JP3535754B2 - B-containing steel excellent in cold workability and delayed fracture resistance, its manufacturing method and bolt - Google Patents

B-containing steel excellent in cold workability and delayed fracture resistance, its manufacturing method and bolt

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Publication number
JP3535754B2
JP3535754B2 JP33781498A JP33781498A JP3535754B2 JP 3535754 B2 JP3535754 B2 JP 3535754B2 JP 33781498 A JP33781498 A JP 33781498A JP 33781498 A JP33781498 A JP 33781498A JP 3535754 B2 JP3535754 B2 JP 3535754B2
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JP
Japan
Prior art keywords
precipitates
containing steel
less
delayed fracture
fracture resistance
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
JP33781498A
Other languages
Japanese (ja)
Other versions
JPH11293401A (en
Inventor
浩 家口
英雄 畠
護 長尾
裕一 並村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kobe Steel Ltd
Original Assignee
Kobe Steel Ltd
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Filing date
Publication date
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Priority to JP33781498A priority Critical patent/JP3535754B2/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Heat Treatment Of Steel (AREA)

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、自動車等の車両用
や産業機械用として使用されるボルト等に多用されてい
るB含有鋼に関するものであり、殊に冷間加工性および
耐遅れ破壊性のいずれにも優れたB含有鋼、およびこう
したB含有鋼を製造する為の有用な方法、並びにこうし
たB含有鋼によって製造されたボルト等に関するもので
ある。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a B-containing steel which is frequently used in bolts and the like used for vehicles such as automobiles and industrial machines, and particularly to cold workability and delayed fracture resistance. And a useful method for producing such a B-containing steel, a bolt produced by such a B-containing steel, and the like.

【0002】[0002]

【従来の技術】鋼材をボルト等の部品に加工する場合に
は、熱間圧延材(熱間圧延ままの鋼材)或はその後軟化
熱処理した鋼材を冷間伸線した後に、冷間鍛造で部品形
状に成形されることが多い。更にその後、鋼材の最終の
機械的性質を満足させるという観点から、焼戻しマルテ
ンサイト組織を得る為の調質処理が施されるのが一般的
である。この様な調質処理後に良好な機械的性質を得る
には、焼入れ性が良好であることが必要であるが、C添
加量を増加したり合金元素を添加することによって焼入
れ性を向上させた場合には、熱間圧延まま材の強度が高
くなり過ぎて冷間加工性が大幅に低下する。その結果、
冷鍛前に軟化熱処理が必要となり、大きなコストアップ
の要因となる。
2. Description of the Related Art When a steel material is processed into parts such as bolts, hot-rolled material (steel material as hot-rolled) or steel material after softening heat treatment is cold-drawn and then cold-forged. Often shaped into a shape. Further, after that, from the viewpoint of satisfying the final mechanical properties of the steel material, it is common to perform a heat treatment for obtaining a tempered martensite structure. In order to obtain good mechanical properties after such heat treatment, it is necessary that the hardenability is good, but the hardenability was improved by increasing the amount of C added or adding an alloying element. In this case, the strength of the as-hot-rolled material becomes too high and the cold workability is significantly reduced. as a result,
Softening heat treatment is required before cold forging, which causes a large cost increase.

【0003】ところで硼素(B)は、少量の添加で焼入
れ性を大幅に向上させる元素であることから、鋼中のC
量を低減させても同一の焼入れ性を確保することがで
き、冷間加工性との両立を図ることが可能となるので、
近年多くの分野で使用されている。Bによる焼入れ性向
上効果を発揮させるには、BNの析出を抑制してフリー
のBとして鋼中に存在させる必要がある。その為には、
NをTiによって固定するのが最も効果的であることが
知られている。しかしながら、このように成分調整した
B含有鋼においても、冷間加工性の更なる向上を図るべ
く熱間圧延まま材の強度低下が要求されており、これま
でにも熱間圧延まま材の金属組織を制御圧延で制御する
ことによって軟質化を狙った技術が数多く提案されてい
る(例えば、特公昭61−59379号、同61−37
333号、特公平7−5960号等)。
By the way, since boron (B) is an element that greatly improves the hardenability by adding a small amount, C in steel is
Even if the amount is reduced, the same hardenability can be secured, and it is possible to achieve both cold workability and
It has been used in many fields in recent years. In order to exert the effect of improving the hardenability by B, it is necessary to suppress the precipitation of BN and to exist in the steel as free B. For that,
It is known that fixing N by Ti is the most effective. However, even in the B-containing steel whose composition has been adjusted in this way, it is required to reduce the strength of the as-hot-rolled material in order to further improve the cold workability. Many techniques aiming at softening by controlling the structure by controlled rolling have been proposed (for example, Japanese Patent Publication Nos. 61-59379 and 61-37).
333, Japanese Patent Publication No. 7-5960, etc.).

【0004】一方、B含有鋼は冷間加工性・焼入れ性が
良好であることが注目され、従来では低合金鋼が使用さ
れていた高強度ボルトに対しても、上記の様なB含有鋼
の適用が検討されている。しかしながら、B含有鋼の場
合には、調質処理中に旧オーステナイト粒径が粗大化し
易いことや、耐遅れ破壊性が低合金鋼と比較して不十分
であり、高強度ボルト用鋼として適用するには課題が残
されている。
On the other hand, it has been noted that B-containing steel has good cold workability and hardenability, and even for high-strength bolts in which low alloy steel has been used in the past, B-containing steel as described above is used. Is being considered. However, in the case of B-containing steel, the former austenite grain size is likely to coarsen during tempering and the delayed fracture resistance is insufficient compared to low alloy steel, so it is applied as a steel for high strength bolts. Challenges remain to be addressed.

