WO2019111648A1 - アルミニウム積層体およびその製造方法 - Google Patents

アルミニウム積層体およびその製造方法 Download PDF

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Publication number
WO2019111648A1
WO2019111648A1 PCT/JP2018/041956 JP2018041956W WO2019111648A1 WO 2019111648 A1 WO2019111648 A1 WO 2019111648A1 JP 2018041956 W JP2018041956 W JP 2018041956W WO 2019111648 A1 WO2019111648 A1 WO 2019111648A1
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Prior art keywords
aluminum
less
thickness
oxide film
anodic oxide
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PCT/JP2018/041956
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English (en)
French (fr)
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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Priority to CN201880076400.7A priority Critical patent/CN111406128B/zh
Priority to KR1020207017618A priority patent/KR102444981B1/ko
Publication of WO2019111648A1 publication Critical patent/WO2019111648A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • 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
    • C25D11/16—Pretreatment, e.g. desmutting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon

Definitions

  • the present invention relates to an aluminum laminate and a method of manufacturing the same.
  • a natural oxide film is formed on the surface of aluminum.
  • natural oxide films are easily corroded by moisture and water. Therefore, in order to protect the surface from corrosion, an anodized film is generally formed on the surface of an aluminum plate used under a corrosive environment which contains moisture, water and the like to corrode aluminum. The corrosion resistance by the anodized film increases as the thickness of the anodized film increases.
  • an aluminum plate is used as a reflector of illumination or a panel for a designable building material.
  • aluminum plates having high gloss and high total reflectance are required.
  • bending may be applied to an appropriate shape.
  • Patent Document 1 discloses an aluminum material provided with a barrier type anodic oxide film having a thickness of 100 nm or more and 500 nm or less. According to Patent Document 1 described above, when the thickness exceeds 500 nm, the influence of absorption of visible light by the anodic oxide film becomes large and the regular reflectivity is inferior, so the thickness of the barrier type anodic oxide film needs to be 500 nm or less And is stated.
  • Patent Document 2 by setting the withstand voltage of the oxide film to a range of 1 V or more and less than 20 V (corresponding to a film thickness of 10 to 200 ⁇ ), it has excellent corrosion resistance and weather resistance. It is disclosed that an aluminum foil excellent in flexibility can be obtained.
  • Patent Document 2 Although the aluminum foil described in Patent Document 2 has flexibility, the thickness of the oxide film is relatively thin, the application that is directly exposed to the outdoor environment is not considered, and the corrosion resistance is insufficient. If the thickness of the oxide film is increased to improve the corrosion resistance, a crack will occur. Moreover, in the said patent document 2, surface hardness, glossiness, total reflectance, and image clarity are not considered.
  • an object of the present invention is to provide an aluminum laminate having high glossiness, high total reflectance and high image clarity, as well as high corrosion resistance, high surface hardness, and high bendability.
  • the present inventors have made the anodic oxide film extremely thick, so that it has high corrosion resistance and high total reflection while having high corrosion resistance and high surface hardness. Rate, high image clarity can be obtained, and the relationship between the value T1 (unit: ⁇ m) of the total thickness of the aluminum laminate and the value T2 (unit: ⁇ m) of the thickness of the anodized film layer is T1 + 10 ⁇ T2 ⁇ 450 It has been found that an aluminum laminate satisfying the following condition can be bent with a minimum diameter of 100 mm or less.
  • the possibility of bending with a minimum diameter of 100 mm or less means that the aluminum laminate is processed for holding for 10 seconds along the outer peripheral surface of a cylinder having a diameter of at least 100 mm and then visually observed on the surface of the anodized film. It means that a crack is not confirmed.
  • the aluminum laminate of the present embodiment has the following features.
  • the aluminum laminate according to the present embodiment is formed in contact with the first surface and the aluminum base having the first surface, and a position away from the first surface in the direction intersecting the first surface.
  • the surface layer including the first surface of the aluminum base includes aluminum having a purity of 99.9% by mass or more and iron of 0.001% by mass or more and 0.052% by mass or less.
  • the surface roughness Ra of the second surface of the first anodized film is 20 nm or less.
  • the average inter-relief distance RSm of the second surface of the first anodized film is less than 30 ⁇ m.
  • the thickness in the intersecting direction of the first anodic oxide film is 9 ⁇ m or more and 26 ⁇ m or less.
  • the value T1 (unit: ⁇ m) of the total thickness in the intersecting direction of the aluminum laminate and the value T2 (unit: ⁇ m) of the thickness in the intersecting direction of the first anodic oxide film are expressed by the relational expression T1 + 10 ⁇ T2. ⁇ 450 is satisfied.
  • the specular reflectance of the aluminum laminate including the same decreases.
  • the regular reflectance at this time does not decrease monotonously as the film thickness increases, but exhibits a tendency of gradually decreasing while repeating a decreasing tendency and an increasing tendency.
  • FIG. 1 of the patent document 1 when the thickness of the anodized film is gradually increased from 0 nm to about 550 nm, the regular reflectance of the aluminum laminate gradually decreases while periodically decreasing and increasing repeatedly. The trend is shown.
