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JP2001098338A - High strength and high formability aluminum alloy sheet with excellent recrystallization grain refinement during high temperature annealing - Google Patents

High strength and high formability aluminum alloy sheet with excellent recrystallization grain refinement during high temperature annealing

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Publication number
JP2001098338A
JP2001098338A JP27429399A JP27429399A JP2001098338A JP 2001098338 A JP2001098338 A JP 2001098338A JP 27429399 A JP27429399 A JP 27429399A JP 27429399 A JP27429399 A JP 27429399A JP 2001098338 A JP2001098338 A JP 2001098338A
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JP
Japan
Prior art keywords
less
grain size
annealing
aluminum alloy
alloy sheet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP27429399A
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Japanese (ja)
Other versions
JP4164206B2 (en
Inventor
Kazunori Kobayashi
一徳 小林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Furukawa Electric Co Ltd
Sky Aluminium Co Ltd
Kobe Steel Ltd
Nippon Light Metal Co Ltd
Sumitomo Light Metal Industries Ltd
MA Aluminum Corp
Original Assignee
Mitsubishi Aluminum Co Ltd
Furukawa Electric Co Ltd
Sky Aluminium Co Ltd
Kobe Steel Ltd
Nippon Light Metal Co Ltd
Sumitomo Light Metal Industries Ltd
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Application filed by Mitsubishi Aluminum Co Ltd, Furukawa Electric Co Ltd, Sky Aluminium Co Ltd, Kobe Steel Ltd, Nippon Light Metal Co Ltd, Sumitomo Light Metal Industries Ltd filed Critical Mitsubishi Aluminum Co Ltd
Priority to JP27429399A priority Critical patent/JP4164206B2/en
Publication of JP2001098338A publication Critical patent/JP2001098338A/en
Application granted granted Critical
Publication of JP4164206B2 publication Critical patent/JP4164206B2/en
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Abstract

(57)【要約】 【課題】 高温の再結晶焼鈍を行っても、焼鈍後の再
結晶粒度を5 μm 以下の超微細粒とすることが可能なAl
-Mg 系Al合金板を提供することを目的とする。 【解決手段】 Mg:3.0〜10.0% 、Mn:0.1〜1.5%を含み
残部Alおよび不可避的不純物からなり、冷間圧延におい
て90% 以上の圧下が加えられるとともに、最終焼鈍後の
再結晶粒度が5 μm 以下であるAl-Mg 系Al合金板であっ
て、組織内に分散析出するAl-Mn 系化合物の最大長さを
500nm 以下とすることである。
(57) [Summary] [Problem] Al capable of forming ultra-fine grains having a recrystallized grain size of 5 μm or less even after high-temperature recrystallization annealing.
It is intended to provide a -Mg-based Al alloy plate. SOLUTION: Mg: 3.0 to 10.0%, Mn: 0.1 to 1.5%, the balance being Al and unavoidable impurities, the reduction of 90% or more is applied in cold rolling, and the recrystallized grain size after final annealing is reduced. In Al-Mg-based Al alloy sheets with a size of 5 μm or less, the maximum length of Al-Mn-based
It should be less than 500nm.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、高温焼鈍時の再結
晶粒微細化に優れた高強度高成形性アルミニウム合金板
(以下、アルミニウムを単にAlと言う)に関するもので
ある。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-strength and high-formability aluminum alloy sheet (hereinafter, aluminum is simply referred to as Al) excellent in refining recrystallized grains during high-temperature annealing.

【0002】[0002]

【従来の技術】鉄道車両、航空機、船舶、自動車、自動
二輪、自転車等の輸送機、或いは圧力容器やタンク等の
化学プラント、更には建築物や構造物等の構造部材や構
造部品として、主として、AA乃至JIS 5052、5056、508
2、5182、5083、5086等の、Mgを3.5% (質量% 、以下同
じ) 以上を含むAl-Mg 系乃至5000系Al合金板が使用され
ている。これらMg含有量の多いAl-Mg 系Al合金板は、優
れた強度や成形性を持ち、溶接性も良好であるため、溶
接構造部材として汎用されている。
2. Description of the Related Art Mainly as transportation equipment such as railway vehicles, aircrafts, ships, automobiles, motorcycles and bicycles, or chemical plants such as pressure vessels and tanks, and also as structural members and structural parts such as buildings and structures. , AA to JIS 5052, 5056, 508
Al-Mg-based to 5000-based Al alloy sheets containing 3.5% (% by mass, the same applies hereinafter) of Mg, such as 2, 5182, 5083, and 5086, are used. These Al-Mg-based Al alloy sheets having a high Mg content have excellent strength and formability and good weldability, and thus are widely used as welded structural members.

【0003】このAl-Mg 系Al合金板は、周知の通り、常
法により、鋳塊を均質化熱処理後、熱間圧延および冷間
圧延により所定の板厚とした後、再結晶焼鈍を行ってAl
合金板とされる。そして、このAl-Mg 系Al合金板の再結
晶粒度は、通常20〜30μm のレベルである。
[0003] As is well known, the Al-Mg-based Al alloy sheet is subjected to a recrystallization annealing after a homogenizing heat treatment of the ingot, a hot rolling and a cold rolling to a predetermined thickness, in a usual manner. Al
It is an alloy plate. The recrystallized grain size of the Al-Mg-based Al alloy sheet is usually at a level of 20 to 30 µm.

【0004】これに対し、近年、このAl-Mg 系Al合金板
の強度や成形性の更なる向上のために、再結晶粒度をよ
り微細化することが研究されている。例えば、特願平11
-268599 号などでは、最大で7.0%までのMgを含有させる
とともに、Fe:0.1〜2.0%、Cr:0.05 〜0.5%、Zr:0.05 〜
0.2%の一種または二種以上を含むAl-Mg 系Al合金につい
て、冷間圧延において90% 以上の大圧下を加えて、再結
晶焼鈍後の再結晶粒度を5 μm 以下の超微細粒とするこ
とが提案されている。
On the other hand, in recent years, to further improve the strength and formability of the Al-Mg-based Al alloy sheet, studies have been made to further refine the recrystallized grain size. For example, Japanese Patent Application No. 11
-268599, etc., contain up to 7.0% Mg, Fe: 0.1-2.0%, Cr: 0.05-0.5%, Zr: 0.05-
For Al-Mg-based Al alloys containing 0.2% or more of one or more types, apply a large reduction of 90% or more in cold rolling to reduce the recrystallized grain size after recrystallization annealing to 5μm or less. It has been proposed.

【0005】この技術は、Mg含有量を極端に多くすると
ともに、冷間圧延において大圧下を加えて、再結晶の核
生成サイトとなる転位やFeを含む化合物粒子を増加さ
せ、更に、Mn、Cr、Zrなどの分散粒子 (析出物) によ
り、粒界の移動による再結晶粒の粗大成長を抑制しよう
とするものである。
In this technique, the Mg content is extremely increased, and a large reduction is applied in the cold rolling to increase the number of dislocations and Fe-containing compound particles serving as nucleation sites for recrystallization. The purpose is to suppress the coarse growth of recrystallized grains due to the movement of grain boundaries by using dispersed particles (precipitates) such as Cr and Zr.