【0005】本発明者らも、B含有鋼を高強度ボルト用
鋼に適用することについて様々な角度から研究を進めて
おり、B含有鋼中の析出物制御の観点から耐遅れ破壊性
の向上を図った技術を開発し、その技術的意義が認めら
れたので先に特許出願している(特願平8−19113
4号)。この技術によって耐遅れ破壊性については優れ
た特性が得られたのであるが、冷間加工性については十
分に考慮しておらず、冷間加工性と耐遅れ破壊性の両立
は達成されなかった。冷間加工性と耐遅れ破壊性の両立
を図る試みとして、例えば特開平8−60245号の技
術も提案されているが、成分バランス調整だけによって
それを達成しようとするものであることから両特性の向
上には限界があり、依然として改良の余地が残されてい
た。
The inventors of the present invention are also conducting research from various angles to apply B-containing steel to steel for high-strength bolts, and improve delayed fracture resistance from the viewpoint of controlling precipitates in B-containing steel. We have developed a technology aimed at achieving this, and since its technical significance was recognized, we applied for a patent first (Japanese Patent Application No. 8-19113).
No. 4). Although this technique provided excellent characteristics for delayed fracture resistance, cold workability was not fully considered, and cold workability and delayed fracture resistance were not achieved at the same time. . As an attempt to achieve both cold workability and delayed fracture resistance, for example, the technique of Japanese Patent Laid-Open No. 8-60245 has been proposed, but since both of these characteristics are intended to be achieved only by adjusting the component balance. There was a limit to the improvement, and there was still room for improvement.

【0006】[0006]

【発明が解決しようとする課題】本発明はこの様な状況
の下でなされたものであり、その目的は、冷間加工性と
耐遅れ破壊性を両立したB含有鋼、およびこうしたB含
有鋼を製造するための有用な方法、並びに上記したB含
有鋼からなるボルト等を提供することにある。
The present invention has been made under such circumstances, and an object thereof is a B-containing steel having both cold workability and delayed fracture resistance, and such a B-containing steel. The present invention provides a useful method for manufacturing a steel, as well as a bolt made of the B-containing steel described above.

【0007】[0007]

【課題を解決するための手段】上記目的を達成し得た本
発明のB含有鋼とは、C:0.10〜0.45%、B:
0.0003〜0.0050%、Ti:0.01〜0.
1%、N:0.0025〜0.010%を含み、 更に他の成分として、Si:0.03〜0.5%、M
n:0.3〜1.5%およびAl:0.01〜0.10
%を含有し、 残部がFeおよび不可避不純物である、 熱間圧延材また
は熱間圧延後に冷間伸線された鋼材であって、下記
(1)および(2)の少なくともいずれかの要件を満足
する点に要旨を有するものである。 (1)抽出残渣法により抽出された粒径:0.1μm超
の析出物に含まれるTi量が、鋼材中に含まれる総Ti
量の60%以上である。 (2)抽出レプリカ法による電子顕微鏡観察によって観
察される粒径:0.0 1〜0.2μmのTi系
析出物の平均個数が、25μm2 の観察視野中
において10〜500個である。
The B-containing steel of the present invention capable of achieving the above object is C: 0.10 to 0.45%, B:
0.0003-0.0050%, Ti: 0.01-0.
1%, N: 0.0025~0.010% only contains, as yet another component, Si: 0.03 to 0.5%, M
n: 0.3 to 1.5% and Al: 0.01 to 0.10.
%, With the balance being Fe and unavoidable impurities, a hot-rolled material or a steel material cold-drawn after hot-rolling, which satisfies at least one of the following requirements (1) and (2): The point is to do. (1) The amount of Ti contained in the precipitate extracted by the extraction residue method and having a particle size of more than 0.1 μm is the total Ti contained in the steel material.
It is 60% or more of the amount. (2) Particle size: 0.01 to 0.2 μm observed by electron microscope observation by the extraction replica method In the observation field of view, the average number of Ti-based precipitates is 25 μm 2.
In 10 to 500.

【0008】上記化学成分を有するB含有鋼において
は、必要に応じて下記(i) 〜(iv)の成分を含有させるこ
とも有効であり、その含有する成分の種類に応じてその
特性が更に改善される。(i) Cu:2%以下(0%を含まない)、Ni:2%以
下(0%を含まない)お よびCr:2%以下(0%
を含まない)よりなる群から選ばれる1種以上(ii) Mo:1%以下(0%を含まない)(iii) Nb:0.005〜0.1%および/またはV:
0.005〜0.3%(iv) Ca:0.0003〜0.001% また上記した要件を満足するB含有を用いて製造するこ
とによって、冷間加工性と耐遅れ破壊性が両立した高強
度ボルトが得られる。
In the B-containing steel having the above-mentioned chemical components, it is effective to include the following components (i) to (iv), if necessary, and the characteristics thereof are further improved depending on the kind of the components contained. Be improved. (i) Cu: 2% or less (not including 0%), Ni: 2% or less (not including 0%) and Cr: 2% or less (0%)
One or more selected from the group consisting of (ii) Mo: 1% or less (not including 0%) (iii) Nb: 0.005 to 0.1% and / or V:
0.005 to 0.3% (iv) Ca: 0.0003 to 0.001% Further, by using a B content that satisfies the above requirements, cold workability and delayed fracture resistance are compatible. High strength bolts can be obtained.