  • the thickness of the anodized film is preferably 150 nm ⁇ 30 nm or 300 nm ⁇ 20 nm.
  • the above tendency is considered to be caused by interference between the reflected light on the first surface of the aluminum base and the reflected light on the second surface of the anodized film.
  • the present inventors have found that the aluminum laminate according to the present embodiment provided with the first anodic oxide film having a thickness of 9 ⁇ m to 26 ⁇ m is an aluminum laminate having an anodic oxide film having a thickness of about 150 nm to 300 nm. It confirmed that it had high visible light total reflectance compared with the body (for details, refer to the example mentioned later).
  • the aluminum laminate has high glossiness, visible light total reflectance and image clarity, and high corrosion resistance, as compared to an aluminum laminate having an anodized film with a thickness of 600 nm to less than 9 ⁇ m. It confirmed that it had (the details refer to the example mentioned later). That is, the present inventors can realize high glossiness, high visible light total reflectance, and high image clarity within a relatively wide numerical range of the thickness of the first anodized film of 9 ⁇ m to 26 ⁇ m. It was confirmed.
  • the present inventors found that the above-mentioned tendency found this time is realized by an action different from the interference action, because the regular reflectance is different from the tendency to decrease gradually while repeating increase and decrease due to the above-mentioned interference. I believe that.
  • the anodized film is preferably a sulfuric acid anodized film.
  • the method of manufacturing the aluminum laminate comprises the steps of preparing an aluminum base having a surface roughness Ra of 15 nm or less on the first side, and using an electrolytic solution containing sulfuric acid on the first side of the aluminum base. And forming a first anodic oxide film having a thickness in a cross direction of 9 ⁇ m or more and 26 ⁇ m or less.
  • an aluminum laminate having high glossiness, high total reflectance and high image clarity, as well as high corrosion resistance, high surface hardness and high bendability.
  • the aluminum laminate 10 As shown in FIG. 1, the aluminum laminate 10 according to the present embodiment includes an aluminum base 1 and a first anodic oxide film 2.
  • the aluminum base 1 has a first surface 1A and a third surface 1B opposite to the first surface 1A.
  • the material which comprises the aluminum base 1 contains aluminum (Al).
  • the aluminum base 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 iron (Fe) of 0.001% by mass or more and 0.052% by mass or less.
  • strength of the aluminum base material 1 falls that content of iron is less than 0.001 mass%.
  • intermetallic compounds such as FeAl 3 easily crystallize out when aluminum is cast. These crystallized products have a lower reflectance in the visible light region than the aluminum base, and cause a decrease in the glossiness and the visible light reflectance as an aluminum base.
  • the surface layer including the first surface 1A of the aluminum substrate 1 may contain, for example, 0.001% by mass or more and 0.09% by mass or less of silicon (Si). Since silicon has a large solid solubility in aluminum and is difficult to form a crystallized product, if the content is such that the crystallized product is not generated, the reflectance in the visible light region is not reduced. In addition, the mechanical strength of the aluminum base 1 in which silicon is solid-solved by 0.001 mass% or more is improved by solid solution strengthening as compared with the mechanical strength of the aluminum base 1 in which silicon is not solid-solved. There is.
  • the aluminum substrate 1 in which silicon is solid-solved by 0.001% by mass or more is rolled of a thinner foil while maintaining the same mechanical strength as the aluminum substrate 1 in which silicon is not dissolved. Can also be easier.
  • the aluminum base material 1 contains silicon more than 0.09 mass%, if the thickness of the first anodic oxide film 2 is increased, the transparency of the first anodic oxide film 2 is reduced and the reflectance is lowered. Furthermore, the hardness of the second surface 2A of the first anodic oxide film 2 also decreases. Therefore, the content of silicon needs to be 0.09% by mass or less.
  • the balance other than Al, Fe, and Si in the surface layer including the first surface 1A of the aluminum base 1 is made of impurities.
  • the impurities are, for example, unavoidable impurities, but may contain, in addition to the unavoidable impurities, trace amounts of impurities that do not significantly affect the gloss, the total reflectance of visible light, the image clarity, and the corrosion resistance.
  • the above-mentioned impurities are, 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.
  • the content of each impurity element is 0.01 mass% or less.
  • the surface layer including the first surface 1A of the aluminum substrate 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.
  • polishing such as physical polishing, electrolytic polishing, chemical polishing or the like, or a rolling roll having a mirror surface is used. There are cold rolling used, etc.
  • electropolishing and chemical polishing are wet methods, and when the surface roughness Ra of the first surface 1A before polishing is as rough as 29 nm or more, the surface roughness Ra of the first surface is 15 nm or less. Even if it grind
  • the surface roughness Ra of the first surface 1A is 15 nm or less by physical polishing or cold rolling.
  • composition of the other portion of the aluminum base 1 other than the surface layer is not particularly limited, and the aluminum base 1 may be configured as a clad material, for example.
  • the first anodic oxide film 2 is formed in contact with the first surface 1A.
  • the first anodic oxide film 2 has a surface in contact with the first surface 1A, and a second surface 2A at a position separated from the first surface 1A in the direction intersecting the first surface 1A.