【0006】[0006]

【発明が解決しようとする課題】この再結晶粒微細化技
術により、実際に、再結晶焼鈍後の再結晶粒度を5 μm
以下の超微細粒としたAl-Mg 系Al合金板の製造が可能と
なる。しかし、この再結晶粒微細化技術では、再結晶粒
度を5 μm 以下とするために、再結晶焼鈍温度を350 ℃
以下の低温とする必要がある。言い換えると、再結晶焼
鈍温度を350 ℃を越える温度とした場合、再結晶粒が粗
大化して、粒度を5 μm 以下とすることができなくな
る。
According to the recrystallized grain refining technique, the recrystallized grain size after recrystallization annealing is actually reduced to 5 μm.
The following ultrafine-grained Al-Mg-based Al alloy sheets can be manufactured. However, in this recrystallized grain refinement technology, the recrystallization annealing temperature is set to 350 ° C. in order to reduce the recrystallized grain size to 5 μm or less.
The following low temperature is required. In other words, if the recrystallization annealing temperature is set to a temperature exceeding 350 ° C., the recrystallized grains become coarse and the grain size cannot be reduced to 5 μm or less.

【0007】この再結晶粒微細化技術では、Mg含有量を
極端に多くするとともに、冷間圧延において大圧下を加
えているため、Al合金板の加工硬化量が極端に大きい。
このため、再結晶焼鈍の際の温度が低温側に制約される
と、焼きなましが不十分となる場合が生じ、前記各種用
途で要求される伸びや絞り高さなどの成形性を満足でき
ない可能性がある。
In this recrystallization grain refinement technique, the Mg content is extremely increased, and a large reduction is applied during cold rolling, so that the work hardening amount of the Al alloy sheet is extremely large.
For this reason, if the temperature during the recrystallization annealing is restricted to a lower temperature side, annealing may be insufficient, and the formability such as elongation and drawing height required in the above various applications may not be satisfied. There is.

【0008】この点、前記特願平11-268599 号でも、最
終焼鈍温度を350 ℃以下の低温とする必要があることが
明記され、その実施例では、この発明範囲内の、Mn:0.2
% 、Fe:1.26%、Cr:0.15%を含むAl-Mg 系Al合金板につい
て、最終焼鈍温度を420 ℃とした場合に、350 ℃未満の
焼鈍温度の発明例に比して、再結晶粒度が5 μm を越え
て粗大化し、Al合金板の成形性などの特性が低下してい
ることが記載されている。
In this respect, Japanese Patent Application No. 11-268599 also discloses that the final annealing temperature must be as low as 350 ° C. or less.
%, Fe: 1.26%, Cr: 0.15%, when the final annealing temperature is 420 ° C., the recrystallized grain size is lower than that of the invention example having an annealing temperature of less than 350 ° C. It is described that the average grain size exceeds 5 μm and the properties such as formability of the Al alloy sheet are deteriorated.

【0009】従って、この再結晶粒微細化技術では、再
結晶焼鈍後の再結晶粒度を5 μm 以下の超微細粒とする
ためは、焼鈍温度を350 ℃未満の低温とする必要があ
る。このため、用途によっては、強度が高すぎる乃至Al
-Mg 系Al合金板特有のSSマークが生じるなど、要求され
る成形性を満足できない場合が生じ、Al合金板の用途が
制約される可能性がある。
Therefore, in this recrystallized grain refining technique, the annealing temperature must be lower than 350 ° C. in order to make the recrystallized grain size after recrystallization annealing smaller than 5 μm. For this reason, depending on the application, the strength is too high or Al
In some cases, the required formability may not be satisfied, such as the generation of SS marks specific to -Mg-based Al alloy sheets, and the applications of the Al alloy sheets may be restricted.

【0010】本発明はこの様な事情に着目してなされた
ものであって、その目的は、高温の再結晶焼鈍を行って
も、焼鈍後の再結晶粒度を5 μm 以下の超微細粒とする
ことが可能なAl-Mg 系Al合金板を提供しようとするもの
である。
The present invention has been made in view of such circumstances, and has as its object to reduce the recrystallized grain size after annealing to ultra-fine grains of 5 μm or less even after high-temperature recrystallization annealing. It is an object of the present invention to provide an Al-Mg-based Al alloy sheet that can be used.

【0011】[0011]

【課題を解決するための手段】この目的を達成するため
に、本発明Al-Mg 系Al合金板の要旨は、Mg:3.0〜10.0%
(質量% 、以下同じ) 、Mn:0.1〜1.5%を含み残部Alおよ
び不可避的不純物からなり、冷間圧延において90% 以上
の圧下が加えられるとともに、最終焼鈍後の再結晶粒度
が5 μm 以下である、Al-Mg 系Al合金板であって、組織
内に分散析出するAl-Mn 系化合物の最大長さを500nm 以
下とすることである。
In order to achieve this object, the gist of the Al-Mg-based Al alloy sheet of the present invention is as follows: Mg: 3.0 to 10.0%
(% By mass, the same applies hereinafter), Mn: 0.1 to 1.5%, the balance consisting of Al and unavoidable impurities, a reduction of 90% or more is applied in cold rolling, and the recrystallization grain size after final annealing is 5 μm or less. In the Al-Mg-based Al alloy plate, the maximum length of the Al-Mn-based compound dispersed and precipitated in the structure is set to 500 nm or less.

【0012】また、選択的添加元素を加えた本発明Al合
金板の別の態様として、前記Al合金板が、更に、Fe:0.1
〜2.0%、Cr:0.05 〜0.2%、Zr:0.05 〜0.2%の一種または
二種以上を含む (請求項2 に対応) 、および/ または、
Ti:0.001〜0.1%、B:1 〜300ppmの一種または二種を含む
(請求項3 に対応) を含むことである。
Further, as another embodiment of the Al alloy sheet of the present invention to which the selective addition element is added, the Al alloy sheet further comprises Fe: 0.1
~ 2.0%, Cr: 0.05 ~ 0.2%, Zr: 0.05 ~ 0.2% containing one or more of (corresponding to claim 2), and / or
Contains one or two types of Ti: 0.001-0.1%, B: 1-300ppm
(Corresponding to claim 3).

【0013】そして、本発明Al合金板の好ましい用途と
しては、焼鈍の温度が350 ℃を越える高温の最終焼鈍に
用いられることである (請求項4 に対応) 。
A preferable use of the Al alloy sheet of the present invention is that it is used for final annealing at a high temperature exceeding 350 ° C. (corresponding to claim 4).

【0014】本発明では、前記特願平11-268599 号の技
術思想を前提としている。即ち、Mg含有量を多くすると
ともに、冷間圧延において大圧下を加えて、再結晶の核
生成サイトとなる転位を増加させ、加えて核生成サイト
となるFeの化合物粒子( 晶出物) を増加させ、更に、M
n、Cr、Zrなどの化合物粒子 (析出物) により、粒界の
移動による再結晶粒の粗大成長を抑制し、最終焼鈍後の
再結晶粒度を5 μm 以下とする技術思想は、前記特願平
11-268599 号と同じである。したがって、本発明では、
後述するMnの必須添加と、Al合金板が90% 以上の大きな
圧下率で冷間圧延されることを前提とする。
The present invention is based on the technical idea of Japanese Patent Application No. 11-268599. That is, while increasing the Mg content, a large reduction is applied in cold rolling to increase the dislocations that serve as nucleation sites for recrystallization, and further reduce Fe compound particles (crystallized products) that serve as nucleation sites. Increase, and M
The technical idea of suppressing the coarse growth of recrystallized grains due to the movement of grain boundaries by using compound particles (precipitates) such as n, Cr, and Zr and reducing the recrystallized grain size after final annealing to 5 μm or less is described in the above-mentioned patent application. flat
Same as 11-268599. Therefore, in the present invention,
It is premised that essential addition of Mn to be described later and that the Al alloy sheet is cold-rolled at a large rolling reduction of 90% or more.

