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JP2008308718A - High strength steel plate and manufacturing method thereof - Google Patents

High strength steel plate and manufacturing method thereof Download PDF

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Publication number
JP2008308718A
JP2008308718A JP2007156539A JP2007156539A JP2008308718A JP 2008308718 A JP2008308718 A JP 2008308718A JP 2007156539 A JP2007156539 A JP 2007156539A JP 2007156539 A JP2007156539 A JP 2007156539A JP 2008308718 A JP2008308718 A JP 2008308718A
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steel sheet
rolling
precipitate
steel
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Hideki Matsuda
英樹 松田
Naohiro Sato
直広 佐藤
Jun Haga
純 芳賀
Sukehisa Kikuchi
祐久 菊地
Kazuhiko Kishi
一彦 岸
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Nippon Steel Corp
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Sumitomo Metal Industries Ltd
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Abstract

【課題】自動車外板パネル用の引張強度390MPa級以上の冷延鋼板と溶融亜鉛めっき鋼板を提供する。
【解決手段】下記鋼組成を有し、Nb/Tiを含有する直径5nm以上の析出物が圧延方向に帯状に分布した析出物列を有し、前記析出物列が板厚方向10μm当たりに1〜30列の範囲で存在し、好ましくは、前記析出物列が、圧延方向断面における圧延方向にNb/Tiを含有する直径5nm以上の析出物を5個/μm以上有するものであり、かつ前記析出物列を除く部分におけるNbまたはTiを含有する直径5nm以上の生成物が圧延方向断面の平均個数で50個/μm以下である。
C:0.0005〜0.010%、Si:1.0%以下、Mn:0.30〜2.5%、P:0.10%以下、S:0.02%以下、sol.Al:0.005〜0.5%、N:0.010%以下、Nb:0.04〜0.20%、およびTi:0.05%以下を含有し、残部がFeおよび不純物からなる。
(Nb/93+Ti/48)/(C/12+N/14)≧1.5 (式1)
【選択図】図3
The present invention provides a cold-rolled steel sheet and a hot-dip galvanized steel sheet having a tensile strength of 390 MPa or more for an automobile outer panel.
SOLUTION: A precipitate having the following steel composition and containing Nb / Ti and having a diameter of 5 nm or more has a precipitate row distributed in a strip shape in the rolling direction, and the precipitate row is 1 per 10 μm in the plate thickness direction. Present in a range of ˜30 rows, preferably the precipitate row has 5 / μm or more precipitates having a diameter of 5 nm or more containing Nb / Ti in the rolling direction in the rolling direction cross section, and The product having a diameter of 5 nm or more containing Nb or Ti in the portion excluding the precipitate row is 50 pieces / μm 2 or less in average number of cross sections in the rolling direction.
C: 0.0005 to 0.010%, Si: 1.0% or less, Mn: 0.30 to 2.5%, P: 0.10% or less, S: 0.02% or less, sol. Al: 0.005 to 0.5%, N: 0.010% or less, Nb: 0.04 to 0.20%, and Ti: 0.05% or less, with the balance being Fe and impurities.
(Nb / 93 + Ti / 48) / (C / 12 + N / 14) ≧ 1.5 (Formula 1)
[Selection] Figure 3

Description

本発明は、引張強度390MPa級以上の鋼板、例えば冷延鋼板や冷延鋼板を原板とした溶融亜鉛めっき鋼板、合金化溶融亜鉛めっき鋼板、電気亜鉛めっき鋼板ならびにそれらの製造方法に関する。とりわけサイドパネル等自動車外板パネルに適した引張強度390MPa級以上の冷延鋼板および溶融亜鉛めっき鋼板、合金化溶融亜鉛めっき鋼板ならびにそれらの製造方法に関する。   The present invention relates to a steel sheet having a tensile strength of 390 MPa or higher, such as a cold-rolled steel sheet or a cold-rolled steel sheet, a hot-dip galvanized steel sheet, an alloyed hot-dip galvanized steel sheet, an electrogalvanized steel sheet, and a production method thereof. More particularly, the present invention relates to a cold-rolled steel sheet, a hot-dip galvanized steel sheet, an alloyed hot-dip galvanized steel sheet, and a method for producing them, which are suitable for an automotive outer panel such as a side panel.

自動車の高強度軽量化のニーズを受けて、自動車外板パネル等に適用される鋼板には、高強度とともに成形性、耐二次加工脆性、および外板パネルとしての表面性状などが要求されている。成形性についてはr値を高くすることや降伏強度についても低下させることが効果的である。近年は高強度鋼板に対しても成形性向上の要求が強い。高いr値を得るには、C含有量が30ppm程度以下の極低炭素鋼をベースとして、TiやNbなどの炭窒化物生成元素を添加することが有効であり、一般的にIF鋼として広く用いられている。   In response to the need for high strength and light weight of automobiles, steel sheets applied to automobile outer panel are required to have high strength, formability, secondary work brittleness, and surface properties as outer panel. Yes. For the formability, it is effective to increase the r value and also decrease the yield strength. In recent years, there is a strong demand for improving formability even for high-strength steel sheets. In order to obtain a high r value, it is effective to add a carbonitride-forming element such as Ti or Nb based on an ultra-low carbon steel having a C content of about 30 ppm or less. It is used.

しかし、IF鋼は結晶粒が粗大になりやすいため、r値を向上させるために焼鈍温度を高温とした場合に、プレス後に肌荒れが発生じて表面性状が劣化する場合がある。また、熱間圧延鋼板の微細化に適した鋼材組成の検討が不十分なこともあって、冷間圧延、焼鈍後のr値の改善は難しかった。   However, IF steel tends to be coarse in crystal grains. Therefore, when the annealing temperature is set to a high temperature in order to improve the r value, rough surface may occur after pressing and surface properties may deteriorate. In addition, it was difficult to improve the r-value after cold rolling and annealing because the examination of the steel composition suitable for miniaturization of the hot rolled steel sheet was insufficient.

一方、高いr値を備えるとともに高い強度を備える鋼板として、IF鋼をベースとしてMn、Pなどの固溶強化元素を添加した鋼板が開発されている。しかし、これらの固溶強化元素の添加は一般に高価であり、鋼板のコストアップを招く。このため、特許文献1には、固溶強化元素を削減する目的で、NbCやTiCで析出強化する技術が開示されている。   On the other hand, as a steel plate having a high r value and a high strength, a steel plate to which solid solution strengthening elements such as Mn and P are added based on IF steel has been developed. However, the addition of these solid solution strengthening elements is generally expensive and causes an increase in the cost of the steel sheet. For this reason, Patent Document 1 discloses a technique of precipitation strengthening with NbC or TiC for the purpose of reducing solid solution strengthening elements.

しかしながら、TiCはAr点以上の高温で生成するため、析出物のサイズが大きく、熱間圧延鋼板組織の微細化によるr値向上の効果や、冷間圧延鋼板組織の微細化による析出強化や表面性状改善の効果は小さい。 However, since TiC is generated at a high temperature of Ar 3 or more, the size of the precipitate is large, the effect of improving the r value by refining the hot rolled steel sheet structure, the precipitation strengthening by refining the cold rolled steel sheet structure, The effect of improving the surface properties is small.

また、TiとNbとを複合添加すると、冷却中にCがTiCとして高温で先に析出してしまうことにより、NbC微細析出物の生成が不十分となる場合があり、プレス成形性に優れた鋼板を製造する技術は十分には確立されていなかった。   In addition, when Ti and Nb are added in combination, C may be precipitated at a high temperature as TiC during cooling, resulting in insufficient generation of NbC fine precipitates, and excellent press formability. The technology for manufacturing steel sheets has not been well established.

特許文献2では、上記問題の解決を目的に、C:0.0040〜0.01%を含有する鋼板にNbを適正に添加することにより、NbCの微細析出物を生成させて組織の細粒化を図り、表面性状、機械特性を向上させる鋼板が開示されている。   In Patent Document 2, for the purpose of solving the above-mentioned problem, Nb is appropriately added to a steel sheet containing C: 0.0040 to 0.01%, thereby generating fine precipitates of NbC and fine grains of the structure. Steel sheets that improve the surface properties and mechanical properties are disclosed.

