WO2017006816A1 - 陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材及びその製造方法 - Google Patents
陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材及びその製造方法 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
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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
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- 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
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- 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
- C22F1/053—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 of alloys with zinc as the next major constituent
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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
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- 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
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- the present invention relates to an aluminum alloy extruded material having an anodized film and excellent in appearance quality, and a method for producing the same, and more particularly, to an aluminum alloy extruded material for an electronic device casing excellent in anodized film property and a method for producing the same. .
- the metal structure is a recrystallized structure
- the streak pattern is reduced, but sufficient aesthetics cannot be obtained.
- the inventor of the present application has conducted extensive research on the cause of streak patterns.
- concentration segregation of elements other than aluminum in the crystal and at the grain boundaries, the crystallization state of the compound, and the recrystallization It was found that the difference in grain size between crystal structures greatly affected.
- the portion where elements other than aluminum are segregated and the portion where there is a crystallized product tend to form an anodic oxide film less easily than other portions. This is considered to be due to the difference in electrical properties due to the effect of concentration segregation. That is, the peritectic elements are concentrated in the crystal grains, the eutectic elements are swept out to the crystal grain boundaries, and concentration segregation occurs between the crystal grains and the crystal grain boundaries.
- the concentration segregation part When extruded, the concentration segregation part is stretched in the extrusion direction as well as the crystal grains of the cast structure, and a thin layer of Zn, Mg main element concentration segregation is formed in a streak shape, and the thickness of the anodized film Is considered to be a cause of visible streaks on the surface of the anodized film.
- crystallized substances are present, but as crystal grains are stretched by extrusion, such crystallized substances are scattered in the extrusion direction, which causes streaks.
- the cast structure is stretched to become a fiber-like structure.
- the concentration segregation part and the crystallized material are also stretched. Even if recrystallization is performed and the crystal structure changes from a fiber-like structure to a recrystallized structure that is equiaxed, the concentration segregation part and the crystallized phase remain and are stretched, so the anodized film It is thought that streaks are visible when processing is performed. Further, it was found that the recrystallized structure also has a streaky portion where crystals with a large difference in crystal grain size are mixed.
- the inventor of the present application has a high strength of 380 MPa or more, but the concentration segregation, excessive crystallization of the compound, and the crystal grain size of the recrystallized structure.
- the range of the optimal alloy composition that suppresses the difference was found.
- An object of the present invention is to provide a 7000 series aluminum alloy extruded material that has a desired strength and is less likely to cause a streak pattern on the surface of an anodized film.
- an aluminum alloy extruded material Zn: 4.0 mass% or more and 7.5 mass% or less, Mg: 1.0 mass% or more and 2.2 mass% or less, Fe: 0.05 mass% or more and 0.20 mass% or less, Cu: 0.30 mass% or less, Ti: 0.005 mass% or more and 0.04 mass% or less, B: 0.001% by mass or more and 0.02% by mass or less, Si: 0.15 mass% or less, Zr: 0.05% by mass or less, Mn: 0.05% by mass or less, Cr: 0.05% by mass or less, V: 0.05 mass% or less, Containing [Zr + Mn + Cr + V + Ti], which is the total content of Zr, Mn, Cr, V and Ti, [Zr + Mn + Cr + V + Ti] ⁇ 0.10 mass% Satisfy the relationship Except for the range where the Zn content is 6.0% by mass or less and the Mg content is 1.2% by mass or less, The balance consists of aluminum and
- a Zn high-concentration phase and a Zn low-concentration phase are present in layers in the anodized surface in parallel to the extrusion direction, and are orthogonal to the extrusion direction.
- the Zn concentration difference is 1% or less in a range of width 0.1 mm or more and 3 mm or less.
- the crystal grain size of the recrystallized structure on the treated surface of the anodized film is an average value of 200 ⁇ m or less, and the maximum crystal grain size is 1 mm or less.
- the aluminum alloy extruded material is characterized in that the area ratio of the intermetallic compound (crystallized product) in the anodized surface is less than 2%.
- the cast material is processed for 1 to 24 hours at a holding condition of the homogenization treatment of 400 to 560 ° C., and the extrusion ratio exceeds 20 in the extrusion process.
- a method for producing an extruded aluminum alloy characterized in that extrusion is performed so that the temperature of the material is 420 ° C. or higher, and the aging treatment is performed at 100 to 180 ° C. for 1 to 30 hours.
- a 7000 series aluminum alloy extruded material having a desired strength and excellent in appearance quality in which a streak pattern is difficult to appear on the surface of an anodized film, and a manufacturing method thereof.
- FIG. 4 is a photograph of the crystal structure of Experimental Example L taken with a polarizing microscope. 4 is a photograph of the crystal structure of Experimental Example H taken with a polarizing microscope. 6 is a photograph of the microstructure of Experimental Example K taken.
- A A graph showing a concentration analysis of Experimental Example B and (b) a mapping diagram. 10 is a graph showing a concentration analysis of Experimental Example G.
