JP2008308703A - Magnesium alloy for continuously casting and rolling, and method for producing magnesium alloy material - Google Patents
Magnesium alloy for continuously casting and rolling, and method for producing magnesium alloy material Download PDFInfo
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Abstract
Description
この発明は、連続鋳造圧延に用いるマグネシウム合金および該マグネシウム合金を用いて連続鋳造圧延によりマグネシウム合金材料を製造する製造方法に関するものである。 The present invention relates to a magnesium alloy used for continuous casting and rolling and a manufacturing method for producing a magnesium alloy material by continuous casting and rolling using the magnesium alloy.
従来、展伸用マグネシウム合金としてＭｇ−Ａｌ−Ｚｎ系のＡＺ３１、ＡＺ４１、ＡＺ６１などが知られており、その材料特性に応じて、モバイル製品の筐体などに使用されている。その製法として、スラブを熱処理と熱間・温間圧延を繰返し薄肉化する方法や、予め押出された薄肉のフラットバーを熱間・温間圧延を繰返し薄肉化し製品板厚としている。他に、双ロール法で直接薄肉の板材を作製し、それを同様に圧延し製品板厚としている（例えば特許文献１、２参照）。 Conventionally, Mg-Al-Zn-based AZ31, AZ41, AZ61, and the like are known as magnifying magnesium alloys, and are used for housings of mobile products according to their material properties. As a manufacturing method thereof, a method of repeatedly thinning a slab by heat treatment and hot / warm rolling repeatedly, or a thin flat bar extruded in advance is repeatedly thinned by hot / warm rolling to obtain a product thickness. In addition, a thin plate material is directly produced by a twin roll method, which is rolled in the same manner to obtain a product plate thickness (see, for example, Patent Documents 1 and 2).
また、マグネシウム合金の機械的性質は結晶粒度に強く依存し、結晶粒が微細になるほど強度および伸びが向上する。従来、微細な結晶粒組織を有するマグネシウム合金板を製造する方法としては、加工熱処理法がよく用いられている。この方法は、熱間加工時の動的再結晶現象、あるいは温間加工の中間および／または後での熱処理時の溶質元素の固溶、析出現象や回復と再結晶現象を制御して、さらに多くの場合、前記の各現象を総合的に制御して結晶粒の微細化を図るものである。また、最近ではＥＣＡＰ（Equal-Channel Angular Pressing）などの強ひずみ加工法も開発されている。
しかしながら、最近になって、モバイル等の筐体に更なる強度が求められるようになり、展伸材の強度増加が必要である。強度増加には、同じＭｇ−Ａｌ−Ｚｎ系の材料を使用する場合は、Ａｌ添加量の高いＡＺ６１やＡＺ９１が有効である。また、本来、鋳物用合金であるＭｇ−Ａｌ系のＡＭ６０やＡＭ８０も有効である。ただし、これら合金は強度は高くなるものの、一方で、変形抵抗が大きいため、押出によるフラットバーの製造では、その押出速度が極端に低くなるとともに、割れが発生し健全な材料が得られない。また、双ロール法で帯状板を製造する場合、Ａｌ添加量の増加につれて溶湯の流動性が低下するため、健全な帯状板の製造が困難である。 However, recently, further strength has been demanded for housings such as mobile phones, and it is necessary to increase the strength of the wrought material. In order to increase the strength, when the same Mg—Al—Zn-based material is used, AZ61 or AZ91 having a high Al addition amount is effective. Further, Mg-Al-based AM60 and AM80, which are originally casting alloys, are also effective. However, although these alloys have high strength, on the other hand, since the deformation resistance is large, in the production of a flat bar by extrusion, the extrusion speed becomes extremely low, and cracks occur and a sound material cannot be obtained. Moreover, when manufacturing a strip | belt board by a twin roll method, since the fluidity | liquidity of a molten metal falls as the amount of Al addition increases, manufacture of a healthy strip | belt board is difficult.
本発明は、上記事情を背景としてなされたものであり、低コストで高強度のマグネシウム合金材料を得ることができる連続鋳造圧延用マグネシウム合金およびマグネシウム合金材料の製造方法を提供することを目的とする。 The present invention has been made against the background of the above circumstances, and an object of the present invention is to provide a magnesium alloy for continuous casting and rolling and a method for producing the magnesium alloy material capable of obtaining a high-strength magnesium alloy material at low cost. .