【0015】しかし、本発明者らは、まず、粒界の移動
による再結晶粒の粗大成長を抑制すべき、Mn、Cr、Zrな
どの化合物粒子乃至分散粒子 (析出物) に、前記350 ℃
以上の高温の再結晶焼鈍時には、350 ℃未満の低温の再
結晶焼鈍時には無い、再結晶粒度の微細化 (粗大化防
止) 効果の差が生じることを知見した。
[0015] However, the present inventors first added the compound particles or dispersed particles (precipitates) such as Mn, Cr, and Zr, which should suppress the coarse growth of recrystallized grains due to the movement of the grain boundaries, to the temperature of 350 ° C.
It was found that a difference in the effect of refining the recrystallized grain size (preventing coarsening) occurs during the above-described high-temperature recrystallization annealing, which does not occur during the low-temperature recrystallization annealing at less than 350 ° C.

【0016】即ち、Mn、Cr、Zrなどの化合物粒子は、周
知の通り、前記Al-Mg 系Al合金鋳塊の均質化熱処理時に
生じるものである。ただ、各々の含有量や鋳造条件およ
び均質化熱処理時の条件によって、特に、化合物粒子の
大きさや形状が異なり、これが、350 ℃以上の高温の再
結晶焼鈍時の再結晶粒度の微細化 (粗大化防止) 効果の
差につながる。
That is, as is well known, compound particles such as Mn, Cr, and Zr are generated during the homogenizing heat treatment of the Al-Mg-based Al alloy ingot. However, the size and shape of the compound particles, in particular, differ depending on the respective contents, casting conditions, and conditions during the homogenization heat treatment, and this leads to the refinement of the recrystallization grain size during recrystallization annealing at 350 ° C or higher (coarse Prevention) leads to a difference in effectiveness.

【0017】特に、Cr、Zrなどの化合物粒子は、Mnの化
合物粒子の大きさに比して、通常は小さい。したがっ
て、通常、結晶粒の成長抑制効果は、Cr、Zrなどの化合
物粒子の方が、Mnの化合物粒子よりも大きいと思われが
ちである。
In particular, compound particles such as Cr and Zr are usually smaller than the size of Mn compound particles. Therefore, it is generally thought that the effect of suppressing the growth of crystal grains is larger in compound particles such as Cr and Zr than in Mn compound particles.

【0018】しかし、一方、Cr、Zrなどの化合物粒子に
は、核生成サイトを減少させる作用もあり、この作用が
大きいと、結晶粒の形状は、球状の等軸状ではなく、圧
延方向に伸長した伸長粒となる。そして、この伸長粒
は、特に、350 ℃以上の高温の再結晶焼鈍時には、より
粗大化しやすい。したがって、この結果が、Cr、Zrなど
の化合物粒子とMnの化合物粒子の再結晶粒度の微細化
(粗大化防止) 効果の差につながっているものと推考さ
れる。
On the other hand, compound particles such as Cr and Zr also have the effect of reducing the number of nucleation sites. If this effect is large, the shape of crystal grains is not spherical and equiaxed, but in the rolling direction. It becomes elongated grains that are elongated. The elongated grains tend to become coarser, especially during recrystallization annealing at a high temperature of 350 ° C. or higher. Therefore, this result indicates that the recrystallized particle size of the compound particles such as Cr and Zr and the compound particles of Mn can be reduced.
(Prevention of coarsening) It is presumed that this leads to a difference in effect.

【0019】このため、Cr、Zrなどの化合物粒子は、35
0 ℃未満の低温の再結晶焼鈍時には再結晶粒度の微細化
効果を発揮するものの、350 ℃以上の高温の再結晶焼鈍
時には再結晶粒度の微細化効果が弱くなる。この結果、
最終焼鈍後のAl-Mg 系Al合金板の再結晶粒度を、通常の
再結晶粒度20〜30μm のレベル以下の微細粒とはできる
ものの、本発明の主目的である5 μm 以下の超微細粒と
することができなくなる。
Therefore, compound particles such as Cr, Zr, etc.
At the time of recrystallization annealing at a low temperature of less than 0 ° C., the effect of refining the recrystallized grain size is exhibited, but at the time of recrystallization annealing at a high temperature of 350 ° C. or more, the effect of refining the recrystallized grain size becomes weak. As a result,
Although the recrystallized grain size of the Al-Mg-based Al alloy sheet after the final annealing can be reduced to a fine grain size less than the normal recrystallized grain size of 20 to 30 μm, the ultra-fine grain size of 5 μm or less which is the main object of the present invention is And cannot be done.

【0020】また、Mnの化合物粒子が粗大化した場合に
は、特に、350 ℃以上の高温の再結晶焼鈍時における、
Mnの化合物粒子自体の再結晶粒度の微細化効果が弱くな
ることも、本発明者らは知見した。そこで、本発明者ら
は、Mn化合物粒子の粗大化の、再結晶粒度の微細化効果
発揮の臨界的な大きさとして、Al-Mg 系Al合金板の結晶
粒内に分散析出するAl-Mg 系化合物の最大長さを500nm
以下とすべきことを更に知見して、本発明をなしたもの
である。
In the case where the Mn compound particles are coarsened, particularly, during recrystallization annealing at a high temperature of 350 ° C. or more,
The present inventors have also found that the effect of refining the recrystallized particle size of the Mn compound particles themselves is weakened. Therefore, the present inventors considered that the critical size of the coarsening of the Mn compound particles and the effect of refining the recrystallized grain size is that Al-Mg dispersed and precipitated in the crystal grains of the Al-Mg-based Al alloy plate. The maximum length of the compound is 500 nm
The present invention has been made by further understanding the following.

【0021】[0021]

【発明の実施の形態】(Al-Mn 系化合物粒子)本発明で言
うAl-Mn 系化合物粒子とは、FeやSiが含まれない場合に
はMnAl6 であり、FeやSiが含まれる場合には、(Fe,Mn)3
SiAl12、(Fe,Mn)Al6等の化合物である。
BEST MODE FOR CARRYING OUT THE INVENTION (Al-Mn-based compound particles) The Al-Mn-based compound particles referred to in the present invention are MnAl 6 when Fe or Si is not contained, and when they contain Fe or Si. Contains (Fe, Mn) 3
Compounds such as SiAl 12 and (Fe, Mn) Al 6 .

【0022】そして、本発明では、これらAl-Mn 系化合
物粒子の最大長さを500nm 以下と規定する。Al-Mn 系化
合物粒子の最大長さが500nm を越えて粗大化した場合、
前記した、Al合金組織内における、Al-Mn 系化合物粒子
の微細分散析出による、350℃以上の高温の再結晶焼鈍
時の再結晶粒度の微細化効果が弱くなる。この結果、最
終焼鈍後のAl-Mg 系Al合金板の再結晶粒度を、通常の再
結晶粒度20〜30μm のレベル以下の微細粒とはできるも
のの、本発明の主目的である5 μm 以下の超微細粒とす
ることができなくなる。
In the present invention, the maximum length of the Al-Mn-based compound particles is specified to be 500 nm or less. When the maximum length of the Al-Mn-based compound particles exceeds 500 nm,
Due to the fine dispersion of Al-Mn-based compound particles in the Al alloy structure, the effect of refining the recrystallized grain size during recrystallization annealing at 350 ° C. or higher is weakened. As a result, although the recrystallized grain size of the Al-Mg-based Al alloy sheet after the final annealing can be reduced to a fine grain of the ordinary recrystallized grain size of 20 to 30 μm or less, the recrystallization grain size of 5 μm or less which is the main object of the present invention is obtained. Ultrafine particles cannot be obtained.

