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JP4683441B2 - Manufacturing method of ultra-fine structure steel - Google Patents
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JP4683441B2 - Manufacturing method of ultra-fine structure steel - Google Patents

Manufacturing method of ultra-fine structure steel Download PDF

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Publication number
JP4683441B2
JP4683441B2 JP2000056478A JP2000056478A JP4683441B2 JP 4683441 B2 JP4683441 B2 JP 4683441B2 JP 2000056478 A JP2000056478 A JP 2000056478A JP 2000056478 A JP2000056478 A JP 2000056478A JP 4683441 B2 JP4683441 B2 JP 4683441B2
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Japan
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rolling
roll
steel
shear strain
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JP2000056478A
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JP2001140016A (en
Inventor
宏 中嶋
年裕 花村
史郎 鳥塚
寿 長井
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Japan Science and Technology Agency
Mitsubishi Heavy Industries Ltd
Nippon Steel Corp
National Institute for Materials Science
National Institute of Japan Science and Technology Agency
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Japan Science and Technology Agency
Mitsubishi Heavy Industries Ltd
Nippon Steel Corp
National Institute for Materials Science
National Institute of Japan Science and Technology Agency
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Description

【0001】
【発明の属する技術分野】
この出願の発明は、超微細組織鋼の製造方法に関するものである。さらに詳しくは、この出願の発明は、高強度、高靱性で、かつ溶接性に優れ、厚さ10mm以上の鋼板としての製造も可能とする、結晶粒2μm以下のフェライト組織を主体とした超微細組織鋼の製造方法に関するものである。
【0002】
【従来の技術とその課題】
フェライト結晶粒の微細化は鋼の靱性を向上させる有力な高強度化手法として知られており、従来よりフェライト組織微細化に関する検討が広く行われてきている。例えば、大圧下での急冷法(CAMP-ISIJ-Vol.11(1998), P1017) をはじめ、逆変態を利用する方法(特開昭58−58224)、繰り返し重ね接合圧延による方法(CAMP-ISIJ-Vol.11(1998), P1031) 、温間圧延・再結晶による方法(CAMP-ISIJ-Vol.11(1998), P1031) が提案されており、これらの方法での厚さ5mm以下の微細組織鋼薄肉材が作製可能であるとされている。また、多パス溝ロール圧延法による直径5mm以上の微細組織棒材が作製可能となってもいる(特願平11−052008号)。
【0003】
しかしながら、以上のような検討と提案にもかかわらず、フェライトを主体として平均粒径が2ミクロン以下の組織を有し、しかも厚さ5mm以上で幅が厚さの10倍以上の、さらには厚さ10mm以上の微細組織鋼板は依然として実現されていないのが実情である。
【0004】
そこで、この出願の発明は、上記のとおりの問題に鑑みてなされたものであって、従来技術の限界を克服し、厚さ5mm以上で幅が厚さの10倍以上の、さらには厚さ10mm以上の鋼板としての製造も可能とする、フェライト主体組織を有し、その平均粒径が2ミクロン以下の超微細組織鋼の新しい製造方法を提供することを課題としている。