【0009】一方、上記目的を達成し得た本発明のB含
有鋼の製造方法とは、下記(a)〜(c)の条件を満足
させつつ操業する点に要旨を有する冷間加工性と耐遅れ
破壊に優れたB含有鋼の製造方法である。 (a)ビレット再加熱温度:950℃以上 (b)仕上げ圧延温度(すなわち最終圧延パス前または
圧延ロール群前の放射温度計で測定可能な表面の平均温
度):700〜900℃ (c)仕上げ圧延後、750℃から650℃までの平均
冷却速度:1℃/秒
On the other hand, the method for producing a B-containing steel of the present invention which has achieved the above-mentioned object is the cold workability which has the gist of operating while satisfying the following conditions (a) to (c). It is a method for producing a B-containing steel excellent in delayed fracture resistance. (A) Billet reheating temperature: 950 ° C. or higher (b) Finish rolling temperature (that is, before the final rolling pass or
Mean surface temperature measurable with a radiation thermometer in front of rolling rolls
Degree) : 700 to 900 ° C (c) After finish rolling, average cooling rate from 750 ° C to 650 ° C: 1 ° C / sec

【0010】[0010]

【発明の実施の形態】上記のようなB含有鋼において
は、焼入れ性の安定確保のためにBNの析出を抑制する
必要があり、Nを固着させるためにTiが添加されてい
る。冷間加工性の向上のためには熱間圧延まま材の強度
低下が必要であるが、Tiは鋼中でTiN、TiC或は
これらと類似の微細析出物となりマトリックスを析出強
化させることがある。冷間加工性を向上させるという観
点からすれば、こうした析出強化をできるかぎり抑制さ
せることが望ましいと言える。しかしながら、これらの
微細析出物は調質後の旧オーステナイト粒径粗大化防止
や耐遅れ破壊性の向上に有効に作用するので、全くゼロ
にすることはできない。
BEST MODE FOR CARRYING OUT THE INVENTION In the B-containing steel as described above, it is necessary to suppress the precipitation of BN in order to ensure the stable hardenability, and Ti is added to fix N. In order to improve the cold workability, it is necessary to reduce the strength of the as-hot-rolled material, but Ti may become TiN, TiC or fine precipitates similar to these in the steel, and precipitation strengthen the matrix. . From the viewpoint of improving the cold workability, it can be said that it is desirable to suppress such precipitation strengthening as much as possible. However, since these fine precipitates effectively act to prevent the coarsening of the austenite grain size after refining and to improve the delayed fracture resistance, they cannot be completely eliminated.

【0011】そこで本発明者らは、結晶粒粗大化防止や
耐遅れ破壊性向上を図りながら、熱間圧延ままの強度低
下に最適な析出物を形成させる為の形態制御を行うこと
が必要であると考え、研究開発を行った。尚従来では上
述の如く、B含有鋼において制御圧延で熱間圧延まま材
の金属組織を制御することによる軟質化を狙った技術
(前記した特公昭61−59379号、特公昭61−3
7333号、特公平7−5960号等)、或は成分バラ
ンスの調整を主に考慮して、冷間加工性と耐遅れ破壊性
の両立を図った特許(前記した特開平8−60245
号)は提案されていたが、析出物の形態制御によって軟
質化と他の特性の両立を試みた例はなかった。
Therefore, the present inventors need to perform morphology control for forming precipitates optimal for strength reduction during hot rolling, while preventing coarsening of crystal grains and improving resistance to delayed fracture. I thought there was, and conducted research and development. Conventionally, as described above, a technology aiming at softening by controlling the metallographic structure of the as-hot-rolled steel by controlled rolling in B-containing steel (the above-mentioned Japanese Patent Publication Nos. 61-59379 and 61-3).
No. 7333, Japanese Examined Patent Publication No. 7-5960, etc.), or a patent in which cold workability and delayed fracture resistance are compatible with each other mainly in consideration of adjustment of component balance (the above-mentioned JP-A-8-60245).
No.) was proposed, but there was no case where attempts were made to achieve both softening and other properties by controlling the morphology of precipitates.

【0012】ところで熱間圧延まま材の強度低下や調質
熱処理中の結晶粒粗大化防止、更には耐遅れ破壊性向上
の全てに微細析出物が影響を及ぼすが、最適な析出物形
態は特性によって異なる。まず熱間圧延まま材の強度
は、フェライト中に析出する微細整合TiCによる影響
が最も大きく、微細整合TiCが多くなると強度が上昇
する。従って、熱間圧延まま材の強度を低下させるに
は、フェライト域で析出するTiC系微細整合析出物を
抑制することが必要である。ビレット再加熱前に析出し
ていた粗大析出物を再固溶させない温度でビレットを再
加熱することで、フェライト域での析出を抑制させるこ
とができるが、この方法では後述するように結晶粒粗大
化と耐遅れ破壊性向上に有効でない。オーステナイト中
で析出する非整合析出物はそれほど強化に寄与しないの
で、この様な析出物を有効に利用することが望ましい。
By the way, the fine precipitates affect the strength reduction of the as-hot-rolled material, the prevention of crystal grain coarsening during heat treatment, and the improvement of delayed fracture resistance. Depends on First, the strength of the as-hot-rolled material is most affected by the finely matched TiC precipitated in the ferrite, and the strength increases as the amount of finely matched TiC increases. Therefore, in order to reduce the strength of the as-hot-rolled material, it is necessary to suppress the TiC-based fine matching precipitates that precipitate in the ferrite region. By reheating the billet at a temperature that does not re-dissolve the coarse precipitates that had precipitated before reheating the billet, it is possible to suppress precipitation in the ferrite region, but with this method, as described below, coarse crystal grains And not effective in improving delayed fracture resistance. Since non-coherent precipitates precipitated in austenite do not contribute to strengthening so much, it is desirable to effectively utilize such precipitates.