すなわち、本発明の連続鋳造圧延用マグネシウム合金のうち、第１の発明は、質量％で、Ａｌ：１〜１１％，Ｍｎ：０．１〜０．５％、Ｓｒ：０．０２〜１．０％を含み、残部がＭｇおよび不可避不純物からなる組成を有することを特徴とする。 That is, among the magnesium alloys for continuous casting and rolling of the present invention, the first invention is mass%, Al: 1 to 11%, Mn: 0.1 to 0.5%, Sr: 0.02 to 1.. The composition is characterized by including 0% and the balance being composed of Mg and inevitable impurities.
第２の本発明の連続鋳造圧延用マグネシウム合金は、前記第１の本発明において、前記組成に、さらに、質量％で、Ｚｎ：０．１〜２．０％を含有することを特徴とする。 The magnesium alloy for continuous casting and rolling according to the second aspect of the present invention is characterized in that, in the first aspect of the present invention, the composition further contains Zn: 0.1 to 2.0% by mass%. .
また、第３の本発明のマグネシウム合金材料の製造方法は、前記第１または第２の本発明の組成のマグネシウム合金溶湯を連続鋳造圧延により急冷凝固させ、帯状板とすることを特徴とする。 A third aspect of the method for producing a magnesium alloy material of the present invention is characterized in that a molten magnesium alloy having the composition of the first or second aspect of the present invention is rapidly solidified by continuous casting and rolling to form a strip plate.
第４の本発明のマグネシウム合金材料の製造方法は、前記第３の本発明において、前記帯状板に均質化処理し、次いで、温間圧延により、または熱間圧延と温間圧延とにより製品板厚とする圧延工程を有し、該圧延工程時に異周速圧延を含み、該圧延工程に用いるロール間の回転速度比（周速比）を１．０〜１．８とすることを特徴とする。 According to a fourth aspect of the present invention, there is provided a method for producing a magnesium alloy material according to the third aspect of the present invention, wherein the strip-shaped plate is homogenized and then warm rolled, or hot rolled and warm rolled. It has a rolling process to make it thick, includes a different peripheral speed rolling at the time of the rolling process, and a rotational speed ratio (peripheral speed ratio) between rolls used in the rolling process is 1.0 to 1.8. To do.
以下に、本発明で規定する組成および製造条件の理由について説明する。なお、以下の成分含有量はいずれも質量％を示している。 The reasons for the composition and production conditions specified in the present invention will be described below. In addition, all the following component content has shown the mass%.
Ａｌ：１〜１１％
Ａｌは、鋳造性、強度等の機械的性質および耐食性の向上を目的として添加される。ただし、Ａｌの添加量が１％未満では、十分な鋳造性、強度および耐食性が得られない。一方、Ａｌの添加量が１１％を超えると、強度増加は飽和する。また、Ａｌ添加量が６％を超えると圧延工程における加工性が徐々に低下し、１１％を超えると圧延が困難になる。
これらの理由によりＡｌの含有量範囲を上記に定める。なお、強度増加の目的では、下限を４％とするのが望ましく、加工性の点から上限を９％とするのが望ましい。
Al: 1 to 11%
Al is added for the purpose of improving mechanical properties such as castability and strength, and corrosion resistance. However, if the addition amount of Al is less than 1%, sufficient castability, strength and corrosion resistance cannot be obtained. On the other hand, when the addition amount of Al exceeds 11%, the strength increase is saturated. On the other hand, if the Al content exceeds 6%, the workability in the rolling process gradually decreases, and if it exceeds 11%, rolling becomes difficult.
For these reasons, the content range of Al is defined above. For the purpose of increasing strength, the lower limit is desirably 4%, and the upper limit is desirably 9% from the viewpoint of workability.