【0023】Al-Mn 系化合物粒子の最大長さは、Al-Mn
系化合物粒子の形状にもよるが、Al-Mn 系化合物粒子の
形状の内、最も長い部分の長さである。例えば、Al-Mn
系化合物粒子が板状の場合には最大の辺の長さ、粒状の
場合には最大の径の長さ等が該当する。
The maximum length of the Al-Mn-based compound particles is Al-Mn
Although it depends on the shape of the Al-Mn-based compound particles, it is the length of the longest part among the shapes of the Al-Mn-based compound particles. For example, Al-Mn
In the case where the system compound particles are plate-shaped, the maximum side length is applicable, and in the case where the system compound particles are granular, the maximum diameter length is applicable.

【0024】これらAl-Mn 系化合物粒子の最大長さの測
定と同定 (検証) は、Al合金組織の10000 倍以上の透過
電子顕微鏡(TEM) による、観察により行う。なお、透過
型電子顕微鏡による測定は、機械研磨で約0.1mm 厚みに
薄肉化した測定用試料を、更に、電解研磨 (ジェットポ
リッシュ) で観察部位の厚さを局部的に0.1 〜0.3 μm
(1000〜3000Å) の薄膜化した部位をTEM で観察して行
う。そして、各視野で測定できるAl-Mn 系化合物粒子の
最大長さを各々計測し、1 視野当たりの化合物粒子の最
大長さを10視野で平均値化したものとする。
The measurement and identification (verification) of the maximum length of the Al-Mn-based compound particles is carried out by observation with a transmission electron microscope (TEM) of 10,000 times or more of the Al alloy structure. In the transmission electron microscope measurement, the thickness of the observation part was locally reduced to 0.1 to 0.3 μm by electropolishing (jet polishing) using a measurement sample thinned to a thickness of about 0.1 mm by mechanical polishing.
(1000-3000Å) The thinned part is observed by TEM. Then, the maximum length of the Al-Mn-based compound particles that can be measured in each visual field is measured, and the maximum length of the compound particles per visual field is averaged in 10 visual fields.

【0025】また、Al合金板の再結晶粒度の測定は、光
学顕微鏡および走査電子顕微鏡(SEM) を用い、切断法に
より行う。より具体的には、直線で切断される結晶粒の
数が100 個以上となるように直線を描き、この直線の長
さを切断された結晶粒の数で除して、再結晶粒度とす
る。
The recrystallized grain size of the Al alloy plate is measured by a cutting method using an optical microscope and a scanning electron microscope (SEM). More specifically, draw a straight line so that the number of crystal grains cut by a straight line is 100 or more, and divide the length of this straight line by the number of cut crystal grains to obtain a recrystallized grain size. .

【0026】(本発明Al合金の化学成分組成)次に、本発
明Al合金における、化学成分組成について説明する。
(Chemical Composition of the Al Alloy of the Present Invention) Next, the chemical composition of the Al alloy of the present invention will be described.

【0027】(本発明Al合金の各元素量) Mg:3.0〜10.0% 。 Mgは、Al合金板に構造材に必要な強度と成形性を固溶強
化により付与するとともに、大圧下による冷間圧延時の
回復を抑制し、最終焼鈍後の再結晶粒度を微細にするた
めに必須の元素である。Mgの3.0%未満の含有では、固溶
強化が十分ではなく、更に大圧下による冷間圧延時の回
復を抑制できず、最終焼鈍後の再結晶粒度の微細化が困
難となる。この結果、必要な強度や成形性が不足する。
また、一方、10.0% を越えて含有されると、鋳造や熱間
圧延などの板の製造自体が困難となり、大圧下による冷
間圧延時のエッジクラックも増大するため、工業的な製
造に適さなくなる。したがって、Mgの含有量は3.0 〜1
0.0% の範囲とする。
(Amount of each element in Al alloy of the present invention) Mg: 3.0 to 10.0%. Mg provides the strength and formability necessary for the structural material to the Al alloy sheet by solid solution strengthening, suppresses recovery during cold rolling under large pressure, and refines the recrystallized grain size after final annealing. It is an essential element. If the content of Mg is less than 3.0%, solid solution strengthening is not sufficient, and furthermore, recovery during cold rolling under large pressure cannot be suppressed, making it difficult to refine the recrystallized grain size after final annealing. As a result, required strength and moldability are insufficient.
On the other hand, if the content exceeds 10.0%, it becomes difficult to produce a sheet itself by casting or hot rolling, and edge cracks during cold rolling under a large pressure increase, which is suitable for industrial production. Disappears. Therefore, the content of Mg is 3.0-1.
The range is 0.0%.

【0028】Mn:0.1〜1.5% Mnは、前記した通り、微細なAl-Mn 系化合物粒子の形成
と、350 ℃以上の高温の再結晶焼鈍 (最終焼鈍後) 後の
再結晶粒度の微細化、特に、再結晶粒度が5 μm 以下の
超微細化のために必要な元素である。Mnの含有量が0.1%
未満では、組織内に形成されるAl-Mn 系化合物粒子の量
(数) が不足し、350 ℃以上の高温の最終焼鈍後の再結
晶粒度を5 μm 以下の超微細化させることができない。
一方、Mnの含有量が1.5%を越えた場合には、結晶粒微細
化効果が飽和し、また、化合物粒子により、Al合金板の
伸びおよび成形性が却って低下する。したがって、Mnの
含有量は0.2 〜1.5%の範囲とする。
Mn: 0.1 to 1.5% Mn, as described above, forms fine Al-Mn-based compound particles and refines the recrystallized grain size after recrystallization annealing at 350 ° C. or higher (after final annealing). In particular, it is an element necessary for ultrafineness with a recrystallized grain size of 5 μm or less. Mn content 0.1%
If less than the amount of Al-Mn-based compound particles formed in the structure
(Number) is insufficient and the recrystallized grain size after final annealing at a high temperature of 350 ° C. or more cannot be reduced to an ultra-fine size of 5 μm or less.
On the other hand, when the content of Mn exceeds 1.5%, the effect of refining crystal grains is saturated, and the elongation and formability of the Al alloy sheet are rather reduced by the compound particles. Therefore, the content of Mn is in the range of 0.2 to 1.5%.

【0029】Fe:0.1〜2.0%、Cr:0.05 〜0.2%、Zr:0.05
〜0.2%。 Fe、Cr、Zrは、再結晶焼鈍後の再結晶粒度の微細化の効
果がある点で同効元素である。
Fe: 0.1-2.0%, Cr: 0.05-0.2%, Zr: 0.05
~ 0.2%. Fe, Cr and Zr are the same elements in that they have the effect of making the recrystallized grain size finer after recrystallization annealing.