【0013】また調質熱処理中の結晶粒粗大化防止に
は、ビレット再加熱時に溶け込まないような粗大な析出
物ではその効果を発揮させることはできない。従って、
再固溶後に微細析出物を再析出させる必要がある。しか
し、フェライト域で析出する微細な析出物を熱間圧延ま
ま材で析出させても、その後の調質処理でオーステナイ
ト域保持中に短時間で再固溶し、或はオストワルド成長
するので、オーステナイトの低温域で析出した析出物と
比較して、結晶粒粗大化防止には効果的とは言えない。
ここでオーステナイトの低温域とは、一般的に900℃
以下のオーステナイト状態を規定し、Ae3 点以下で未
変態状態のオーステナイトも含めたものである。
Further, in order to prevent the crystal grain coarsening during the heat treatment for tempering, the effect cannot be exerted with a coarse precipitate which does not melt during reheating of the billet. Therefore,
It is necessary to reprecipitate fine precipitates after re-dissolving. However, even if a fine precipitate that precipitates in the ferrite region is precipitated in the as-hot-rolled material, it will re-dissolve in a short time during the holding of the austenite region in the subsequent tempering treatment, or it will grow in Ostwald, so austenite will grow. It cannot be said that it is effective in preventing the coarsening of crystal grains as compared with the precipitates deposited in the low temperature region.
Here, the low temperature range of austenite is generally 900 ° C.
The following austenite states are defined, and austenite in the untransformed state with Ae 3 point or less is also included.

【0014】更に、耐遅れ破壊性の向上については、T
iC系析出物を水素のトラップサイトとして利用し、有
害な拡散性水素量を減少させることが有効であることが
知られている。TiC系析出物による水素トラッピング
は、該析出物とマトリックスとの界面で起こると考えら
れているので、比表面積を増大させる析出物サイズ減少
は、トラッピング能力をアップし、耐遅れ破壊性の向上
に有効であると考えられる。しかし、耐遅れ破壊性が問
題になるのは、調質後であるので、その時点での析出物
形態が重要となる。従って、圧延後にいくら微細な析出
物を多数析出させても、オーステナイト域保持中に再固
溶、またはオストワルド成長で粗大化するので有効に利
用されない。つまり、フェライト域で析出した微細析出
物は、オーステナイト低温域で析出した析出物と比較し
て、水素トラッピングの向上は期待できない。またビレ
ット再加熱前に析出していた粗大析出物は、調質時に粗
大なまま残されるので、耐遅れ破壊性向上の効果が小さ
い。
Further, regarding the improvement of delayed fracture resistance, T
It is known that it is effective to use the iC-based precipitate as a hydrogen trap site to reduce the amount of harmful diffusible hydrogen. Since hydrogen trapping due to TiC-based precipitates is considered to occur at the interface between the precipitates and the matrix, decreasing the precipitate size that increases the specific surface area improves the trapping ability and improves delayed fracture resistance. Considered to be effective. However, delayed fracture resistance becomes a problem after refining, so the precipitate morphology at that time is important. Therefore, no matter how many fine precipitates are deposited after rolling, they are not effectively utilized because they are re-dissolved during holding the austenite region or coarsen by Ostwald ripening. That is, the fine precipitates precipitated in the ferrite region cannot be expected to improve hydrogen trapping as compared with the precipitates precipitated in the low temperature austenite region. In addition, since the coarse precipitates that have been precipitated before the billet is reheated remain coarse during tempering, the effect of improving delayed fracture resistance is small.

【0015】以上の知見に基づき、熱間圧延まま材の強
度低下、結晶粒粗大化防止、耐遅れ破壊性向上の全ての
要求を満足させるためには、オーステナイト域の低温領
域で析出する程度の大きさの析出物を多量析出させるこ
とが有効であることが判明した。具体的には、後述する
様に化学成分組成を適切に調整した熱間圧延材または熱
間圧延後の冷間伸線された鋼材において、下記(1)お
よび(2)の少なくともいずれかの要件を満足させるこ
とにより、上記した全ての要求特性を満足させ得ること
が判明した。 (1)抽出残渣法により抽出された粒径:0.1μm超
の析出物に含まれるTi量が、鋼材中に含まれる総Ti
量の60%以上である。 (2)抽出レプリカ法による電子顕微鏡観察によって観
察される粒径:0.01〜0.2μmのTi系析出物の
平均個数が、25μm2 の観察視野中において10〜5
00個である。
Based on the above findings, in order to satisfy all the requirements of strength reduction of the as-hot-rolled material, prevention of crystal grain coarsening, and improvement of delayed fracture resistance, precipitation in the low temperature region of the austenite region is sufficient. It has been found that it is effective to deposit a large amount of precipitates. Specifically, in a hot-rolled material whose chemical composition has been appropriately adjusted as described below or a cold-drawn steel material after hot-rolling, at least one of the following requirements (1) and (2) It has been found that all the required characteristics described above can be satisfied by satisfying the above. (1) The amount of Ti contained in the precipitate extracted by the extraction residue method and having a particle size of more than 0.1 μm is the total Ti contained in the steel material.
It is 60% or more of the amount. (2) Particle size observed by electron microscope observation by the extraction replica method: 0.01 to 0.2 μm The average number of Ti-based precipitates is 10 to 5 in the observation field of 25 μm 2.
It is 00.