Ｍｎ：０．１〜０．５％
Ｍｎは、耐食性を低下させる元素の影響を緩和する効果を有するものであるので、積極的に添加する。すなわち、Ｍｎを添加することによって、耐食性を低下させる不純物元素であるＦｅの影響を緩和することができる。０．１％以上の含有により、この効果を効果的に得ることができる。ただし、０．５％を超えて含有すると連続鋳造圧延時に粗大な金属間化合物が生成し、圧延性が悪化するので、Ｍｎの含有量を０．１〜０．５％に定める。
Mn: 0.1 to 0.5%
Since Mn has an effect of mitigating the influence of elements that lower the corrosion resistance, it is positively added. That is, by adding Mn, the influence of Fe, which is an impurity element that lowers the corrosion resistance, can be mitigated. By containing 0.1% or more, this effect can be effectively obtained. However, if the content exceeds 0.5%, a coarse intermetallic compound is produced during continuous casting and rolling, and the rollability deteriorates, so the Mn content is set to 0.1 to 0.5%.
Ｓｒ：０．０２〜１．０％
Ｓｒは、マグネシウムとの原子半径差が大きいことから、わずかな固溶においてもその固溶硬化の影響が大きい。また、ＡｌとＡｌ−Ｓｒ系の化合物を形成し、強度の増加がはかれる。更に、Ｓｒにはマグネシウム合金溶湯の表面張力を低下させる作用があり、その結果、溶湯の流動性が改善され、連続鋳造圧延に際し、健全な帯状板を得ることが可能になる。ただし、Ｓｒが０．０２％未満では、上記作用が十分に得られず、１．０％を超えても、その作用は飽和するので、Ｓｒの含有量を上記範囲とする。なお、同様の理由で下限を０．０５％、上限を０．６％とするのが望ましい。
Sr: 0.02 to 1.0%
Since Sr has a large atomic radius difference from magnesium, the effect of solid solution hardening is large even in a slight solid solution. Further, Al and an Al—Sr compound are formed, and the strength is increased. Furthermore, Sr has the effect | action which reduces the surface tension of a magnesium alloy molten metal, As a result, the fluidity | liquidity of a molten metal is improved and it becomes possible to obtain a healthy strip | belt board in the case of continuous casting rolling. However, if the Sr is less than 0.02%, the above effect cannot be obtained sufficiently. If the Sr exceeds 1.0%, the action is saturated, so the Sr content is set in the above range. For the same reason, it is desirable to set the lower limit to 0.05% and the upper limit to 0.6%.
Ｚｎ：０．１〜２．０％
Ｚｎは、Ａｌと同様に、鋳造性と強度等の機械的性質の向上に寄与するので、所望により含有させる。Ｚｎの添加量が２．０％を超えると、鋳造性が低下する。また、Ｚｎの添加量が０．１％未満では、強度が低下することがあり、その結果としてプレス成形性が低下することがある。したがって、Ｚｎは、０．１〜２．０％の範囲内で添加されていることが好ましい。
Zn: 0.1 to 2.0%
Zn, like Al, contributes to improvement of mechanical properties such as castability and strength, and is thus contained as desired. If the added amount of Zn exceeds 2.0%, the castability deteriorates. Further, if the added amount of Zn is less than 0.1%, the strength may decrease, and as a result, the press formability may decrease. Therefore, it is preferable that Zn is added within a range of 0.1 to 2.0%.
次に、本発明のマグネシウム合金薄板の製造方法は、マグネシウム合金溶湯を連続鋳造圧延（好ましくは双ロール法）により、例えば、板厚３〜１０ｍｍの帯状板にする方法である。連続鋳造により得られた帯状板には好ましくは、均質化処理をし、熱間圧延した後、もしくは、熱間圧延し、均質化処理した後に、温間圧延により製品板厚とする工程において、上下ロールの回転速度比が１．０〜１．８で温間圧延する。前記熱間および／あるいは温間圧延工程途中に中間焼鈍を行うことも可能である。 Next, the manufacturing method of the magnesium alloy thin plate of this invention is a method of making a magnesium alloy molten metal into a strip | belt plate of 3-10 mm in thickness by continuous casting rolling (preferably twin roll method). Preferably, the strip-shaped plate obtained by continuous casting is subjected to homogenization treatment and hot rolling, or after hot rolling and homogenization treatment, and in the step of product plate thickness by warm rolling, Warm rolling is performed at a rotational speed ratio of the upper and lower rolls of 1.0 to 1.8. Intermediate annealing may be performed during the hot and / or warm rolling process.