  • the first anodic oxide film 2 is formed by anodizing the first surface 1A of the aluminum base 1.
  • the anodizing treatment may be any known anodizing treatment method, and is, for example, 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 anodizing 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 transparent.
  • the thickness in the intersecting direction of the first anodic oxide film 2 is 9 ⁇ m or more and 26 ⁇ m or less.
  • the thickness in the intersecting direction of the first anodized film 2 is the distance between the surface of the first anodized film 2 in contact with the first surface 1A and the second surface 2A.
  • the thickness in the intersecting direction of the anodized film is smaller than 9 ⁇ m, the light incident on the second surface of the anodized film is reflected by the first surface of the aluminum base, and the second light of the incident light. It interferes with the reflected light on the surface.
  • interference color or white turbidity occurs on the second surface of the anodized film, and the aluminum laminate can not realize high glossiness, high visible light total reflectance, or high image clarity.
  • the thickness in the crossing direction of the first anodic oxide film 2 is smaller than 9 ⁇ m, the corrosion resistance required for the aluminum laminate 10 used outdoors can not be satisfied, and the second surface 2A The surface hardness also decreases.
  • the thickness in the intersecting direction of the first anodic oxide film 2 is larger than 26 ⁇ m, the dissolution of the anodic oxide film also proceeds during the anodic oxidation treatment, so the film quality of the first anodic oxide film 2 is deteriorated. The surface hardness of the second surface 2A is reduced.
  • the second surface 2A has high glossiness, high visible light total reflectance, and high image clarity. It also has high surface hardness.
  • the thickness in the crossing direction of the first anodic oxide film 2 is 12 ⁇ m or more and 20 ⁇ m or less.
  • the aluminum laminate 10 provided with such a first anodic oxide film 2 has improved productivity and has high glossiness, high total reflectance and high image clarity on the second surface 2A, and high corrosion resistance. have.
  • Surface roughness Ra of 2nd surface 2A of the 1st anodic oxide film 2 is 20 nm or less. Part of the light incident on the aluminum laminate 10 is reflected by the second surface 2 A of the first anodic oxide film 2, and the remaining portion is refracted by the second surface 2 A to reach the first surface 1 A of the aluminum substrate 1. When the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 exceeds 20 nm, the light reflected by the second surface 2A or the light refracted by the second surface 2A diffuses, thereby the second surface The glossiness and total reflectance of 2A decrease.
  • the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 may be such that arithmetic mean roughness Ra defined in JIS B0601 (2001 edition) and ISO 4287 (1997 edition) can be applied to the surface Is a value calculated by expanding in three dimensions.
  • the average inter-relief distance RSm of the second surface 2A of the first anodic oxide film 2 is less than 30 ⁇ m.
  • the average inter-recess distance RSm in any two directions orthogonal to each other in the second surface 2A is less than 30 ⁇ m.
  • the average inter-relief distance RSm of the second surface 2A in the rolling direction (RD direction) of the aluminum substrate 1 and the direction (TD direction) orthogonal thereto is Less than 30 ⁇ m.
  • the average inter-relief distance RSm of the second surface 2A of the first anodic oxide film 2 is 30 ⁇ m or more, the image clarity of the second surface 2A decreases.
  • the second surface 2A of the first anodic oxide film 2 has high image clarity.
  • the average distance between irregularities is defined by JIS standard JIS B0601 (2001 edition).
  • the surface roughness Ra of the first surface 1A of the aluminum substrate 1 is reduced in order to make the surface roughness Ra of the second surface 2A of the first anodic oxide film 2 and the average inter-relief distance RSm within the above numerical range. Is preferred.
  • the surface roughness Ra of the first surface 1A of the aluminum base 1 is 15 nm or less.
  • Value T1 (unit: ⁇ m, see FIG. 1) of the total thickness in the crossing direction of the aluminum laminate 10
  • value T2 (unit: ⁇ m, FIG. 1) of the thickness in the crossing direction of the first anodic oxide film 2 Reference) satisfies the relational expression T1 + 10 ⁇ T2 ⁇ 450.
  • the inventors of the present invention have found that, in an aluminum laminate having T1 + 10 ⁇ T2 exceeding 450, which does not satisfy the above relational expression, the anodic oxide film is cracked when bending is performed so that the minimum diameter is 100 mm or less. confirmed.
  • the inventors of the present invention have the above-described features, and the aluminum laminated body satisfying the above-mentioned relational expression suppresses the generation of cracks even when bending is performed to make the minimum diameter 100 mm or less. Found out that
  • the inventors intensively studied an aluminum laminate having high glossiness, high total reflectance, high image clarity, high corrosion resistance, high surface hardness, and high bendability.
  • 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 of 0.001% by mass to 0.052% by mass, and the first anode
  • the surface roughness Ra of the second surface 2A of the oxide film 2 is 20 nm or less, and the average inter-relief distance RSm of the second surface 2A of the first anodic oxide film 2 is less than 30 ⁇ m.