【0030】Feは、Al-Fe 系の化合物粒子 (晶出物) を
形成し、再結晶焼鈍 (最終焼鈍後)時の核生成サイトと
なって、再結晶粒度の微細化の効果を発揮する元素であ
る。0.1%未満の含有ではこの効果が不足し、一方、2.0%
を越えた場合には、却って、再結晶焼鈍後のAl合金板の
成形性や伸びなどを低下させる。したがって、Feの含有
量は0.1 〜2.0%の範囲とする。
Fe forms Al-Fe-based compound particles (crystals), becomes a nucleation site during recrystallization annealing (after final annealing), and exerts the effect of refining the recrystallization particle size. Element. If the content is less than 0.1%, this effect is insufficient, while 2.0%
On the other hand, if it exceeds, the formability, elongation, etc. of the Al alloy sheet after recrystallization annealing are reduced. Therefore, the content of Fe is set in the range of 0.1 to 2.0%.

【0031】Cr、Zrは、前記Mnと同様に、Al-Cr 系、Al
-Zr 系の化合物粒子を形成し、再結晶焼鈍 (最終焼鈍
後) 後の再結晶粒度の微細化の効果がある同効元素であ
る。前記した通り、これらの再結晶粒度の微細化元素
は、350 ℃以上の高温の最終焼鈍後の再結晶粒度を5 μ
m 以下にする効果はないものの、350 ℃未満の低温の再
結晶焼鈍時には、焼鈍後の再結晶粒度を5 μm 以下にす
る微細化効果を発揮する。したがって、選択的に含ませ
る場合には、Mnを必須とし、これに加えて、一種または
2 種以上を組み合わせて用いる。
Cr and Zr are, like Mn, Al-Cr based, Al
-Zr-based compound particles that form the same particles and have the effect of refining the recrystallized grain size after recrystallization annealing (after final annealing). As described above, these recrystallized grains have a recrystallized grain size of 5 μm after final annealing at a high temperature of 350 ° C. or more.
Although it does not have the effect of reducing the particle size to less than m, during recrystallization annealing at a low temperature of less than 350 ° C., it exerts a refining effect of reducing the recrystallized grain size after annealing to 5 μm or less. Therefore, in the case of selective inclusion, Mn is required, and in addition to this,
Use a combination of two or more.

【0032】各々の下限量未満では、結晶粒内に形成さ
れる各々の化合物粒子の数乃至量が不足し、再結晶焼鈍
時の再結晶粒度を5 μm 以下にする微細化効果が無い。
一方で、各々の上限量を越えた場合には、結晶粒微細化
効果が飽和し、また、粗大な晶出物を生成し、却って、
Al合金板の破壊靱性および疲労特性、あるいは伸びや成
形性などを劣化させる。したがって、各々の含有量は、
Cr:0.05 〜0.2%、Zr:0.05 〜0.2%の範囲とする。
If the amount is less than each lower limit, the number or amount of each compound particle formed in the crystal grain is insufficient, and there is no effect of miniaturizing the recrystallized grain size during recrystallization annealing to 5 μm or less.
On the other hand, if the respective upper limits are exceeded, the crystal grain refining effect is saturated, and a coarse crystallized substance is generated.
Deterioration of fracture toughness and fatigue properties, elongation, formability, etc. of Al alloy sheets. Therefore, each content,
Cr: 0.05 to 0.2%, Zr: 0.05 to 0.2%.

【0033】Ti:0.001 〜0.1%、B:1 〜300ppm。 Ti、B は鋳塊の結晶粒を微細化する効果がある。このた
め、特にTiは通常添加する元素である。Tiの0.001%未
満、B の1ppm未満の含有では、この効果が得られず、一
方、Tiを0.1%を越えて、またB を300ppmを越えて含有す
ると、粗大な晶出物を形成する。したがって、Ti、B を
一種または二種含有する場合、Tiの含有量は0.001 〜0.
1%の範囲、B の含有量は1 〜300ppmの範囲と、各々する
ことが好ましい。
Ti: 0.001 to 0.1%, B: 1 to 300 ppm. Ti and B have the effect of refining the crystal grains of the ingot. For this reason, Ti is an element usually added. If the content of Ti is less than 0.001% and the content of B is less than 1 ppm, this effect cannot be obtained. On the other hand, if the content of Ti exceeds 0.1% and the content of B exceeds 300 ppm, coarse crystals are formed. Therefore, when one or two types of Ti and B are contained, the content of Ti is 0.001 to 0.
The content of B is preferably in the range of 1 to 300 ppm, and the content of B is preferably in the range of 1 to 300 ppm.

【0034】(本発明Al合金板の製造方法)Al合金板自体
は常法により製造可能であるものの、最終焼鈍処理時お
よび最終焼鈍処理後の、Al合金板の結晶粒内のAl-Mn 系
化合物の最大長さを500nm 以下とするため、また、最終
焼鈍後の再結晶粒度が5 μm 以下とするための好ましい
工程条件について以下に説明する。
(Method of Manufacturing Al Alloy Sheet of the Present Invention) Although the Al alloy sheet itself can be manufactured by an ordinary method, the Al-Mn system in the crystal grains of the Al alloy sheet at the time of final annealing and after the final annealing is performed. Preferred process conditions for setting the maximum length of the compound to 500 nm or less and for setting the recrystallized grain size after final annealing to 5 μm or less are described below.

【0035】Al-Mn 系化合物粒子の固溶と析出とを初期
に支配する鋳造工程においては、固溶を促進して、析出
を抑制することが好ましい。このためには、鋳造の際の
冷却速度が早い方が好ましい。この点、固定式水冷鋳型
を有する半連続鋳造法(DC鋳造法)よりは、回転式水
冷鋳型などを有する双ロール法、ベルトキャスター法、
3C法、ブロック法等の連鋳では、凝固時の冷却速度 (液
相線温度から固相線温度まで) を2 ℃/sec〜10℃/secと
することが可能となる。
In the casting step in which the solid solution and precipitation of the Al-Mn compound particles are initially controlled, it is preferable to promote the solid solution and suppress the precipitation. For this purpose, it is preferable that the cooling rate during casting be high. In this regard, rather than a semi-continuous casting method having a fixed water-cooled mold (DC casting method), a twin-roll method having a rotary water-cooled mold, a belt caster method,
In continuous casting such as the 3C method and the block method, the cooling rate during solidification (from the liquidus temperature to the solidus temperature) can be 2 ° C / sec to 10 ° C / sec.

【0036】これらAl合金鋳塊の熱間圧延前の均質化熱
処理において、Al-Mn 系化合物粒子を微細にかつ多数析
出させるためには、均質化熱処理温度を430 〜520 ℃程
度とすることが好ましい。処理温度が520 ℃以上では、
Al-Mn 系化合物粒子が粗大化する可能性が大きい。ま
た、均質化熱処理温度が430 ℃未満では、固溶による均
質化自体の効果が不足する。
In the homogenizing heat treatment of these Al alloy ingots before hot rolling, in order to precipitate a large number of Al-Mn-based compound particles, the homogenizing heat treatment temperature should be about 430 to 520 ° C. preferable. At processing temperatures above 520 ° C,
Al-Mn-based compound particles are likely to become coarse. If the temperature of the heat treatment for homogenization is lower than 430 ° C., the effect of the homogenization itself by solid solution is insufficient.