【0005】
【課題を解決するための手段】
この出願の発明は、上記の課題を解決するために、第1には、鋼をAc3以上に加熱してオーステナイト化した後に、準安定オーステナイト域の温度で、終了温度が550℃以上を保持している間に累積減面率が70%以上の圧延を、上下のロール軸が平面位置で1°以上の角度で交差した状態で行い、被圧延材にロール軸方向のせん断歪みを与え、フェライトを主体とした平均粒径2ミクロン以下の等軸組織を有する超微細組織鋼を製造することを特徴としている。
【0006】
この出願の発明は、第2には、上記第1の特徴において、前記せん断歪みを4以上とすることを特徴とし、第3には、上記第の特徴において、複数回の圧延により前記せん断歪み2以上を得ることを特徴としている。
この出願の発明は、第4には、上記第1の特徴において、化学組成(質量%)として、C:0.8%以下、Si:0.5%以下、Mn:3.0%以下、P:0.02%以下、S:0.02%以下、であり、Ti、MgまたはAlの1種または2種以上が単独または混合で0.3%以下含有することを特徴としてもいる。
【0007】
【発明の実施の形態】
この出願の発明は、上記のとおりの特徴を有するものであるが、以下にその実施の形態について説明する。
【0008】
この出願の発明の方法においては、上下のロール軸が平面位置で交差した状態で圧延することにしているが、この場合の交差の状態は、たとえば図1に例示したように、被圧延材としての板材(1)の上側に配置される上ロール(2A)と、下側に配置される下ロール(2B)の各々のロール軸が、図1に示したような平面配置位置において、板材(1)中心線に直交する直交線に対する角度(θ θ)の設定により平面的には交差した状態にあることを意味している。
【0009】
そして、この発明の製造方法では、この角度θ1 およびθ2 が、各々、1°以上となるようにしている。より実際的には、この角度θ1 およびθ2 は、各々、20°程度までとすることが望ましい。そして、この交差角度θ1 およびθ2 は同一もしくは実質的に同一であることが好ましい。
【0010】
また、交差角度θ1 およびθ2 は、累積減面率80%以上の圧延を行った場合に、被圧延材が5mm以上の厚さの場合のロール軸方向のせん断歪みが0.5以上となる角度であることが望ましい。
【0011】
そして、たとえば図2に例示したような、中央部が湾曲状に窪んだ鼓型のロールを用いることによって圧延材の板厚を平坦にしつつ、せん断歪みを効果的に与えることができる。通常のフラットなロールをクロスさせると上下ロールの間隔は(圧延される板の形状に相当)ロールの幅方向中央が狭く両端部になるに従ってひろがり、あたかもロールにクラウン(湾曲形状)が施されたようになる。このため圧延した場合、図3のように、ロール中央部の間隔(B)が端部(A)に比べて圧延材の変形抵抗により大きく広がり、あたかもロール間隔が一定となったような作用がある。これは、クロス圧延の原理と言えるものであるが、大きくクロス角を取った場合でもこのロール間隔形状は次式で表わすことができる。そのため図2にような湾曲形状のロールの場合の曲率はこの式に従い、ロール間隔が一定となる様に逆の形状をロールに与えることになる。
【0012】
【数1】

Figure 0004683441
【0013】
組織の微細化においては、以上のようなロール圧延の場合、圧延方向でのせん断歪みが4以上となるようにすることが特に好適でもある。
【0014】
この出願の発明の方法において、交差状態にあるロール(クロスロール)での圧延は、鋼をAc3点以上に加熱してオーステナイト化した後に、たとえばAc3点以下の準安定オーステナイト温度域で、かつ終了時の温度が550℃を保持している間の累積減面率が70%以下となるようにして行う。
【0015】
フェライト粒を主体とする組織とするためには準安定オーステナイト温度域での圧延が欠かせないのであり、また、圧延終了温度を550℃以上とするのは、組織の微細化を得るために必要だからである。圧延終了温度が550℃以下では、組織は伸長するのみで再結晶による組織の微細化が生じない。
【0016】
ロールによる圧延は、ワンパス圧延でもよいし、多パス圧延であってもよい。多パス圧延、すなわち複数回の圧延においては1パスと比べて以下の式に示すような大きなせん断歪みを得ることが可能である。
【0017】
【数2】
Figure 0004683441
【0018】
そのため、1パスが低圧下量でも2回以上の多パス圧延による大きなせん断歪みが得られる。
【0019】
以上のとおりのこの出願の発明によって、厚5mm以上、さらには10mm以上の鋼板材としても、2ミクロン以下のフェライト主体の微細組織、特に、高強度化に寄与する等軸組織を有する、超微細組織鋼が提供されることになる。
【0020】
この出願の発明において対象とすることのできる鋼については、その組成に特段の限定はないが、好適なものとしては、組成(質量%)は以下のとおりである。
すなわち、C:0.8%以下、Si:0.5%以下、Mn:3.0%以下、P:0.02%以下、S:0.02%以下、Ti、MgまたはAlの1種または2種以上が単独または混合0.3%以下の割合で含有するものが例示される。