  • an aluminum laminate having a thickness in the crossing direction of 9 ⁇ m to 26 ⁇ m had high glossiness, high total reflectance, high image clarity, high corrosion resistance, and high surface hardness. Furthermore, the present inventors have found that the bending workability of such an aluminum laminate, that is, the difficulty in generating cracks when subjected to bending, is the value T1 of the overall thickness of the aluminum laminate and the first anode. It was found to be correlated with the value T2 of the thickness of the oxide film 2 (details will be described later in the examples).
  • the above T1 and the above T2 of the aluminum laminate 10 can be arbitrarily set as long as the thickness of the first anodic oxide film 2 is 9 ⁇ m to 26 ⁇ m and the above relational expression T1 + 10 ⁇ T2 ⁇ 450 is satisfied.
  • the aluminum laminate 10 preferably satisfies T1 + 10 ⁇ T2 ⁇ 400, more preferably satisfies T1 + 10 ⁇ T2 ⁇ 350, and more preferably satisfies T1 + 10 ⁇ T2 ⁇ 300, from the viewpoint of improving bending workability. Do.
  • the lower limit value of the above 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 9 ⁇ m or more.
  • the lower limit value of T1 + 10 ⁇ T2 may be, for example, 150 or 100.
  • the thickness value of the aluminum base 1 in the intersecting direction is T3 (unit: ⁇ m)
  • the value T1 is the value T3 of the thickness of the aluminum base 1
  • the value T 2 of the thickness of the first anodized film 2 satisfies the relational expression T3 + 11 ⁇ T2 ⁇ 450.
  • an ingot is prepared (step (S10)). Specifically, a molten aluminum of a predetermined composition is prepared, and the ingot is cast (for example, semi-continuous casting) by solidifying the molten aluminum.
  • the content of the metal element such as Fe, Mn, or Si in the molten metal is controlled such that the aluminum purity in the surface layer of the aluminum base 1 is 99.9 mass% or more.
  • the content of Fe in the molten metal is controlled such that the content of Fe in the surface layer of the aluminum base 1 is 0.001% by mass or more and 0.052% by mass or less.
  • the content of Si in the molten metal is controlled such that the content of Fe in the surface layer of the aluminum base 1 is 0.001% by mass or more and 0.09% by mass or less.
  • the homogenization heat treatment is performed on the obtained ingot (step (S20)).
  • the homogenization heat treatment may be performed under general operating conditions, and is performed, for example, under the conditions of a heating temperature of 400 ° C. or more and 630 ° C. or less and a heating time of 1 hour or more and 20 hours or less.
  • step (S30) A hot-rolled material having a predetermined thickness W1 is obtained by this process. Hot rolling may be performed one or more times.
  • the said thin plate-like ingot may be cold-rolled not via this process.
  • the hot-rolled material obtained by hot rolling is cold-rolled (step (S40)).
  • a cold-rolled material having a predetermined thickness W2 (a material to be rolled in the final finish cold rolling process (S50)) is obtained.
  • cold rolling is performed, for example, multiple times with an intermediate annealing process in between.
  • the first cold rolling step (S40A) is first performed on the hot-rolled material to form a rolled material thinner than the thickness W1 of the hot-rolled material and thicker than the thickness W2 of the cold-rolled material.
  • an intermediate annealing step (S40B) is performed on the obtained rolled material.
  • middle annealing should just be in the range of general operation conditions, for example, it is performed on the conditions which make annealing temperature 50 to 500 degreeC and annealing time be 1 second or more and 20 hours or less.
  • a second cold rolling step (S40C) is performed on the annealed rolled material to form a cold rolled material having a thickness W2.
  • the cold rolled material is subjected to final finish cold rolling (step (S50)).
  • the final finish cold rolling of the material to be rolled is performed using a rolling roll.
  • a rolling roll has a roll surface which rolls in contact with a material to be rolled. It is preferable that surface roughness Ra of the roll surface of at least one rolling roll is 50 nm or less among a pair of rolling rolls arrange
  • the surface roughness Ra of the first surface of the resulting aluminum substrate is 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.
  • the aluminum base 1 is prepared.
  • step (S60) the first anodic oxide film 2 is formed on the first surface 1A of the obtained aluminum base 1 (step (S60)).
  • This step (S60) can be carried out 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 electrolyte, and the aluminum substrate 1 is immersed in this to serve as an anode.
  • the other electrode immersed in the electrolytic solution is used as a cathode and electric current is applied between them.
  • Each condition of the anodizing treatment method is that the thickness of the first anodic oxide film 2 is 9 ⁇ m or more and 26 ⁇ m or less, the surface roughness Ra of the second surface 2A is 20 nm or less, and the average inter-relief distance RSm of the second surface 2A is less than 30 ⁇ m To be selected appropriately.
  • a sulfuric acid bath is used for the electrolyte.
  • the aluminum laminate 10 according to the present embodiment shown in FIG. 1 can be obtained.
  • the surface layer including the first surface 1A of the aluminum base material 1 may not contain Si. As described above, Si contributes to the improvement of the mechanical strength of the aluminum base 1, but if it can ensure the mechanical strength required by other parameters such as thickness, the aluminum base 1 contains Si. You do not have to. In this case, the total content of the above-mentioned impurities constituting the balance other than Al and Fe in the surface layer including the first surface 1A of the aluminum base material 1 may be 0.10 mass% or less.