しかし、そのような鋼板は、サイドパネル、ドア、フード、ルーフ等自動車外板パネルへの適用を考慮すると、しわや面歪みが顕在化しやすいものであり、また伸びが低く、耐二次加工脆性も十分ではなかった。
特開平10−46289号公報 特開2000−303145号公報
However, when considering application to automotive outer panel such as side panels, doors, hoods, roofs, etc., such steel sheets are prone to wrinkles and surface distortions, have low elongation, and are resistant to secondary processing. Was not enough.
Japanese Patent Laid-Open No. 10-46289 JP 2000-303145 A

上述したように、従来技術にあっては、まだ、強度、成形性及び表面性状のすべてを高品質で満足する高強度冷延鋼板や高強度亜鉛めっき鋼板が得られていない。
本発明は、例えば、フード、ドア、フェンダー、サイドパネル等の自動車外板パネルに要求される高いプレス成形性を備える、引張強度390MPa級以上の高強度冷延鋼板および溶融亜鉛めっき鋼板ならびにそれらの製造方法を提供することを目的とする。
As described above, in the prior art, a high-strength cold-rolled steel sheet and a high-strength galvanized steel sheet that satisfy all of the strength, formability, and surface properties with high quality have not yet been obtained.
The present invention is, for example, a high strength cold-rolled steel sheet and hot-dip galvanized steel sheet having a high tensile formability of 390 MPa class and high press formability required for automobile outer panel such as a hood, door, fender, side panel, and the like. An object is to provide a manufacturing method.

本発明者らは、まず、サイドパネル、フード、ドア、フェンダー等の自動車外板パネルに要求される高プレス成形性を検討した。
これらの用途に供されるブランク材は、鋼板からプレス加工で製造される自動車部品のなかでも最大クラスのサイズのため、小物部品のようなスリットコイルからではなく、コイル幅のまま、それも最大クラスの広幅コイルから、ほぼ長方形にブランクカットしたものが若干トリムされたものである。
The present inventors first examined high press formability required for automobile outer panel such as side panels, hoods, doors, and fenders.
The blank material used for these applications is the largest class of automotive parts manufactured by pressing from steel plates, so it is not the slit coil like small parts, it is the maximum coil width. The wide coil of the class, which is blank cut into a nearly rectangular shape, is trimmed slightly.

ここで、本発明者らは着目したことは、例えば、サイドパネルは、しわや割れが発生し易い部分となるフロントドア、リアドア開口部の四隅のコーナーがコイル圧延方向に対し45°方向に位置すること、また、フード、ドア、フェンダーも、四隅のコーナー部近辺がしわや割れが発生し易い部分であり、その位置がコイル圧延方向に対し45°方向に位置することである。   Here, the present inventors have focused on, for example, that the side panel has a corner at the four corners of the front door and the rear door opening that are likely to be wrinkled or cracked at 45 ° with respect to the coil rolling direction. In addition, the hood, the door, and the fender are also portions where the wrinkles and cracks are likely to occur near the corners of the four corners, and the positions thereof are located in the 45 ° direction with respect to the coil rolling direction.

図1は、自動車のサイドパネルをプレスする際のブランク材における、割れやしわ危険位置を示す説明図である。
サイドパネル、ドア、フード、ルーフ等自動車外板パネルは、大型かつ概ね長方形のブランク材を用いるため、鋼板コイルに対して0°または90°方向に板取りされる。その結果、図1に示すように、鋼板の圧延方向に対して45°方向がプレス時の割れやしわ危険位置に合致する。
Drawing 1 is an explanatory view showing a crack and a wrinkle danger position in a blank material at the time of pressing a side panel of a car.
Automobile outer panel such as side panels, doors, hoods, roofs, etc. are stripped in the direction of 0 ° or 90 ° with respect to the steel plate coil because a large and generally rectangular blank material is used. As a result, as shown in FIG. 1, the 45 ° direction with respect to the rolling direction of the steel sheet coincides with a crack or wrinkle danger position during pressing.

ここに、本発明者らは、鋼板全体についての過剰な高成形性を要求することなしに、斯かる大型プレス加工用に適した鋼板を得るために次のことを着想した。
(i) 鋼板における機械特性の面内異方性に起因して、圧延方向に対して45°方向の機械特性が0°方向や90°方向より著しく劣ると、割れやしわなどのプレス不具合が生じ易くなること、そして
(ii) 45°方向の機械特性を向上させて、成形難易度が高く、しわや割れが発生し易いサイドパネル、フード、ドア、フェンダー等のコーナー部における成形性を向上させること。
Here, the present inventors have conceived the following in order to obtain a steel plate suitable for such a large press work without requiring excessively high formability of the entire steel plate.
(i) Due to the in-plane anisotropy of the mechanical properties of the steel sheet, if the mechanical properties in the 45 ° direction with respect to the rolling direction are significantly inferior to the 0 ° direction or the 90 ° direction, press defects such as cracks and wrinkles will occur. To be prone to occur, and
(ii) Improving the mechanical properties in the 45 ° direction to improve the formability at corners of side panels, hoods, doors, fenders, etc., which are highly difficult to form and easily wrinkle and crack.

すなわち、本発明者らは、圧延方向に対して45°方向の機械特性が優れ、かつ0°、45°、90°方向での機械特性差を小さくすることにより、プレス成形性が良好な、自動車のサイドパネル、フード、ドア、フェンダー等の大型プレス部品の成形に最適な鋼板とすることを着想した。   That is, the inventors have excellent mechanical properties in the 45 ° direction with respect to the rolling direction and good press formability by reducing the mechanical property difference in the 0 °, 45 °, and 90 ° directions. The idea was to make the steel plate optimal for molding large press parts such as automobile side panels, hoods, doors, and fenders.

上記課題を解決するため、本発明者らは鋼組成、製造条件について鋭意検討を行い、Nb、Ti系の微細析出物の析出状態を制御することにより、高強度化と同時に本発明の特徴である45°方向の機械特性が優れた異方性バランスを実現することができることを見出し、本発明を完成するに至った。   In order to solve the above-mentioned problems, the present inventors diligently investigated the steel composition and production conditions, and controlled the precipitation state of Nb and Ti-based fine precipitates, thereby improving the strength and at the same time the features of the present invention. The present inventors have found that an anisotropic balance with excellent mechanical properties in a certain 45 ° direction can be realized, and have completed the present invention.

本発明は次の通りである。
(1)NbまたはTiを含有する直径5nm以上の析出物が圧延方向に帯状に分布した析出物列を有し、前記析出物列が圧延方向断面における板厚方向10μm当たりに1〜30列の範囲で存在する鋼組織を備えることを特徴とする鋼板。
The present invention is as follows.
(1) Precipitates having a diameter of 5 nm or more containing Nb or Ti have a precipitate row distributed in a strip shape in the rolling direction, and the precipitate row is 1 to 30 rows per 10 μm in the plate thickness direction in the rolling direction section. A steel sheet comprising a steel structure existing in a range.

(2)前記析出物列が、圧延方向断面における圧延方向の単位長さ当たりにNbまたはTiを含有する直径5nm以上の析出物を5個/μm以上有するものであり、かつ前記析出物列を除く部分におけるNbまたはTiを含有する直径5nm以上の析出物が圧延方向断面の単位面積当たりの平均個数で50個/μm以下であることを特徴とする上記(1)に記載の鋼板。 (2) The precipitate row has 5 / μm or more of precipitates having a diameter of 5 nm or more containing Nb or Ti per unit length in the rolling direction in a cross section in the rolling direction, and the precipitate row is The steel sheet according to (1), wherein precipitates having a diameter of 5 nm or more containing Nb or Ti in an excluded portion are 50 pieces / μm 2 or less in average number per unit area of the cross section in the rolling direction.

(3)質量%で、C:0.0005〜0.010%、Si:1.0%以下、Mn:0.30〜2.5%、P:0.10%以下、S:0.02%以下、sol.Al:0.005〜0.5%、N:0.010%以下、Nb:0.04〜0.20%、およびTi:0〜0.1%を含有し、残部がFeおよび不純物からなり、下記式1を満たす鋼組成を備えることを特徴とする上記(1)または(2)に記載の鋼板。   (3) By mass%, C: 0.0005 to 0.010%, Si: 1.0% or less, Mn: 0.30 to 2.5%, P: 0.10% or less, S: 0.02 % Or less, sol. Al: 0.005 to 0.5%, N: 0.010% or less, Nb: 0.04 to 0.20%, and Ti: 0 to 0.1%, with the balance being Fe and impurities The steel plate according to (1) or (2) above, which has a steel composition satisfying the following formula 1.

(Nb/93+Ti/48)/(C/12+N/14)≧1.5 (式1)
ここで、Nb、Ti、C、Nは各元素の含有量(単位:質量%)を表す。
(4)前記鋼組成が、質量%で、B:0.002%以下をさらに含有することを特徴とする上記(3)に記載の鋼板。
(Nb / 93 + Ti / 48) / (C / 12 + N / 14) ≧ 1.5 (Formula 1)
Here, Nb, Ti, C, and N represent the content (unit: mass%) of each element.
(4) The steel sheet according to (3), wherein the steel composition further contains B: 0.002% or less in terms of mass%.

(5)前記鋼組成が、質量%で、Cr:1%以下、Mo:1%以下、V:1%以下、Cu:1%以下およびNi:1%以下からなる群から選ばれた1種または2種以上をさらに含有することを特徴とする上記(3)または(4)に記載の鋼板。   (5) The steel composition is one type selected from the group consisting of Cr: 1% or less, Mo: 1% or less, V: 1% or less, Cu: 1% or less, and Ni: 1% or less in mass%. Or the steel plate as described in said (3) or (4) characterized by further containing 2 or more types.