以下に実施例を示し、さらに詳しくこの出願の発明について説明する。
【0021】
【実施例】
<実施例1>
材質SM490で、化学組成がC:0.13,Si:0.40,Mn:1.39,P:0.01,S:0.02,Al:0.03,Ti:0.1,Nb:0.03(mass%)であり、大きさが50×60×300mmの鋼板を供試材とした。この供試材を、Ac3点以上の900℃に10分間保持してオーステナイト化し、その後空冷し、供試材鋼板の中心温度が750℃から650℃にある間に、累積減面率が70%以上になるように、延加工を行った。
【0022】
圧延装置は、図1のように、上下2本のロールからなり、ロール軸が交差するように配置され、鋼板にせん断歪みを与えるものとした。
【0023】
上下のロールは、通常の円柱状のロールで交差角をもって交差状に配置され、鋼板にせん断歪み(多軸)を与える。
【0024】
この場合の交差角(クロス角)、すなわちθ1 =θ2 の場合のθ1 およびθ2 の各々の角度とせん断変形量(mm)との関係を示したものが図4である。
【0025】
圧延処理の条件は次のとおりとした。また、比較のためのクロス角度0°の場合の圧延条件も次に示した。
【0026】
A材(発明材)
クロス角度:1.5°、圧延速度:10m/min、ロール径:260mm
パススケジュール:50−35−25−18−10mm、圧延後処理:水冷。
【0027】
B材(比較材)
クロス角度:0°、圧延速度:10m/min、ロール径:260mm
パススケジュール:50−35−25−18−10mm、圧延後処理:水冷。
【0028】
図5(a)、(b)は、各々上記のA材、B材に係る圧延方向に垂直な断面の組織観察結果を示し、それぞれ表面より1mm位置、2.5mm位置(1/4厚さ部)の組織を示したものである。
【0029】
A材(本発明材)は、図5(a)に示すように、表面より1mm、2.5mm(1/4厚さ部)で、断面全面で微細で、特に表層部で等軸な1.3−1.6ミクロンのフェライト粒主体の組織であることが確認された。
【0030】
これに対し、B材(比較材)は、図5(b)に示すように、同じ位置において、断面全面で均一な1.3−1.8ミクロンのフェライト粒主体の組織であるが表層部で伸長した組織であることが確認された。
【0031】
これにより、クロス角度1.5°でクロス圧延した発明材は、クロス角度0°の圧延を行った比較材に比べ、粒径が微細等軸で断面全面が2ミクロン以下の超微細組となっていることがわかる。
【0032】
【表1】
Figure 0004683441
【0033】
<実施例2>
実施例1において、クロス角度を10°として同様にして圧延を行った。圧延速度は5m/minとした。この場合、ロールは図2のように中央が湾曲状に窪んだ鼓型のロール形状を有している。
【0034】
粒径0.5−1.0ミクロンのフェライト粒を主体とする等軸組織を有する超微細組織鋼を得た(表1)。
<実施例3>
実施例1において、通常の円柱状ロールを用いて、クロス角度5°として同様の条件で圧延を得た。
【0035】
粒径1.1−1.3ミクロンのフェライト粒を主体とする等軸組織を有する超微細組織鋼を得た(表1)。
【0036】
【発明の効果】
以上詳しく説明したように、この出願の発明によれば、通常の圧延のように一定方向での圧延が可能とされるとともに、板厚5mm以上、さらには10mm以上の鋼板材としても、極めて強度の高いフェライト組織を主体とした平均粒径2ミクロン以下の微細等軸組織の鋼板材を得ることができる。
【図面の簡単な説明】
【図1】クロス圧延装置の交差状態での上下ロールの配置を例示した平面図である。
【図2】鼓型ロールの配置とその作用について例示した図である。
【図3】クロス圧延の原理と湾曲状の曲率について説明した図である。
【図4】実施例1の装置の場合のクロス角度とせん断変形量との関係を例示した図である。
【図5】クロス角度1.5°でのクロス圧延を行った試料の組織および、クロス角度0°での圧延を行った試料の組織を示す図である。[0001]
BACKGROUND OF THE INVENTION
The invention of this application relates to a method for producing ultrafine structure steel. More specifically, the invention of this application, high strength, high toughness, and excellent weldability, the production of a 10mm thick or more thick steel material is also possible, and mainly the grain size 2μm following ferrite structure The present invention relates to a method for producing a manufactured ultrafine structure steel.
