JP2000273563A - Aluminum alloy rolled sheet whose color tone after anodic oxidation treatment is gray and stable and its production - Google Patents
Aluminum alloy rolled sheet whose color tone after anodic oxidation treatment is gray and stable and its productionInfo
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- JP2000273563A JP2000273563A JP7403299A JP7403299A JP2000273563A JP 2000273563 A JP2000273563 A JP 2000273563A JP 7403299 A JP7403299 A JP 7403299A JP 7403299 A JP7403299 A JP 7403299A JP 2000273563 A JP2000273563 A JP 2000273563A
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は陽極酸化処理を施
して使用される用途のアルミニウム合金圧延板、特に建
築内装材などの建材、あるいは器物、容器、各種電気機
器・計測器の筐体、電気機械装置のパネル、装飾品など
に使用されるアルミニウム合金圧延板およびその製造方
法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rolled aluminum alloy plate to be used after being subjected to an anodic oxidation treatment, in particular, a building material such as a building interior material, a container, a housing of various electric devices and measuring instruments, The present invention relates to a rolled aluminum alloy plate used for a panel of a mechanical device, a decorative article, and the like, and a method for producing the same.
【０００２】[0002]
【従来の技術】一般に建材などに使用されるアルミニウ
ム合金圧延板は、耐食性の観点から陽極酸化処理を施す
のが通常である。またこのような用途では、美観のため
に陽極酸化処理後の色調として灰色系の色調が求められ
ることが多い。そしてこのような要望を満たすため、通
常の陽極酸化処理のままで灰色系の色調が得られるアル
ミニウム合金圧延板の製造方法として、既に特許第２５
４４２３３号に示される「陽極酸化処理後の色調が青灰
色のアルミニウム合金およびその製造方法」の発明が提
案され、また特開平９−７１８３１号に示される「陽極
酸化処理後の色調が黄みと赤みの少ないグレー色のアル
ミニウム合金板およびその製造方法」の発明が提案され
ている。2. Description of the Related Art Generally, a rolled aluminum alloy plate used for building materials is usually subjected to an anodic oxidation treatment from the viewpoint of corrosion resistance. In such applications, a gray color tone is often required as a color tone after anodizing for aesthetics. In order to satisfy such a demand, a method for manufacturing an aluminum alloy rolled plate capable of obtaining a grayish color tone with ordinary anodic oxidation treatment has already been disclosed in Japanese Patent No.
The invention of "Aluminum alloy having a bluish gray color after anodizing treatment and a method for producing the same" disclosed in JP-A-44233 has been proposed, and "The color tone after anodizing treatment is yellowish" described in JP-A-9-71831. And a method of manufacturing the same with a reddish gray aluminum alloy plate.
【０００３】[0003]
【発明が解決しようとする課題】ところで建材の用途の
うちでも、カーテンウォールやそのほかの外装材などに
おいては、高い耐食性が求められるため、一般に２０μ
ｍ程度と比較的厚く陽極酸化皮膜を形成することが行な
われているが、内装材などに使用する場合、外装材ほど
には耐食性が要求されないため、外装材の場合の１／２
程度、すなわち１０μｍ程度の陽極酸化皮膜厚みで充分
とされている。しかるに、厚み２０μｍ程度の比較的厚
い陽極酸化皮膜を形成する場合は、前記各提案の方法で
得られたアルミニウム合金圧延板でも、通常の陽極酸化
処理を適用することにより安定して灰色の色調の陽極酸
化皮膜を得ることが可能であるが、前記各提案の方法に
より得られたアルミニウム合金圧延板に対して、通常の
陽極酸化処理により厚み１０μｍ程度の薄い陽極酸化皮
膜を生成させた場合、灰色の色調を得ることは困難であ
り、せいぜい淡い灰色（淡灰色）を呈するに過ぎない。
このように耐食性の観点からは陽極酸化皮膜厚が１０μ
ｍ程度で足りる内装材の場合も、安定した灰色の色調を
得るにやむを得ず２０μｍ程度の厚い陽極酸化皮膜を生
成させていたのが実情である。Among construction materials, curtain walls and other exterior materials are required to have high corrosion resistance.
The anodic oxide film is formed to be relatively thick as about m, but when used for interior materials, etc., it is not required to be as corrosion-resistant as exterior materials.
An anodic oxide film thickness of about 10 μm is sufficient. However, when a relatively thick anodic oxide film having a thickness of about 20 μm is formed, even a rolled aluminum alloy plate obtained by each of the above-mentioned proposed methods can stably obtain a gray color by applying a normal anodic oxidation treatment. Although it is possible to obtain an anodic oxide film, when a thin anodic oxide film having a thickness of about 10 μm is formed on a rolled aluminum alloy plate obtained by each of the above-mentioned proposed methods by ordinary anodic oxidation treatment, gray It is difficult to obtain a color tone of at most, and at most it exhibits a pale gray (light gray).
Thus, from the viewpoint of corrosion resistance, the thickness of the anodic oxide film is 10 μm.
In the case of an interior material that requires only about m, a thick anodic oxide film of about 20 μm is unavoidably generated to obtain a stable gray color tone.
【０００４】また内装材の用途では、外装材などと比較
して精細でかつより立体的なデザインが要求されること
が多く、例えば陽極酸化処理の前工程として９０°曲げ
以上の１００〜１８０°の苛酷な曲げ加工が必要とされ
ることが多い。このように苛酷な曲げ加工が要求される
用途に対して前記各提案の方法により得られたアルミニ
ウム合金圧延板を適用した場合、強度が不足したり曲げ
加工時に割れたり肌荒れが生じたりすることがある。ま
た内装材の用途では、外装材などと比較して、外観品質
についてもより高品質であることが求められることが多
いが、前述の各提案の方法により得られたアルミニウム
合金圧延板では、この点でも不充分であった。[0004] In addition, in the use of interior materials, a finer and more three-dimensional design is often required as compared with exterior materials and the like. Severe bending is often required. When the rolled aluminum alloy sheet obtained by each of the above-mentioned proposed methods is applied to applications requiring such severe bending, the strength may be insufficient or cracking or rough surface may occur during bending. is there. In addition, in the use of interior materials, it is often required that the appearance quality be higher than that of exterior materials, but in the rolled aluminum alloy plate obtained by the above-mentioned proposed methods, The point was also insufficient.
【０００５】すなわち、前記各提案の方法により得られ
たアルミニウム合金圧延板の場合、鋳塊加熱処理温度が
低い領域では、比較的大きなＡｌ−Ｍｎ系針状析出物が
不均一に析出し、それに起因して陽極酸化処理後の表面
に筋目状の模様、すなわちいわゆる「筋目不良」と称さ
れる外観不良が生じたり、またＭｇ量が少ない領域では
結晶粒が大きくなって曲げ加工時に肌荒れ不良を生じた
り、中間焼鈍後の冷間圧延率の大小によっては強度と伸
びのバランスが崩れて、強度不足が生じたり逆に苛酷な
曲げ条件下での曲げ加工時に割れが生じたりすることが
ある。That is, in the case of the rolled aluminum alloy sheet obtained by each of the above-mentioned proposed methods, relatively large Al-Mn needle-like precipitates are non-uniformly deposited in a region where the ingot heat treatment temperature is low, and Due to this, a streak-like pattern, that is, a poor appearance called so-called “streak defect” occurs on the surface after the anodizing treatment, and in a region where the amount of Mg is small, crystal grains become large and rough surface failure occurs during bending. Depending on the magnitude of the cold rolling reduction after the intermediate annealing, the balance between strength and elongation may be lost, resulting in insufficient strength or, conversely, cracking during bending under severe bending conditions.
【０００６】そこで本発明者は、２０μｍ未満の例えば
１０μｍ程度の薄い陽極酸化皮膜を生成した場合でも、
陽極酸化皮膜の色調として安定に灰色を呈し、しかも筋
目不良が生じにくく、さらには従来材と同等以上の強度
で曲げ加工性を従来よりも格段に向上させたアルミニウ
ム合金圧延板を製造する方法を特願平１０−０５０１３
９に提案した。しかしながらこの提案では、Ｓｉ含有量
の規制が一部不適切だったため、また最終板における金
属組織状態と陽極酸化処理後の色調の関係を完全に把握
できていなかったため、量産を繰り返すと一部におい
て、陽極酸化処理後の色調が変動するものもあった。Therefore, the inventor of the present invention has proposed that even when a thin anodic oxide film of less than 20 μm, for example, about 10 μm is formed,
A method of manufacturing a rolled aluminum alloy plate that stably exhibits gray as the color of the anodic oxide film, hardly causes streaking defects, and has much higher bending workability than conventional materials with strength equal to or higher than conventional materials Japanese Patent Application No. 10-05013
9 proposed. However, in this proposal, the regulation of the Si content was partially inadequate, and the relationship between the metallographic state of the final plate and the color tone after anodizing was not completely understood. In some cases, the color tone after the anodic oxidation treatment fluctuated.