【0016】次に、上記(1),(2)の要件の限定理
由について説明する。固溶Ti或はフェライト域で析出
する超微細析出物は、孔径:0.1μmのフィルターを
通過するので、抽出残渣法では測定できない。従って、
抽出残渣法で抽出された析出物中のTi量は、ビレット
再加熱時に再固溶しなかった粗大析出物とオーステナイ
ト相で新たに析出した析出物に固定されているTi量の
総和である。このTi量が、鋼材中に含まれる総Ti量
の60%未満では、フェライト中に微細なTi系析出物
が多数析出することを示しており、圧延ままの強度が高
くなる。より好ましくは、80%以上とするのが良い。
尚ここで対象とする粒径:0.1μm超の析出物とは、
Ti系析出物は勿論のこと、Ti系でない析出物(Ti
を含まない析出物)をも含めた意味である。これは、抽
出残渣法では、Tiを含まない析出物(例えば、セメン
タイト)だけを分離することが難しいからである。
Next, the reasons for limiting the requirements (1) and (2) will be described. Ultrafine precipitates that precipitate in the solid solution Ti or ferrite region cannot be measured by the extraction residue method because they pass through a filter having a pore size of 0.1 μm. Therefore,
The amount of Ti in the precipitate extracted by the extraction residue method is the sum of the amount of Ti fixed in the coarse precipitate that has not been re-dissolved during billet reheating and the precipitate that is newly precipitated in the austenite phase. If the amount of Ti is less than 60% of the total amount of Ti contained in the steel material, it indicates that a large number of fine Ti-based precipitates are precipitated in the ferrite, and the as-rolled strength is increased. More preferably, it is 80% or more.
In addition, the target particle size: a precipitate having a particle size of more than 0.1 μm is
Not only Ti-based precipitates but also non-Ti-based precipitates (Ti
It is also meant to include precipitates not containing). This is because it is difficult to separate only Ti-free precipitates (for example, cementite) by the extraction residue method.

【0017】オーステナイト域で析出するTi系析出物
のサイズは、粒径が0.01〜0.2μmとなる。粒径
が0.01μm未満のTi系析出物は、主にフェライト
域で析出する整合析出物であり、熱間圧延まま材の強度
を上げるので問題となる。また粒径が0.2μmを超え
る様な析出物は、結晶粒粗大化防止や耐遅れ破壊性向上
に寄与しない。こうしたことから、粒径が0.01μm
以上、0.2μm以下のTi系析出物を多数析出させる
ことが熱間圧延まま材の強度低下、結晶粒粗大化防止、
並びに耐遅れ破壊性向上の全てを満足させるのに有効で
ある。こうした効果と発揮させる為には、粒径が上記の
範囲にあるTi系析出物が、25μm2の観察視野中に
おいて平均個数で10個以上含有させる必要がある。こ
のTi系析出物の平均個数は、より望ましくは20個以
上とするのが良い。
The size of the Ti-based precipitate that precipitates in the austenite region is 0.01 to 0.2 μm. A Ti-based precipitate having a grain size of less than 0.01 μm is a coherent precipitate that mainly precipitates in the ferrite region, and raises the strength of the as-hot-rolled material, which poses a problem. Further, a precipitate having a grain size of more than 0.2 μm does not contribute to prevention of crystal grain coarsening or improvement of delayed fracture resistance. Therefore, the particle size is 0.01 μm
As described above, depositing a large number of Ti-based precipitates having a size of 0.2 μm or less prevents the strength of the as-hot-rolled material from decreasing and prevents the crystal grains from coarsening.
In addition, it is effective in satisfying all of the improvement of delayed fracture resistance. In order to exert such an effect, it is necessary to contain 10 or more Ti-based precipitates having a grain size within the above range on average in the observation visual field of 25 μm 2 . More preferably, the average number of Ti-based precipitates is 20 or more.

【0018】一方、平均個数の上限を500個としたの
は、これ以上の析出物数を得るにはTi添加量が多量に
必要になり、靱性等に悪影響を及ぼす可能性があるこ
と、およびTi添加の効率が悪くなるので、これを上限
とした。尚Ti系析出物数の好ましい上限は、平均個数
で300個である。
On the other hand, the upper limit of the average number is set to 500, because a large amount of Ti must be added to obtain a larger number of precipitates, which may adversely affect toughness and the like. Since the efficiency of Ti addition becomes poor, this was made the upper limit. The preferable upper limit of the number of Ti-based precipitates is 300 on average.

【0019】本発明で対象とするTi系析出物とは、例
えばTiC,TiN,TiS,Ti 422 およびこ
れらの複合析出物、並びにこれらにNb,Mo,V等が
一部含まれた析出物の総称である。また本発明で「Ti
系析出物」と規定した理由は、下記(I)〜(III) に示す
通りである。 (I) Ti系析出物は、CとNの両方を個々の析出物で異
なった量で含有するTi(C,N)となっていることが
多いが、CとNの分離が困難であること、(II)Nb,M
o,V等と複合した析出物も、Tiを主成分としている
限り、特性に及ぼす影響はNbやVが含むまれない析出
物と大きな相違がなく、Ti系と称しても良いこと、(I
II) 上述したいくつかの析出物は、その種類で析出する
温度領域が異なるが、サイズ領域はオーバーラップする
ことがあり、特性に及ぼす影響では同一サイズでは特に
分離して考える必要がない。
Examples of the Ti-based precipitates that are the subject of the present invention include
For example TiC, TiN, TiS, Ti Four C2 S2 Toko
These composite precipitates, as well as Nb, Mo, V, etc.
It is a generic term for some of the precipitates included. Further, in the present invention, "Ti
The reasons for defining "system precipitates" are shown in (I) to (III) below.
On the street. (I) Ti-based precipitates differ in both C and N due to individual precipitates.
Ti (C, N) contained in the amount
Many, but it is difficult to separate C and N, (II) Nb, M
The precipitate compounded with o, V, etc. also has Ti as the main component.
As long as it has no influence on the characteristics, it does not contain Nb or V
There is no big difference with the product, and it may be called Ti system, (I
II) Some of the above-mentioned precipitates are deposited in that type.
Temperature regions are different, but size regions overlap
The same size may affect the characteristics.
There is no need to think separately.

【0020】以上の様な観点から析出物を析出させなが
ら、全ての要求特性を満足させるのに必要な本発明鋼の
化学成分組成の規定限定理由を次に示す。
From the above viewpoints, the reasons for limiting the definition of the chemical composition of the steel of the present invention necessary for satisfying all the required properties while precipitating the precipitates are shown below.