[0002]
[Prior art and its problems]
Refinement of ferrite crystal grains is known as a powerful technique for enhancing the toughness of steel, and studies on refinement of ferrite structure have been widely conducted. For example, a rapid cooling method under large pressure (CAMP-ISIJ-Vol.11 (1998), P1017), a method using reverse transformation (Japanese Patent Laid-Open No. 58-58224), a method by repeated lap joint rolling (CAMP-ISIJ -Vol.11 (1998), P1031) and methods by warm rolling and recrystallization (CAMP-ISIJ-Vol.11 (1998), P1031) have been proposed. It is said that a thin steel sheet can be produced. Further, it is possible to produce a fine-structured bar having a diameter of 5 mm or more by a multi-pass groove roll rolling method (Japanese Patent Application No. 11-052008).
[0003]
However, despite the above examinations and proposals, it has a structure mainly composed of ferrite and having an average particle size of 2 microns or less, and is 5 mm or more in thickness and 10 times the width or more. The actual situation is that a microstructure steel plate having a thickness of 10 mm or more has not been realized yet.
[0004]
Therefore, the invention of this application has been made in view of the problems as described above, which overcomes the limitations of the prior art, has a thickness of 5 mm or more, a width of 10 times the thickness, or even a thickness. It is an object of the present invention to provide a new method for producing ultrafine structure steel having a ferrite main structure and an average particle diameter of 2 microns or less, which can be produced as a steel sheet of 10 mm or more.
[0005]
[Means for Solving the Problems]
In order to solve the above-mentioned problem, the invention of this application firstly, after heating the steel to Ac3 or higher and austenitizing, the end temperature is maintained at 550 ° C. or higher at the temperature in the metastable austenite region. During rolling, rolling with a cumulative area reduction of 70% or more is performed in a state where the upper and lower roll axes intersect at an angle of 1 ° or more at the plane position, and a shear strain in the roll axis direction is given to the material to be rolled, It is characterized by producing ultra-fine structure steel having an equiaxed structure with an average particle diameter of 2 microns or less mainly composed of.
[0006]
The invention of this application is characterized in that, secondly, in the first feature, the shear strain is 4 or more, and third, in the first feature, the shearing is performed by a plurality of rollings. It is characterized by obtaining a strain of 2 or more.
The invention of this application, fourthly, in the first feature, as a chemical composition (mass%), C: 0.8% or less, Si: 0.5% or less, Mn: 3.0% or less, P: 0.02% or less, S: 0.02% or less, and one or two or more of Ti, Mg, or Al are contained alone or in a mixture of 0.3% or less.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
The invention of this application has the features as described above, and an embodiment thereof will be described below.
[0008]
In the method of the invention of this application, rolling is performed with the upper and lower roll axes intersecting at a planar position. In this case, for example, as illustrated in FIG. The roll shafts of the upper roll (2A) arranged on the upper side of the plate material (1) and the lower roll (2B) arranged on the lower side are arranged in a plane arrangement position as shown in FIG. angle (theta 1 with respect to the orthogonal line perpendicular to the center line of 1), by setting the theta 2), which means that in a state of intersecting the plane.
[0009]
In the manufacturing method of the present invention, the angles θ 1 and θ 2 are each set to 1 ° or more. More practically, the angles θ 1 and θ 2 are each desirably up to about 20 °. The crossing angles θ 1 and θ 2 are preferably the same or substantially the same.
[0010]
In addition, the crossing angles θ 1 and θ 2 have a shear strain in the roll axis direction of 0.5 or more when the material to be rolled has a thickness of 5 mm or more when rolling with a cumulative area reduction of 80% or more. It is desirable that the angle be
[0011]
Then, for example, by using a drum-shaped roll having a concave central portion as illustrated in FIG. 2, shear strain can be effectively applied while flattening the plate thickness of the rolled material. When a normal flat roll is crossed, the distance between the upper and lower rolls (corresponding to the shape of the rolled sheet) is increased as the center in the width direction of the roll becomes narrower and becomes both ends, and the roll is crowned (curved) It becomes like this. For this reason, when rolled, as shown in FIG. 3, the distance (B) at the center of the roll is greatly expanded due to the deformation resistance of the rolled material as compared with the end (A), as if the distance between the rolls is constant. is there. This can be said to be the principle of cross rolling, but even when a large cross angle is taken, this roll interval shape can be expressed by the following equation. For this reason, the curvature in the case of a roll having a curved shape as shown in FIG. 2 follows this formula and gives the roll an opposite shape so that the roll interval is constant.
[0012]
[Expression 1]
Figure 0004683441
[0013]
In the refinement of the structure, in the case of roll rolling as described above, it is particularly preferable that the shear strain in the rolling direction is 4 or more.