- A A graph showing concentration analysis of Experimental Example H and (b) a mapping diagram.
- the aluminum alloy extruded material having an anodized film according to this embodiment is an aluminum alloy extruded material, Zn: 4.0 mass% or more and 7.5 mass% or less, Mg: 1.0 mass% or more and 2.2 mass% or less, Fe: 0.05 mass% or more and 0.20 mass% or less, Cu: 0.30 mass% or less, Ti: 0.005 mass% or more and 0.04 mass% or less, B: 0.001% by mass or more and 0.02% by mass or less, Si: 0.15 mass% or less, Zr: 0.05% by mass or less, Mn: 0.05% by mass or less, Cr: 0.05% by mass or less, V: 0.05 mass% or less, Containing [Zr + Mn + Cr + V + Ti], which is the total content of Zr, Mn, Cr, V and Ti, [Zr + Mn + Cr + V + Ti] ⁇ 0.10 mass% Satisfy the relationship Except for the range where the Zn content is
- the aluminum alloy extruded material having the above-described configuration has a desired strength and an effect that a streak pattern is difficult to appear on the surface of the anodized film. Below, each element which concerns on the aluminum alloy extrusion material of this embodiment is demonstrated.
- the aluminum alloy extruded material according to the present embodiment has a Zn content of 4.0% by mass to 7.5% by mass, more preferably 4.0% by mass to 7.0% by mass, More preferably, it is 4.0 mass% or more and 6.0 mass% or less, More preferably, it is 4.0 mass% or more and less than 5.5 mass%, Most preferably, it is 4.0 mass% or more and 5.0 mass%. % Or less.
- the Mg content is 1.0% by mass or more and 2.2% by mass or less, more preferably 1.2% by mass or more and 2.2% by mass or less. More preferably, it is 1.3 mass% or more and 2.2 mass% or less, More preferably, it is 1.4 mass% or more and 2.2 mass% or less, Most preferably, it is 1.5 mass% or more and 2.2 mass% or less. % Or less.
- the Zn content is 6.0% by mass or less
- the Mg content is 1.2% by mass or more, and when the Zn content is less than 5.5% by mass, the Mg content is 1.6% by mass. The above is preferable.
- the Fe content is 0.05% by mass or more and 0.20% by mass or less.
- the Fe content is 0.05% by mass or more, coarse recrystallization of the cast structure can be suppressed during the homogenization treatment. If there is a coarse crystal structure in the ingot, non-uniform deformation is likely to occur during the extrusion process, and it becomes difficult to keep the dimensions of the extruded material within a predetermined size (accuracy, twist and bend). Furthermore, if there is a coarse crystal structure in the billet, recrystallized grain structures having different sizes are likely to be mixed even in an equiaxed recrystallized structure during recrystallization after extrusion. Such a structure is arranged in layers, which causes a difference in color tone in a stripe shape.
- the content of Fe is 0.20% by mass or less, it can be suppressed that Fe forms a compound with other elements to form an excessive crystallized product and a streak pattern is generated.
- the Fe content is more preferably 0.15% by mass or less, and the above effect is further enhanced within this range.
- the Cu content is 0.30 mass% or less. If the Cu content exceeds 0.30% by mass, the anodized film tends to be yellowish and the corrosion resistance tends to deteriorate.
- the Cu content is more than 0.15% by mass, mechanical strength and stress corrosion cracking resistance (SCC) are improved.
- the Ti content is 0.005 mass% or more and 0.04 mass% or less. Further, in the aluminum alloy extruded material according to this embodiment, the content of B is 0.001% by mass or more and 0.02% by mass or less.
- the crystal of the cast structure in the alloy is coarse, non-uniform deformation is likely to occur during extrusion, and concentration segregation and non-uniform grain size of the recrystallized structure are likely to occur. At this time, it is added as a grain refiner. When only Ti is added, it dissolves in the matrix phase and the effect as a finer becomes small. Further, since concentration segregation inside the crystal tends to occur, it is preferable to add as a TiB 2 compound using a rod hardener as a refining agent. On the other hand, excessive addition of Ti or B causes excessive crystallization as a compound and causes streak patterns, so the upper limit of the addition amount is required.
- the Si content is 0.15% by mass or less. Since Si forms a Mg and Mg—Si-based compound and contributes to the streak pattern, it is preferably regulated to 0.15% or less. Moreover, it is more preferable that content of Si is 0.1 mass% or less. If content of Si is this range, said effect will increase more.
- Zr zirconium, Mn: manganese, Cr: chromium, V: vanadium
- Mn, Cr, and V have an action of suppressing recrystallization during extrusion, their content is preferably 0.05% by mass or less, more preferably 0.02% by mass or less. It is.
- These elements also have the effect of suppressing the diffusion of Zn.