【0021】C:0.10〜0.45% Cは、強度付与に有効な元素であり、こうした効果を発
揮させる為には0.10%以上含有させる必要がある。
しかしながら、過剰に含有させると焼入れ後の靱性が低
下するので、0.45%以下にする必要がある。尚C含
有量の好ましい下限は0.15%であり、好ましい上限
は0.40%である。
C: 0.10 to 0.45% C is an element effective in imparting strength, and in order to exert such effects, it is necessary to contain C by 0.10% or more.
However, if it is contained excessively, the toughness after quenching decreases, so 0.45% or less is necessary. The preferable lower limit of the C content is 0.15%, and the preferable upper limit is 0.40%.

【0022】B:0.0003〜0.0050% Bは微量の添加で焼入れ性を向上させる効果がある。こ
うした効果を発揮させる為には、0.0003%以上含
有させる必要がある。しかしながら、過剰に含有させる
と、その効果が飽和するばかりか靱性や加工性が劣化す
るので0.0050%以下にする必要がある。尚B含有
量の好ましい下限は0.0005%であり、好ましい上
限は0.002%である。
B: 0.0003 to 0.0050% B has the effect of improving the hardenability by adding a trace amount. In order to exert such effects, it is necessary to contain 0.0003% or more. However, if it is contained excessively, not only the effect is saturated but also the toughness and workability are deteriorated, so it is necessary to make it 0.0050% or less. The preferable lower limit of the B content is 0.0005%, and the preferable upper limit thereof is 0.002%.

【0023】Ti:0.01〜0.1% TiはBの焼入れ性効果を確保する為に必要な元素であ
る。また結晶粒微細化や耐遅れ破壊性の向上に有効な元
素である。こうした効果を発揮させる為には、少なくと
も0.01%以上含有させる必要がある。しかしなが
ら、過剰に含有させるとTi系析出物が粗大化し、靱性
や疲労強度に悪影響を及ぼす可能性があること、および
熱間圧延まま材の強度が増加する可能性があるので、そ
の含有量は0.1%以下にする必要がある。尚Ti含有
量の好ましい下限は0.025%であり、好ましい上限
は0.07%である。
Ti: 0.01 to 0.1% Ti is an element necessary for ensuring the hardenability effect of B. Further, it is an element effective for refining crystal grains and improving delayed fracture resistance. In order to exert such effects, it is necessary to contain at least 0.01% or more. However, if it is contained excessively, Ti-based precipitates are coarsened, which may adversely affect toughness and fatigue strength, and the strength of the as-hot-rolled material may increase. It should be 0.1% or less. The preferable lower limit of the Ti content is 0.025%, and the preferable upper limit thereof is 0.07%.

【0024】N:0.0025〜0.010% Nは、Bによる焼入れ性向上効果を確保させる為にはで
きるだけ少ない方が良い。また多過ぎると粒径の大きい
TiNが形成し易くなり、鋼材の靱性や疲労強度に悪影
響を及ぼす可能があるので、上限を0.010%とする
必要がある。しかしながら、Nの含有量が0.0025
%未満では、微細なTiC系析出物がフェライト域で多
数発生し、熱間圧延まま材の強度が高くなるので、これ
を下限とした。尚N含有量の好ましい下限は0.004
0%であり、好ましい上限は0.0070%である。
N: 0.0025 to 0.010% N is preferably as small as possible in order to secure the hardenability improving effect of B. On the other hand, if the amount is too large, TiN having a large grain size is likely to be formed, which may adversely affect the toughness and fatigue strength of the steel material. Therefore, the upper limit needs to be 0.010%. However, the N content is 0.0025
If it is less than%, a large number of fine TiC-based precipitates are generated in the ferrite region, and the strength of the as-hot-rolled material increases, so this was made the lower limit. The preferable lower limit of the N content is 0.004.
It is 0%, and the preferable upper limit is 0.0070%.

【0025】本発明のB含有鋼の基本的な化学成分組成
は上記の通りであり、残部はFeおよび不可避不純物で
あるが、必要よってSi,Mn,Al,Cu,Ni,C
r,Mo,Nb,V,Ca等の合金元素を添加すること
も有効である。これらの元素を添加するときの成分限定
理由は、下記の通りである。尚本発明のB含有鋼には、
これら以外にもB含有鋼の特性を阻害しない程度の微量
成分を含み得るものであり、こうしたB含有鋼も本発明
の技術的範囲に含まれるものである。
The basic chemical composition of the B-containing steel of the present invention is as described above, the balance being Fe and unavoidable impurities, but if necessary Si, Mn, Al, Cu, Ni, C
It is also effective to add alloying elements such as r, Mo, Nb, V and Ca. The reasons for limiting the components when adding these elements are as follows. The B-containing steel of the present invention includes
In addition to these, trace amounts of components that do not impair the characteristics of B-containing steel may be contained, and such B-containing steel is also included in the technical scope of the present invention.

【0026】Si:0.03〜0.5% Siは脱酸剤として有効であり、その効果を発揮させる
為には0.03%以上含有させる必要がある。しかしな
がら、過剰に含有させると延性や冷間加工性が悪くなる
ので、0.5%以下とする必要がある。尚Si含有量の
好ましい下限は0.05%であり、好ましい上限は0.
40%である。
Si: 0.03 to 0.5% Si is effective as a deoxidizer, and it is necessary to contain Si in an amount of 0.03% or more in order to exert its effect. However, if it is contained excessively, ductility and cold workability deteriorate, so it is necessary to set it to 0.5% or less. The preferable lower limit of the Si content is 0.05%, and the preferable upper limit is 0.1.
40%.