【０００７】[0007]
【課題を解決するための手段】前述のような課題を解決
するため、本発明者は鋭意実験・研究を重ねた結果、合
金の成分組成を適切に設定すると同時に、製造プロセス
条件、特に鋳塊加熱条件、熱間圧延条件、中間焼鈍条
件、最終冷間圧延条件を適切に選定して、最終板におけ
る金属組織状態を適切なものとすることにより、前述の
課題を解決し得ることを見出し、この発明をなすに至っ
た。Means for Solving the Problems In order to solve the above-mentioned problems, the present inventors have conducted intensive experiments and researches. As a result, the present inventors have determined that the composition of the alloy is appropriately set, and at the same time, the manufacturing process conditions, especially the ingot By appropriately selecting heating conditions, hot rolling conditions, intermediate annealing conditions, and final cold rolling conditions, and by making the metal structure state in the final sheet appropriate, it has been found that the above-described problems can be solved. The present invention has been made.
【０００８】具体的には請求項１の発明の陽極酸化処理
後の色調が灰色で安定なアルミニウム合金圧延板は、
Ｍｎ１．３〜１．５％（重量％、以下同じ）、Ｍｇ０．
４〜１．２％、Ｆｅ０．２％以下を含有し、Ｓｉ０．０
５％未満に規制し、残部がＡｌおよび不可避的不純物よ
りなり、かつ、１μｍ未満の大きさのＡｌ−Ｍｎ−Ｓｉ
系粒状析出物の析出がなく、１〜８μｍの大きさのＡｌ
−Ｍｎ系針状析出物が１０００〜４０００個／０．２ｍ
ｍ2 の範囲内の密度で析出しており、しかも平均結晶
粒径が８０μｍ以下で、耐力が９５Ｎ／ｍｍ2 以上で
あることを特徴とする。Specifically, the rolled aluminum alloy plate having a stable gray tone after the anodizing treatment according to the first aspect of the present invention is:
Mn 1.3-1.5% (wt%, the same applies hereinafter), Mg0.
4 to 1.2%, Fe 0.2% or less, Si 0.0
Al-Mn-Si of less than 5%, with the balance being Al and unavoidable impurities and having a size of less than 1 µm
Al with a size of 1 to 8 μm without precipitation of systemic granular precipitates
-1000 to 4000 Mn-based needle precipitates / 0.2 m
m 2, the average crystal grain size is 80 μm or less, and the proof stress is 95 N / mm 2 or more.
【０００９】そして、請求項２の発明では、アルミニウ
ム合金に、前記各成分のほか、さらに０．００３〜０．
１５％のＴｉを単独でもしくは０．０００１〜０．０１
％のＢと組合されて含有することを特徴とする。According to the second aspect of the present invention, in addition to the above-described components, the aluminum alloy may further contain 0.003-0.
15% Ti alone or 0.0001 to 0.01%
% In combination with B.
【００１０】さらに、請求項３の発明の陽極酸化処理後
の色調が灰色で安定なアルミニウム合金圧延板の製造方
法は、請求項１または請求項２記載の化学組成を有する
Ａｌ合金の鋳塊に、５８０〜６３０℃の範囲内の温度で
１〜２４時間保持する加熱処理を施し、次いで前記加熱
処理における処理温度以下で熱間圧延を開始して、その
熱間圧延を３００℃以下で終了し、その後１〜５０℃／
秒の昇温速度で４００〜６００℃の範囲内の温度に加熱
して０〜１０分保持した後１〜５０℃／秒の冷却速度で
冷却する中間焼鈍を施し、さらに２〜３０％の圧延率で
冷間圧延を施し、これにより１μｍ未満の大きさのＡｌ
−Ｍｎ−Ｓｉ系粒状析出物の析出がなく、１〜８μｍの
大きさのＡｌ−Ｍｎ系針状析出物が１０００〜４０００
個／０．２ｍｍ2 の範囲内の密度で析出しており、し
かも平均結晶粒径が８０μｍ以下で、耐力が９５Ｎ／ｍ
ｍ2 以上であることを特徴とする。Further, according to the third aspect of the present invention, there is provided a method for producing a rolled aluminum alloy plate having a stable gray tone after the anodizing treatment, wherein the ingot of the Al alloy having the chemical composition according to the first or second aspect is provided. , A heat treatment of holding at a temperature in the range of 580 to 630 ° C. for 1 to 24 hours, then starting hot rolling at a temperature lower than the processing temperature in the heat treatment, and finishing the hot rolling at 300 ° C. or lower. , Then 1-50 ° C /
The steel sheet is heated to a temperature in the range of 400 to 600 ° C. at a heating rate of 2 seconds, held for 0 to 10 minutes, and then subjected to intermediate annealing for cooling at a cooling rate of 1 to 50 ° C./sec. Cold rolling at a rate of less than 1 μm
-No precipitation of Mn-Si-based granular precipitates, and 1000 to 4000 Al-Mn-based needle-like precipitates having a size of 1 to 8 µm.
Grains / precipitate at a density within the range of 0.2 mm 2 , with an average crystal grain size of 80 μm or less and a proof stress of 95 N / m 2.
m 2 or more.
【００１１】さらにまた請求項４の発明は、請求項３に
記載のアルミニウム合金圧延板の製造方法において、熱
間圧延後、中間焼鈍の前に一次冷間圧延を施すことを特
徴とするものである。A fourth aspect of the present invention is the method for producing a rolled aluminum alloy sheet according to the third aspect, wherein primary cold rolling is performed after hot rolling and before intermediate annealing. is there.
【００１２】[0012]
【発明の実施の形態】先ずこの発明における成分組成の
限定理由について説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS First, the reasons for limiting the component composition in the present invention will be described.
【００１３】Ｍｎ：ＭｎはＡｌ−Ｍｎ系の金属間化合物
析出物を生成して、陽極酸化処理後の色調を決定するた
めに重要な元素である。すなわち、Ｍｎは鋳造時に鋳塊
のマトリックス中に固溶し、その後の鋳塊加熱時にＡｌ
−Ｍｎ系金属間化合物として析出し、この析出物が最終
板まで残存し、陽極酸化処理後も皮膜中に残存して灰色
の色調を呈するに寄与する。ここで、１０μｍ程度の厚
みの陽極酸化皮膜においては、１〜８μｍの大きさのＡ
ｌ−Ｍｎ系針状析出物の密度が１０００個／０．２ｍｍ
2 未満では充分な灰色とならずに淡灰色となり、一方
４０００個／０．２ｍｍ2 を越えれば灰色が濃過ぎて
濃灰色〜黒色となり、したがって安定した灰色の色調を
得るためには、１〜８μｍの大きさのＡｌ−Ｍｎ系針状
析出物の密度が１０００〜４０００個／０．２ｍｍ2
の範囲内となることが必要である。そして、１〜８μｍ
の大きさのＡｌ−Ｍｎ系針状析出物の密度が１０００個
／０．２ｍｍ2 未満となるのは合金中のＭｎ量が１．
３％未満となる場合であり、一方その密度が４０００個
／０．２ｍｍ2 を越えるのは合金中のＭｎ量が１．５
％を越える場合であり、したがって陽極酸化処理後の色
調を安定した灰色とすべく１〜８μｍの大きさのＡｌ−
Ｍｎ系針状析出物の密度を１０００〜４０００個／０．
２ｍｍ2 とするためには、Ｍｎ量を１．３〜１．５％
の範囲内とする必要がある。Mn: Mn is an important element for forming an Al-Mn intermetallic compound precipitate to determine the color tone after anodizing. That is, Mn dissolves in the matrix of the ingot during casting, and Al
-Precipitates as a Mn-based intermetallic compound, and the precipitate remains up to the final plate, remains in the film even after the anodizing treatment, and contributes to exhibiting a gray color tone. Here, in an anodic oxide film having a thickness of about 10 μm, A having a size of 1 to 8 μm is used.
The density of the l-Mn needle-like precipitates is 1000 / 0.2 mm
If it is less than 2 , the color is not sufficiently gray and becomes light gray, whereas if it exceeds 4000 / 0.2 mm 2 , the gray is too dark and becomes dark gray to black. The density of the Al-Mn-based acicular precipitate having a size of 8 µm is 1000 to 4000 particles / 0.2 mm 2.