- [Zr + Mn + Cr + V + Ti] which is the total content of Zr, Mn, Cr, V and Ti, preferably satisfies the relationship [Zr + Mn + Cr + V + Ti] ⁇ 0.10 mass%. If the amount added exceeds the specified range, recrystallization will be suppressed and a non-recrystallized structure may be formed, and grain growth may occur. Therefore, even if all are added, the content is preferably 0.10% by mass or less, more preferably 0.09% by mass or less, and still more preferably 0.08% by mass or less. More preferably, it is 0.07 mass% or less, Most preferably, it is 0.05 mass% or less.
- the crystal structure is preferably a recrystallized structure having a uniform crystal grain size.
- the alloy components, casting HO conditions, and extrusion conditions are controlled.
- the form of the crystal structure can be confirmed by a method of coating with a borohydrofluoric acid aqueous solution and observing with a polarizing microscope.
- the aluminum alloy extruded material according to this embodiment is excellent in anodized film property and is preferably used as a housing material for electronic equipment.
- the method for producing an aluminum alloy extruded material according to another embodiment of the present invention is an aluminum alloy extruded material, which is Zn: 4.0% by mass to 7.5% by mass, Mg: 1.0% by mass to 2%. 0.2 mass% or less, Fe: 0.05 mass% or more and 0.20 mass% or less, Cu: 0.30 mass% or less, Ti: 0.005 mass% or more and 0.04 mass% or less, B: 0.001 % By mass or more and 0.02% by mass or less, Si: 0.15% by mass or less, Zr: 0.05% by mass or less, Mn: 0.05% by mass or less, Cr: 0.05% by mass or less, V: 0.00%.
- [Zr + Mn + Cr + V + Ti] which is a total of the contents of Zr, Mn, Cr, V and Ti, [Zr + Mn + Cr + V + Ti] ⁇ 0.10 mass% Except for the range where the Zn content is 6.0 mass% or less and the Mg content is 1.2 mass% or less, the balance is made of aluminum and inevitable impurities, and the metal structure is a recrystallized structure.
- a method for producing an aluminum alloy extruded material having an anodized film The casting material is processed at a holding condition of homogenization treatment at 400 to 560 ° C.
- the aging treatment step is characterized by treating at 100 to 180 ° C. for 1 to 30 hours.
- a molten aluminum alloy having the above alloy composition is prepared, and a known molten metal treatment such as degassing treatment, degassing treatment, and filtering is performed. Then, a cylindrical ingot (billet) is obtained by a DC casting method or the like.
- a micronizing agent made of an Al-Ti-B alloy into the molten metal.
- the finer added to the molten metal is preferably such that Ti and B do not exceed the above ranges in the alloy composition.
- the molten metal is preferably poured into the mold uniformly so that the casting temperature is uniform in the mold.
- HOT TOP (hot top) casting or the like is preferably used.
- the billet diameter is small, preferably 14 inches or less.
- the diameter of the billet is large, cooling of the billet center portion is slowed, and the structure of the billet center portion tends to be coarse. If the cast structure is coarse, it is difficult not only to eliminate concentration segregation during the homogenization process, but also to make the crystal structure finer in the extrusion process.
- the billet obtained in the casting process is subjected to a homogenization process (HO process).
- HO process homogenization process
- the homogenization temperature is preferably 400 to 560 ° C. for 1 hour to 24 hours. If the condition of the homogenization treatment is within this range, the homogenization is sufficiently performed.
- the homogenization temperature for 24 hours exceeds 560 ° C., the ingot crystal grows, the extrudability is lowered, the crystal grains of the extruded material are coarsened, and the recrystallized structure is locally coarsened, The difference in the grain size of the recrystallized structure becomes large, and a pattern is generated during the anodic oxide coating.
- the homogenization temperature is more preferably 540 ° C. or lower. Even if the homogenization treatment is performed for more than 24 hours, no further effect can be expected and only the production cost is required.
- homogenization is preferably performed at 470 ° C. or higher, and more preferably at 500 ° C.
- the cooling rate after the homogenization treatment is low, the solid solution element is likely to be precipitated. Therefore, it is preferable to cool at an average cooling rate from the HO temperature to 150 ° C. at 100 ° C./h or more.
- the billet that has been subjected to the homogenization treatment is extruded to obtain a predetermined processed material.
- the extrusion ratio in the extrusion process is preferably 20 or more.
- the extrusion ratio in the extrusion process is more preferably 40 or more. This is because the extension of the crystal causes a gradual change in concentration (concentration segregation is likely to be improved if the interval between high-concentration parts or low-concentration parts is close), and the appearance after the anodized film is a streak pattern. It is because it becomes difficult to generate
- the formation of streaks due to the difference in crystal structure can be suppressed by setting the average grain size to 200 ⁇ m or less and the maximum crystal grain size to 1 mm or less. Since the crystal size of the extruded material becomes finer as the billet temperature is extruded at a lower temperature, the billet temperature is desirably set in consideration of the extrusion pressure and the shape material temperature, and is preferably 480 ° C. or less.
- the extrusion conditions (billet temperature, die temperature, container temperature, extrusion pressure, extrusion speed, etc.) such that the temperature at the die outlet is 400 ° C. or higher. If the temperature of the extruded material at the die outlet is low, high strength may not be obtained.