  • the aluminum laminate 11 may further include a second anodic oxide film 3 provided to be in contact with the third surface 1B of the aluminum base 1.
  • the second anodic oxide film 3 has a fourth surface 3B at a position distant from the third surface 1B in the intersecting direction. That is, the aluminum laminate 11 includes the aluminum base 1 and the first anodic oxide coating 2 and the second anodic oxide coating 3 provided so as to sandwich the aluminum base 1.
  • the value T1 of the total thickness is the value T3 (unit: ⁇ m) of the thickness of the aluminum substrate 1 and the value T2 (unit: ⁇ m) of the thickness of the first anodic oxide film 2 And the thickness T2 (unit: ⁇ m) of the second anodic oxide film 3 in the intersecting direction.
  • the thickness of the second anodic oxide film 3 is equal to or less than the thickness of the first anodic oxide film 2.
  • the thickness of the second anodic oxide film 3 is 9 ⁇ m or more and 26 ⁇ m or less.
  • the aluminum laminate 11 satisfies the relational expression T1 + 10 ⁇ T2 ⁇ 450. That is, the aluminum laminated body 11 satisfies the relational expression T1 + 10 ⁇ T4 ⁇ T1 + 10 ⁇ T2 ⁇ 450.
  • the aluminum laminate 11 satisfying the above relational expression can exhibit the same effects as the aluminum laminate 10 according to the first embodiment, and has high bending workability.
  • the aluminum laminate 11 satisfies the relational expression T1 + 10 ⁇ (T2 + T4) ⁇ 450.
  • the surface layer including the third surface 1B of the aluminum base 1 has an aluminum purity of 99.9% by mass or more, 0.001% by mass or more, similarly to the surface layer including the first surface 1A. .052 mass% or less of iron is included.
  • Such an aluminum base 1 can be prepared by the same method as the steps (S10) to (S50) of the method for manufacturing the aluminum laminate 10 described above.
  • the second anodic oxide film 3 has the surface roughness Ra of the fourth surface 3B of 20 nm or less as in the case of the first anodic oxide film 2, and the average inter-relief distance RSm of the fourth surface 3B. Is less than 30 ⁇ m.
  • Such a second anodic oxide film 3 can be formed by the same method as the above step (S60) of the method of manufacturing the aluminum laminate 10 described above.
  • the second surface 2A of the first anodic oxide film 2 and the fourth surface 3B of the second anodic oxide film 3 have high glossiness, high total reflectance and high image clarity.
  • the composition of the surface layer including the third surface 1B of the aluminum base 1 may be different from the composition of the surface layer including the first surface 1A, but is preferably the same.
  • the aluminum substrate 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 therebetween, for example, as in a clad material. .
  • the aluminum base material obtained by final finish cold rolling is polished after the step (S50) and before the step (S60).
  • the process (S70) of processing may be implemented.
  • the surface of the aluminum base to be the first side 1A is polished to form the aluminum base 1 having the first side 1A.
  • the surface to be the first surface 1A and the surface to be the third surface 1B are polished to form the aluminum base 1 having the first surface 1A and the third surface 1B. Be done.
  • the polishing method may be selected from physical polishing, electro polishing, chemical polishing and the like, but is not limited thereto. Preferably, physical polishing is performed in this step (S70).
  • the step of forming the aluminum substrate obtained by the final finish cold rolling into a predetermined shape is performed after the step (S50) and before the step (S60). It may be done. Alternatively, after the step (S60), a step of molding the aluminum laminates 10 and 11 obtained in the step (S60) may be performed. Further, after the step (S60), a step of forming a film on at least one surface of the aluminum laminate 10, for example, on the third surface 1B of the aluminum base 1 may be performed.
  • the material constituting the film is at least one selected from the group consisting of resin, metal, ceramic and the like.
  • the film is, for example, an adhesive layer, and after the step of forming the film, the step of adhering the aluminum laminates 10 and 11 to another member or a wall or the like may be performed via the film. Further, after the step (S60), the porous portion of at least one of the first anodic oxide film 2 and the second anodic oxide film 3 of the aluminum laminates 10 and 11 obtained in the step (S60) is subjected to coloring treatment And, sealing treatment may be applied, or only sealing treatment may be applied.
  • the coloring treatment may be any method, but may be, for example, a method of adsorbing a dye or a pigment, or may be a secondary electrolytic coloring method.
  • samples of the reflecting members of the example of the present embodiment and the comparative example were manufactured, and their glossiness, total reflectance, image clarity and corrosion resistance were evaluated.
  • the aluminum substrates of Examples and Comparative Examples were produced according to the production steps shown below.
  • the aluminum ingot obtained by DC casting was subjected to homogenization heat treatment in a heating furnace. Then, it hot-rolled until thickness became about 6.5 mm. A plurality of cold rollings were performed on the obtained hot-rolled material until the thickness reached a predetermined value. A plurality of cold rolling steps were carried out with intermediate annealing interposed therebetween to produce an aluminum base having a thickness shown in Tables 1 and 2.
  • Example 1 to 9, 12 to 18 and Comparative Examples 1 to 12, 27, 28 in the final finish cold rolling rolling was performed using a rolling roll having a surface roughness Ra of 40 nm.