Must be within the range. And 1 to 8 μm
The density of the Al-Mn needle-like precipitates having a size of less than 1000 / 0.2 mm 2 is that the Mn content in the alloy is 1.
On the other hand, when the density exceeds 4000 / 0.2 mm 2 , the Mn content in the alloy is less than 1.5%.
%, So that the color tone after the anodizing treatment becomes a stable gray with an Al—
The density of Mn-based needle-like precipitates is 1000 to 4000 particles / 0.
In order to make it 2 mm 2 , the Mn content is 1.3 to 1.5%
Must be within the range.
【００１４】Ｍｇ：Ｍｇは強度向上に寄与する元素であ
る。Ｍｇ量が０．４％未満では曲げ加工性は良好である
が、充分な強度が得られず、一方１．２％を越えれば強
度が高過ぎて曲げ加工性が不充分となる。したがってＭ
ｇ量は０．４〜１．２％の範囲内とした。Mg: Mg is an element that contributes to improving strength. If the Mg content is less than 0.4%, the bending workability is good, but sufficient strength cannot be obtained, while if it exceeds 1.2%, the strength is too high and the bending workability becomes insufficient. Therefore M
The g amount was in the range of 0.4 to 1.2%.
【００１５】Ｆｅ：Ｆｅは中間焼鈍時において再結晶粒
を微細化する有益な作用を有するが、その一方では鋳造
時においてＡｌ−Ｍｎ−Ｆｅ系金属間化合物を生成させ
て鋳塊マトリックス中へのＭｎ固溶量を減少させ、これ
により鋳塊加熱時のＡｌ−Ｍｎ系析出物の析出を妨げる
有害な作用も有する。特にＦｅ量が０．２％を越えれば
鋳塊加熱時におるＡｌ−Ｍｎ系析出物の析出が著しく減
少し、１０μｍ程度の厚みの陽極酸化皮膜では灰色とな
りにくい。したがってＦｅ量は０．２％以下とした。Fe: Fe has a beneficial effect of refining the recrystallized grains during the intermediate annealing. On the other hand, Fe forms an Al—Mn—Fe intermetallic compound during casting to form the alloy in the ingot matrix. It also has a detrimental effect of reducing the amount of Mn solid solution, thereby preventing the precipitation of Al-Mn-based precipitates during heating of the ingot. In particular, if the Fe content exceeds 0.2%, the precipitation of Al-Mn-based precipitates during the heating of the ingot is significantly reduced, and the anodic oxide film having a thickness of about 10 µm hardly becomes gray. Therefore, the amount of Fe was set to 0.2% or less.
【００１６】Ｓｉ：Ｓｉも陽極酸化処理後の色調に影響
を与える元素である。Ｓｉ量が０．０５％以上では１μ
ｍ未満の大きさのＡｌ−Ｍｎ−Ｓｉ系粒状析出物がＳｉ
量に比例して増加し、陽極酸化処理後の色調もＡｌ−Ｍ
ｎ−Ｓｉ系粒状析出物の分布密度に比例して黄色味がか
った灰色となってしまう。したがって陽極酸化処理後の
色調変動を小さくするには１μｍ未満の大きさのＡｌ−
Ｍｎ−Ｓｉ系粒状析出物を析出させないことが必要であ
り、そのためのＳｉ量は０．０５％未満である。Si: Si is also an element that affects the color tone after anodizing. 1μ when Si content is 0.05% or more
m-sized Al-Mn-Si-based granular precipitates
The amount increases in proportion to the amount, and the color tone after anodizing treatment is also Al-M
It becomes yellowish gray in proportion to the distribution density of the n-Si-based granular precipitates. Therefore, in order to reduce color tone fluctuations after anodizing, Al-
It is necessary not to precipitate Mn-Si-based granular precipitates, and the amount of Si for that purpose is less than 0.05%.
【００１７】このほか一般にＡｌ合金の不可避的不純物
としては、Ｃｒ，Ｃｕ，Ｚｎ，Ｚｒ，Ｖなどがあるが、
このうちＣｒ，Ｃｕは陽極酸化処理後の色調にある程度
影響を与えるから、少量に規制することが好ましい。す
なわちＣｒは０．０５％を、Ｃｕは０．１％を越えれ
ば、陽極酸化処理後の色調が黄色味がかるから、不純物
としてのＣｒ量は０．０５％以下、Ｃｕ量は０．１％以
下に規制することが好ましい。一方、Ｚｎ，Ｚｒ，Ｖは
いずれも陽極酸化処理後の色調に本質的な影響を与えな
いが、Ｚｎが１．０％を越えれば耐食性が低下し、また
ＺｒおよびＶがそれぞれ０．３％を越えれば粗大金属間
化合物が生成されて曲げ加工性が阻害されるから、不純
物としてのＺｎ量は１．０％以下、Ｚｒ量およびＶ量は
それぞれ０．３％以下に規制することが好ましい。In general, inevitable impurities of Al alloy include Cr, Cu, Zn, Zr, and V.
Among them, Cr and Cu have some influence on the color tone after the anodizing treatment, so that it is preferable to restrict them to a small amount. That is, if the content of Cr exceeds 0.05% and the content of Cu exceeds 0.1%, the color tone after anodizing becomes yellowish, so that the Cr content as an impurity is 0.05% or less and the Cu content is 0.1%. It is preferable to regulate as follows. On the other hand, Zn, Zr, and V do not substantially affect the color tone after the anodizing treatment. However, if Zn exceeds 1.0%, the corrosion resistance is reduced, and Zr and V each become 0.3%. If the ratio exceeds the above range, a coarse intermetallic compound is generated and the bending workability is impaired. Therefore, it is preferable that the Zn content as impurities is regulated to 1.0% or less, and the Zr content and V content are each regulated to 0.3% or less. .
【００１８】さらに、一般にＡｌ合金においては、鋳塊
組織の微細化のためにＴｉを単独で、あるいはＴｉをＢ
と組合せて添加する場合があるが、この発明の場合もこ
れらを添加しても良い。但し、Ｔｉ量が０．００３％未
満では鋳塊組織微細化の効果が得られず、一方Ｔｉ量が
０．１５％を越えればＴｉＡｌ３ の粗大金属間化合物
が生成されて曲げ加工性が阻害されるから、Ｔｉを添加
する場合のＴｉ量は０．００３〜０．１５％の範囲内と
する。またＴｉとともにＢを添加する場合のＢ量は、
０．０００１％未満では鋳塊組織微細化の効果が得られ
ず、一方０．０１％を越えれば粗大なＴｉＢ２ が生成
されて曲げ加工性が阻害されるから、Ｔｉと組合せてＢ
を添加する場合のＢ量は０．０００１〜０．０１％の範
囲内とする。Further, in general, in an Al alloy, Ti alone or Ti is added in order to refine the ingot structure.
May be added in combination, but also in the case of the present invention, these may be added. However, if the amount of Ti is less than 0.003%, the effect of refining the ingot structure cannot be obtained, while if the amount of Ti exceeds 0.15%, a coarse intermetallic compound of TiAl3 is generated and the bending workability is impaired. Therefore, the amount of Ti when Ti is added is in the range of 0.003 to 0.15%. The amount of B when B is added together with Ti is as follows:
If the content is less than 0.0001%, the effect of refining the ingot structure cannot be obtained. On the other hand, if the content exceeds 0.01%, coarse TiB2 is generated and bending workability is impaired.
Is added in the range of 0.0001 to 0.01%.
【００１９】またＭｇを含有する合金において溶湯酸化
防止のためにＢｅを添加することがあるが、本発明にお
いてもＢｅの添加は許容される。Ｂｅを添加する場合の
Ｂｅ量は、０．０００１％未満では溶湯酸化防止の効果
が得られず、一方０．０５％を越えてＢｅを添加しても
上記効果は飽和するだけで経済的に無駄となるから、Ｂ
ｅを添加する場合のＢｅ量は０．０００１〜０．０５％
の範囲内とする。In some cases, Be is added to an alloy containing Mg in order to prevent oxidation of the molten metal. However, the addition of Be is also permitted in the present invention. If the amount of Be in the case of adding Be is less than 0.0001%, the effect of preventing molten metal oxidation cannot be obtained. On the other hand, if the amount of Be exceeds 0.05%, the above effect is only saturated and economical. It's wasted, B
The amount of Be when e is added is 0.0001 to 0.05%
Within the range.