- the extruded material after coming out of the die is cooled so that the cooling rate in the temperature range of up to 200 ° C. after the extrusion is 0.3 to 20 ° C./s. If the cooling rate satisfies this condition, high strength can be obtained and good stress corrosion cracking resistance can be obtained.
- Aging treatment is performed on the extruded material.
- the holding temperature in the aging treatment step is 1 to 30 hours under the condition of 100 to 180 ° C.
- the aging treatment may be performed in two stages in order to obtain higher strength and stress corrosion cracking resistance.
- An extruded material obtained by sequentially passing through a casting process, a homogenization process, an extrusion process, and an aging process is cut into a predetermined shape and then anodized.
- the anodized film treatment is performed under known conditions.
- the homogenization treatment step is performed at a holding temperature of 400 ° C. to 560 ° C.
- the extrusion step is performed at an extrusion ratio of 20 or more. It is characterized in that the outlet temperature is 420 ° C. or higher, the cooling rate between after extrusion and 200 ° C. is 0.3 to 20 ° C./s, and the aging treatment step is performed under the condition of holding temperature 100 ° C. to 180 ° C.
- a method for producing an aluminum alloy extruded material having an anodic oxide coating is provided.
- Billets having the components of Experimental Examples A to N shown in [Table 1] below were obtained.
- the diameter of the billet was 325 mm.
- These billets were subjected to HO treatment under the conditions of [Table 2] and then extruded under the conditions of [Table 2].
- Extrusion was performed under the condition of a billet temperature of 400 ° C., (a) was a flat bar with a width of 100 mm and a thickness of 10 mm, and (b) was performed with two extruded shapes, a flat bar with a width of 120 mm and a thickness of 25 mm.
- heat treatment was performed under the conditions described in Table 2. After the heat treatment, tempering was performed under the conditions of A to J and L to N for T5 (after extrusion, artificial aging) and K for T6 (after solution treatment, artificial aging).
- the crystal grain size after casting and after HO was measured by the cross line method, and those having crystal grains with a size exceeding 1 mm were marked as x.
- the intersecting line method means that a straight line is drawn in an arbitrary direction from an image taken with an optical microscope, and the number of crystal grain boundaries intersecting with the straight line is n, and the length of the straight line is divided by (n-1). Thus, the average crystal grain size is calculated.
- the surface of the aluminum alloy test material was chamfered (buffed) in an amount corresponding to 20% of the wall thickness, and the anodized film treatment was performed on the chamfered surface.
- the treatment conditions for the anodized film treatment were 1.5 A / dm 2 in a 15% sulfuric acid aqueous solution at 20 ° C., and the film thickness was about 5 ⁇ m.
- the color tone was judged based on the fact that the gloss retention before and after the treatment was 40% or more, and the L value was 78 or more and the b value was 1 or less. Those satisfying the above values were marked with ⁇ , and those not satisfying were marked with x. In addition, the presence or absence of streak patterns was evaluated. In “ ⁇ ”, a streak pattern hardly occurred, and in “ ⁇ ”, a thin streak pattern was observed in a limited part. In “X”, a dark streak pattern was generated. The color tone is based on the value of JIS Z8730.
- the surface of the aluminum alloy test material was chamfered in an amount corresponding to 20% of the wall thickness, and the mirror surface was polished and coated with a borohydrofluoric acid aqueous solution.
- the structure was observed with a polarizing microscope to determine the structure.
- the observation surface is an L-LT surface (a wide surface among the surfaces parallel to the extrusion direction).
- a to G and L to N were equiaxed crystals in which recrystallized structures were observed, and the aspect ratio (average crystal diameter in the extrusion length direction / average crystal diameter in the direction perpendicular to the extrusion) was 2 or less.
- the aspect ratio average crystal diameter in the extrusion length direction / average crystal diameter in the direction perpendicular to the extrusion
- HK it was a fiber-like crystal structure.
- a to E and G, M, and N in which recrystallized structures were observed had uniform fine crystals with an average grain size of 200 ⁇ m or less measured by the intersection method. Coarse crystal grains exceeding 1 mm were present. Crystal growth is confirmed in the ingot structure after F and L HO, and this is the effect.
- the surface of the aluminum alloy test material was chamfered in an amount corresponding to 20% of the wall thickness, and after polishing to a mirror surface, the area occupied by the crystallized material was measured with an image analyzer and an optical microscope.
- the observation surface is an L-LT surface (a wide surface among the surfaces parallel to the extrusion direction).
- Stress corrosion cracking test Only A to E, M, and N were subjected to stress corrosion cracking tests in accordance with JIS H8711.
- a stress corresponding to 50% of 0.2% proof stress was applied in the direction perpendicular to the extrusion direction.
- the corrosive solution was immersed in 3.5% NaCl at 25 ° C. for 10 minutes and then dried for 50 minutes for one cycle.
- the test was conducted for 30 days, and the material without cracks was set as a pass “ ⁇ ”. A, M, and N are inferior in the results of the SCC test, which is thought to be due to the low Cu content.