(6)前記鋼板の表面にめっき層を備えることを特徴とする上記(1)〜(5)の何れかに記載の鋼板。
(7)上記(3)〜(5)の何れかに記載の鋼組成を有する溶鋼を鋳造して鋳片とする鋳造工程、前記鋳片を熱間圧延して熱間圧延鋼板とする熱間圧延工程、前記熱間圧延鋼板を冷間圧延して冷間圧延鋼板とする冷間圧延工程、および前記冷間圧延鋼板を焼鈍して鋼板とする焼鈍工程を備える鋼板の製造方法において、前記鋳造工程における液相線温度から固相線温度の間の平均冷却速度CR(℃/秒)を下記式2を満足する範囲とし、前記熱間圧延工程における熱間圧延に供する鋳片の温度を1000〜1280℃、仕上圧延温度をAr〜1000℃、巻取温度を400〜650℃とし、前記冷間圧延工程における圧下率を50%以上とし、前記焼鈍工程における焼鈍温度を780〜900℃とすることを特徴とする鋼板の製造方法。
(6) The steel sheet according to any one of (1) to (5) above, wherein a plating layer is provided on the surface of the steel sheet.
(7) A casting process in which the molten steel having the steel composition described in any one of (3) to (5) above is cast into a slab, and the hot slab is hot-rolled into a hot-rolled steel sheet. In the method for producing a steel sheet, comprising: a rolling process, a cold rolling process for cold rolling the hot rolled steel sheet into a cold rolled steel sheet, and an annealing process for annealing the cold rolled steel sheet into a steel sheet. The average cooling rate CR (° C./second) between the liquidus temperature and the solidus temperature in the process is in a range satisfying the following formula 2, and the temperature of the slab used for hot rolling in the hot rolling process is 1000. To 1280 ° C., the finishing rolling temperature is Ar 3 to 1000 ° C., the coiling temperature is 400 to 650 ° C., the rolling reduction in the cold rolling step is 50% or more, and the annealing temperature in the annealing step is 780 to 900 ° C. A method for producing a steel sheet, comprising:

0.33≦(t/t)×770×CR−0.41≦10 (式2)
ここで、tは鋳片厚、tは最終の冷延鋼板厚である。
(8)前記焼鈍工程ののちに、さらにめっきを施すめっき工程を備えることを特徴とする上記(7)に記載の鋼板の製造方法。
0.33 ≦ (t 2 / t 1 ) × 770 × CR −0.41 ≦ 10 (Formula 2)
Here, t 1 is IhenAtsu, t 2 is the cold-rolled steel sheet thickness of the final.
(8) The method for producing a steel sheet according to (7) above, further comprising a plating step of performing plating after the annealing step.

本発明によれば、プレス成形性、耐二次加工脆性、鋼板表面品質に優れる鋼板が得られ、それらをサイドパネル、ドア、フェンダーなどの自動車外板に適用すると、それら部品のプレス加工で面歪み、しわ、割れが発生し易い主応力方向の圧延方向に対して45°方向の材料特性が特に優れたものが得られる。   According to the present invention, steel sheets having excellent press formability, secondary work brittleness resistance, and steel sheet surface quality can be obtained, and when they are applied to automobile outer plates such as side panels, doors, fenders, etc. A material having particularly excellent material properties in the direction of 45 ° with respect to the rolling direction of the main stress direction in which distortion, wrinkles and cracks are likely to occur can be obtained.

このように本発明によれば、適材適所の異方性をもった最適な高強度冷延鋼板を製造することができ、産業上、極めて有益である。
この鋼板は、自動車外板としてのみならず、加工用冷延鋼板、加工用表面処理鋼板としても適用できる。その表面処理としては、亜鉛めっき(合金系を含む)、すずめっき、ほうろう樹脂被覆等がある。また、本発明鋼板には、焼鈍または亜鉛めっき後、特殊な処理を施して、化成処理性、溶接性、プレス成形性および耐食性等の改善を行ってもよい。
As described above, according to the present invention, an optimum high-strength cold-rolled steel sheet having anisotropy at an appropriate position for an appropriate material can be produced, which is extremely useful industrially.
This steel sheet can be applied not only as an automobile outer sheet but also as a cold-rolled steel sheet for processing and a surface-treated steel sheet for processing. Examples of the surface treatment include zinc plating (including alloy system), tin plating, enamel resin coating, and the like. The steel sheet of the present invention may be subjected to special treatment after annealing or galvanization to improve chemical conversion properties, weldability, press formability, corrosion resistance, and the like.

本発明にかかる高強度鋼板について、析出物列で規定されるその組織、機械的特性、さらに鋼組成の限定理由について以下説明する。なお、以下、本明細書において鋼板として例えば0.5〜2.0mm程度の鋼板を例にとって本発明を説明し、また鋼組成を示す「%」は特にことわりがない限り、「質量%」である。   Regarding the high-strength steel sheet according to the present invention, the structure, mechanical properties, and reasons for limiting the steel composition defined by the precipitate row will be described below. In the following description, the present invention will be described by taking, for example, a steel sheet of about 0.5 to 2.0 mm as a steel sheet in this specification, and “%” indicating the steel composition is “% by mass” unless otherwise specified. is there.

鋼板組織
析出物
本発明においては、圧延方向に対して45°方向の降伏強度が300MPa以下、圧延方向に対して45°方向のr値が1.50以上、そして圧延方向に対して90°方向の引張強度が390MPa以上の鋼板を得るため、直径5nm以上のNbまたはTiを含有する析出物が圧延方向に帯状に分布した析出物列を、その析出物列が板厚方向10μm当たりに1〜30列の範囲で配するようにする。
Steel plate structure Precipitate In the present invention, the yield strength in the 45 ° direction relative to the rolling direction is 300 MPa or less, the r value in the 45 ° direction relative to the rolling direction is 1.50 or more, and the 90 ° direction relative to the rolling direction In order to obtain a steel sheet having a tensile strength of 390 MPa or more, a precipitate row containing Nb or Ti having a diameter of 5 nm or more distributed in a strip shape in the rolling direction, the precipitate row is 1 to 10 μm per 10 μm in the plate thickness direction. It is arranged in the range of 30 rows.

なお、本発明における冷間圧延時には、主として鋳造工程の冷却段階で生じた析出物は冷間圧延に際して圧延方向に伸び、一部、分断されることで本発明に云う析出物列が生じるのである。   In the cold rolling according to the present invention, the precipitates generated mainly in the cooling stage of the casting process extend in the rolling direction during the cold rolling and are partially divided to form the precipitate row according to the present invention. .

本発明におけるNbまたはTiを含有する析出物は、特に制限されないが、TiC、NbC、TiNおよびそれらの複合したもの、MnOを核にNbCが析出したもの、さらには、TiS、Ti422やそれらにMnSが複合したもの、FeTiPなどがある。これからも分かるように、本発明に云う「NbまたはTiを含有する」とは、介在物、つまり化合物の形態でNbおよび/またはTiが含まれているという意味である。 The precipitate containing Nb or Ti in the present invention is not particularly limited, but TiC, NbC, TiN and their composites, NbC precipitated with MnO as a nucleus, and TiS, Ti 4 C 2 S 2 and those in which MnS is combined, FeTiP, and the like. As can be seen from the above, the term “containing Nb or Ti” in the present invention means that Nb and / or Ti is contained in the form of inclusions, that is, compounds.

なお、本発明で規定する析出物の析出状態は、鋼板の表面から板厚10%、および鋼板厚の中心から板厚10%の両部分を除いた領域で満足されていればよい。表面から板厚10%および中心から板厚10%の両部分の析出状態が本発明の規定を外れていても、それらを除いた領域で満足していれば、鋼板全体としては本発明の目的とする特性を確保できる。   In addition, the precipitation state of the precipitate prescribed | regulated by this invention should just be satisfy | filled in the area | region remove | excluding both the plate thickness 10% from the surface of a steel plate, and the plate thickness 10% from the center of steel plate thickness. Even if the precipitation state of both portions of the plate thickness of 10% from the surface and the plate thickness of 10% from the center is not within the scope of the present invention, if the region excluding them is satisfied, the entire steel plate is an object of the present invention. The following characteristics can be secured.

本発明では直径5nm以上のNb、Ti系析出物について規定しているが、それより小さい極微細なNb、Ti系析出物は転位に切断されて、次に来る同じすべり面の転位に対して妨げとなりえず、以下に述べる効果に寄与しないためである。   In the present invention, Nb and Ti-based precipitates having a diameter of 5 nm or more are specified. This is because it cannot interfere with the effects described below.