【００２０】さらにこの発明では、最終的に得られる最
終板（陽極酸化処理前の板）について、その組織条件お
よび特性値を規定しており、これらについて以下に説明
する。Further, in the present invention, the texture conditions and characteristic values of the finally obtained final plate (plate before anodizing treatment) are defined, and these will be described below.
【００２１】最終板においては、１〜８μｍの大きさの
Ａｌ−Ｍｎ系針状析出物の密度が１０００〜４０００個
／０．２ｍｍ2 の範囲内であることと、１μｍ未満の
大きさのＡｌ−Ｍｎ−Ｓｉ系粒状析出物を析出させない
ことが必要であり、このように１〜８μｍの大きさのＡ
ｌ−Ｍｎ系針状析出物の密度範囲の選定と、１μｍ未満
の大きさのＡｌ−Ｍｎ−Ｓｉ系粒状析出物を析出させな
いことによって、前述のように１０μｍ程度の薄い膜厚
の陽極酸化皮膜で灰色で安定な色調を得ることができ
る。ここで、最終板においては、１μｍ未満および８μ
ｍを超える大きさのＡｌ−Ｍｎ系針状析出物は、この発
明で規定する成分組成、鋳塊加熱処理条件の範囲内では
実質的に存在しない。さらにＳｉ量が０．０５％以上で
は１μｍ未満のＡｌ−Ｍｎ−Ｓｉ系粒状析出物は存在す
るが、本発明では、Ｓｉ量を０．０５％未満に規制した
のでＡｌ−Ｍｎ−Ｓｉ系粒状析出物は存在しない。した
がってこの発明では、特に大きさが１〜８μｍの範囲内
のＡｌ−Ｍｎ系針状析出物の密度と１μｍ未満のＡｌ−
Ｍｎ−Ｓｉ系粒状析出物を析出させないことを規定した
のである。なおここでＡｌ−Ｍｎ系針状析出物の「大き
さ」とは、その最大長さ方向の長さを意味し、Ａｌ−Ｍ
ｎ−Ｓｉ系粒状析出物の「大きさ」とは最大直径を意味
するものとする。In the final plate, the density of Al-Mn based needle-like precipitates having a size of 1 to 8 µm is in the range of 1000 to 4000 / 0.2 mm 2 , -It is necessary not to precipitate the Mn-Si-based granular precipitates, and thus, A having a size of 1 to 8 μm is required.
By selecting the density range of the l-Mn needle-like precipitates and not depositing Al-Mn-Si-based granular precipitates having a size of less than 1 µm, as described above, the anodic oxide film having a thin film thickness of about 10 µm as described above. And a stable gray tone can be obtained. Here, in the final plate, less than 1 μm and 8 μm
Al-Mn needle-like precipitates having a size exceeding m are substantially absent within the range of the component composition and the ingot heat treatment conditions specified in the present invention. Further, when the amount of Si is 0.05% or more, there are Al-Mn-Si-based granular precipitates having a particle size of less than 1 µm. However, in the present invention, the amount of Al-Mn-Si-based granular particles is regulated to less than 0.05%. No precipitate is present. Therefore, in the present invention, in particular, the density of the Al-Mn-based acicular precipitate having a size in the range of 1 to 8 µm and the Al-
It is stipulated that no Mn-Si-based particulate precipitate is deposited. Here, the “size” of the Al—Mn-based needle-like precipitate means the length in the maximum length direction, and
The "size" of the n-Si-based granular precipitate means the maximum diameter.
【００２２】また最終板における平均結晶粒径は８０μ
ｍ以下である必要がある。平均結晶粒径は曲げ加工時に
おける肌荒れの発生に影響を与え、その値が小さいほど
肌荒れが発生しにくくなる。そして特に平均結晶粒径を
８０μｍ以下とすることによって、９０°曲げ以上の１
００〜１８０°の苛酷な曲げ加工でも肌荒れの発生を確
実に防止することができる。The average crystal grain size in the final plate is 80 μm.
m. The average crystal grain size affects the occurrence of surface roughness during bending, and the smaller the value is, the less likely it is for the surface roughness to occur. In particular, by setting the average crystal grain size to 80 μm or less, the 1
The occurrence of rough skin can be reliably prevented even in severe bending at a temperature of 00 to 180 °.
【００２３】さらに最終板における耐力は９５Ｎ／ｍｍ
2 以上であることが必要である。すなわち耐力が９５
Ｎ／ｍｍ2 以上であれば、従来並の強度となり、従来
材と同様な用途に適用することが可能となるのである。Further, the yield strength of the final plate is 95 N / mm.
Must be at least 2 . That is, the proof stress is 95
If it is N / mm 2 or more, the strength becomes the same as that of the conventional material, and it can be applied to the same use as the conventional material.
【００２４】次にこの発明の製造方法における各プロセ
スについて説明する。Next, each process in the manufacturing method of the present invention will be described.
【００２５】先ず前述のような成分組成のアルミニウム
合金を鋳造して鋳塊を得る。この鋳造方法は特に限定さ
れるものではなく、常法に従えば良いが、通常はＤＣ鋳
造法（半連続鋳造法）が好ましい。First, an ingot is obtained by casting an aluminum alloy having the above-mentioned composition. This casting method is not particularly limited, and may be in accordance with an ordinary method, but DC casting (semi-continuous casting) is usually preferred.
【００２６】鋳塊に対しては加熱処理を施す。この鋳塊
加熱処理は、最終板に対する陽極酸化処理によって灰色
の色調を得るに必要なＡｌ−Ｍｎ系析出物を析出させる
ための処理である。この鋳塊加熱処理の温度が５８０℃
未満では、最終板の状態で１〜８μｍ程度の大きさの針
状析出物は分布も粗く不均一なため、陽極酸化処理後に
筋目不良が生じるおそれがある。そして鋳塊加熱処理の
温度が５８０℃以上となれば、１〜８μｍの針状析出物
の分布が均一化されて筋目不良が生じにくくなる。さら
に鋳塊加熱処理の温度が６３０℃を越えれば共晶融解が
生じるおそれがある。したがって筋目不良の発生を防止
するためには、鋳塊加熱処理温度を５８０〜６３０℃の
範囲内とする必要がある。鋳塊加熱処理の保持温度は、
１時間未満では充分にＡｌ−Ｍｎ系析出物が析出され
ず、一方２４時間を越えて長時間加熱保持しても、Ａｌ
−Ｍｎ系析出物の析出は飽和状態となり、経済性を損な
うだけである。したがって鋳塊加熱処理の加熱保持時間
は１〜２４時間とした。ここで、１０μｍ程度の比較的
薄い陽極酸化皮膜において安定した灰色を得るために
は、既に述べたように最終板における１〜８μｍの大き
さの針状析出物の分布密度が１０００〜４０００個／
０．２ｍｍ2 であることが必要であり、合金のＭｎ量
を１．３〜１．５％としかつ上述のような条件の鋳塊加
熱処理を施すことによって、Ａｌ−Ｍｎ系針状析出物の
分布密度の要件を満たすことができる。The ingot is subjected to a heat treatment. This ingot heat treatment is a treatment for precipitating Al-Mn-based precipitates necessary for obtaining a gray color by anodizing the final plate. The temperature of this ingot heat treatment is 580 ° C
If it is less than 1, in the state of the final plate, the needle-like precipitate having a size of about 1 to 8 μm has a coarse and uneven distribution, and therefore, there is a possibility that a streak defect may occur after the anodizing treatment. When the temperature of the ingot heat treatment is 580 ° C. or higher, the distribution of needle-like precipitates having a size of 1 to 8 μm is uniformed, and poor streaking is less likely to occur. If the temperature of the ingot heat treatment exceeds 630 ° C., eutectic melting may occur. Therefore, in order to prevent the occurrence of defective streaks, the ingot heat treatment temperature must be within the range of 580 to 630 ° C. The holding temperature of the ingot heat treatment is
If the time is less than 1 hour, the Al-Mn-based precipitate is not sufficiently deposited.
The precipitation of -Mn-based precipitates becomes saturated and only impairs economic efficiency. Therefore, the heating holding time of the ingot heating treatment was set to 1 to 24 hours. Here, in order to obtain a stable gray color in a relatively thin anodic oxide film of about 10 μm, as described above, the distribution density of needle-like precipitates having a size of 1 to 8 μm in the final plate is 1000 to 4000 particles /
0.2 mm 2 , the Mn content of the alloy is set to 1.3 to 1.5%, and the ingot heat treatment is performed under the above-described conditions, whereby the Al—Mn acicular precipitates are obtained. Can satisfy the requirement of the distribution density.