連続鋳造圧延
この工程は、マグネシウム合金の溶湯を、例えば、水冷された一対のロールの間に供給し、連続的に薄い帯状板に鋳造圧延する工程である。本発明においては、この製造方法によって、極めて効率的なマグネシウム合金板の製造を可能にしたものである。
連続鋳造圧延の冷却速度としては、２００〜５５０℃／秒の範囲が好ましい。２００℃／秒未満では、急冷による作用を十分に得られない。一方、５５０℃／秒を超える条件では、ノズル内で凝固を生じやすくなり板の製造がストップしてしまう。
Continuous casting and rolling This step is a step in which a molten magnesium alloy is supplied between, for example, a pair of water-cooled rolls and continuously cast and rolled into a thin strip. In the present invention, this manufacturing method makes it possible to manufacture an extremely efficient magnesium alloy sheet.
The cooling rate for continuous casting and rolling is preferably in the range of 200 to 550 ° C / second. If it is less than 200 ° C./second, the effect of rapid cooling cannot be obtained sufficiently. On the other hand, under conditions exceeding 550 ° C./second, solidification easily occurs in the nozzle, and the production of the plate is stopped.
均質化処理
この熱処理は急冷凝固された連続鋳造圧延板におけるＡｌ（Ｚｎ）溶質元素のデンドライト・セル境界および板厚中心部での高濃度の偏析を解消する熱処理である。熱処理条件としては３７０〜４７０℃の温度範囲で１時間以上行うのが好ましい。この熱処理により上記偏析が解消され、その後の圧延性に優れたマグネシウム合金板を得ることができる。該均質化処理は、圧延工程前または熱間圧延と温間圧延との間に行うことができる。
Homogenization treatment This heat treatment is a heat treatment for eliminating high concentration segregation at the dendrite cell boundary and the center of the plate thickness of the Al (Zn) solute element in the rapidly cast solidified continuous cast rolled plate. As heat treatment conditions, it is preferable to carry out at a temperature range of 370 to 470 ° C. for 1 hour or longer. By this heat treatment, the segregation is eliminated, and a magnesium alloy sheet excellent in the subsequent rollability can be obtained. The homogenization treatment can be performed before the rolling process or between hot rolling and warm rolling.
熱間／温間圧延工程
圧延工程は、所定の厚さの連続鋳造圧延板を所定の厚さのマグネシウム合金板に加工するための工程である。ここで、３００℃以上での圧延を熱間圧延、３００℃未満での圧延を温間圧延とする。圧延工程は、温間圧延工程のみであっても良く、熱間圧延後に温間圧延を行う工程であってもよいが、いずれにしても最終製品板厚は温間圧延により得られる。最終温間圧延工程での圧下率としては、５０％以上の圧下率を特に好ましく適用できる。この圧下率は、一回（一パス）の圧延であっても複数回（複数パス）の圧延であってもよく特に限定されない。
Hot / warm rolling process The rolling process is a process for processing a continuous cast rolled sheet having a predetermined thickness into a magnesium alloy sheet having a predetermined thickness. Here, rolling at 300 ° C. or higher is hot rolling, and rolling at less than 300 ° C. is warm rolling. The rolling process may be only a warm rolling process or a process of performing warm rolling after hot rolling, but in any case, the final product sheet thickness can be obtained by warm rolling. As the rolling reduction in the final warm rolling step, a rolling reduction of 50% or more can be particularly preferably applied. This rolling reduction may be one time (one pass) or a plurality of times (multiple passes), and is not particularly limited.
温間圧延および温間異周速圧延
周速比１．０の圧延において５．０μｍまでの微細な結晶粒が得られるが、周速比を上げることで、せん断変形を付与し、それ以下の微細粒が得られる。ただし、周速比が１．８より大きくなると、結晶粒微細化への効果がそれほど向上しないばかりでなく、操業が困難になるおそれがあるので、圧延工程での周速比は１．０〜１．８が好ましい。
Warm rolling and warm different peripheral speed rolling Fine grains up to 5.0 μm are obtained in rolling with a peripheral speed ratio of 1.0, but by increasing the peripheral speed ratio, shear deformation is imparted, and below that Fine grains are obtained. However, if the peripheral speed ratio is larger than 1.8, not only the effect on crystal grain refinement is not improved so much, but also the operation may be difficult, so the peripheral speed ratio in the rolling process is 1.0 to 1.8 is preferred.