  • rolling was performed using a rolling roll having a surface roughness Ra of 50 nm in final finish cold rolling.
  • Comparative Examples 15 to 22 rolling was performed using a rolling roll having a surface roughness Ra of 100 nm in final finish cold rolling.
  • Comparative Examples 23 to 26 rolling was performed using a rolling roll having a surface roughness Ra of 150 nm in final finish cold rolling.
  • the surface to be the first surface of the aluminum substrate obtained by the final finish cold rolling (the surface rolled to the rolling roll)
  • electrolytic polishing was performed.
  • the electropolishing was performed by immersing the above aluminum substrate in an aqueous solution containing 60% by volume of phosphoric acid and 20% by volume of sulfuric acid at a bath temperature of 70 ° C. for 20 minutes under the condition of a current density of 2000 A / m 2 .
  • the homogenization heat treatment was performed under the conditions of a heating temperature of 400 ° C. or more and 630 ° C. or less and a heating time of 1 hour or more and 20 hours or less.
  • the intermediate annealing was performed under the conditions of an annealing temperature of 50 ° C. to 500 ° C. and an annealing time of 1 second to 20 hours.
  • Surface roughness Ra of the 1st surface of the aluminum base material of each Example was 15 nm or less.
  • the average inter-concave-convex distance RSm of the first surface of the aluminum base material of each example was 30 ⁇ m or less.
  • Anodizing treatment was performed on the aluminum base obtained as described above.
  • the electrolyte was an aqueous solution containing 15% by volume of sulfuric acid and having a bath temperature of 21 ° C.
  • Each sample was immersed in the electrolyte to form an anode, and a current density of 130 mA / m 2 was passed between the sample and the cathode for a predetermined time to carry out anodizing treatment.
  • the anodizing treatment time of each sample was taken as the time for obtaining an anodized coating layer of a predetermined thickness. That is, the anodizing conditions for each sample were the same except for the anodizing time.
  • sealing treatment was performed on all the samples under the same conditions.
  • the sealing treatment is carried out by immersing each sample on which an anodic oxide film is formed in an aqueous solution containing nickel acetate at a concentration of 5 g / L and oxalic acid at a concentration of 5 g / L at a bath temperature of 90 ° C. It was carried out by immersing in pure water for 20 minutes.
  • the thickness of the obtained anodized film was measured with a FTA 3.3H probe using a Fischer Instruments eddy current film thickness meter ISOSCOPE FMP10. Further, the thickness of the obtained aluminum laminate was measured by using a digital micrometer MDC-MX IP65 manufactured by Mitutoyo Corporation.
  • the observation of the surface asperity with an atomic force microscope was performed using a scanning probe microscope AFM 5000 II manufactured by Hitachi High-Tech Science Co., Ltd. with a surface shape of 80 ⁇ m ⁇ 80 ⁇ m in a rectangular force field mode (noncontact) mode.
  • the inclination of the sample was corrected by cubic slope automatic inclination correction which performs fitting by obtaining a curved surface by least square approximation, and the surface roughness Ra was measured.
  • the surface roughness Ra is calculated by extending the arithmetic mean 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 surface asperity distance RSm was measured using the SURFCOM 1400D manufactured by Tokyo Seimitsu Co., Ltd.
  • the arithmetic surface asperity distance RSm defined in JIS B0601 (2001 edition) and ISO 4287 (1997 edition) was measured.
  • the measurement type is roughness measurement, shape removal is the least-squares linear method, the evaluation length is 4 mm, the cutoff type is 2RC phase non-assisted, and the cutoff wavelength ⁇ c is 0.1 ⁇ m Ra obtained in this measurement In the case of less than 0.25 mm, and in the case of 0.1 ⁇ m or more, it was measured as 0.8 mm.
  • the measurement was performed in two directions of the rolling direction (RD) and the direction (TD) perpendicular to the rolling direction, and the values in each direction were evaluated.
  • the glossiness was measured using a Gloss meter VG7000 manufactured by Nippon Denshoku Kogyo Co., Ltd. at a light incident angle of 60 °.
  • the glossiness was measured in two directions, ie, the rolling direction (RD) and the direction perpendicular to the rolling direction (TD), and the values in each direction were evaluated. The higher the degree of gloss, the metallic gloss is obtained.
  • the total reflectance is measured using a UV-visible spectrophotometer V570 manufactured by JASCO Corporation, using a standard white plate Spectralon for integrating sphere manufactured by Labsphere as a reference, in the wavelength range of 250 nm to 2000 nm. It was measured. From the obtained total reflectance measurement values, an average value of visible light in a wavelength range of 400 nm to 800 nm was determined. The measurement of the total reflectance was measured in two directions of a rolling direction (RD) and a direction (TD) perpendicular to the rolling direction, and the total reflectance was evaluated as an average value of these.
  • RD rolling direction
  • TD direction
  • an all-in-one gloss meter IQ3 manufactured by RHOPOINT INSTRUMENTS was used, and a DOI value according to ASTM D5767 was evaluated as image clarity.
  • the measurement was performed in two directions of the rolling direction (RD) and the direction (TD) perpendicular to the rolling direction, and the values in each direction were evaluated.