【0037】熱間圧延は常法により可能であるが、後述
する冷間圧延の圧下率に対し、熱間圧延の加工度も影響
を与える。後述する冷間圧延の加工度 (圧下率) を高く
するために、最終板厚が同じ場合、熱間圧延終了時の板
厚が厚い方が好ましい。また熱間圧延時に導入されるひ
ずみ( 転位密度) が大きくすることが好ましく、このた
めに、熱間圧延終了温度は低い方が好ましい。
Although hot rolling can be performed by a conventional method, the working ratio of hot rolling also affects the rolling reduction of cold rolling described below. In order to increase the working ratio (reduction ratio) of cold rolling described later, when the final plate thickness is the same, it is preferable that the plate thickness at the end of hot rolling be large. Further, it is preferable to increase the strain (dislocation density) introduced during hot rolling, and therefore, it is preferable that the hot rolling end temperature is lower.

【0038】引き続く冷間圧延の圧下率は、最終焼鈍後
の再結晶粒度が5 μm 以下とするために重要である。通
常の冷間圧延Al-Mg 系Al合金板の再結晶粒度が、通常20
〜30μm のレベルであるのは、Mg含有量が比較的低いこ
とと、この冷間圧延の圧下率が大きくても90% 未満のレ
ベルであることによる。このため、本発明では、90%以
上の圧下率で冷間圧延することが必要で、これ未満の圧
下率では、最終焼鈍後の再結晶粒度を5 μm 以下とする
ことができない。90% 以上の圧下率で冷間圧延すること
により、転位を高密度で導入するとともに局部変形領域
を高密度に形成して、これらを再結晶の核生成サイトと
して作用させ、最終焼鈍後の再結晶粒度を5 μm 以下と
することが可能となる。
The rolling reduction in the subsequent cold rolling is important to keep the recrystallized grain size after final annealing to 5 μm or less. The recrystallization grain size of a normal cold-rolled Al-Mg-based Al alloy sheet is
The level of 3030 μm is attributable to the relatively low Mg content and the level of the cold rolling reduction of less than 90% at most. Therefore, in the present invention, it is necessary to perform cold rolling at a rolling reduction of 90% or more, and at a rolling reduction of less than this, the recrystallized grain size after final annealing cannot be reduced to 5 μm or less. By cold rolling at a rolling reduction of 90% or more, dislocations are introduced at a high density, local deformation regions are formed at a high density, and these act as nucleation sites for recrystallization. The crystal grain size can be reduced to 5 μm or less.

【0039】冷間圧延の際の中間焼鈍および冷間圧延後
の最終焼鈍 (再結晶焼鈍) は、バッチ式の熱処理炉或い
は連続式熱処理炉により、製品板に要求される機械的特
性や成形性などの要求特性に応じた、温度と時間により
行う。
The intermediate annealing during the cold rolling and the final annealing (recrystallization annealing) after the cold rolling are carried out by a batch type heat treatment furnace or a continuous type heat treatment furnace by using the mechanical properties and formability required for the product sheet. It is performed by temperature and time according to the required characteristics such as.

【0040】なお、高温焼鈍によっても再現性よく再結
晶粒度の超微細化を行うために、高温の最終焼鈍の前
に、Al-Mn 系化合物を再現性よく微細化しておくために
は、単に化学成分や通常の基本的な製造工程だけではな
く、鋳塊の鋳造における冷却速度や均質化熱処理条件を
合わせて考慮して、Al-Mn 系化合物の大きさを制御する
ことが重要である。言い換えると、他の条件が同じで
も、鋳造における冷却速度や均質化熱処理条件が異なる
場合には、Al-Mn 系化合物の大きさがかなり異なってく
る。
In order to make the recrystallized grain size ultra-fine with good reproducibility even by high-temperature annealing, it is necessary to simply make the Al-Mn-based compound fine with good reproducibility before final annealing at high temperature. It is important to control the size of the Al-Mn-based compound in consideration of not only the chemical composition and the ordinary basic manufacturing process, but also the cooling rate and the homogenizing heat treatment conditions in casting the ingot. In other words, even if the other conditions are the same, the size of the Al-Mn-based compound will be significantly different if the cooling rate and the homogenizing heat treatment conditions in casting are different.

【0041】[0041]

【実施例】次に、本発明方法の実施例を説明する。表1
に示すNo.A〜J までの、化学成分組成を有するAl-Mg 系
Al合金を用い、表2 に示す通り、種々製造条件を変えて
Al合金板の供試材を製造した。
Next, an embodiment of the method of the present invention will be described. table 1
Al-Mg system with chemical composition of No.A to J shown in
Using an Al alloy and changing various manufacturing conditions as shown in Table 2.
The test material of the Al alloy plate was manufactured.

【0042】因みに、表1 の内、A 〜C は本発明範囲内
の組成で、Mn量を変えた発明例である。また、D 〜G は
本発明範囲内の組成で、Fe、Cr、Zrの一種または二種以
上を添加した発明例で、D はMg量が上限の発明例、E は
Mg量が比較的少ない発明例である。更に、H 〜J は本発
明範囲外の組成で、H はMn等の微細化元素を含まない比
較例、I はMnが下限量未満で、Fe、Cr、Zrの三種を添加
した比較例、J はMg量が下限量未満の比較例である。
Incidentally, in Table 1, A to C are compositions within the scope of the present invention, and are examples of the invention in which the amount of Mn is changed. D to G are compositions within the scope of the present invention, and are examples of the invention to which one or more of Fe, Cr, and Zr are added, D is an invention example in which the amount of Mg is the upper limit, and E is
It is an invention example in which the amount of Mg is relatively small. Further, H to J are compositions outside the range of the present invention, H is a comparative example not containing a refining element such as Mn, I is a comparative example in which Mn is less than the lower limit and Fe, Cr, and Zr are added. J is a comparative example in which the amount of Mg is less than the lower limit.

【0043】Al合金板の具体的な製造方法は、Al-Mg 系
Al合金鋳塊をDC鋳造法 (冷却速度 5℃/ 秒) により50mm
厚みの鋳塊に溶製した後、表2 に示す各温度で、4 時間
の均質化熱処理 (昇温速度は共通して50℃/ 秒) を施し
た。そして、この熱処理温度から熱間圧延を開始し、30
0 ℃で圧延を終了し、厚さ10mmまで熱間圧延した。更
に、これらの熱延板を、厚さ0.4 〜1.5mm まで、最大96
% の大圧下率から85% の圧下率まで、表2 に示す圧下率
で冷間圧延した。そして、この冷間圧延板をソルトバス
を用いて、表2 に示す温度で20秒間 (昇温速度は共通し
て100 ℃/ 秒) 最終焼鈍 (再結晶焼鈍) を施した。
A specific method of manufacturing an Al alloy plate is an Al-Mg-based
50mm of Al alloy ingot by DC casting method (cooling rate 5 ℃ / sec)
After being melted into thick ingots, they were subjected to a homogenizing heat treatment (at a common heating rate of 50 ° C / sec) for 4 hours at each temperature shown in Table 2. Then, hot rolling was started from this heat treatment temperature,
The rolling was completed at 0 ° C. and hot-rolled to a thickness of 10 mm. Furthermore, these hot-rolled sheets can be reduced to a thickness of 0.4 to
Cold rolling was performed at a reduction ratio shown in Table 2 from a large reduction ratio of 85% to a reduction ratio of 85%. Then, the cold-rolled sheet was subjected to final annealing (recrystallization annealing) at a temperature shown in Table 2 for 20 seconds (heating rate was 100 ° C./second in common) using a salt bath.