本発明における、圧延方向に対して45°方向の降伏強度が低くなり、r値が高くなるというメカニズムについては必ずしも明らかでないが、従来知られている集合組織の影響以外に、析出物が影響する可能性が推測される。即ち、圧延方向に並んだ前記の析出物列と、それらに挟まれた析出物の少ない領域が存在することにより、転位の運動の妨げとなる析出物が少ない領域において低い応力で降伏し始めることが推測される。さらに、その析出物列と析出物の少ない領域は圧延方向に沿って連続的に広がっているため、圧延方向にすべる向きは他の方向より変形が容易であり、圧延方向に対して45〜90゜方向にかけては引張試験をした際の幅縮みが大きく、r値が大きくなるという可能性が推測される。   In the present invention, the mechanism that the yield strength in the 45 ° direction with respect to the rolling direction is lowered and the r value is increased is not necessarily clear, but precipitates influence other than the influence of the conventionally known texture. The possibility is guessed. That is, the presence of the above-described precipitate row arranged in the rolling direction and a region with a small amount of precipitates sandwiched between them starts to yield at a low stress in a region where there are few precipitates that hinder the movement of dislocations. Is guessed. Further, since the precipitate row and the region with few precipitates continuously spread along the rolling direction, the direction of sliding in the rolling direction is easier to deform than the other directions, and 45 to 90 with respect to the rolling direction. In the direction of °, the width shrinkage during the tensile test is large, and the possibility that the r value becomes large is estimated.

析出物列が板厚方向10μm当たりに1列未満になると転位がどの向きにも動きやすくなり、30列を超えると転位の圧延方向への運動も他の方向と同様に妨げられるようになり、いずれの場合も45°方向の機械特性の向上が得られない。好ましくは、析出物列を板厚方向10μm当たりに5〜20列とするのがよい。   When the number of precipitates is less than 1 row per 10 μm in the plate thickness direction, dislocations can easily move in any direction, and when the number of rows exceeds 30 rows, movement of dislocations in the rolling direction is prevented in the same manner as other directions. In either case, the improvement of the mechanical characteristics in the 45 ° direction cannot be obtained. Preferably, the number of precipitates is 5 to 20 per 10 μm in the plate thickness direction.

なお、析出物列の板幅方向の分布は、もっと大きな間隔で存在しているため、転位の動きへの影響に対しては板厚方向の分布が支配的である。よって、本発明では板厚方向断面での析出物列の数を規定する。   In addition, since the distribution in the plate width direction of the precipitate row exists at a larger interval, the distribution in the plate thickness direction is dominant with respect to the influence on the movement of dislocations. Therefore, in the present invention, the number of precipitate rows in the cross section in the plate thickness direction is defined.

また、好ましくは前記析出物列が、NbまたはTiを含有する直径5nm以上の析出物を圧延方向断面の単位長さ当たりに5個/μm以上有するものであり、かつ析出物列を除く部分は、NbまたはTiを含有する直径5nm以上の析出物が圧延方向断面の単位面積当たりの平均個数で50個/μm以下であるのが良い。析出物列中のNbまたはTiを含有する直径5nm以上の析出物が5個/μm未満であると前述したような転位の運動に対する析出物列としての機能を果たしにくくなり、45°方向の機械特性の向上に寄与しなくなる。また、析出物列を除く部分が、NbまたはTiを含有する直径5nm以上の析出物を圧延方向断面の単位面積当たりの平均個数で50個/μmを超えて有すると、転位の圧延方向への運動も他の方向と同様に妨げられるようになり、45°方向の機械特性の向上が得にくくなる。 Preferably, the precipitate row has Nb or Ti-containing precipitates having a diameter of 5 nm or more per unit length of the cross section in the rolling direction, and the portion excluding the precipitate row is The average number of precipitates containing 5 nm or more in diameter containing Nb or Ti per unit area of the cross section in the rolling direction is preferably 50 / μm 2 or less. When the number of precipitates having a diameter of 5 nm or more containing Nb or Ti in the precipitate row is less than 5 / μm, it becomes difficult to perform the function as the precipitate row with respect to the movement of dislocation as described above. Does not contribute to improvement of characteristics. Further, if the portion excluding the precipitate row has Nb or Ti-containing precipitates having a diameter of 5 nm or more in an average number per unit area of the cross section in the rolling direction of more than 50 / μm 2 , the dislocation direction is changed to the rolling direction. This movement is also hindered in the same manner as in other directions, and it becomes difficult to improve the mechanical characteristics in the 45 ° direction.

さらに好ましくは、前記の析出物列が、NbまたはTiを含有する直径5nm以上の析出物を圧延方向断面の単位長さ当たりに10個/μm以上有するのが良く、析出物列を除く部分は、NbまたはTiを含有する直径5nm以上の析出物が圧延方向断面の単位面積当たりの平均個数で30個/μm以下であるのが良い。 More preferably, the precipitate row has Nb or Ti-containing precipitates having a diameter of 5 nm or more per unit length of the cross section in the rolling direction, and the portion excluding the precipitate row is Nb or Ti-containing precipitates having a diameter of 5 nm or more are preferably 30 pieces / μm 2 or less in average number per unit area of the cross section in the rolling direction.

析出物列に入る析出物とそれ以外の析出物とは、単位長さ当たりの析出物の存在頻度が圧延方向が板厚方向の10倍以上になっている箇所を析出物列とみなし、その注目する析出物列の中心線から、それと隣接する析出物列の中心線まで距離の0.1倍以内に位置している析出物を、その析出物列に含まれる析出物とみなすことをもって識別することとする。   Precipitates entering the precipitate row and the other precipitates are regarded as a precipitate row where the presence frequency of precipitates per unit length is 10 times or more in the rolling direction in the sheet thickness direction. Identify a precipitate located within 0.1 times the distance from the center line of the target precipitate line to the center line of the adjacent precipitate line as a precipitate included in the precipitate line I decided to.

なお、本発明の鋼板の組織はフェライトを主体としているが、フェライト平均結晶粒径が大き過ぎると、プレス後に肌荒れが発生して表面性状が劣化する場合があるため、さほど問題とならない範囲として30μm以下であるのが好ましい。一方、フェライト平均結晶粒径が3μm未満であると、転位が結晶粒界で止められる影響が大きくなり、前記析出物列による影響が相対的に小さくなって、45°方向の機械特性の向上が得られなくなる恐れがあるため、フェライト平均結晶粒径は3μm以上であることが好ましい。   The structure of the steel sheet of the present invention is mainly composed of ferrite, but if the average grain size of ferrite is too large, rough surface may occur after pressing and the surface properties may deteriorate, so that it does not matter so much as 30 μm. It is preferable that: On the other hand, if the ferrite average crystal grain size is less than 3 μm, the effect of dislocations being stopped at the grain boundaries is increased, the effect of the precipitate row is relatively reduced, and the mechanical properties in the 45 ° direction are improved. The ferrite average crystal grain size is preferably 3 μm or more because there is a risk that it will not be obtained.

本発明において、析出物の形態および成分の分析は、特に具体的手段が規定されるものではないが、基準的方法としては、エネルギー分散型X線分光法による分析でTiまたはNbの存在を確認することができ、析出物の数等は透過型電子顕微鏡による断面観察を行なえばよい。そのときの倍率は10万倍とする。
機械的特性
本発明にかかる鋼板においては、圧延方向に対して45°方向の降伏強度が300MPa以下、圧延方向に対して45°方向のr値が1.50以上であり、圧延方向に対して90°方向の引張強度が390MPa以上である。
In the present invention, there are no specific means for the analysis of the form and components of the precipitate, but as a standard method, the presence of Ti or Nb is confirmed by analysis by energy dispersive X-ray spectroscopy. The number of precipitates and the like may be observed through a cross section using a transmission electron microscope. The magnification at that time is 100,000.
Mechanical properties In the steel sheet according to the present invention, the yield strength in the 45 ° direction with respect to the rolling direction is 300 MPa or less, and the r value in the 45 ° direction with respect to the rolling direction is 1.50 or more. The tensile strength in the 90 ° direction is 390 MPa or more.

析出物の形態の制御は、まず鋼組成の選択、連続鋳造時の冷却速度、最終製品に至るまでの圧下率等によって行なうことができる。本発明にかかる鋼板にみられる析出物は大部分が炭化物と窒化物であるため、例えば、析出物の量は鋼組成によりほぼ決まり、その大きさは連続鋳造後の凝固過程での粒成長により、そして圧延等の加工段階での加工方法、そしてそのときの加工率等によって変わる。   The control of the form of the precipitate can be performed by first selecting the steel composition, the cooling rate during continuous casting, the reduction rate until reaching the final product, and the like. Since most of the precipitates found in the steel sheet according to the present invention are carbides and nitrides, for example, the amount of precipitates is almost determined by the steel composition, the size of which depends on the grain growth in the solidification process after continuous casting. And the processing method at the processing stage such as rolling, and the processing rate at that time.