【0027】Mn:0.3〜1.5% Mnは、脱酸、脱硫剤および焼入れ性向上元素として有
効であり、その効果を発揮させる為には0.3%以上含
有させる必要がある。しかしながら、過剰に含有させる
と偏析による組織の不均一が生じ、焼入れ後の靱性低下
や、冷間加工性の低下が生じるので、1.5%以下とす
る必要がある。尚Mn含有量の好ましい下限は0.5%
であり、好ましい上限は1.2%である。
Mn: 0.3 to 1.5% Mn is effective as a deoxidizing agent, a desulfurizing agent and an element for improving hardenability, and 0.3% or more is required to exert its effect. However, if it is contained excessively, the structure becomes nonuniform due to segregation, and the toughness after quenching and the cold workability deteriorate. Therefore, it is necessary to set it to 1.5% or less. The preferable lower limit of the Mn content is 0.5%.
And the preferable upper limit is 1.2%.

【0028】Al:0.01〜0.10% Alは、脱硫剤として有効であり、またAlNとしてN
を固定する効果も発揮する。これらの効果を発揮させる
為には、Alは0.01%以上含有させる必要がある。
しかしながら、過剰に含有させると却って靱性を阻害す
るので、0.10%以下とする必要がある。尚Al含有
量の好ましい下限は0.015%であり、好ましい上限
は0.06%である。
Al: 0.01 to 0.10% Al is effective as a desulfurizing agent, and N is used as AlN.
Also exerts the effect of fixing. In order to exert these effects, Al needs to be contained by 0.01% or more.
However, if it is contained excessively, the toughness is adversely affected, so it is necessary to set it to 0.10% or less. The preferable lower limit of the Al content is 0.015%, and the preferable upper limit is 0.06%.

【0029】Cu:2%以下(0%を含まない)、N
i:2%以下(0%を含まない)およびCr:2%以下
(0%を含まない)よりなる群から選択される1種以上 これらの元素は、焼入れ性向上と耐食性向上による耐遅
れ破壊性の向上に有効な元素である。しかしながら、多
量に添加すると熱間圧延まま材の強度が高くなり過ぎる
ので、いずれも2%以下にする必要がある。
Cu: 2% or less (not including 0%), N
i: 1% or more selected from the group consisting of 2% or less (not including 0%) and Cr: 2% or less (not including 0%) These elements are delayed fracture resistant due to improvement in hardenability and corrosion resistance. It is an element effective in improving the properties. However, if added in a large amount, the strength of the as-hot-rolled material becomes too high, so it is necessary to make it 2% or less in all cases.

【0030】Mo:1%以下(0%を含まない) Moは、焼入れ性向上に有効な元素であるが、多量に添
加すると熱間圧延まま材の強度が高くなり過ぎるので、
1%以下にする必要がある。
Mo: 1% or less (not including 0%) Mo is an element effective for improving hardenability, but if added in a large amount, the strength of the as-hot-rolled material becomes too high.
It should be 1% or less.

【0031】Nb:0.005〜0.1%および/また
はV:0.005〜0.3% NbとVは、結晶粒の微細化や耐遅れ破壊性の向上に有
効な元素であり、こうした効果を発揮させる為には、い
ずれも0.005%以上含有させる必要がある。しかし
ながら、過剰に添加すると熱間圧延まま材の強度が必要
以上に高くなるので、Nbで0.1%以下、Vで0.3
%以下にする必要がある。
Nb: 0.005 to 0.1% and / or V: 0.005 to 0.3% Nb and V are elements effective for refining crystal grains and improving delayed fracture resistance. In order to exert such an effect, it is necessary to contain 0.005% or more in each case. However, if added excessively, the strength of the as-hot-rolled material becomes unnecessarily high, so Nb is 0.1% or less and V is 0.3% or less.
Must be less than or equal to%.

【0032】Ca:0.0003〜0.001% Caは、硫化物系介在物の形態制御(例えば、特開昭5
8−84960号)やCaxy の生成(例えば、特開
平6−212345号)に有効であることは知られてい
るが、これらの効果以外にも電子を放出して回りの鉄同
士の結合力を高める効果があり、これによって粒界の結
合力を高めて水素脆性を抑制する効果を発揮する。また
水素トップサイトとなる析出物の形態を制御することに
よって、耐遅れ破壊性を向上させるのにも寄与する。こ
れらの効果を発揮させるためには、Ca含有量は0.0
003%以上とする必要があるが、過剰になると粗大な
介在物が生成し、却って遅れ破壊性を劣化させるので
0.001%以下にする必要がある。
Ca: 0.0003 to 0.001% Ca controls the morphology of sulfide-based inclusions (see, for example, Japanese Patent Laid-Open No.
8-84960) and Ca x P y generation (for example, JP-A-6-212345), but in addition to these effects, electrons are emitted to cause the surrounding iron It has the effect of increasing the bond strength, and thereby exerts the effect of increasing the bond strength at the grain boundaries and suppressing hydrogen embrittlement. Further, by controlling the morphology of precipitates which become hydrogen top sites, it contributes to improve delayed fracture resistance. In order to exert these effects, the Ca content is 0.0
The content must be 003% or more, but if it becomes excessive, coarse inclusions will be generated, which will rather deteriorate the delayed fracture property, so it must be 0.001% or less.