【0044】因みに、表2 の内、No.1〜3 は、表1 のA
の本発明範囲内の組成のAl合金板を用い、最終焼鈍を35
0 〜500 ℃まで変えた発明例である。No.4は、A の本発
明範囲内の組成のAl合金板を用い、冷間圧延圧下率が本
発明下限の90% とした発明例である。No.5は、A の本発
明範囲内の組成のAl合金板を用い、均質化熱処理の温度
が470 ℃と比較的低い発明例である。No.6〜11は、表1
のB 〜G までの本発明範囲内の組成のAl合金板を用い、
製造条件を全く同じとした発明例である。
In Table 2, Nos. 1 to 3 correspond to A in Table 1.
Using an Al alloy plate having a composition within the scope of the present invention,
This is an example of the invention in which the temperature is changed from 0 to 500 ° C. No. 4 is an invention example in which an Al alloy sheet having a composition within the range of the present invention of A was used and the cold rolling reduction was 90% of the lower limit of the present invention. No. 5 is an invention example in which an Al alloy plate having a composition within the range of the present invention of A is used and the temperature of the homogenization heat treatment is relatively low at 470 ° C. No. 6 to 11 are shown in Table 1.
Using an Al alloy plate having a composition within the range of the present invention from B to G,
This is an invention example in which the manufacturing conditions are exactly the same.

【0045】更に、表2 の内、No.12 〜14は、表1 のH
〜J までの本発明範囲外の組成のAl合金板を用い、製造
条件を発明例No.1と全く同じとした比較例である。ま
た、No.15 は、表1 のA の本発明範囲内の組成のAl合金
板を用い、冷間圧延圧下率が本発明下限未満の85% とし
た比較例である。そして、No.16 は、均質化熱処理の温
度を540 ℃と比較的高くした比較例である。
Further, in Table 2, Nos. 12 to 14 correspond to H in Table 1.
This is a comparative example in which Al alloy plates having compositions out of the range of the present invention from No. 1 to No. J were used, and the production conditions were exactly the same as those of Invention Example No. 1. No. 15 is a comparative example in which an Al alloy plate having a composition within the range of the present invention A in Table 1 was used and the cold rolling reduction was 85%, which is less than the lower limit of the present invention. No. 16 is a comparative example in which the temperature of the homogenizing heat treatment was relatively high at 540 ° C.

【0046】(Al-Mn 系化合物粒子の測定)各例のAl合金
板の再結晶粒内のAl-Mn 系化合物粒子の同定と最大長
さ、さらに再結晶粒の大きさ (再結晶粒度) を各々前記
した測定方法により測定した。これらの結果を表2 に示
す。
(Measurement of Al-Mn-based compound particles) Identification and maximum length of Al-Mn-based compound particles in recrystallized grains of Al alloy plate of each example, and size of recrystallized grains (recrystallized grain size) Was measured by the measurement method described above. Table 2 shows the results.

【0047】(Al合金板の特性評価)また、引張試験(JIS
Z 2241 法) にて引張試験を行い、引張強さ (σB ) 、
耐力 (σ0.2)、伸び(%) を測定した。これらの結果を表
2 に示す。
(Evaluation of characteristics of Al alloy plate) Further, a tensile test (JIS
Z 2241 method) to conduct a tensile test, and the tensile strength (σ B )
The proof stress (σ 0.2 ) and elongation (%) were measured. These results are tabulated.
See Figure 2.

【0048】また、前記各供試板のプレス成形性を評価
するために、供試板よりブランク材を採取して、 LDHO
測定用の金型 (直径50.8mmφの球頭パンチ) を用いて、
簡易的な球頭張出試験を行い、その際に割れを生じずに
成形できた LDHO (最大張出高さ) を求めた。これらの
結果も表2 に示す。
Further, in order to evaluate the press formability of each of the test plates, a blank was sampled from the test plates, and LDH O
Using a mold for measurement (ball-head punch with a diameter of 50.8 mmφ),
Perform simple spherical head overhanging test was determined was molded LDH O (fully extended height) without causing cracks at that time. Table 2 also shows these results.

【0049】表2 から明らかな通り、発明例No.1〜11
は、最終焼鈍が350 ℃以上の500 ℃の高温となっても、
Al合金板の再結晶粒内のAl-Mn 系化合物粒子の最大長さ
が500nm 以下であり、再結晶粒度が5 μm 以下の超微細
粒となっている。この結果、表2 に示す通り、優れた引
張強さ (σB ) 、耐力 (σ0.2)、伸び(%) とともに、高
い成形限界高さを示している。また、発明例No.11 は、
最終焼鈍が320 ℃の低温の際にも、再結晶粒度が勿論5
μm 以下の超微細粒となることを示している。したがっ
て、この結果から、本発明Al合金板は、最終焼鈍温度
を、低温から高温まで、要求特性に応じて適宜選択でき
る利点を有することも示している。
As is clear from Table 2, Invention Examples Nos. 1 to 11
Means that even if the final annealing reaches a high temperature of 500
The maximum length of the Al-Mn-based compound particles in the recrystallized grains of the Al alloy plate is 500 nm or less, and the recrystallized grains are ultra-fine grains of 5 μm or less. As a result, as shown in Table 2, it shows a high forming limit height as well as excellent tensile strength (σ B ), proof stress (σ 0.2 ) and elongation (%). In addition, Invention Example No. 11
Even when the final annealing is at a low temperature of 320 ° C, the recrystallized
This indicates that the particles become ultra-fine particles of μm or less. Therefore, the results also show that the Al alloy sheet of the present invention has an advantage that the final annealing temperature can be appropriately selected from a low temperature to a high temperature according to required characteristics.

【0050】また、発明例No.3の結果は、前記特願平11
-268599 号の実施例 (Mnを含むAl-Mg 系Al合金板の最終
焼鈍温度が高い場合に再結晶粒度が5 μm を越えて粗大
化)の傾向なり方向を裏付けている。
The results of Invention Example No. 3 are described in Japanese Patent Application No.
The example of -268599 (the recrystallization grain size exceeds 5 μm when the final annealing temperature of the Al-Mg-based Al alloy sheet containing Mn is high) becomes larger.