【００２７】上述のような鋳塊加熱処理の後には、熱間
圧延を施す。この熱間圧延は、鋳塊加熱温度以下の温度
で開始し、再結晶温度以下で終了させる。この発明で用
いている合金の場合、再結晶温度はほぼ３００℃である
から、熱間圧延終了温度は３００℃以下とする。熱間圧
延終了温度が３００℃を越える場合、熱間圧延終了後の
熱間圧延板に部分再結晶粒や粗大再結晶粒が残り、その
ためその後の中間焼鈍で微細な均一再結晶組織が得難く
なり、陽極酸化処理後の表面に結晶組織の不均一に起因
する筋目不良が生じやすくなるから、熱間圧延は３００
℃以下で終了させる必要がある。After the ingot heating treatment as described above, hot rolling is performed. The hot rolling starts at a temperature equal to or lower than the ingot heating temperature and ends at a temperature equal to or lower than the recrystallization temperature. In the case of the alloy used in the present invention, since the recrystallization temperature is approximately 300 ° C., the hot rolling end temperature is set to 300 ° C. or less. When the hot rolling end temperature exceeds 300 ° C., partially recrystallized grains or coarse recrystallized grains remain in the hot-rolled sheet after the hot rolling, and it is difficult to obtain a fine uniform recrystallized structure by subsequent intermediate annealing. In this case, the surface after the anodizing treatment is liable to cause streaking defects due to the non-uniform crystal structure.
It is necessary to end at or below ° C.
【００２８】熱間圧延終了後には、直ちに中間焼鈍を施
しても良く、また必要に応じて冷間圧延（一次冷間圧
延）を施してから中間焼鈍を行なっても良い。すなわち
最終板の板幅方向および長さ方向の板厚精度が厳しく要
求される場合などには、熱間圧延後に一次冷間圧延を施
してから中間焼鈍を行なっても良く、このような中間焼
鈍前の冷間圧延はこの発明の目的に対して本質的な影響
は与えない。After completion of the hot rolling, intermediate annealing may be performed immediately, or if necessary, cold rolling (primary cold rolling) may be performed before intermediate annealing. That is, in the case where the thickness accuracy of the final sheet in the sheet width direction and the length direction is strictly required, the intermediate annealing may be performed after performing the primary cold rolling after the hot rolling. The previous cold rolling has no substantial effect on the purpose of the present invention.
【００２９】熱間圧延後、あるいは熱間圧延および一次
冷間圧延を施した後の中間焼鈍は、組織を微細かつ均一
に再結晶させて、曲げ加工時の肌荒れ発生防止のために
必要な工程である。この発明で規定する平均結晶粒径８
０μｍ以下の微細再結晶粒組織を得るためには、急速昇
温、急速冷却の条件で中間焼鈍を行なう必要がある。具
体的には、昇温速度、冷却速度が１℃／秒未満では平均
結晶粒径８０μｍ以下の微細再結晶粒組織を得ることが
困難となり、曲げ加工時に肌荒れが生じやすくなるか
ら、中間焼鈍後の昇温速度、冷却速度はともに１℃／秒
以上とする必要がある。一方昇温速度および冷却速度が
より高ければ平均結晶粒径が８０μｍ以下の微細再結晶
粒組織を得ることは可能であるが、５０℃／秒を越えれ
ば焼鈍時における板の変形が生じやすくなり、また量産
規模での工業的な実施も困難となる。したがって中間焼
鈍の昇温速度、冷却速度はともに１〜５０℃／秒の範囲
内とした。なおこのような１〜５０℃／秒の急速昇温、
急速冷却の中間焼鈍は、連続焼鈍炉によって行なうこと
ができる。バッチ炉による焼鈍では、昇温速度、冷却速
度がともに２０〜６０℃／ｈｒと極めて遅く、そのため
平均結晶粒径が８０μｍ以下の微細再結晶粒組織が得ら
れず、曲げ加工時に肌荒れが生じるおそれが高い。一方
連続焼鈍による中間焼鈍は短時間加熱となるため、中間
焼鈍温度が４００℃未満では充分に再結晶せず、６００
℃を越えれば粗大再結晶粒が生じて曲げ加工性が阻害さ
れるから、中間焼鈍温度は４００〜６００℃の範囲内と
する。また４００〜６００℃の加熱温度での保持が１０
分を越えれば生産性が低下するから、保持時間は１０分
以下とする。なお保持を０分、すなわち保持なしとして
も良いことはもちろんである。Intermediate annealing after hot rolling, or after hot rolling and primary cold rolling, is a step required to recrystallize the structure finely and uniformly to prevent the occurrence of rough surface during bending. It is. Average crystal grain size defined by the present invention 8
In order to obtain a fine recrystallized grain structure of 0 μm or less, it is necessary to perform intermediate annealing under conditions of rapid temperature rise and rapid cooling. Specifically, if the heating rate and the cooling rate are less than 1 ° C./sec, it becomes difficult to obtain a fine recrystallized grain structure having an average crystal grain size of 80 μm or less, and the surface is likely to be roughened during bending. It is necessary that both the rate of temperature rise and the rate of cooling be 1 ° C./sec or more. On the other hand, if the heating rate and the cooling rate are higher, it is possible to obtain a fine recrystallized grain structure having an average crystal grain size of 80 μm or less, but if it exceeds 50 ° C./sec, the sheet tends to be deformed during annealing. In addition, industrial implementation on a mass production scale becomes difficult. Therefore, both the temperature rising rate and the cooling rate of the intermediate annealing were set in the range of 1 to 50 ° C./sec. In addition, such a rapid temperature rise of 1 to 50 ° C./sec,
The rapid cooling intermediate annealing can be performed by a continuous annealing furnace. In the annealing in a batch furnace, the rate of temperature rise and the rate of cooling are both as extremely slow as 20 to 60 ° C./hr, so that a fine recrystallized grain structure having an average crystal grain size of 80 μm or less cannot be obtained, and surface roughening may occur during bending. Is high. On the other hand, since intermediate annealing by continuous annealing is heating for a short time, recrystallization is not sufficiently performed when the intermediate annealing temperature is less than 400 ° C.
If the temperature exceeds ℃, coarse recrystallized grains are generated and bending workability is impaired. Therefore, the intermediate annealing temperature is set in the range of 400 to 600 ℃. Also, holding at a heating temperature of 400 to 600 ° C. is 10
If the time exceeds minutes, the productivity decreases, so the holding time is set to 10 minutes or less. Needless to say, the holding may be performed for 0 minute, that is, without holding.
【００３０】中間焼鈍後には最終板厚とするために冷間
圧延を行なう。この冷間圧延は強度向上のために必要な
工程である。冷間圧延率が２％未満では最終板の耐力が
９５Ｎ／ｍｍ2 を下廻り、一方３０％を越えれば強度
と曲げ加工性のバランスが崩れて、強度は高くなるもの
の曲げ加工性が低下し、いずれの場合もこの発明の目的
を達成できない。したがって中間焼鈍後の冷間圧延率は
２〜３０％の範囲内とする。After the intermediate annealing, cold rolling is performed to obtain a final sheet thickness. This cold rolling is a necessary step for improving the strength. If the cold rolling ratio is less than 2%, the yield strength of the final sheet is less than 95 N / mm 2 , while if it exceeds 30%, the balance between strength and bending workability is lost, and although bending strength is increased, strength is reduced, In any case, the object of the present invention cannot be achieved. Therefore, the cold rolling reduction after the intermediate annealing is in the range of 2 to 30%.
【００３１】以上のようにして得られた冷間圧延後の最
終板厚の圧延板を内装材等に用いるにあたっては、陽極
酸化処理を施す。この陽極酸化処理の条件は特に限定さ
れるものではないが、経済性等から最も一般的な硫酸電
解浴を用いることが望ましい。具体的には、例えばＨ２
ＳＯ４ 濃度が１０〜２５ｖｏｌ％程度の硫酸浴を用
い、浴温１０〜３０℃程度、電流密度１．０〜２．５Ａ
／ｄｍ2 程度の条件で陽極酸化処理を施せば良い。陽
極酸化処理による皮膜厚は特に限定しないが、この発明
の方法の場合、１０μｍ程度の薄い皮膜厚でも灰色で安
定な色調が安定して得られることを大きな特徴としてお
り、その意味から、２０μｍ未満の皮膜厚、特に６〜１
５μｍの膜厚の場合にこの発明の効果を最大限に発揮す
ることができる。When the rolled sheet having the final thickness after cold rolling obtained as described above is used as an interior material or the like, anodizing treatment is performed. The conditions of this anodizing treatment are not particularly limited, but it is desirable to use the most common sulfuric acid electrolytic bath from the viewpoint of economy and the like. Specifically, for example, H2
Using a sulfuric acid bath having an SO4 concentration of about 10 to 25 vol%, a bath temperature of about 10 to 30 ° C., and a current density of 1.0 to 2.5 A
Anodizing treatment may be performed under the condition of about / dm 2 . The thickness of the film formed by the anodizing treatment is not particularly limited. However, the method of the present invention is characterized in that a gray and stable color tone can be stably obtained even with a film thickness as thin as about 10 μm. Film thickness, especially 6-1
The effect of the present invention can be maximized when the film thickness is 5 μm.