前述のように、冷間圧延時には析出物は圧延方向に伸び、一部、分断されることで本発明に云う析出物列が生じるのである。
鋼組成
C:0.0005〜0.010%
CはNb、Tiと結合し、Nb、Ti系の微細析出物を形成する。C含有量を適正化することは本発明の特徴とする析出物列の析出状態を実現するために重要である。Cが0.0005%未満では析出物が少な過ぎ、0.010%を超えると析出物が多過ぎて、本発明の特徴とする析出状態が得られないため、0.0005〜0.010%とする。好ましくは、0.0005〜0.004%である。
As described above, during cold rolling, the precipitates extend in the rolling direction and are partially divided to form a precipitate row according to the present invention.
Steel composition C: 0.0005 to 0.010%
C combines with Nb and Ti to form Nb and Ti-based fine precipitates. It is important to optimize the C content in order to realize the precipitation state of the precipitate row, which is a feature of the present invention. When C is less than 0.0005%, there are too few precipitates, and when it exceeds 0.010%, there are too many precipitates, and the precipitation state characteristic of the present invention cannot be obtained, so 0.0005 to 0.010% And Preferably, it is 0.0005 to 0.004%.

Si:1.0%以下
Siは固溶強化により高強度化するために添加することができるが、1.0%を超えて含有するとr値の劣化が大きい。従って、1.0%以下とする。
Si: 1.0% or less Si can be added to increase the strength by solid solution strengthening, but if it exceeds 1.0%, the r value is greatly deteriorated. Therefore, it is 1.0% or less.

Mn:0.30〜2.5%
Mnは固溶強化により高強度化し、耐二次加工脆性に悪影響を及ぼすSを固定するため含有させる。0.30%未満では、狙いとする高強度が図れない。また、耐二次加工脆性をより良好にするためには0.8%以上とすることが望ましい。2.5%超えではr値と伸びを劣化させるので0.30〜2.5%とする。
Mn: 0.30 to 2.5%
Mn is added to increase the strength by solid solution strengthening and to fix S which adversely affects secondary work brittleness resistance. If it is less than 0.30%, the targeted high strength cannot be achieved. Moreover, in order to make secondary work brittleness resistance better, it is desirable to set it as 0.8% or more. If it exceeds 2.5%, the r value and elongation deteriorate, so 0.30 to 2.5% is set.

P:0.10%以下
Pは固溶強化により高強度化するため含有させることができる。0.10%を超えると耐二次加工脆性が極端に劣化するため0.10%以下とする。好ましくは0.07%以下とするのがよい。
P: 0.10% or less P can be contained in order to increase the strength by solid solution strengthening. If it exceeds 0.10%, the secondary work brittleness resistance is extremely deteriorated, so the content is made 0.10% or less. Preferably it is 0.07% or less.

S:0.02%以下
Sは不純物として存在するが、0.02%を超えると熱間圧延時に疵が発生しやすくなり表面性状が悪化するため、0.02%以下とする。
S: 0.02% or less S is present as an impurity, but if it exceeds 0.02%, wrinkles are likely to occur during hot rolling and the surface properties deteriorate, so the content is made 0.02% or less.

sol.Al:0.005〜0.5%
Alは脱酸のため含有させる。sol.Alが0.005%未満では脱酸が十分でなく、0.5%を超えて含有させてもコストが嵩むばかりで効果が無いため、0.005〜0.5%とする。
sol. Al: 0.005 to 0.5%
Al is included for deoxidation. sol. When Al is less than 0.005%, deoxidation is not sufficient, and even if contained over 0.5%, the cost is increased and there is no effect, so 0.005 to 0.5% is made.

N:0.010%以下
Nは過剰に含有すると、固溶状態のまま残ってストレッチャーストレインや降伏強度の上昇を生じる場合があるほか、TiがN当量以上添加されている場合でも、Nが0.010%を超えて存在するとTiNが高温から析出して析出物が粗大化しやすくなり、本発明の特徴とする析出状態が得られない場合がある。よって、Nは0.010%以下に限定する。
N: 0.010% or less If N is excessively contained, it may remain in a solid solution state, resulting in an increase in stretcher strain or yield strength. If the content exceeds 0.010%, TiN precipitates from a high temperature and the precipitate tends to be coarsened, and the precipitation state characteristic of the present invention may not be obtained. Therefore, N is limited to 0.010% or less.

Nb:0.04〜0.20%
NbはCなどと結合、複合化して、Nb、Ti系の微細析出物を形成する。Nbを適正化することは本発明の特徴とする析出物列の析出状態を得るために極めて重要である。Nb、Tiは、極めて微細な炭窒化物が得られるという点で析出強化に好適な元素であるが、本発明はさらに鋳造工程において凝固の際の分配係数が小さいことを利用して、凝固時の冷却条件を適正な範囲に制御することによりデンドライトアーム間にミクロ偏析させることを特徴としている。このミクロ偏析を圧延工程で引き延ばすとともに、熱間圧延後のホットランテーブル上やコイル巻取後、および冷間圧延後の焼鈍工程でNb、Ti炭窒化物を析出させ、本発明の特徴である圧延方向に帯状に分布した析出物列を実現している。
Nb: 0.04 to 0.20%
Nb combines with C and the like to form a composite precipitate of Nb and Ti. Optimizing Nb is extremely important in order to obtain the precipitation state of the precipitate row, which is a feature of the present invention. Nb and Ti are elements suitable for precipitation strengthening in that extremely fine carbonitrides can be obtained, but the present invention further utilizes a small distribution coefficient during solidification in the casting process, It is characterized by microsegregation between the dendrite arms by controlling the cooling condition of the material within an appropriate range. The microsegregation is extended in the rolling process, and Nb and Ti carbonitrides are deposited on the hot run table after hot rolling, after coil winding, and in the annealing process after cold rolling, which is a feature of the present invention. A series of precipitates distributed in a strip shape in the direction is realized.

析出物列を効果的に得るためには、分配係数がより小さいNbの利用が必須であり、0.04%未満では析出物列を得るのに十分なNbの濃化が得られない。0.20%を超えてNbを含有させると、固溶Nbの増加により降伏強度が上昇して加工時にしわが生じやすくなる。   In order to effectively obtain a precipitate row, it is essential to use Nb having a smaller distribution coefficient. If it is less than 0.04%, Nb concentration sufficient to obtain a precipitate row cannot be obtained. When Nb is contained exceeding 0.20%, the yield strength increases due to an increase in solid solution Nb and wrinkles are likely to occur during processing.

Ti:0〜0.1%
一方、Tiも分配係数が小さい元素であるが、Nbに比べると大きく、Ti添加したものはNb単独添加の場合に比べて析出物列と析出物列を除く部分との析出物密度の差が小さくなる場合があるため、Tiを過剰に含有させることは避けるべきである。よって、必要により含有させればよく、そのとき含有させても良い上限を0.1%とする。好ましくは0.05%以下である。
Ti: 0 to 0.1%
On the other hand, Ti is also an element having a small distribution coefficient, but it is larger than Nb, and the Ti addition has a difference in the precipitate density between the precipitate row and the portion excluding the precipitate row as compared with the case of adding Nb alone. Since it may be small, excessive Ti content should be avoided. Therefore, it may be contained if necessary, and the upper limit that may be contained at that time is 0.1%. Preferably it is 0.05% or less.

(Nb/93+Ti/48)/(C/12+N/14)≧1.5
(Nb/93+Ti/48)/(C/12+N/14)が1.5未満では、熱間圧延鋼板の段階での固溶C量が多くなり、最終製品のr値が低下して、サイドパネル、フード、ドア、フェンダー等に必要な深絞り性が得られない場合があるため、上述のように規定する。
(Nb / 93 + Ti / 48) / (C / 12 + N / 14) ≧ 1.5
If (Nb / 93 + Ti / 48) / (C / 12 + N / 14) is less than 1.5, the amount of solute C in the hot rolled steel sheet stage increases, and the r value of the final product decreases, and the side panel Since the deep drawability required for hoods, doors, fenders, etc. may not be obtained, it is specified as described above.

B:0.002%以下
Bは二次加工脆化を防止するために含有させることができる。0.002%を超えて含有させるとr値および伸びが著しく劣化するので、0.002%以下とする。 0.0002%未満では効果が小さいため、含有させる場合は0.0002%以上とすることが好ましい。
B: 0.002% or less B can be contained in order to prevent secondary processing embrittlement. If the content exceeds 0.002%, the r value and the elongation deteriorate significantly, so the content is made 0.002% or less. If the content is less than 0.0002%, the effect is small.