中間焼鈍
中間焼鈍工程は、熱間圧延工程と温間圧延工程の間に、あるいは温間圧延の圧下率が８０％を超える場合に温間圧延途中に好ましく設けられるものである。一の温間圧延工程での圧下率が８０％以下であっても、二以上の温間圧延工程でのトータルの圧下率が８０％を超える場合には、中間焼鈍工程を設け、その後に最終温間圧延工程を設けることが好ましい。中間焼鈍の条件としては、２００〜３００℃、１時間を例示することができる。中間焼鈍を行うと、平均粒径５μｍ以下の微細粒組織を確実に得ることができる。
Intermediate annealing The intermediate annealing step is preferably provided between the hot rolling step and the warm rolling step or during the warm rolling when the rolling reduction of the warm rolling exceeds 80%. Even if the reduction ratio in one warm rolling process is 80% or less, if the total reduction ratio in two or more warm rolling processes exceeds 80%, an intermediate annealing process is provided, and then the final It is preferable to provide a warm rolling process. Examples of the conditions for the intermediate annealing include 200 to 300 ° C. and 1 hour. When the intermediate annealing is performed, a fine grain structure having an average particle diameter of 5 μm or less can be obtained with certainty.
以上説明したように、本発明の連続鋳造圧延用マグネシウム合金は、質量％で、Ａｌ：１〜１１％，Ｍｎ：０．１〜０．５％、Ｓｒ：０．０２〜１．０％を含み、残部がＭｇおよび不可避不純物からなる組成を有するので、高い強度特性を有し、連続鋳造圧延においても良好な流動性により健全な組織を有することができる。 As described above, the magnesium alloy for continuous casting and rolling of the present invention is, in mass%, Al: 1 to 11%, Mn: 0.1 to 0.5%, Sr: 0.02 to 1.0%. In addition, since the remainder has a composition composed of Mg and inevitable impurities, it has high strength characteristics and can have a sound structure due to good fluidity even in continuous casting and rolling.
また、本発明のマグネシウム合金材料の製造方法は、上記組成のマグネシウム合金溶湯を連続鋳造圧延により急冷凝固させ、帯状板とするので、合金の良好な流動性によって健全な帯状板が得られ、さらには従来の製造法より、高強度なマグネシウム合金材料を簡単に製造することができる。 In addition, since the magnesium alloy material manufacturing method of the present invention rapidly solidifies the magnesium alloy melt having the above composition by continuous casting and rolling to form a strip, a healthy strip can be obtained by the good fluidity of the alloy. Can easily produce a high-strength magnesium alloy material than the conventional production method.
以下に、本発明の一実施形態を説明する。
質量％で、Ａｌ：１〜１１％，Ｍｎ：０．１〜０．５％、Ｓｒ：０．０２〜１．０％を含み、所望によりＺｎ：０．１〜２．０％を含有し、残部がＭｇおよび不可避不純物からなる組成を有するアルミニウム合金を用意し、該アルミニウム合金を溶解し、好適には双ロールによる連続鋳造圧延により、２００〜５５０℃／秒の冷却速度で急冷して帯状板を製造する。該帯状板は、例えば３〜１０ｍｍの板厚とする。
上記帯状板は、後述する圧延工程により製品板厚にまで圧延される。この圧延工程前または圧延工程における熱間圧延後、温間圧延前に、均質化処理を行うのが望ましい。均質化処理は、例えば３７０〜４７０℃で１時間以上加熱することにより行うことができる。
Hereinafter, an embodiment of the present invention will be described.
In mass%, Al: 1 to 11%, Mn: 0.1 to 0.5%, Sr: 0.02 to 1.0%, optionally containing Zn: 0.1 to 2.0% An aluminum alloy having a composition consisting of Mg and inevitable impurities is prepared, the aluminum alloy is melted, and is preferably quenched by continuous casting and rolling with twin rolls at a cooling rate of 200 to 550 ° C./sec. Manufacture a board. The strip plate has a thickness of 3 to 10 mm, for example.