  • the surface hardness was evaluated by Vickers hardness.
  • the Vickers hardness in the direction (depth direction) intersecting with the second surface of the anodic oxide film of each of the obtained Examples and Comparative Examples was measured.
  • the Vickers hardness was determined by using a Vickers hardness tester HMV-1 manufactured by Shimadzu Corporation with the scratch resistance of the surface as an index, and pressing the test force at 490.3 mN for 5 seconds under a pressure with a diamond indenter. Conducted and obtained HV0.05 value.
  • the corrosion resistance was subjected to a cass test and evaluated according to the following contents.
  • the Cass test was conducted under the test conditions described in JIS H8681-2 (1999), and the test time was assumed for outdoor use with reference to the application example described in Section 6.2.2 of JIS H8601 (1999). It was 32 hours. Evaluation is based on the criteria described in JIS H8681-2 (1999 edition), and as described in JIS H8601 (1999 edition) section 6.3, passing rating number 9 or higher (A in Tables 3 and 4), rating number 9 Less than is considered as rejection (F in Tables 3 and 4).
  • the bending workability was evaluated by observing the presence or absence of a crack in each anodic oxide film for each of the above-described samples subjected to bending.
  • test pieces of each example and comparative example were cut out in a rolling direction (RD) of 100 mm and 150 mm in a direction (TD) perpendicular to the rolling direction. Furthermore, a plurality of cylinders having different diameters in stages were prepared. Next, each piece cut out was put 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. When no cracks were found in the anodized film in visual observation, the surface of the anodized film was observed visually after being held for 10 seconds along the outer peripheral surface of the cylinder having a diameter smaller than that of the previously used cylinder.
  • the minimum diameter in Tables 3 and 4 shows the minimum value (unit: mm) of the diameter of the cylinder used for the above-mentioned bending processing in which a crack was not confirmed in an anodic oxide film about each specimen.
  • FIG. 5 is a graph showing the results of the bending test, the horizontal axis shows the value of the left side T1 + 10 ⁇ T2 of the above-mentioned relational expression of each sample, and the vertical axis shows the minimum diameter in Table 3 and Table 4 Unit: mm) is shown.
  • the inventors used the above-mentioned bending in which no crack was found in the anodic oxide film in the bending test for each of the samples of Examples 1 to 18 and Comparative Examples 1 to 28.
  • the shortest value (unit: mm) of the diameter of the cylinder is the value of the total thickness of the aluminum base material and the anodized film in the intersecting direction as T1, and the value of the thickness of the anodized film in the intersecting direction as T2. It was found to be correlated with the value T1 + 10 ⁇ T2 at the time of The correlation coefficient R 2 was over 0.92. As shown in FIG.
  • the first anodic oxide film 2 has cracks. It was not confirmed. Furthermore, in the embodiments 6, 8, 12, 13 and 15 in which the above value T1 + 10 ⁇ T2 is 300 or less, the first anodized film 2 is obtained by bending along the outer peripheral surface of the cylinder having a diameter of 80 mm. No cracks were observed. On the other hand, in Comparative Examples 9, 10, 16 to 18, 20 to 22, 27, 28 not satisfying the above relational expression, the anodized film is formed by bending along the outer peripheral surface of a cylinder having a diameter of 100 mm or more. Crack was confirmed.
  • the present inventors confirmed that high bending workability is realized as long as the above-mentioned relational expression is satisfied even if the thickness T2 of the anodized film is a relatively thick aluminum laminate of 9 ⁇ m or more.
  • Example 17 the thickness of the anodized film is 17.5 ⁇ m as in Comparative Example 9, but the thickness of the aluminum base is 100 ⁇ m smaller than that of Comparative Example 9.
  • Example 17 satisfying the above relational expression no crack was observed even when wound around the outer periphery of a cylinder having a diameter of 73 mm in a bending test.
  • Comparative Example 9 not satisfying the above relational expression a crack was confirmed when wound around the outer periphery of a cylinder having a diameter of 100 mm in a bending test.
  • 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 substrate and the anodized film.
  • Anodized films have lower ductility than aluminum substrates. Therefore, the anodized film is considered to have a high influence on the bending processability as compared to the aluminum base.
  • the bendability does not significantly change depending on the increase or decrease.
  • Example 7 the aluminum substrate 1 is 140 ⁇ m thicker than in Example 12, but the anodized film has the same thickness, and it satisfies the above-mentioned relational expression as in Example 12. is there. In Example 7, no crack was observed even when wound around the outer circumference of a cylinder having a diameter of 96 mm in a bending test.
  • Comparative Example 9 the thickness and the like of the aluminum base are equal to those in Examples 6 and 7, but only the thickness T2 is thicker by about 8 ⁇ m and does not satisfy the above relational expression It is. As described above, in Comparative Example 9, cracks were observed when wound around the outer periphery of a cylinder having a diameter of 100 mm in a bending test.
  • Examples 1 to 18 each have an aluminum base containing 99.9% by mass or more and 0.001% by mass or more and 0.052% by mass or less of iron, and an aluminum base having a thickness of 9 ⁇ m or more and 26 ⁇ m or less.