Cr:1%以下、Mo:1%以下、V:1%以下、Cu:1%以下、Ni:1%以下からなる群から選ばれた1種または2種以上
これらの元素は強度確保のため含有させても良い。各元素の含有量が1%を超えると強度向上の効果が飽和してコストが嵩むため各元素の含有量を1%以下とする。好ましくは0.5%以下である。
製造方法
鋳造の際の液相線温度から固相線温度の間の平均冷却速度CR(℃/秒)と鋳片厚t、最終の冷延鋼板厚tとの関係:0.33≦(t/t)×770×CR−0.41≦10
本発明の特徴である、NbまたはTiを含有する直径5nm以上の析出物が圧延方向に帯状に分布した析出物列が板厚方向10μm当たりに1〜30列配した状態にするために、凝固時の冷却速度を制御することは極めて重要である。鋳造の際の凝固時に液相線温度から固相線温度の間の平均冷却速度CR(℃/秒)、鋳片厚t、最終の鋼板厚tとの関係で、(t/t)×770×CR−0.41が10を超えると、Nbの偏析帯の間隔が大きくなり、最終製品において45°方向の機械特性を向上させるのに必要なNb、Ti系析出物の析出状態を得ることができない。一方、(t/t)×770×CR−0.41が0.33より小さくなると、Nbの偏析帯の間隔が小さ過ぎて、最終製品において45°方向の機械特性を向上させるのに必要なNb、Ti系析出物の析出状態を得ることができない。
Cr: 1% or less, Mo: 1% or less, V: 1% or less, Cu: 1% or less, Ni: 1% or less selected from the group consisting of Ni: 1% or less These elements are for securing strength It may be included. If the content of each element exceeds 1%, the effect of improving the strength is saturated and the cost increases, so the content of each element is set to 1% or less. Preferably it is 0.5% or less.
Production method Relationship between average cooling rate CR (° C./second) between liquidus temperature and solidus temperature during casting, slab thickness t 1 , final cold-rolled steel plate thickness t 2 : 0.33 ≦ (T 2 / t 1 ) × 770 × CR −0.41 ≦ 10
In order to obtain a state in which 1 to 30 rows of precipitates in which a precipitate having a diameter of 5 nm or more containing Nb or Ti is distributed in a strip shape in the rolling direction is arranged in 1 to 30 rows per 10 μm in the thickness direction, which is a feature of the present invention. It is very important to control the cooling rate of the hour. In relation to the average cooling rate CR (° C./sec) between the liquidus temperature and the solidus temperature during solidification during casting, the slab thickness t 1 , and the final steel plate thickness t 2 , (t 2 / t 1 ) When X770 × CR- 0.41 exceeds 10, the interval between the segregation bands of Nb becomes large, and precipitation of Nb and Ti-based precipitates necessary for improving the mechanical properties in the 45 ° direction in the final product Can't get state. On the other hand, if (t 2 / t 1 ) × 770 × CR −0.41 is smaller than 0.33, the interval between the segregation bands of Nb is too small to improve the mechanical properties in the 45 ° direction in the final product. The necessary precipitation state of Nb and Ti-based precipitates cannot be obtained.

なお、上記の鋳造の際の冷却速度は、鋳片の表面から鋳片厚10%、および鋳片厚の中心から鋳片厚10%の両部分を除いた領域で満足されていればよい。表面から鋳片厚10%および中心から鋳片厚10%の両部分の冷却速度が本発明の規定を外れていても、それらを除いた領域で満足していれば、本発明の目的とする特性を確保できる。   In addition, the cooling rate at the time of said casting should just be satisfy | filled in the area | region except the both parts of slab thickness 10% from the slab surface, and slab thickness 10% from the center of slab thickness. The object of the present invention is that if the cooling rate of both portions of the slab thickness 10% from the surface and the slab thickness 10% from the center is satisfied in the region excluding them, even if they are out of the scope of the present invention. Characteristics can be secured.

熱間圧延に供する鋳片の温度:1000〜1280℃
本発明では所定の成分を有する鋳片を連続鋳造後直ちに、または再加熱後、粗熱間圧延を行う。いずれの場合でも熱間圧延に供する温度を1000〜1280℃とする。1000℃未満の場合、変形抵抗が高く熱間圧延が困難で、1280℃を超えると過剰にスケールが生成し、表面性状を劣化させるため、1000〜1280℃とする。
Temperature of slab to be subjected to hot rolling: 1000 to 1280 ° C
In the present invention, a slab having a predetermined component is subjected to rough hot rolling immediately after continuous casting or after reheating. In any case, the temperature used for hot rolling is 1000 to 1280 ° C. When the temperature is less than 1000 ° C., deformation resistance is high and hot rolling is difficult, and when it exceeds 1280 ° C., scales are excessively generated and the surface properties are deteriorated, so the temperature is set to 1000 to 1280 ° C.

なお、粗熱間圧延と仕上熱間圧延の合間に1280℃を超えない範囲で加熱を行ってもよく、本発明の効果が失われることはない。
仕上圧延温度:Ar〜1000℃
仕上熱間圧延の仕上温度がAr未満では表層の析出物が粗大化するため、r値を損なう。1000℃を超えると、スケールにより表面性状が劣化するため、仕上圧延温度はAr3〜1000℃とする。
In addition, you may heat in the range which does not exceed 1280 degreeC between rough hot rolling and finishing hot rolling, and the effect of this invention is not lost.
Finish rolling temperature: Ar 3 ~1000
When the finish hot rolling finish temperature is less than Ar 3 , the surface layer precipitates become coarse, and the r value is impaired. If the temperature exceeds 1000 ° C., the surface properties deteriorate due to the scale, so the finish rolling temperature is Ar 3 to 1000 ° C.

巻取温度:400〜650℃
巻取温度が400℃未満では、巻取後に炭化物の生成が十分に生じないため、r値が低下する。650℃を超える場合、粗大な析出物が生成し、強度が低下する場合があるため、400〜650℃とする。
Winding temperature: 400-650 ° C
If the coiling temperature is less than 400 ° C., carbides are not sufficiently generated after coiling, and the r value is lowered. When it exceeds 650 ° C., coarse precipitates are formed and the strength may be lowered, so the temperature is set to 400 to 650 ° C.

冷間圧延の圧延率:50%以上
r値を向上させるため、冷間圧延の圧延率を50%以上とする。
焼鈍温度:780〜900℃
高いr値を得るため、冷間圧延後、780〜900℃の温度域で均熱し、焼鈍を行う。
焼鈍温度が780℃未満および900℃を超えると、r値の低下や降伏強度の上昇をもたらすため、780〜900℃とする。
Cold rolling rolling ratio: 50% or more In order to improve the r value, the cold rolling rolling ratio is 50% or more.
Annealing temperature: 780-900 ° C
In order to obtain a high r value, after cold rolling, soaking is performed in a temperature range of 780 to 900 ° C. and annealing is performed.
When the annealing temperature is less than 780 ° C. and exceeds 900 ° C., the r value is decreased and the yield strength is increased.

このようにして得られた冷延鋼板は自動車外板パネルの成形に要求される優れたプレス成形性を備え、引張強度390MPa以上を有する。
本発明によれば、好ましくは、上記冷延鋼板にさらに亜鉛などの金属をめっきして金属めっき鋼板としてもよい。めっきの形態としては電気めっき、溶融金属めっき、などがある。実用上からは、そのような金属めっき鋼板としては、代表的には、電気亜鉛めっき鋼板、溶融亜鉛めっき鋼板、合金化溶融亜鉛めっき鋼板などがある。
The cold-rolled steel sheet thus obtained has excellent press formability required for forming an automobile outer panel, and has a tensile strength of 390 MPa or more.
According to the present invention, preferably, the cold-rolled steel sheet may be further plated with a metal such as zinc to form a metal-plated steel sheet. Examples of plating forms include electroplating and molten metal plating. From a practical standpoint, representative examples of such metal-plated steel sheets include electrogalvanized steel sheets, hot-dip galvanized steel sheets, and alloyed hot-dip galvanized steel sheets.

そのようなめっき鋼板の製造方法については、慣用の方法にしたがえばよく、本発明においては特に制限されない。   About the manufacturing method of such a plated steel plate, what is necessary is just to follow a conventional method, and it does not restrict | limit in particular in this invention.

表1に示す化学成分を含有する供試材No.1〜30の鋼板を下記要領で試作した。
連続鋳造により鋳片厚270mmのスラブとし、スラブ加熱後、熱間圧延により粗圧延後板厚40mm、仕上圧延後板厚3.2mmとし、その後、冷却して巻き取った。さらに0.65mmまで冷間圧延し、連続焼鈍を施した。一部の試験材はさらに電気亜鉛めっきまたは溶融亜鉛めっきを片面当り45g/mの付着量で実施した。溶融亜鉛めっき鋼板のさらに一部は470〜550℃で合金化処理を行い、合金化溶融亜鉛めっき鋼板とした。
Specimen No. containing chemical components shown in Table 1 1 to 30 steel plates were prototyped as follows.
A slab having a slab thickness of 270 mm was formed by continuous casting, and after slab heating, the plate thickness after rough rolling was 40 mm and the plate thickness after finish rolling was 3.2 mm by hot rolling, and then cooled and wound. Further, it was cold-rolled to 0.65 mm and subjected to continuous annealing. Some test materials were further subjected to electrogalvanization or hot dip galvanization with an adhesion amount of 45 g / m 2 per side. Further part of the hot dip galvanized steel sheet was alloyed at 470 to 550 ° C. to obtain an alloyed hot dip galvanized steel sheet.