The strip plate is rolled to a product plate thickness by a rolling process described later. It is desirable to perform a homogenization treatment before the rolling process or after hot rolling in the rolling process and before warm rolling. A homogenization process can be performed by heating at 370-470 degreeC for 1 hour or more, for example.
上記圧延工程は、温間圧延または、熱間工程と温間圧延とを行う工程により行うことができる。なお、該圧延工程では、異周速圧延を含むことにより材料に剪断変形を与えて結晶粒の微細化を図るのが望ましい。圧延工程では、周速比を１．０〜１．８とするのが好ましい。製品板厚は、温間圧延において、５０％以下の圧下率の最終圧延（一パスまたは複数パス）により得られる。 The said rolling process can be performed by the process of performing warm rolling or a hot process and warm rolling. In the rolling process, it is desirable to refine the crystal grains by applying shear rolling to the material by including different peripheral speed rolling. In the rolling step, the peripheral speed ratio is preferably 1.0 to 1.8. The product sheet thickness is obtained by final rolling (one pass or multiple passes) with a reduction rate of 50% or less in warm rolling.
また、上記圧延工程では、中間焼鈍を介在させることができる。該中間焼鈍は、熱間圧延工程と温間圧延工程の間で行ったり、温間圧延の途中に行うことができ、温間圧延の途中で行う場合には温間圧延の圧下率が８０％を超える場合に、好ましく設けられる。
中間焼鈍は、例えば２００〜３００℃、１時間の加熱により行うことができる。
Moreover, intermediate annealing can be interposed in the said rolling process. The intermediate annealing can be performed between the hot rolling process and the warm rolling process, or can be performed in the middle of the warm rolling. When performing in the middle of the warm rolling, the rolling reduction of the warm rolling is 80%. Is preferably provided.
The intermediate annealing can be performed, for example, by heating at 200 to 300 ° C. for 1 hour.
最終板厚のマグネシウム合金材料は、例えば３〜１０ｍｍの板厚とされるが、本発明としては、この板厚に限定をされるものではない。 最終板厚のマグネシウム合金材料のさらに２次加工などを経て種々の用途に用いることができ、例えば前記したようにモバイル品の筺体などに利用することができる。 The final thickness of the magnesium alloy material is 3 to 10 mm, for example, but the present invention is not limited to this thickness. The final thickness of the magnesium alloy material can be used for various applications through further secondary processing, for example, as described above, and can be used for mobile products.
以下に、実施例と比較例によって本発明を更に詳しく説明する。
双ロール法（冷却速度３５０℃／秒）により、表１に示す合金組成（残部Ｍｇおよび不可避不純物）からなるマグネシウム合金溶湯から、厚さ５ｍｍの帯状板を連続鋳造圧延した。得られた鋳造圧延板を４００℃で２４時間の均質化処理を施した後、熱間圧延、温間圧延により厚さ１．０５ｍｍの板とし、その後、周速比を変量した温間異周速圧延で厚さ０．８ｍｍの薄板に製造した。
Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples.
By a twin roll method (cooling rate 350 ° C./second), a 5 mm thick strip was continuously cast and rolled from a molten magnesium alloy having the alloy composition (remaining Mg and inevitable impurities) shown in Table 1. The obtained cast rolled plate was subjected to a homogenization treatment at 400 ° C. for 24 hours, and then made into a plate having a thickness of 1.05 mm by hot rolling and warm rolling. A thin plate having a thickness of 0.8 mm was produced by rapid rolling.
表に示されるように、本発明の製造方法により製造された実施例の供試材は、連続鋳造圧延時に割れもなく、高い強度、伸び特性を有していた。一方、比較例の供試材は、Ａｌの量が少なく、Ｓｒも添加されていない比較例Ｎｏ．６では、強度が低く、Ａｌをある程度含有するものでは強度特性は良好であるものの、Ｓｒが添加されていないので連続鋳造圧延で得られる帯状板に割れの発生が見られた。 As shown in the table, the sample materials of Examples produced by the production method of the present invention were free from cracks during continuous casting and rolling, and had high strength and elongation characteristics. On the other hand, the test material of the comparative example has a small amount of Al and no comparative example No. Sr. In No. 6, although the strength was low and the strength characteristics were good when Al was contained to some extent, cracks were found in the strip obtained by continuous casting and rolling because Sr was not added.
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