- FIG. 2 shows the microstructure of Experimental Example B (Inventive Example). It can be seen that the crystallized substance is diffused and no extreme continuity of the compound is observed.
- 3 (a) and 3 (b) are obtained by observing the crystal structure of the sample cross section of Experimental Example L (Comparative Example) with a polarizing microscope. It can be seen that the size of the crystal grains varies depending on the observation location, and partially coarse crystal grains are formed. This is because the recrystallized structure is locally coarsened depending on the temperature condition of the HO treatment.
- FIG. 4 is an observation of the crystal structure of Experimental Example H (Comparative Example). It can be seen that the crystal structure is a fiber structure.
- FIG. 5 is an observation of the microstructure of Experimental Example K (Comparative Example). The content of Fe, Cu, Mg and Cr is large, and the portion where the crystallized material segregates is stretched by extrusion processing, and the continuity of the compound can be seen in a streak shape.
- FIG. 6 is a graph showing a Zn concentration analysis and mapping diagram of Experimental Example B (Inventive Example). Zn concentration segregation in a width of 3 mm is 1.0% by mass or less.
- FIG. 7 is a graph showing the Zn concentration distribution of Experimental Example G (Comparative Example), and FIG. 8 is a graph showing the Zn concentration distribution and mapping diagram of Experimental Example H (Comparative Example).
- Experimental Examples G and H which are comparative examples, have locations where concentration segregation in which the Zn concentration exceeds 1.0 mass% occurs within a width of 3 mm. Further, it can be seen from the mapping diagram that the concentration segregation is layered.
- an aluminum alloy extruded material that satisfies these conditions can be preferably used for a housing of an electronic device such as a portable personal computer, a mobile phone, and a smartphone.
- the extrusion ratio of A to D, M, and N is larger than that of E, that is, the degree of processing is high, so that the surface uniformity is higher.
- G has a lack of Ti and B which are crystal refining agents during casting, and the ingot structure after casting becomes coarse.
- concentration segregation of Zn is not sufficiently eliminated, and concentration segregation occurs in which the Zn concentration difference exceeds 1% in the range of more than 0.1 mm and 3 mm or less. Streaks occurred after the oxide film treatment.
- the Zr addition amount exceeds the upper limit, and the diffusion of Zn is inhibited by Zr because the crystal structure of the extruded material is maintained in the fiber structure due to the pinning effect, and even when homogenization is performed. Zn concentration segregation was not sufficiently eliminated, and streaks were generated after the anodic oxide film treatment of the extruded material. Furthermore, although I has a high Zn content, the mechanical strength is low even in a fiber structure because the Mg content is low.
- J also has a Zr addition amount, a Cr addition amount, and a Mn addition amount exceeding the upper limit values, and the diffusion of Zn is inhibited by the fact that the crystal structure of the extruded material is maintained in the fiber structure due to the pinning effect, and Zr is homogeneous. Zn concentration segregation is not sufficiently eliminated even when the oxidization treatment is performed, and concentration segregation in which the Zn concentration difference exceeds 1% occurs in the range of more than 0.1 mm and 3 mm or less. There has occurred.
- J has a high Mg content
- the mechanical strength is low even in a fiber structure because the Zn content is low.
- the Mn content is large, the crystal structure of the extruded material is maintained in the fiber structure due to the pinning effect, and the diffusion of Zn is inhibited by Mn. Even if homogenization is performed, the Zn concentration is sufficiently segregated. However, concentration segregation in which the Zn concentration difference exceeded 1% occurred in a range exceeding 0.1 mm and 3 mm or less, and streaks were generated after the anodic oxide film treatment of the extruded material.
- the HO temperature exceeded the upper limit temperature, and the crystal structure of the ingot grew.
- some crystal grains exceeding 1 mm were generated, and the crystal grain size of the extruded material was uneven.
- streaks were generated after the anodized film treatment.