[0014]
In the method of the invention of this application, rolling with a roll in a crossed state (cross roll) is finished at a metastable austenite temperature range of, for example, Ac3 point or less after heating the steel to Ac3 point or higher and austenitizing. The cumulative area reduction rate while maintaining the temperature at 550 ° C. is 70% or less.
[0015]
Rolling in the metastable austenite temperature range is indispensable in order to make the structure mainly composed of ferrite grains, and setting the rolling end temperature to 550 ° C. or higher is necessary to obtain a refined structure. That's why. When the rolling end temperature is 550 ° C. or lower, the structure only expands and the structure is not refined by recrystallization.
[0016]
Rolling with a roll may be one-pass rolling or multi-pass rolling. In multi-pass rolling, that is, rolling a plurality of times, it is possible to obtain a large shear strain as shown in the following equation as compared with one pass.
[0017]
[Expression 2]
Figure 0004683441
[0018]
Therefore, even if one pass is under a low pressure, a large shear strain is obtained by multi-pass rolling twice or more.
[0019]
According to the invention of this application as described above, the thickness of 5 mm or more, and even a thick steel plate material of 10 mm or more has a fine structure mainly composed of ferrite of 2 microns or less, particularly an equiaxed structure that contributes to high strength, Ultra fine structure steel will be provided.
[0020]
There is no particular limitation on the composition of the steel that can be the subject of the invention of this application, but the composition (% by mass) is preferably as follows.
That is, C: 0.8% or less, Si: 0.5% or less, Mn: 3.0% or less, P: 0.02% or less, S: 0.02% or less, one of Ti, Mg, or Al or those of two or more is contained in an amount of 0.3% or less alone or mixed are exemplified.
Examples will be shown below, and the invention of this application will be described in more detail.
[0021]
【Example】
<Example 1>
The material is SM490, and the chemical composition is C: 0.13, Si: 0.40, Mn: 1.39, P: 0.01, S: 0.02, Al: 0.03, Ti: 0.1, Nb. : 0.03 (mass%), and a steel plate having a size of 50 × 60 × 300 mm was used as a test material. This specimen was austenitized by holding at 900 ° C. for 10 minutes or more at Ac 3 point and then air-cooled. While the center temperature of the specimen steel sheet was from 750 ° C. to 650 ° C., the cumulative area reduction was 70%. The rolling process was performed so that it might become above.
[0022]
As shown in FIG. 1, the rolling apparatus is composed of two upper and lower rolls, arranged so that roll axes intersect, and imparts shear strain to the steel sheet.
[0023]
The upper and lower rolls are ordinary cylindrical rolls arranged in an intersecting manner with an intersecting angle, and apply shear strain (multiaxial) to the steel sheet.
[0024]
FIG. 4 shows the relationship between the crossing angle (crossing angle) in this case, that is, the angle of each of θ 1 and θ 2 when θ 1 = θ 2 and the amount of shear deformation (mm).
[0025]
The conditions for the rolling treatment were as follows. The rolling conditions for a cross angle of 0 ° for comparison are also shown below.
[0026]
A material (Invention material)
Cross angle: 1.5 °, rolling speed: 10 m / min, roll diameter: 260 mm
Pass schedule: 50-35-25-18-10 mm, post-rolling treatment: water cooling.
[0027]
B material (comparative material)
Cross angle: 0 °, rolling speed: 10 m / min, roll diameter: 260 mm
Pass schedule: 50-35-25-18-10 mm, post-rolling treatment: water cooling.
[0028]
5 (a) and 5 (b) show the structure observation results of the cross sections perpendicular to the rolling direction of the A material and B material, respectively, and are 1 mm position and 2.5 mm position (1/4 thickness from the surface), respectively. Part)).
[0029]
As shown in FIG. 5 (a), the A material (the material of the present invention) is 1 mm and 2.5 mm (1/4 thickness portion) from the surface, is fine on the entire cross section, and is particularly equiaxed in the surface layer portion. It was confirmed that the structure was mainly composed of 3-1.6 micron ferrite grains.
[0030]
On the other hand, as shown in FIG. 5B, the B material (comparative material) has a structure composed mainly of ferrite grains of 1.3 to 1.8 microns which is uniform over the entire cross section at the same position. It was confirmed that the tissue was elongated in.
