes a display such as a liquid crystal, an organic EL, and electronic paper, a thin film solar cell, and a touch panel.
  • 1 Aluminum substrate, 1A 1st surface, 1B 3rd surface, 2nd first anodized film, 2A 2nd surface, 3rd 2nd anodized film, 3B 4th surface, 4 substrate, 10 and 11 aluminum laminate.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne un corps multicouche en aluminium (10) comprenant : un matériau de base en aluminium (1) qui possède une première surface (1A) ; et un film de revêtement en oxyde anodique (2) qui est formé de manière à être en contact avec la première surface (1A) et qui possède une deuxième surface (2A), laquelle se trouve à une certaine distance de la première surface (1A) dans une direction qui croise la première surface (1A). La couche de surface du matériau de base en aluminium (1), qui comprend la première surface (1A), contient de l'aluminium qui présente une pureté égale ou supérieure à 99,9 % massiques et contient de 0,001 % massique à 0,02 % massique (inclus) de fer. La deuxième surface (2A) du film de revêtement en oxyde anodique (2) présente une rugosité de surface Ra inférieure ou égale à 15 nm. Le film de revêtement en oxyde anodique (2) présente une épaisseur de 2 µm à 20 µm (inclus) dans la direction de l'intersection. L'épaisseur totale T1 (unité : μm) du corps multicouche en aluminium (1) dans la direction de l'intersection et l'épaisseur T2 (unité : µm) du film de revêtement en oxyde anodique (2) dans la direction de l'intersection satisfont l'expression relationnelle : T1 + 10 × T2 ≤ 230. Le film de revêtement en oxyde anodique (2) présente une valeur d'admittance Y de degré d'étanchéité inférieure à 100 μS.
PCT/JP2019/003392 2018-02-26 2019-01-31 Corps multicouche en aluminium et son procédé de production WO2019163466A1 (fr)

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JP2011171379A (ja) * 2010-02-16 2011-09-01 Fujifilm Corp 金属複合基板およびその製造方法
JP2012033853A (ja) * 2010-04-28 2012-02-16 Fujifilm Corp 絶縁性光反射基板
JP2012201891A (ja) * 2011-03-23 2012-10-22 Fujifilm Corp 絶縁基板ならびにそれを用いた配線基板、半導体パッケージおよびｌｅｄパッケージ
JP2013253317A (ja) * 2012-05-08 2013-12-19 Fujifilm Corp 半導体装置用基板、半導体装置、調光型照明装置、自己発光表示装置、太陽電池および反射型液晶表示装置
JP2015196867A (ja) * 2014-03-31 2015-11-09 株式会社神戸製鋼所 アルミニウム合金板

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JP5833987B2 (ja) * 2012-07-26 2015-12-16 株式会社神戸製鋼所 陽極酸化処理性に優れたアルミニウム合金および陽極酸化処理アルミニウム合金部材
JP6308848B2 (ja) 2014-04-08 2018-04-11 三菱アルミニウム株式会社 陽極酸化皮膜付アルミニウム基板の製造方法

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JPH0475208A (ja) * 1990-07-17 1992-03-10 Sumitomo Electric Ind Ltd 無機絶縁電線
JP2011171379A (ja) * 2010-02-16 2011-09-01 Fujifilm Corp 金属複合基板およびその製造方法
JP2012033853A (ja) * 2010-04-28 2012-02-16 Fujifilm Corp 絶縁性光反射基板
JP2012201891A (ja) * 2011-03-23 2012-10-22 Fujifilm Corp 絶縁基板ならびにそれを用いた配線基板、半導体パッケージおよびｌｅｄパッケージ
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JP2015196867A (ja) * 2014-03-31 2015-11-09 株式会社神戸製鋼所 アルミニウム合金板

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