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Abstract
Description
また、再結晶組織においても、結晶粒径の差が大きい結晶が混在している箇所も筋状に見えることがわかった。
Zn:4.0質量%以上7.5質量%以下、
Mg:1.0質量%以上2.2質量%以下、
Fe:0.05質量%以上0.20質量%以下、
Cu:0.30質量%以下、
Ti:0.005質量%以上0.04質量%以下、
B:0.001質量%以上0.02質量%以下、
Si:0.15質量%以下、
Zr:0.05質量%以下、
Mn:0.05質量%以下、
Cr:0.05質量%以下、
V:0.05質量%以下、
を含有し、
Zr、Mn、Cr、V及びTiの含有量の合計である[Zr+Mn+Cr+V+Ti]が、
[Zr+Mn+Cr+V+Ti]≦0.10質量%
の関係を満たし、
Znの含有量が6.0質量%以下かつMgの含有量が1.2質量%以下の範囲を除き、
残部がアルミニウムと不可避不純物からなり、
金属組織が再結晶組織である陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材が提供される。
本実施形態に係る陽極酸化皮膜を有するアルミニウム合金押出材は、アルミニウム合金押出材であって、
Zn:4.0質量%以上7.5質量%以下、
Mg:1.0質量%以上2.2質量%以下、
Fe:0.05質量%以上0.20質量%以下、
Cu:0.30質量%以下、
Ti:0.005質量%以上0.04質量%以下、
B:0.001質量%以上0.02質量%以下、
Si:0.15質量%以下、
Zr:0.05質量%以下、
Mn:0.05質量%以下、
Cr:0.05質量%以下、
V:0.05質量%以下、
を含有し、
Zr、Mn、Cr、V及びTiの含有量の合計である[Zr+Mn+Cr+V+Ti]が、
[Zr+Mn+Cr+V+Ti]≦0.10質量%
の関係を満たし、
Znの含有量が6.0質量%以下かつMgの含有量が1.2質量%以下の範囲を除き、
残部がアルミニウムと不可避不純物からなり、
金属組織が再結晶組織であることを特徴とする。
以下に、本実施形態のアルミニウム合金押出材に係る各元素について説明する。
Zn及びMgは、Zn‐Mg相として析出し、合金の高強度化に寄与する。Znの含有量が4.0質量%以上の場合、十分な強度を得ることができ、Znの含有量が7.5質量%以下であれば、良好な耐食性が得られる。
本実施形態に係るアルミニウム合金押出材は、Znの含有量が、4.0質量%以上7.5質量%以下であり、より好ましくは4.0質量%以上7.0質量%以下であり、さらに好ましくは4.0質量%以上6.0質量%以下であり、よりさらに好ましくは4.0質量%以上5.5質量%未満であり、最も好ましくは4.0質量%以上5.0質量%以下である。
Mgの含有量が1.0質量%以上であれば、十分な強度を得ることができ、Mgの含有量が2.2質量%以下であれば、良好な押出加工性が得られる。
本実施形態に係るアルミニウム合金押出材は、Mgの含有量が、1.0質量%以上2.2質量%以下であり、より好ましくは1.2質量%以上2.2質量%以下であり、さらに好ましくは1.3質量%以上2.2質量%以下であり、よりさらに好ましくは1.4質量%以上2.2質量%以下であり、最も好ましくは1.5質量%以上2.2質量%以下である。
但し、Zn含有量が6.0%質量以下の場合、Mgの含有量を1.2質量%以上、Zn含有量が5.5質量%未満の場合、Mgの含有量を1.6質量%以上とすることが好ましい。
本実施形態に係るアルミニウム合金押出材は、Feの含有量が、0.05質量%以上0.20質量%以下である。
本実施形態に係るアルミニウム合金押出材は、Cuの含有量が、0.30質量%以下である。Cuの含有量が、0.30質量%を超えると、陽極酸化皮膜に黄色味を帯びやすく、また耐食性も悪化しやすい。
本実施形態に係るアルミニウム合金押出材は、Tiの含有量が、0.005質量%以上0.04質量%以下である。また、本実施形態に係るアルミニウム合金押出材は、Bの含有量が、0.001質量%以上0.02質量%以下である。
Tiのみを添加した場合、母相中に固溶してしまい、微細化剤としての作用が小さくなる。また結晶内部への濃度偏析が起こりやすくなるので、ロッドハードナーを微細化剤として用いてTiB2化合物として添加することが好ましい。一方、TiやBを過剰に添加すると化合物として過剰に晶出し、スジ模様の原因となるので添加量の上限規制が必要となる。
本実施形態に係るアルミニウム合金押出材は、Siの含有量が、0.15質量%以下である。Siは、MgとMg‐Si系化合物を形成してスジ模様の一因となるため、0.15%以下に規制することが好ましい。
また、Siの含有量が、0.1質量%以下であることが、より好ましい。Siの含有量がこの範囲であれば、上記の効果がより高まる。
Zr、Mn、Cr、Vは、押出加工時の再結晶化を抑制する作用があるので、それぞれの含有量が0.05質量%以下であることが好ましく、より好ましくは0.02質量%以下である。またこれらの元素は、Znの拡散を抑制する作用もある。
これらの添加量が規定範囲を超えて添加した場合には、再結晶化を抑制し非再結晶組織を形成したり、結晶粒成長を起こす原因となり、更には粗大な過剰な晶出物の原因となるので、全てを合計しても含有量が0.10質量%以下であることが好ましく、より好ましくは0.09質量%以下であり、さらに好ましくは0.08質量%以下であり、よりさらに好ましくは0.07質量%以下であり、最も好ましくは0.05質量%以下である。