【0051】一方、表2 の内、表1 のH 〜J までの本発
明範囲外の組成のAl合金板を用い、製造条件を発明例N
o.1と全く同じとした比較例No.12 、13は、Al-Mn 系化
合物粒子自体が無いか、または量が少なく、比較例No.1
4 はMg量が少ないために、いずれも再結晶の核生成サイ
トが不足し、350 ℃以上の高温の再結晶焼鈍時に再結晶
粒度が5 μm 以下の超微細粒とすることができない。ま
た、表1 のA の本発明範囲内の組成のAl合金板を用い、
冷間圧延圧下率が本発明下限未満の85% とした比較例N
o.15 は、再結晶の核生成サイトが不足し、350 ℃以上
の高温の再結晶焼鈍時に再結晶粒度が5 μm 以下の超微
細粒とすることができない。更に、表1 のA の本発明範
囲内の組成のAl合金板を用い、均質化熱処理温度を540
℃の高温とした比較例No.16 は、Al-Mn 系化合物粒子の
最大長さが500nm を超え、350 ℃以上の高温の再結晶焼
鈍時に再結晶粒度が5 μm 以下の超微細粒とすることが
できない。そして、この結果、これら各比較例はいずれ
も表2 に示す通り、引張強さ (σ B ) 、耐力 (σ0.2)、
伸び(%) 、成形限界高さが、発明例に比して著しく劣っ
ている。
On the other hand, in Table 2, the present invention from H to J in Table 1
Manufacturing conditions using Invention alloy N
Comparative Examples Nos. 12 and 13 which were completely the same as o.1 were Al-Mn based
No or small amount of compound particles per se, Comparative Example No. 1
No. 4 has a small amount of Mg, so all of them have a nucleation site for recrystallization.
Shortage, recrystallization during high temperature recrystallization annealing at 350 ° C or higher
It cannot be made into ultra-fine particles with a particle size of 5 μm or less. Ma
Further, using an Al alloy plate having a composition within the range of the present invention A in Table 1,
Comparative Example N where the cold rolling reduction was 85%, which is less than the lower limit of the present invention.
o.15 lacks nucleation sites for recrystallization,
Ultra fine particles with a recrystallized grain size of 5 μm or less during high temperature recrystallization annealing
Cannot be fine. Further, the present invention of A of Table 1
Using an Al alloy plate with the composition in the box, set the homogenization heat treatment temperature to 540.
Comparative Example No. 16 in which the temperature was as high as
High temperature recrystallization at 350 ° C or more with a maximum length exceeding 500nm
Ultra-fine grains with a recrystallized grain size of 5 μm or less during dulling
Can not. As a result, each of these comparative examples
As shown in Table 2, the tensile strength (σ B), Proof stress (σ0.2),
Elongation (%) and molding limit height are significantly inferior to the invention examples
ing.

【0052】したがって、これらの結果から、本発明の
要件の臨界的な意義や好ましい製造条件の意義が分か
る。また、再結晶焼鈍温度、そして合金組成や製造条件
によって、Al-Mn 系化合物粒子の最大長さや再結晶粒度
が大きく異なり、本発明のAl-Mn 系化合物粒子の最大長
さの規定によって始めて、350 ℃以上の高温の再結晶焼
鈍時の再結晶粒度5 μm 以下が保証されることが分か
る。
Therefore, these results reveal the critical significance of the requirements of the present invention and the significance of the preferred production conditions. Further, the maximum length and the recrystallized grain size of the Al-Mn-based compound particles greatly differ depending on the recrystallization annealing temperature, the alloy composition, and the manufacturing conditions. Only by defining the maximum length of the Al-Mn-based compound particles of the present invention, It can be seen that a recrystallization grain size of 5 μm or less during recrystallization annealing at a high temperature of 350 ° C. or more is guaranteed.

【0053】[0053]

【表1】 [Table 1]

【0054】[0054]

【表2】 [Table 2]

【0055】[0055]

【発明の効果】本発明によれば、高温の再結晶焼鈍を行
っても、焼鈍後の再結晶粒度を5 μm以下の超微細粒と
することが可能なAl-Mg 系Al合金板を提供することがで
きる。この結果、輸送機用のAl合金材の用途を大きく拡
大できる点で工業的な価値が大きい。
According to the present invention, there is provided an Al-Mg-based Al alloy sheet capable of forming ultra-fine grains having a recrystallized grain size of 5 μm or less even after high-temperature recrystallization annealing. can do. As a result, the industrial value is great in that the applications of the Al alloy material for transport aircraft can be greatly expanded.

───────────────────────────────────────────────────── 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 1/00 630 C22F 1/00 630K 685 685 694 694A 694B (71)出願人 000004743 日本軽金属株式会社 東京都品川区東品川二丁目2番20号 (71)出願人 000005290 古河電気工業株式会社 東京都千代田区丸の内2丁目6番1号 (71)出願人 000176707 三菱アルミニウム株式会社 東京都港区芝2丁目3番3号 (72)発明者 小林 一徳 神戸市西区高塚台1丁目5番5号 株式会 社神戸製鋼所神戸総合技術研究所内──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22F 1/00 630 C22F 1/00 630K 685 685 694 694A 694B (71) Applicant 000004743 Nippon Light Metal Co., Ltd. Tokyo Furukawa Electric Co., Ltd. 2-6-1 Marunouchi, Chiyoda-ku, Tokyo (71) Applicant 000176707 Mitsubishi Aluminum Co., Ltd. 2-3-3 Shiba, Minato-ku, Tokyo No.3 (72) Inventor Kazunori Kobayashi 1-5-5 Takatsukadai, Nishi-ku, Kobe-shi Kobe Steel, Ltd.Kobe Research Institute

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 Mg:3.0〜10.0% (質量% 、以下同じ) 、
Mn:0.1〜1.5%を含み残部Alおよび不可避的不純物からな
り、冷間圧延において90% 以上の圧下が加えられるとと
もに、最終焼鈍後の再結晶粒度が5 μm 以下である、Al
-Mg 系アルミニウム合金板であって、組織内に分散析出
するAl-Mn 系化合物の最大長さが500nm 以下であること
を特徴とする高温焼鈍時の再結晶粒微細化に優れた高強
度高成形性アルミニウム合金板。
(1) Mg: 3.0 to 10.0% (% by mass, the same applies hereinafter),
Mn: 0.1 to 1.5%, the balance being Al and unavoidable impurities.In the cold rolling, a reduction of 90% or more is applied, and the recrystallized grain size after final annealing is 5 μm or less.
-Mg-based aluminum alloy sheet, characterized in that the maximum length of the Al-Mn-based compound dispersed and precipitated in the structure is 500 nm or less, and high strength with excellent recrystallization grain refinement during high temperature annealing Formable aluminum alloy plate.
【請求項2】 前記アルミニウム合金板が、更に、Fe:
0.1〜2.0%、Cr:0.05〜0.2%、Zr:0.05 〜0.2%の一種また
は二種以上を含む請求項1に記載の高温焼鈍時の再結晶
粒微細化に優れた高強度高成形性アルミニウム合金板。
2. The method according to claim 1, wherein the aluminum alloy plate further comprises Fe:
The high-strength high-formability aluminum having excellent refining grain refining during high-temperature annealing according to claim 1, comprising one or more of 0.1 to 2.0%, Cr: 0.05 to 0.2%, and Zr: 0.05 to 0.2%. Alloy plate.
【請求項3】 前記アルミニウム合金板が、更に、Ti:
0.001〜0.1%、B:1 〜300ppmの一種または二種を含む請
求項1または2に記載の高温焼鈍時の再結晶粒微細化に
優れた高強度高成形性アルミニウム合金板。
3. The method according to claim 2, wherein the aluminum alloy plate further comprises Ti:
The high-strength high-formability aluminum alloy sheet according to claim 1 or 2, which contains one or two kinds of 0.001 to 0.1% and B: 1 to 300 ppm.
【請求項4】 前記焼鈍温度が350 ℃を越える請求項1
乃至3のいずれか1項に記載の高温焼鈍時の再結晶粒微
細化に優れた高強度高成形性アルミニウム合金板。
4. The method according to claim 1, wherein the annealing temperature exceeds 350 ° C.
4. A high-strength, high-formability aluminum alloy sheet excellent in refining recrystallized grains during high-temperature annealing according to any one of 3 to 3 above.
JP27429399A 1999-09-28 1999-09-28 High-strength, high-formability aluminum alloy sheet with excellent recrystallization grain refinement during high-temperature annealing Expired - Fee Related JP4164206B2 (en)

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