冷延鋼板と電気亜鉛めっき鋼板については連続焼鈍後、溶融亜鉛めっき鋼板と合金化溶融亜鉛めっき鋼板についてはめっき後に伸び率0.9%の調質圧延を施した。
図2は、試験材の観察断面の位置を模式的に示す説明図である。
The cold-rolled steel sheet and the electrogalvanized steel sheet were subjected to temper rolling with an elongation rate of 0.9% after the continuous annealing and the hot-dip galvanized steel sheet and the alloyed hot-dip galvanized steel sheet after plating.
FIG. 2 is an explanatory diagram schematically showing the position of the observation cross section of the test material.

得られた各種鋼板について、図2に斜線領域で示す、圧延方向に沿った断面について透過型電子顕微鏡を用いてレプリカ法で析出物の観察を行なうとともに、めっき密着性、耐二次加工脆性、表面性状および成形性を調査した。図2において、斜線領域で示す圧延方向断面におけるY軸方向が板厚方向であり、X軸方向が圧延方向である。   About the obtained various steel sheets, while observing precipitates by a replica method using a transmission electron microscope with respect to a cross section along the rolling direction, which is indicated by a hatched region in FIG. 2, plating adhesion, secondary work brittleness resistance, The surface properties and moldability were investigated. In FIG. 2, the Y-axis direction in the cross section in the rolling direction indicated by the hatched area is the plate thickness direction, and the X-axis direction is the rolling direction.

析出物列中の析出物密度、析出物列を除く部分の析出物密度の測定は、1μm四方の任意の10視野について観察を行い、その平均値を求めた。
図3は、結果の1例として試験番号3の場合の電子顕微鏡写真を示す。
For the measurement of the precipitate density in the precipitate row and the precipitate density in the portion excluding the precipitate row, observation was performed for any 10 fields of view of 1 μm square, and the average value was obtained.
FIG. 3 shows an electron micrograph of test number 3 as an example of the results.

図3からは、本発明鋼の特徴である、圧延方向に帯状に分布した析出物列が観察される。図示写真の析出物はX線回折による同定の結果、NbCを主体としたNb、Ti系析出物であった。この視野中に観察される2本の析出物列は、直径5nm以上のNbまたはTiを含有する析出物を、それぞれ15個/μm(図中、上側の列)、28個/μm(図中、下側の列)有している。一方、析出物列を除く部分は、直径5nm以上のNbまたはTiを含有する析出物を5個/μm有している。 From FIG. 3, a string of precipitates distributed in a strip shape in the rolling direction, which is a feature of the steel of the present invention, is observed. As a result of identification by X-ray diffraction, the precipitates in the photograph shown were Nb and Ti based precipitates mainly composed of NbC. The two precipitate rows observed in this field of view are 15 / μm (upper row in the drawing) and 28 / μm (upper row in the drawing) containing Nb or Ti having a diameter of 5 nm or more. , Lower row). On the other hand, the portion excluding the precipitate row has 5 precipitates / μm 2 containing Nb or Ti having a diameter of 5 nm or more.

なお、図3の場合、析出物列は、厚さ方向1μm当たりでいえば、2列となるから、これを10視野について行い、それを合計することで厚さ方向10μm 当たりの析出物列の列数が算出される。  In the case of FIG. 3, there are two precipitate rows per 1 μm in the thickness direction, so this is performed for 10 fields of view, and by summing them, the number of precipitate rows per 10 μm in the thickness direction The number of columns is calculated.

耐二次加工脆性は、直径50mmの円筒ポンチを用いて絞り比1.8で絞り加工を行い、各温度に保持した後、円錐台にセットして100kgの錘を高さ1mより落錘させ、破面観察から脆性破壊が発生する上限温度(以下、耐二次加工脆化温度と呼ぶ)を調査した。耐二次加工脆化温度が−50℃以下のものを本発明の適合範囲とした。   The secondary work brittleness resistance is drawn using a cylindrical punch with a diameter of 50 mm and drawn at a drawing ratio of 1.8. After holding at each temperature, it is set on a truncated cone and a weight of 100 kg is dropped from a height of 1 m. From the observation of the fracture surface, the upper limit temperature at which brittle fracture occurs (hereinafter referred to as secondary work embrittlement resistance temperature) was investigated. A material having a secondary work embrittlement resistance of −50 ° C. or less was regarded as a conforming range of the present invention.

めっき密着性は、180°密着曲げし、曲げ加工部にセロテープ(登録商標)を接着、剥離し、テープに付着した剥離めっき量を自動車外装用途として基準を満たすか否かにより判定した。
表面性状は、めっき表面の外観を自動車外装用途の基準を満たすか否かを目視で判定した。
The plating adhesion was determined by whether or not the adhesive plating was performed by 180 ° adhesion, cellotape (registered trademark) was adhered to and peeled off from the bent portion, and the amount of peeled plating adhered to the tape satisfied the standard for automotive exterior use.
The surface property was determined by visual observation as to whether or not the appearance of the plating surface satisfies the standards for automotive exterior applications.

成形性は、図4に示すように、サイドパネルのセンターピラー部を模したT字型テスト型を用いて、絞り深さ25mmでプレス加工を施し、割れ、しわの有無を評価した。
製造条件および機械的特性を調査した結果を表1に示す。めっき鋼板のr値測定はめっき層の影響を除去するため、塩酸によりめっき層のみ溶解除去した後に実施した。圧延方向に対して45゜方向のr値が1.50以上であっても他の方向のr値が極端に低ければ、プレス成形において割れが発生しやすくなるため、平均r値が1.50以上のものを本発明の適合範囲とした。ここで、平均r値=(r+2r45+r90)/4、r、r45、r90はそれぞれ圧延方向に対して0゜、45゜、90゜のr値である。
As shown in FIG. 4, the moldability was evaluated by using a T-shaped test die simulating the center pillar portion of the side panel at a drawing depth of 25 mm and evaluating the presence or absence of cracks and wrinkles.
Table 1 shows the results of investigating the manufacturing conditions and mechanical properties. The r value of the plated steel sheet was measured after dissolving and removing only the plating layer with hydrochloric acid in order to remove the influence of the plating layer. Even if the r value in the 45 ° direction with respect to the rolling direction is 1.50 or more, if the r value in the other direction is extremely low, cracks are likely to occur in press forming, so the average r value is 1.50. The above is regarded as the applicable range of the present invention. Here, the average r value = (r 0 + 2r 45 + r 90 ) / 4, r 0 , r 45 , and r 90 are r values of 0 °, 45 °, and 90 ° with respect to the rolling direction, respectively.

本発明の成分範囲の鋼板は強度、r値、耐二次加工脆性、成形性のすべてに優れ、自動車外板用に最適である。
図5には、析出物の分布と45°方向r値との関係を、表1に示す結果に基づいてグラフにして示す。本発明の範囲内の析出物分布のときに45°方向のr値1.50以上が得られることが分かる。
The steel sheet of the component range of the present invention is excellent in all of strength, r value, secondary work brittleness resistance and formability, and is optimal for an automobile outer sheet.
FIG. 5 is a graph showing the relationship between the distribution of precipitates and the 45 ° direction r value based on the results shown in Table 1. It can be seen that an r value of 1.50 or more in the 45 ° direction is obtained when the precipitate distribution is within the range of the present invention.

自動車のサイドパネルをプレスする際の、割れやしわ危険位置の模式的説明図である。It is a typical explanatory view of a crack and a wrinkle danger position at the time of pressing a side panel of a car. 実施例の試験材の観察断面の位置の概略説明図である。It is a schematic explanatory drawing of the position of the observation cross section of the test material of an Example. 圧延方向断面の析出物観察例を示すレプリカ法による透過型電子顕微鏡写真である(10万倍)。It is the transmission electron micrograph by the replica method which shows the example of precipitate observation of a rolling direction cross section (100,000 times). T字型テスト型の平面図である。It is a top view of a T-shaped test type. 実施例の結果を示すグラフである。It is a graph which shows the result of an Example.