ファイバー状の組織は、陽極酸化皮膜処理を行った場合、陽極酸化皮膜の表面にスジ模様が生じる原因となる。そのため、結晶組織は、結晶粒径が揃った、再結晶組織であることが好ましい。このような微細な再結晶組織が形成させるために、合金成分、鋳造HO条件、押出条件を制御する。結晶組織の形態は、ホウフッ化水素酸水溶液で皮膜処理し、偏光顕微鏡で観察といった方法で確認することができる。
陽極酸化処理面において、押出方向に平行して層状に存在するZn高濃度層とZn低濃度層の幅が0.1mmを超え、3mm以下の範囲においてZn濃度差が1%超える場合に、陽極酸化皮膜処理を行った際に、高濃度部と低濃度部の皮膜形態に差が生じ、その差が筋状模様に見えやすくなる。0.1mm幅の範囲での濃度偏析では、幅が狭すぎて、スジと認識され難い。また、3mmを超える緩やかな濃度偏析もスジとして認識されにくい。
陽極酸化皮膜処理面の再結晶組織の結晶粒サイズが不均一であると、そこで濃度偏析が生じ、筋模様状に見える。
陽極酸化処理面に占める金属間化合物(晶出物)の面積率が2%以上であると、押出加工時に結晶粒が引き伸ばされた際に、押出方向に平行に点在するように移動させられた金属間化合物(晶出物)が筋模様状に見える。
また、本発明によれば、アルミニウム合金押出材の製造方法が提供される。下記の実施形態は、上記実施形態と基本的な構成は同様である。
[Zr+Mn+Cr+V+Ti]≦0.10質量%
の関係を満たし、Znの含有量が6.0質量%以下かつMgの含有量が1.2質量%以下の範囲を除き、残部がアルミニウムと不可避不純物からなり、金属組織が再結晶組織であり、陽極酸化皮膜を有するアルミニウム合金押出材の製造方法であって、
鋳造材を均質化処理の保持条件が400~560℃で、1~24時間で処理し、
押出工程で押出比が20を超えて押出加工し、押出加工中の形材の温度が420℃以上になるように押出し、
時効処理工程が100~180℃で1~30時間で処理することを特徴とする。
鋳造工程では、上記の合金組成を有するアルミニウム合金溶湯を準備し、脱滓処理や脱ガス処理、フィルタリング等の公知の溶湯処理を行う。そして、DC鋳造法等で、円柱状の鋳塊(ビレット)を得る。
上記の鋳造工程で得られたビレットに均質化処理(HO処理)を施す。均質化処理によって、元素の濃度偏析が解消され、晶出物が減少する。
押出工程では、均質化処理を行ったビレットに押出加工を施して、所定の加工材とする。
押出加工の押出比は20以上であることが好ましい。押出加工の押出比はより好ましくは40以上である。これは、結晶が延ばされることで、濃度変化が緩やか(高濃度部間あるいは低濃度部間の間隔が密であると濃度偏析が改善されやすい)になり、陽極酸化皮膜後の外観でスジ模様が発生し難くなるためである。
ダイスから出た後の押出材は、押出後~200℃の温度範囲の冷却速度が、0.3~20℃/sとなるように冷却する。冷却速度が、この条件を満たせば、高い強度が得られ、かつ良好な耐応力腐食割れ性を得ることができる。
押出加工を行った加工材を時効処理する。時効処理工程における保持温度は100~180℃の条件で、1~30時間で処理する。また時効処理は、より高強度、耐応力腐食割れ性を得るためには、2段階の時効処理を行っても良い。
鋳造工程、均質化処理工程、押出工程、時効処理工程を順次経ることで得られた押出材は、所定の形状に切削加工された後、陽極酸化皮膜処理が施される。陽極酸化皮膜処理は、公知の条件で行われる。
下記[表1]の実験例A~Nの成分のビレットを得た。ビレットの直径は325mmであった。これらのビレットを[表2]の条件でHO処理をした後、[表2]の条件で押出加工を行った。押出加工は、ビレット温度400℃の条件で行い、(a)は幅100mm、厚さ10mmフラットバー、(b)は幅120mm、厚さ25mmフラットバーと、2つの押出し形状で行った。
押出材をJIS 14B号試験片に加工し、引張試験を実施した。引張試験では、0.2%耐力≧380MPaであるものを合格とした。
アルミニウム合金試験材の表面を肉厚の20%にあたる量を面削(バフ研磨)し、面削面に陽極酸化皮膜処理を実施した。陽極酸化皮膜処理の処理条件は、20℃、15%硫酸水溶液中で1.5A/dm2で、皮膜厚さ約5μmとした。
アルミニウム合金試験材の表面を肉厚の20%にあたる量を面削し、鏡面に研磨後にホウフッ化水素酸水溶液中で皮膜処理し、偏光顕微鏡で組織を観察し組織を判定した。観察面はL-LT面(押出方向に平行である面の中で、広幅な面)である。
アルミニウム合金試験材の表面を肉厚の20%にあたる量を面削し、鏡面に研磨後に画像解析装置と光学顕微鏡により、晶出物の占有面積を測定した。観察面はL-LT面(押出方向に平行である面の中で、広幅な面)である。
A~E、M、Nについてのみ、JIS H8711に準拠し、応力腐食割れ試験を実施した。応力腐食割れ試験では、押出方向と直角方向に0.2%耐力の50%にあたる応力を負荷した。腐食液は3.5%NaCl、25℃、10分間浸漬後、50分間乾燥で1サイクルとした。30日間試験を行い、割れの無い材料を合格「○」とした。A、M、Nは、SCC試験の結果が劣るが、これはCu含有量が少ないためであると考えられる。
アルミニウム合金試験材の表面を3mm面削し、研磨後に島津製作所製EPMA-1610を用いて、下記の条件で元素分析を行った。Znの濃度を計測するために、その測定においてはZn含有量の異なる標準試料を使用して、あらかじめZnの検量線を作成して、検量線法にて定量化を行った。ライン上に測定した元素濃度値の最高値と最低値の差を濃度偏析値とした。