【００３２】ここで、陽極酸化処理後の色調について
は、ハンターの色差式（ＪＩＳ Ｚ８７３０参照）によ
る明度指数Ｌとクロマティクネス指数ａ，ｂの値によっ
て評価することができる。すなわち、明度指数のＬ値は
高いほど白く、一方クロマティクネス指数は着色度につ
いてのものであって、そのａ値は高いほど赤味が強く、
ｂ値は高いほど黄味が強いことをあらわす。Here, the color tone after the anodizing treatment can be evaluated by the values of the lightness index L and the chromaticness indexes a and b according to the Hunter's color difference formula (see JIS Z8730). In other words, the higher the L value of the lightness index, the whiter the color index is, while the chromaticness index is about the degree of coloring, and the higher the a value, the stronger the redness,
The higher the b value, the stronger the yellow color.
【００３３】そしてこの発明において、陽極酸化皮膜が
１０μｍ程度の薄い膜厚でＬ値変動の小さい安定した灰
色を有する色調とは、皮膜厚が６〜１５μｍの場合のＬ
値が６０〜７７の範囲内であって、しかも皮膜厚を一定
とした場合のＬ値の変動範囲が３以内、ａ値およびｂ値
がいずれも−１〜＋１の範囲内の無彩色を目標としてい
る。さらに詳細に各皮膜厚での色調のＬ値、ａ値、ｂ値
の目標値を示せば、 皮膜厚６μｍの場合 Ｌ値：７４〜７７、 ａ値およびｂ値：−１〜＋１ 皮膜厚９μｍの場合 Ｌ値：７０〜７３、 ａ値およびｂ値：−１〜＋１ 皮膜厚１５μｍの場合 Ｌ値：６０〜６３、 ａ値およびｂ値：−１〜＋１ となる。そしてこの発明のアルミニウム合金圧延板に通
常の硫酸浴による陽極酸化処理を施せば、上述のような
目標値を容易に達成して、特にＬ値変動が小さく安定し
た灰色を呈する６〜１５μｍの厚みの陽極酸化皮膜を得
ることができる。In the present invention, the color tone in which the anodic oxide film has a small thickness of about 10 μm and has a stable gray color with a small variation in L value is defined as a color tone when the film thickness is 6 to 15 μm.
The target is an achromatic color in which the value is within the range of 60 to 77, the variation of the L value is within 3 when the film thickness is constant, and the a value and the b value are all within the range of -1 to +1. And If the target values of the L value, a value, and b value of the color tone at each film thickness are shown in more detail, when the film thickness is 6 μm: L value: 74 to 77, a value and b value: −1 to +1 Film thickness 9 μm In the case of L value: 70 to 73, a value and b value: −1 to +1 In the case of a film thickness of 15 μm L value: 60 to 63, a value and b value: −1 to +1 If the aluminum alloy rolled sheet of the present invention is subjected to anodic oxidation treatment using a normal sulfuric acid bath, the above-described target value can be easily achieved, and in particular, a thickness of 6 to 15 μm that exhibits a stable gray with small L value fluctuations Can be obtained.
【００３４】[0034]
【実施例】表１に化学組成が示される合金符号Ａ〜Ｌの
各合金の溶湯を常法に従って溶製し、ＤＣ鋳造法によっ
て５５０ｍｍ×１２００ｍｍ×４０００ｍｍのスラブを
鋳造した。得られた各スラブについて面削後、表２の製
造条件番号１〜２０に示すような各条件で鋳塊加熱処理
を施し、続いてその加熱温度以下の温度で熱間圧延を開
始し、表２中に示す温度で熱間圧延を終了させ、板厚４
ｍｍの熱延板とした。各熱延板に対し、製造条件番号１
９，２０を除いた製造条件番号１〜１８の場合は板厚
２．２ｍｍまで一次冷間圧延を施してから中間焼鈍を施
した。製造条件番号１９，２０の場合は一次冷間圧延を
行なわずに、熱延板に対し直接中間焼鈍を施した。中間
焼鈍は、製造条件番号１〜１２，１４〜２０の場合は、
昇温速度、冷却速度が１〜５０℃／秒の範囲内の連続焼
鈍炉により５００℃で保持なしの条件で行ない、製造条
件番号１３の場合は比較例として４００℃×２ｈｒのバ
ッチ焼鈍を適用した。これらの中間焼鈍後、製造条件番
号１〜１３，１６〜１８の場合は板厚２．０ｍｍまで冷
間圧延を施して最終板とし、製造条件１５の場合は板厚
１．３ｍｍまで冷間圧延を施して最終板とし、さらに製
造条件番号１４の場合は冷間圧延を施さずに中間焼鈍の
まま最終板とした。また製造条件番号１９の場合は中間
焼鈍後３．６ｍｍまで、製造条件番号２０の場合は３．
２ｍｍまで、それぞれ冷間圧延を施して最終板とした。EXAMPLE A melt of each of the alloy symbols A to L whose chemical compositions are shown in Table 1 was melted according to a conventional method, and a slab of 550 mm × 1200 mm × 4000 mm was cast by DC casting. After facing the obtained slabs, ingot heat treatment was performed under the respective conditions as shown in production condition numbers 1 to 20 in Table 2, and then hot rolling was started at a temperature lower than the heating temperature, and The hot rolling was completed at the temperature shown in FIG.
mm hot rolled sheet. Manufacturing condition number 1 for each hot rolled sheet
In the case of Manufacturing Condition Nos. 1 to 18 excluding 9 and 20, the steel sheet was subjected to primary cold rolling to a sheet thickness of 2.2 mm and then to intermediate annealing. In the case of Production Condition Nos. 19 and 20, intermediate annealing was directly performed on the hot-rolled sheet without performing primary cold rolling. The intermediate annealing is performed in the case of manufacturing condition numbers 1 to 12 and 14 to 20,
A continuous annealing furnace in which the heating rate and the cooling rate are in the range of 1 to 50 ° C./sec is performed at 500 ° C. without holding. In the case of the production condition No. 13, batch annealing of 400 ° C. × 2 hr is applied as a comparative example. did. After these intermediate annealings, in the case of production condition numbers 1 to 13, 16 to 18, cold rolling is performed to a plate thickness of 2.0 mm to obtain a final plate, and in the case of production condition 15, cold rolling is performed to a plate thickness of 1.3 mm. To produce a final sheet, and in the case of Production Condition No. 14, the final sheet was subjected to intermediate annealing without cold rolling. Further, in the case of the manufacturing condition number 19, up to 3.6 mm after the intermediate annealing, and in the case of the manufacturing condition number 20, it is 3.
Each was subjected to cold rolling to 2 mm to obtain a final plate.
【００３５】各最終板について、引張試験により耐力を
測定し、また曲げ性について、曲げ加工の苛酷な条件の
１３５°曲げ試験（先端半径０．１ｍｍＲ）により評価
し、さらに結晶粒径について、表面の結晶粒を切断法に
より調べて平均結晶粒径を求めた。さらに、最大長さ１
〜８μｍのＡｌ−Ｍｎ系針状析出物および１μｍ未満の
Ａｌ−Ｍｎ−Ｓｉ系粒状析出物の密度を、透過電子顕微
鏡と光学顕微鏡とを併用して調べた。With respect to each final plate, the proof stress was measured by a tensile test, and the bendability was evaluated by a 135 ° bending test (tip radius 0.1 mmR) under severe bending conditions. Was examined by a cutting method to determine an average crystal grain size. In addition, the maximum length 1
The densities of ８8 μm Al—Mn-based needle-like precipitates and Al—Mn—Si-based granular precipitates of less than 1 μm were examined using both a transmission electron microscope and an optical microscope.