[0031]
As a result, the inventive material cross-rolled at a cross angle of 1.5 ° is an ultra-fine group having a fine equiaxed grain size and an entire cross-section of 2 microns or less compared to a comparative material rolled at a cross angle of 0 °. You can see that
[0032]
[Table 1]
Figure 0004683441
[0033]
<Example 2>
In Example 1, rolling was performed in the same manner with a cross angle of 10 °. The rolling speed was 5 m / min. In this case, the roll has a drum-shaped roll shape with the center recessed in a curved shape as shown in FIG.
[0034]
Ultra-fine structure steel having an equiaxed structure mainly composed of ferrite grains having a particle size of 0.5 to 1.0 microns was obtained (Table 1).
<Example 3>
In Example 1, using a normal cylindrical roll, rolling was obtained under the same conditions with a cross angle of 5 °.
[0035]
Ultra-fine structure steel having an equiaxed structure mainly composed of ferrite grains having a particle size of 1.1 to 1.3 microns was obtained (Table 1).
[0036]
【The invention's effect】
As described above in detail, according to the inventions of this application, with the possible rolling at a constant direction as a normal rolling, thickness 5mm or more, more even more thick steel plate 10 mm, It is possible to obtain a steel plate material having a fine equiaxed structure with an average particle size of 2 microns or less mainly composed of an extremely high ferrite structure.
[Brief description of the drawings]
FIG. 1 is a plan view illustrating the arrangement of upper and lower rolls in a crossing state of a cross rolling apparatus.
FIG. 2 is a diagram illustrating the arrangement of drum-shaped rolls and the operation thereof.
FIG. 3 is a diagram illustrating the principle of cross rolling and a curved curvature .
4 is a diagram illustrating the relationship between the cross angle and the amount of shear deformation in the case of the apparatus of Example 1. FIG.
FIG. 5 is a diagram showing a structure of a sample subjected to cross rolling at a cross angle of 1.5 ° and a structure of a sample subjected to rolling at a cross angle of 0 °.

Claims (4)

鋼をAc3以上に加熱してオーステナイト化した後に、準安定オーステナイト域の温度で、終了温度が550℃以上を保持している間に累積減面率が70%以上の圧延を、上下のロール軸が平面位置で1°以上の角度で交差した状態で行い、被圧延材にロール軸方向のせん断歪みを与え、フェライトを主体とした平均粒径2ミクロン以下の等軸組織を有する超微細組織鋼を製造することを特徴とする超微細組織鋼の製造方法。  After the steel is heated to Ac3 or higher and austenitized, rolling with a cumulative area reduction of 70% or higher is performed at the temperature of the metastable austenite region while the end temperature is maintained at 550 ° C. or higher. Is performed in a state of crossing at an angle of 1 ° or more at the plane position, giving a shear strain in the roll axis direction to the material to be rolled, and having an equiaxed structure mainly composed of ferrite and having an average grain size of 2 microns or less. A process for producing ultra-fine structure steel, characterized in that 前記せん断歪みを4以上とすることを特徴とする請求項1に記載の超微細組織鋼の製造方法。  The method for producing ultrafine structure steel according to claim 1, wherein the shear strain is 4 or more. 複数回の圧延により前記せん断歪み2以上を得ることを特徴とする請求項に記載の超微細粒組織鋼の製造方法。The method for producing ultrafine-grained steel according to claim 1 , wherein the shear strain is 2 or more by rolling a plurality of times. 化学組成(質量%)として、
C:0.8%以下、
Si:0.5%以下、
Mn:3.0%以下、
P:0.02%以下、
S:0.02%以下、
であり、Ti、MgまたはAlの1種または2種以上が単独または混合で0.3%以下含有することを特徴とする請求項1に記載の超微細組織鋼の製造方法。
As chemical composition (mass%)
C: 0.8% or less,
Si: 0.5% or less,
Mn: 3.0% or less,
P: 0.02% or less,
S: 0.02% or less,
The method for producing an ultrafine structure steel according to claim 1, wherein one or more of Ti, Mg, or Al is contained alone or in a mixture of 0.3% or less.
JP2000056478A 1999-08-31 2000-03-01 Manufacturing method of ultra-fine structure steel Expired - Fee Related JP4683441B2 (en)

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