Claims (8)

NbまたはTiを含有する直径5nm以上の析出物が圧延方向に帯状に分布した析出物列を有し、前記析出物列が圧延方向断面における板厚方向10μm当たりに1〜30列の範囲で存在する鋼組織を備えることを特徴とする鋼板。 Nb or Ti-containing precipitates having a diameter of 5 nm or more have a precipitate row distributed in a strip shape in the rolling direction, and the precipitate row exists in a range of 1 to 30 rows per 10 μm in the plate thickness direction in the rolling direction section. A steel sheet characterized by comprising a steel structure to be used. 前記析出物列が、圧延方向断面における圧延方向の単位長さ当たりにNbまたはTiを含有する直径5nm以上の析出物を5個/μm以上有するものであり、かつ前記析出物列を除く部分におけるNbまたはTiを含有する直径5nm以上の析出物が圧延方向断面の単位面積当たりの平均個数で50個/μm2以下であることを特徴とする請求項1に記載の鋼板。 The precipitate row has 5 / μm or more of precipitates having a diameter of 5 nm or more and containing Nb or Ti per unit length in the rolling direction in a cross section in the rolling direction, and in a portion excluding the precipitate row. 2. The steel sheet according to claim 1, wherein the number of precipitates containing Nb or Ti and having a diameter of 5 nm or more is 50 / μm 2 or less in average number per unit area of the cross section in the rolling direction. 質量%で、C:0.0005〜0.010%、Si:1.0%以下、Mn:0.30〜2.5%、P:0.10%以下、S:0.02%以下、sol.Al:0.005〜0.5%、N:0.010%以下、Nb:0.04〜0.20%、およびTi:0〜0.1%を含有し、残部がFeおよび不純物からなり、下記式1を満たす鋼組成を備えることを特徴とする請求項1または2に記載の鋼板。
(Nb/93+Ti/48)/(C/12+N/14)≧1.5 (式1)
ここで、Nb、Ti、C、Nは各元素の含有量(単位:質量%)を表す。
In mass%, C: 0.0005 to 0.010%, Si: 1.0% or less, Mn: 0.30 to 2.5%, P: 0.10% or less, S: 0.02% or less, sol. Al: 0.005 to 0.5%, N: 0.010% or less, Nb: 0.04 to 0.20%, and Ti: 0 to 0.1%, with the balance being Fe and impurities The steel plate according to claim 1 or 2, comprising a steel composition satisfying the following formula (1).
(Nb / 93 + Ti / 48) / (C / 12 + N / 14) ≧ 1.5 (Formula 1)
Here, Nb, Ti, C, and N represent the content (unit: mass%) of each element.
前記鋼組成が、Feの一部に代えて、質量%で、B:0.002%以下をさらに含有することを特徴とする請求項3に記載の鋼板。 The steel sheet according to claim 3, wherein the steel composition further contains B: 0.002% or less in mass% instead of part of Fe. 前記鋼組成が、Feの一部に代えて、質量%で、Cr:1%以下、Mo:1%以下、V:1%以下、Cu:1%以下およびNi:1%以下からなる群から選ばれた1種または2種以上をさらに含有することを特徴とする請求項3または4に記載の鋼板。 The steel composition is, instead of a part of Fe, in mass%, Cr: 1% or less, Mo: 1% or less, V: 1% or less, Cu: 1% or less, and Ni: 1% or less. The steel sheet according to claim 3 or 4, further comprising one or more selected. 前記鋼板の表面にめっき層を備えることを特徴とする請求項1〜5の何れかに記載の鋼板。 The steel plate according to claim 1, further comprising a plating layer on a surface of the steel plate. 請求項3〜5の何れかに記載の鋼組成を有する溶鋼を鋳造して鋳片とする鋳造工程、前記鋳片を熱間圧延して熱間圧延鋼板とする熱間圧延工程、前記熱間圧延鋼板を冷間圧延して冷間圧延鋼板とする冷間圧延工程、および前記冷間圧延鋼板を焼鈍して鋼板とする焼鈍工程を備える鋼板の製造方法において、前記鋳造工程における液相線温度から固相線温度の間の平均冷却速度CR(℃/秒)を下記式2を満足する範囲とし、前記熱間圧延工程における熱間圧延に供する鋳片の温度を1000〜1280℃、仕上圧延温度をAr〜1000℃、巻取温度を400〜650℃とし、前記冷間圧延工程における圧下率を50%以上とし、前記焼鈍工程における焼鈍温度を780〜900℃とすることを特徴とする鋼板の製造方法。
0.33≦(t/t)×770×CR−0.41≦10 (式2)
ここで、tは鋳片厚、tは最終の冷延鋼板厚である。
A casting process in which the molten steel having the steel composition according to any one of claims 3 to 5 is cast into a slab, a hot rolling process in which the slab is hot-rolled into a hot-rolled steel sheet, the hot In a method for producing a steel sheet comprising a cold rolling step for cold rolling a rolled steel plate to obtain a cold rolled steel plate, and an annealing step for annealing the cold rolled steel plate to obtain a steel plate, the liquidus temperature in the casting step The average cooling rate CR (° C./second) between the solidus temperature and the solidus temperature is in a range satisfying the following formula 2, and the temperature of the slab used for hot rolling in the hot rolling step is 1000 to 1280 ° C., and finish rolling. The temperature is Ar 3 to 1000 ° C., the coiling temperature is 400 to 650 ° C., the rolling reduction in the cold rolling step is 50% or more, and the annealing temperature in the annealing step is 780 to 900 ° C. A method of manufacturing a steel sheet.
0.33 ≦ (t 2 / t 1 ) × 770 × CR −0.41 ≦ 10 (Formula 2)
Here, t 1 is IhenAtsu, t 2 is the cold-rolled steel sheet thickness of the final.
前記焼鈍工程ののちに、さらにめっきを施すめっき工程を備えることを特徴とする請求項7に記載の鋼板の製造方法。 The method for manufacturing a steel sheet according to claim 7, further comprising a plating step of performing plating after the annealing step.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014028998A (en) * 2012-07-31 2014-02-13 Nippon Steel & Sumitomo Metal Cold rolled steel sheet, electrogalvanized cold rolled steel sheet, hot-dip galvanized cold rolled steel sheet and galvannealed cold rolled steel sheet having excellent deep drawability, and method of manufacturing the same
JP2020509244A (en) * 2016-12-22 2020-03-26 ポスコPosco Cold rolled steel sheet excellent in corrosion resistance and workability and method for producing the same
CN111850394A (en) * 2020-06-30 2020-10-30 邯郸钢铁集团有限责任公司 Tensile strength 830 MPa-grade hot-galvanized bundle strip steel and preparation method thereof
JPWO2023140239A1 (en) * 2022-01-21 2023-07-27

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001131692A (en) * 1999-11-05 2001-05-15 Nkk Corp High-strength cold-rolled steel sheet, high-strength galvanized steel sheet excellent in surface properties and press formability, and method for producing the same
JP2002003994A (en) * 2000-06-20 2002-01-09 Nkk Corp High strength thin steel sheet and high strength galvanized steel sheet
JP2005187939A (en) * 2003-12-05 2005-07-14 Jfe Steel Kk High-strength cold-rolled steel sheet and manufacturing method thereof
JP2006037162A (en) * 2004-07-27 2006-02-09 Sumitomo Metal Ind Ltd Hot rolled steel sheet and manufacturing method thereof
JP2006291272A (en) * 2005-04-08 2006-10-26 Sumitomo Metal Ind Ltd High-strength cold-rolled steel sheet, hot-dip galvanized steel sheet, and production method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001131692A (en) * 1999-11-05 2001-05-15 Nkk Corp High-strength cold-rolled steel sheet, high-strength galvanized steel sheet excellent in surface properties and press formability, and method for producing the same
JP2002003994A (en) * 2000-06-20 2002-01-09 Nkk Corp High strength thin steel sheet and high strength galvanized steel sheet
JP2005187939A (en) * 2003-12-05 2005-07-14 Jfe Steel Kk High-strength cold-rolled steel sheet and manufacturing method thereof
JP2006037162A (en) * 2004-07-27 2006-02-09 Sumitomo Metal Ind Ltd Hot rolled steel sheet and manufacturing method thereof
JP2006291272A (en) * 2005-04-08 2006-10-26 Sumitomo Metal Ind Ltd High-strength cold-rolled steel sheet, hot-dip galvanized steel sheet, and production method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014028998A (en) * 2012-07-31 2014-02-13 Nippon Steel & Sumitomo Metal Cold rolled steel sheet, electrogalvanized cold rolled steel sheet, hot-dip galvanized cold rolled steel sheet and galvannealed cold rolled steel sheet having excellent deep drawability, and method of manufacturing the same
JP2020509244A (en) * 2016-12-22 2020-03-26 ポスコPosco Cold rolled steel sheet excellent in corrosion resistance and workability and method for producing the same
CN111850394A (en) * 2020-06-30 2020-10-30 邯郸钢铁集团有限责任公司 Tensile strength 830 MPa-grade hot-galvanized bundle strip steel and preparation method thereof
JPWO2023140239A1 (en) * 2022-01-21 2023-07-27
WO2023140239A1 (en) * 2022-01-21 2023-07-27 日本製鉄株式会社 Cold-rolled steel sheet and manufacturing method thereof
JP7659212B2 (en) 2022-01-21 2025-04-09 日本製鉄株式会社 Cold-rolled steel sheet and its manufacturing method

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