加速電圧 :15kV
照射電流 :200nA
ビーム径 :1μm(最小)
sweep condition:LINE x3000
(電子線走査条件:進行方向に対して垂直に3000倍(100μm程度)の範囲で線状に電子線を走査しながら測定)
データ数 :300points
ステップサイズ :10μm
長さ :3000μm(3mm)
測定時間 :2秒/point
図5は、実験例K(比較例)のミクロ組織を観察したものである。Fe、Cu、Mg、Crの含有量が多く、晶出物が偏析した箇所が、押出加工によって引き伸ばされ、スジ状に化合物の連続性が見える。
図6は、実験例B(発明例)のZn濃度分析およびマッピング図を示すグラフである。3mm幅におけるZn濃度偏析は1.0質量%以下である。また図7は、実験例G(比較例)のZn濃度分布、図8は、実験例H(比較例)のZn濃度分布およびマッピング図を示すグラフである。比較例である実験例G、Hは、3mm幅の間にZnの濃度が、1.0質量%を超える濃度偏析が生じている箇所があることがわかる。また、マッピング図より濃度偏析が層状になっていることがわかる。
なお、A~D、M、Nの押出比はEと比較して大きい、すなわち加工度が高いため、表面の均一性はより高い結果となった。
Claims (7)
- アルミニウム合金押出材であって、
Zn:4.0質量%以上7.5質量%以下、
Mg:1.0質量%以上2.2質量%以下、
Fe:0.05質量%以上0.20質量%以下、
Cu:0.30質量%以下、
Ti:0.005質量%以上0.04質量%以下、
B:0.001質量%以上0.02質量%以下、
Si:0.15質量%以下、
Zr:0.05質量%以下、
Mn:0.05質量%以下、
Cr:0.05質量%以下、
V:0.05質量%以下、
を含有し、
Zr、Mn、Cr、V及びTiの含有量の合計である[Zr+Mn+Cr+V+Ti]が、
[Zr+Mn+Cr+V+Ti]≦0.10質量%
の関係を満たし、
Znの含有量が6.0質量%以下かつMgの含有量が1.2質量%以下の範囲を除き、
残部がアルミニウムと不可避不純物からなり、
金属組織が再結晶組織である陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。 - Znの含有量が4.0質量%以上5.5質量%未満である、請求項1に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。
- Mgの含有量が1.0質量%以上1.6質量%以下である、請求項1又は2に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。
- 陽極酸化処理面において、押出方向に平行してZn高濃度相とZn低濃度相が層状に存在し、押出方向に直交する方向において、幅0.1mm以上3mm以下の範囲においてZn濃度差が1%以下であることを特徴とする請求項1から3の何れか一項に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。
- 陽極酸化皮膜処理面の再結晶組織の結晶粒サイズが平均値で200μm以下であり、最大結晶粒サイズが1mm以下あることを特徴とする請求項1から4の何れか一項に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。
- 陽極酸化処理面に占める晶出物の面積率が2%未満であることを特徴とする請求項1から5の何れか一項に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材。
- 鋳造材を、均質化処理の保持条件が400~560℃で、1~24時間で処理し、
押出工程で押出比が20を超えて押出加工し、押出加工中の形材の温度が420℃以上になるように押出し、
時効処理工程が100~180℃で1~30時間で処理することを特徴とする請求項1から6の何れか一項に記載の陽極酸化皮膜を有する外観品質に優れたアルミニウム合金押出材の製造方法。
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JP2015040320A (ja) * | 2013-08-21 | 2015-03-02 | 株式会社Uacj | 高強度アルミニウム合金及びその製造方法 |
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JP2018090839A (ja) * | 2016-11-30 | 2018-06-14 | アイシン軽金属株式会社 | 押出材用アルミニウム合金及びそれを用いた押出材並びに押出材の製造方法 |
JP7093611B2 (ja) | 2016-11-30 | 2022-06-30 | アイシン軽金属株式会社 | 押出材用アルミニウム合金及びそれを用いた押出材並びに押出材の製造方法 |
EP3594369A4 (en) * | 2017-03-07 | 2020-12-16 | LG Electronics Inc. -1- | ALUMINUM ALLOY |
CN113403507A (zh) * | 2021-06-21 | 2021-09-17 | 合肥标兵新材料科技有限公司 | 电子产品用高强高阳极氧化效果的6系铝合金制备方法 |
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