【００３６】さらに各最終板について、１０％ＮａＯＨ
水溶液でエッチングし、水洗後硝酸でデスマット処理し
た後、次のような条件で陽極酸化処理を施した。すなわ
ち、Ｈ２ ＳＯ４ 濃度１５ｖｏｌ％の硫酸浴を用い
て、浴温２０℃、電流密度１．５Ａ／ｄｍ2 で陽極酸
化処理を行ない、それぞれ９μｍの陽極酸化処理皮膜を
生成させた。Further, for each final plate, 10% NaOH
After etching with an aqueous solution, washing with water and desmutting with nitric acid, an anodic oxidation treatment was performed under the following conditions. That is, using a sulfuric acid bath having an H2SO4 concentration of 15 vol%, anodizing treatment was performed at a bath temperature of 20 [deg.] C. and a current density of 1.5 A / dm < 2 > to form anodized films of 9 [mu] m each.
【００３７】各板の陽極酸化処理皮膜の表面色調につい
て、スガ試験機製多光分光測色計ＭＳＣ−ＩＳ−２ＤＨ
を用い、色調はハンターの色差式による明度指数Ｌ、ク
ロマティクネス指数ａ，ｂで評価し、筋目は目視にて評
価した。これらの結果を表３に示す。なお表３中におい
て、１３５°曲げの評価は、○印は割れなし（合格）、
△印は肌荒れ発生（不合格）、×印は割れ発生（不合
格）を示す。With respect to the surface tone of the anodized film on each plate, a multi-spectrophotometer MSC-IS-2DH manufactured by Suga Test Instruments was used.
The color tone was evaluated by a lightness index L and a chromaticness index a and b according to a Hunter's color difference formula, and the streak was visually evaluated. Table 3 shows the results. In Table 3, the evaluation of 135 ° bending was as follows: ○ indicates no crack (pass);
The mark “Δ” indicates occurrence of rough skin (fail), and the mark “X” indicates occurrence of crack (fail).
【００３８】[0038]
【表１】 [Table 1]
【００３９】[0039]
【表２】 [Table 2]
【００４０】[0040]
【表３】 [Table 3]
【００４１】以下にこれらの個々の結果について説明す
る。In the following, these individual results will be described.
【００４２】製造条件番号１，４，５，１６〜２０の各
材料は、いずれも成分組成および製造プロセスの両者が
この発明で規定する条件を満たす発明例であり、表３に
示すように耐力は９５Ｎ／ｍｍ2 以上の従来材と同等
以上の強度を示し、一方曲げ性については、苛酷な１３
５°曲げ試験でも割れや肌荒れが発生せず、しかも９μ
ｍと薄い陽極酸化処理皮膜でも灰色で安定した色調が得
られる優れた材料となっていることが明らかである。Each of the production condition numbers 1, 4, 5, and 16 to 20 is an invention example in which both the component composition and the production process satisfy the conditions specified in the present invention. Shows a strength equal to or more than that of the conventional material of 95 N / mm 2 or more, while a bending property of 13
No cracking or roughening even in 5 ° bending test, and 9μ
It is clear that this is an excellent material that can obtain a stable gray color tone even with an anodized film as thin as m.
【００４３】一方製造条件番号２，３，６〜１０の材料
は、いずれもこの発明で規定する製造プロセス条件は満
たしているが、成分組成条件を満たさない比較例であ
る。このうち製造条件番号２はＭｎ量がこの発明で規定
する成分範囲よりも低い合金Ｂを用い、製造条件番号３
はＭｎ量がこの発明で規定する成分範囲よりも高い合金
Ｃを用いたものであり、前者の場合はＭｎ量が少ないた
め１〜８μｍのＡｌ−Ｍｎ系針状析出物の密度が低過ぎ
てＬ値が目標範囲を上廻ってしまい、後者の場合はＭｎ
量が多いため１〜８μｍのＡｌ−Ｍｎ系針状析出物の密
度が高過ぎてＬ値が目標範囲を下廻ってしまった。一方
製造条件番号６はＭｇ量がこの発明で規定する成分範囲
よりも低い合金Ｆを用い、製造条件番号７はＭｇ量がこ
の発明で規定する成分範囲よりも高い合金Ｇを用いたも
のであり、前者の場合はＭｇ量が少ないため耐力が９５
Ｎ／ｍｍ2 以下の低強度となり、後者の場合はＭｇ量
が多いため耐力が高過ぎて曲げ加工性が低下してしまっ
た。さらに製造条件番号８はＦｅ量がこの発明で規定す
る成分範囲よりも高い合金Ｈを用い、製造条件番号９お
よび１０はＳｉ量がこの発明で規定する成分範囲よりも
高い合金ＩおよびＪを用いたものであり、前者の場合は
Ｆｅ量が多いためＡｌ−Ｍｎ−Ｆｅ系金属間化合物が増
加して１〜８μｍのＡｌ−Ｍｎ系針状析出物の密度が低
くなって、Ｌ値が目標範囲を上廻ってしまい、後者の場
合はＳｉ量が多いため１μｍ未満の大きさのＡｌ−Ｍｎ
−Ｓｉ系粒状析出物が析出してｂ値が上りＬ値が目標範
囲を下廻ってしまった。On the other hand, the materials of Production Condition Nos. 2, 3, and 6 to 10 are comparative examples which satisfy the production process conditions specified in the present invention but do not satisfy the component composition conditions. Among them, Production Condition No. 2 used Alloy B whose Mn content was lower than the component range specified in the present invention, and Production Condition No. 3
Is alloy C having a higher Mn content than the component range specified in the present invention. In the former case, the density of the Al-Mn-based acicular precipitate of 1 to 8 μm is too low because the Mn content is small. The L value exceeds the target range, and in the latter case, Mn
Since the amount was large, the density of the Al-Mn-based acicular precipitate of 1 to 8 µm was too high, and the L value fell below the target range. On the other hand, Production Condition No. 6 uses Alloy F whose Mg content is lower than the component range specified in the present invention, and Manufacturing Condition No. 7 uses Alloy G whose Mg content is higher than the component range specified in the present invention. In the former case, the yield strength is 95 because the amount of Mg is small.
The strength was as low as N / mm 2 or less, and in the latter case, the yield was too high due to the large amount of Mg, and the bending workability was reduced. Further, Production Condition No. 8 uses Alloy H whose Fe content is higher than the component range specified in the present invention, and Manufacturing Condition Nos. 9 and 10 uses Alloys I and J whose Si content is higher than the component range specified in the present invention. In the former case, since the amount of Fe is large, the Al-Mn-Fe-based intermetallic compound increases and the density of the Al-Mn-based needle-like precipitate of 1 to 8 µm decreases, and the L value reaches the target. In the latter case, since the amount of Si is large, Al—Mn having a size of less than 1 μm
-Si-based granular precipitates precipitated, the b value rose, and the L value fell below the target range.
【００４４】一方製造条件番号１１〜１５はこの発明で
規定する成分組成条件を満たした合金（製造条件番号１
３のみ合金Ｄ、他は合金Ａ）を用いてはいるが、製造プ
ロセス条件がこの発明で規定する条件から外れた比較例
である。このうち製造条件番号１１は鋳塊加熱温度が低
過ぎて、１〜８μｍのＡｌ−Ｍｎ系針状析出物が不均一
に分布してその密度が低下したため、Ｌ値が目標範囲を
上廻り、筋目不良が発生した。また製造条件番号１２は
熱間圧延終了温度が高過ぎて熱間圧延終了時に部分再結
晶が生じ、それが中間焼鈍の再結晶粒にも影響して混粒
組織となってしまい、筋目不良が発生した。さらに製造
条件番号１３は中間焼鈍をバッチ炉で行なったため、再
結晶粒が粗大化して曲げ加工時に肌荒れが発生した。そ
してまた製造条件番号１４は中間焼鈍後に冷間圧延を行
なわなかったため耐力が９５Ｎ／ｍｍ2 以下の低強度
となってしまった。一方製造条件番号１５は冷間圧延率
が高過ぎて高耐力となったため、曲げ加工で割れてしま
った。On the other hand, Production Condition Nos. 11 to 15 correspond to alloys satisfying the component composition conditions specified in the present invention (Production Condition No. 1).
Although Comparative Example 3 uses alloy D and others use alloy A), this is a comparative example in which the manufacturing process conditions deviate from the conditions specified in the present invention. Among these, the production condition No. 11 was such that the ingot heating temperature was too low, the Al-Mn-based acicular precipitates of 1 to 8 µm were unevenly distributed and the density thereof was lowered, so that the L value exceeded the target range, A poor streak occurred. In Production Condition No. 12, the hot rolling end temperature is too high, and partial recrystallization occurs at the end of hot rolling, which also affects the recrystallized grains of the intermediate annealing, resulting in a mixed grain structure, which results in poor streaks. Occurred. Further, in the manufacturing condition No. 13, the intermediate annealing was performed in a batch furnace, so that the recrystallized grains became coarse and the surface became rough during bending. In production condition No. 14, since cold rolling was not performed after the intermediate annealing, the yield strength was low, that is, 95 N / mm 2 or less. On the other hand, in production condition No. 15, the cold rolling reduction was too high, resulting in a high yield strength, and thus cracked by bending.