  • the surface roughness Ra of the two surfaces is 20 nm or less, and the average inter-recession distance RSm in the RD direction and the TD direction of the second surface is less than 30 ⁇ m.
  • Examples 1 to 18 the glossiness is 63% or more in the RD direction and the TD direction, the visible light total reflectance is 83% or more, and the DOI value is 80 or more in the RD direction and the TD direction. , High total reflectance and high image clarity and high bending workability. Furthermore, Examples 1 to 18 pass the Vickers hardness of 300 HV or more, pass the Cass test, have high corrosion resistance, and in Examples 1 to 18, the thickness of the anodic oxide film is in the range of 9 ⁇ m to 26 ⁇ m. No tendency was observed that the gloss, the visible light total reflectance, and the image clarity decreased with the increase of.
  • Comparative Examples 1 to 12, 27 and 28 have the same conditions of final finish cold rolling as Examples 1 to 9 and 12 to 18, but at least the chemical composition of aluminum, the thickness of the aluminum base, The presence or absence of electrolytic polishing, the thickness of the anodized film, and any of the above-mentioned relational expressions do not satisfy the above-mentioned respective numerical ranges.
  • Comparative Example 1 in which the aluminum purity of the aluminum base is 99.9% by mass or more but the Fe content of the aluminum base is more than 0.052% by mass has a glossiness of less than 63%, and a high glossiness Did not have. This is considered to be due to the fact that a large amount of intermetallic compound containing Fe is crystallized on the first surface of the aluminum base of Comparative Example 1, thereby reducing the gloss of the aluminum base.
  • Comparative Examples 10 in which only the thickness of the anodized film is different from those in Examples 6 and 7 and the thickness exceeds 26 ⁇ m have a Vickers hardness of 290 HV or less, a low surface hardness, and a sufficiently high corrosion resistance Not scratchable).
  • Comparative Examples 13 and 14 in which only the thickness of the anodized film is different from Examples 10 and 11 and the thickness is less than 9 ⁇ m, the glossiness in the TD direction is less than 63%, and the total visible light reflectance is 83. It was less than 10% and did not have high glossiness and high visible light total reflectance. It is considered that this is due to the interference of the light incident on the second surface of the anodized film with the light reflected on the first surface of the aluminum base and the light reflected on the second surface of the incident light. Furthermore, Comparative Examples 13 and 14 had Vickers hardness of 290 HV or less, failed the cast test, and did not have high corrosion resistance.
  • Comparative Examples 15 to 18 the surface roughness Ra of the second surface of the anodized film was more than 20 nm, and the average inter-recession distance RSm in the RD direction and the TD direction of the second surface was 30 ⁇ m or more.
  • the Comparative Examples 15 to 18 had glosses of less than 63% in the RD direction and TD direction and less than 83% of the total visible light reflectance, and did not have high glossiness and high total visible light reflectance. Furthermore, in Comparative Examples 15 to 18, it was confirmed that the DOI value in the TD direction tends to decrease as the thickness of the anodized film increases. In Comparative Examples 16 to 18 in which the thickness of the anodized film was 7.2 ⁇ m or more, the DOI value in the TD direction was 80 or less, and did not have high image clarity.
  • Comparative Examples 19 to 22 although the surface roughness Ra of the second surface of the anodized film is 20 nm or less, the average inter-recession distance RSm in the RD direction and the TD direction of the second surface is 30 ⁇ m or more.
  • the average inter-concave-convex distance RSm in the TD direction of the surface was longer than the average inter-concave-convex distance RSm in the TD direction and was 57 ⁇ m or more.
  • the comparative examples 19 to 22 had DOI values of less than 80 in the TD direction and did not have high image clarity. Furthermore, in Comparative Examples 19 to 22, it was confirmed that the Vickers hardness tends to decrease as the thickness of the anodized film becomes thinner. Comparative Examples 19 and 20 in which the thickness of the anodized film was less than 9 ⁇ m had a Vickers hardness of 290 HV or less, failed the cast test, and did not have high corrosion resistance.
  • Comparative Examples 23 to 26 the surface roughness Ra of the second surface of the anodized film was over 74 nm, and the average inter-recession distance RSm in the RD direction and the TD direction of the second surface was 30 ⁇ m or more. In particular, the average inter-concavity and convexity distance RSm in the TD direction of the second surfaces of Comparative Examples 23 to 26 was 300 ⁇ m or more. In Comparative Examples 22 to 25, the glossiness in the RD direction and the TD direction is less than 63%, the visible light total reflectance is less than 83%, and the DOI value in the TD direction is 80 or less. It did not have reflectivity and high image clarity.
  • the present embodiment can provide an aluminum laminate having high glossiness, high total reflectance and high image clarity and high corrosion resistance.
  • the aluminum laminate according to the present embodiment is particularly suitable for a reflector for lighting and a panel for a building material used in a corrosive environment including a large amount of moisture and water such as a kitchen or outdoor.
  • SYMBOLS 1 aluminum base material, 1A 1st surface, 1B 3rd surface, 2 1st anodized film, 2A 2nd surface, 3 2nd anodized film, 3B 4th surface, 4 board

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