【００４５】[0045]
【発明の効果】前述の実施例からも明らかなように、こ
の発明の製造方法によれば、特に曲げ加工性が良好であ
って強度も耐力９５Ｎ／ｍｍ2 以上と従来材なみで、
しかも１０μｍ程度の薄い陽極酸化皮膜でもＬ値変動の
小さい安定した灰色を呈するアルミニウム合金圧延板を
得ることができる。そしてこの発明により得られたアル
ミニウム合金圧延板を陽極酸化処理を施した灰色の建
材、特に内装材や、そのほか器物、各種電気機器・計測
器の筐体やパネル、装飾品等に使用すれば、厳しい曲げ
加工の施工デザインでも可能となり、かつ薄い陽極酸化
皮膜でＬ値変動が小さく安定した灰色を呈するところか
ら、陽極酸化処理コストの低減も可能となる。As is clear from the above-described embodiment, according to the manufacturing method of the present invention, the bending workability is particularly good and the strength is 95 N / mm 2 or more, which is equivalent to that of the conventional material.
Moreover, even with a thin anodic oxide film having a thickness of about 10 μm, a rolled aluminum alloy plate exhibiting a stable gray color with small L value fluctuation can be obtained. And if the aluminum alloy rolled plate obtained by the present invention is used for gray building materials subjected to anodizing treatment, especially interior materials, and other objects, housings and panels of various electric instruments and measuring instruments, decorative articles, etc. It is possible even with a severe bending work design, and since the thin anodic oxide film shows a stable gray with a small variation in the L value, the anodizing treatment cost can be reduced.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｆ 1/00 ６８２ Ｃ２２Ｆ 1/00 ６８２ ６８３ ６８３ ６８４ ６８４Ａ ６８５ ６８５ ６９１ ６９１Ａ ６９１Ｂ ６９１Ｃ ６９２ ６９２Ａ ６９４ ６９４Ａ ６９４Ｂ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22F 1/00 682 C22F 1/00 682 683 683 684 684A 685 685 691 691A 691B 691C 692 692A 694 694A 694B
Claims (4)
じ）、Ｍｇ０．４〜１．２％、Ｆｅ０．２％以下を含有
し、Ｓｉ０．０５％未満に規制し、残部がＡｌおよび不
可避的不純物よりなり、かつ、１μｍ未満の大きさのＡ
ｌ−Ｍｎ−Ｓｉ系粒状析出物の析出がなく、１〜８μｍ
の大きさのＡｌ−Ｍｎ系針状析出物が１０００〜４００
０個／０．２ｍｍ2 の範囲内の密度で析出しており、
しかも平均結晶粒径が８０μｍ以下で、耐力が９５Ｎ／
ｍｍ2 以上であることを特徴とする、陽極酸化処理後
の色調が灰色で安定なアルミニウム合金圧延板。1. Mn contains 1.3 to 1.5% (weight%, the same applies hereinafter), Mg 0.4 to 1.2%, Fe 0.2% or less, and is regulated to less than 0.05% of Si, and the balance is less than 0.05%. A consisting of Al and unavoidable impurities and having a size of less than 1 μm
No precipitation of 1-Mn-Si-based granular precipitates, 1-8 μm
Al-Mn based needle-like precipitates having a size of 1000 to 400
0 / precipitated at a density in the range of 0.2 mm 2 ,
Moreover, the average crystal grain size is 80 μm or less, and the yield strength is 95 N /
A rolled aluminum alloy plate having a stable gray tone after anodic oxidation treatment, characterized in that the thickness is not less than 2 mm 2 .
単独でもしくは０．０００１〜０．０１％のＢと組合さ
れて含有することを特徴とする、請求項１記載の陽極酸
化処理後の色調が灰色で安定なアルミニウム合金圧延
板。2. Anodizing treatment according to claim 1, further comprising 0.003 to 0.15% of Ti alone or in combination with 0.0001 to 0.01% of B. Rolled aluminum alloy plate with stable gray tone.
を有するＡｌ合金の鋳塊に、５８０〜６３０℃の範囲内
の温度で１〜２４時間保持する加熱処理を施し、次いで
前記加熱処理における処理温度以下で熱間圧延を開始し
て、その熱間圧延を３００℃以下で終了し、その後１〜
５０℃／秒の昇温速度で４００〜６００℃の範囲内の温
度に加熱して０〜１０分保持した後１〜５０℃／秒の冷
却速度で冷却する中間焼鈍を施し、さらに２〜３０％の
圧延率で冷間圧延を施し、これにより１μｍ未満の大き
さのＡｌ−Ｍｎ−Ｓｉ系粒状析出物の析出がなく、１〜
８μｍの大きさのＡｌ−Ｍｎ系針状析出物が１０００〜
４０００個／０．２ｍｍ 2 の範囲内の密度で析出して
おり、しかも平均結晶粒径が８０μｍ以下で、耐力が９
５Ｎ／ｍｍ2 以上であることを特徴とする、陽極酸化
処理後の色調が灰色で安定なアルミニウム合金圧延板の
製造方法。3. The chemical composition according to claim 1 or claim 2.
In the range of 580 to 630 ° C for ingots of Al alloy having
Heat treatment for 1 to 24 hours at the temperature of
Start hot rolling below the processing temperature in the heat treatment
The hot rolling is completed at 300 ° C. or less,
A temperature in the range of 400 to 600 ° C. at a rate of 50 ° C./sec.
After heating and holding for 0 to 10 minutes, cool at 1 to 50 ° C / sec.
Intermediate annealing for cooling at the cooling speed
Cold-rolled at a reduction rate, thereby reducing the size to less than 1 μm.
No Al-Mn-Si-based granular precipitates were deposited.
Al-Mn-based acicular precipitates having a size of 8 µm
4000 pieces / 0.2mm Two With a density within the range of
With an average crystal grain size of 80 μm or less and a proof stress of 9
5N / mmTwo Characterized by the above, anodizing
Rolled aluminum alloy plate with stable gray color after treatment
Production method.
延を施すことを特徴とする、請求項３に記載の陽極酸化
処理後の色調が灰色で安定なアルミニウム合金圧延板の
製造方法。4. The production of a rolled aluminum alloy sheet having a stable gray tone after anodizing according to claim 3, wherein primary cold rolling is performed after hot rolling and before intermediate annealing. Method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07403299A JP4040787B2 (en) | 1999-03-18 | 1999-03-18 | Aluminum alloy rolled plate with stable gray color after anodization and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000273563A true JP2000273563A (en) | 2000-10-03 |
| JP4040787B2 JP4040787B2 (en) | 2008-01-30 |
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| JP2006322035A (en) * | 2005-05-18 | 2006-11-30 | Furukawa Sky Kk | Rolled sheet of aluminum alloy for painted roof material and manufacturing method therefor |
| JP2009209426A (en) * | 2008-03-05 | 2009-09-17 | Sumitomo Light Metal Ind Ltd | Aluminum alloy material for housing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006322035A (en) * | 2005-05-18 | 2006-11-30 | Furukawa Sky Kk | Rolled sheet of aluminum alloy for painted roof material and manufacturing method therefor |
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| EP2177638A1 (en) * | 2008-10-15 | 2010-04-21 | "Impexmetal" S.A. | Aluminium alloy, in particular for heat exchangers manufacturing |
| EP2653577A2 (en) | 2012-04-20 | 2013-10-23 | Sumitomo Light Metal Industries, Ltd. | Aluminum alloy sheet that exhibits excellent surface quality after anodizing and method for producing the same |
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| EP2695959A1 (en) | 2012-08-08 | 2014-02-12 | Sumitomo Light Metal Industries, Ltd. | Aluminum alloy sheet that exhibits excellent surface quality after anodizing and method for producing the same |
| KR20140020185A (en) | 2012-08-08 | 2014-02-18 | 스미토모 게이 긴조쿠 고교 가부시키가이샤 | Aluminum alloy sheet that exhibits excellent surface quality after anodizing and method for producing the same |
| JP2017147292A (en) * | 2016-02-16 | 2017-08-24 | レノボ・シンガポール・プライベート・リミテッド | Method for manufacturing housing member |
| US10285294B2 (en) | 2016-02-16 | 2019-05-07 | Lenovo (Singapore) Pte Ltd | Method for producing a chassis member usable in a chassis of an electronic device |
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|---|---|
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