【0033】次に、本発明の製造方法について説明す
る。本発明のB含有鋼を製造するに当たっては、下記の
(a)〜(c)の条件を満足させつつ操業する必要があ
るが、これらの条件を設定した理由は下記の通りであ
る。 (a)ビレット再加熱温度:950℃以上 (b)仕上げ圧延温度:700〜900℃ (c)仕上げ圧延後、750℃から650℃までの平均
冷却速度:1℃/秒以下
Next, the manufacturing method of the present invention will be described. In producing the B-containing steel of the present invention, it is necessary to operate while satisfying the following conditions (a) to (c), and the reason for setting these conditions is as follows. (A) Billet reheating temperature: 950 ° C or higher (b) Finish rolling temperature: 700 to 900 ° C (c) After finish rolling, average cooling rate from 750 ° C to 650 ° C: 1 ° C / sec or less

【0034】結晶粒粗大化防止や耐遅れ破壊性向上に必
要な量のTi系析出物をオーステナイトの低温域で析出
させる為には、まずTiをオーステナイト域に固溶させ
る必要がある。その為には、ビレットの再加熱温度を9
50℃以上とする必要がある。この温度が950℃未満
では、固溶量が不十分であり、それまでに存在していた
大型析出物だけとなり、望んでいるサイズのTi系析出
物が生成されなくなる。この温度は、好ましくは100
0℃以上とするのが良い。
In order to precipitate Ti-based precipitates in an amount necessary for preventing crystal grain coarsening and improving delayed fracture resistance in a low temperature range of austenite, it is first necessary to form a solid solution of Ti in the austenite range. To do this, set the billet reheating temperature to 9
It is necessary to set the temperature to 50 ° C or higher. If this temperature is lower than 950 ° C., the amount of solid solution is insufficient, and only the large-scale precipitates that have existed up to that point are formed, and Ti-based precipitates of the desired size are not formed. This temperature is preferably 100
It is better to set it to 0 ° C or higher.

【0035】次に、Ti系析出物をオーステナイト域で
析出させる必要がある。Ti系析出物のオーステナイト
域での析出は、一般的にかなりの長時間を要するが、析
出の核となるオーステナイト結晶粒界の面積増大、即ち
オーステナイト結晶粒微細化と、残留歪を残した状態に
させることで、実用上十分な時間で析出させることがで
きる。オーステナイト結晶粒微細化と残留歪の残存の為
には、仕上げ圧延温度の低減が必要であり、こうした観
点からその上限を900℃とした。900℃を超える温
度では、オーステナイト結晶粒が粗大化し、かつ残留歪
も残存しないので、オーステナイト域でのTi系析出物
が析出しない。しかしながら、低温過ぎると、圧延荷重
の増大や表面疵の発生増大があり、非現実的となるので
その下限を700℃とした。ここで、仕上げ圧延温度と
は、最終圧延パス前または圧延ロール群前の放射温度計
で測定可能な表面の平均温度とした。
Next, it is necessary to precipitate Ti-based precipitates in the austenite region. Precipitation of Ti-based precipitates in the austenite region generally takes a considerably long time, but the area of the austenite crystal grain boundaries, which is the nucleus of precipitation, increases, that is, the austenite crystal grains are refined and residual strain remains. By setting it to, it is possible to deposit in a practically sufficient time. In order to refine the austenite grains and to leave residual strain, it is necessary to reduce the finish rolling temperature. From this viewpoint, the upper limit was set to 900 ° C. At temperatures above 900 ° C., austenite crystal grains become coarse and residual strain does not remain, so that Ti-based precipitates in the austenite region do not deposit. However, if the temperature is too low, the rolling load increases and the surface flaws increase, which becomes unrealistic. Therefore, the lower limit is set to 700 ° C. Here, the finish rolling temperature is the average temperature of the surface that can be measured by the radiation thermometer before the final rolling pass or before the group of rolling rolls.

【0036】尚B含有鋼の製造方法として、特開平8−
60245号の方法も提案されているが、この方法は冷
間加工性を向上させる為に、仕上げ圧延温度を900℃
以上と規定したものである。そしてこの要件は、仕上げ
圧延温度が900℃よりも低くなると、微細組織となっ
て強度が高くなり、冷間加工性が悪くなると説明してい
る。これに対し本発明では、Ti析出物を積極的に利用
することによって、軟質化だけでなく結晶粒粗大化防止
と耐遅れ破壊性向上を狙ったものであり、こうした観点
から加熱温度を規定している。またこの温度範囲では、
仕上げ圧延温度低下による強度増大効果は確かにある
が、本発明で記述した析出物制御による軟質化の方が効
果は大きく、トータルとしては仕上げ圧延温度を700
〜900℃の範囲とすることの方が効果が大きいことが
判明した。
As a method for producing B-containing steel, Japanese Patent Laid-Open No. 8-
Although the method of No. 60245 has also been proposed, this method has a finish rolling temperature of 900 ° C. in order to improve cold workability.
It is defined as above. This requirement explains that when the finish rolling temperature is lower than 900 ° C., the structure becomes a fine structure, the strength is increased, and the cold workability is deteriorated. On the other hand, the present invention aims to prevent not only softening but also crystal grain coarsening and improvement of delayed fracture resistance by positively utilizing Ti precipitates, and the heating temperature is regulated from such a viewpoint. ing. Also in this temperature range,
There is certainly an effect of increasing the strength by lowering the finish rolling temperature, but the effect of softening by controlling the precipitate described in the present invention is more significant, and the total finishing rolling temperature is 700
It was found that the effect is greater when the temperature is in the range of up to 900 ° C.

【0037】本発明では、仕上げ圧延後、750℃から
650℃までの平均冷却速度を1℃/秒以下とする必要
があるが、これはオーステナイト域でのTi析出物の析
出を促進させる為に十分な時間を確保するためである。
特性向上に重要となるサイズ領域の析出は、750〜6
50℃で起こるので、この領域での冷却速度が特に重要
になる。仕上げ温度から750℃までの冷却は、微細オ
ーステナイト結晶粒の粗大化防止の為に急冷した方が良
いが、Ti析出物の析出を促進させる為にこの領域も徐
冷しても良い。尚仕上げ圧延温度を規定の最低である7
00℃で圧延すると、加工発熱によって750℃程度ま
で素材温度が上昇する。また650℃よりも下がると、
オーステナイトの半分以上が変態を終了するので、徐冷
を打ち切っても良い。
In the present invention, after finish rolling, the average cooling rate from 750 ° C. to 650 ° C. is required to be 1 ° C./sec or less. This is to accelerate the precipitation of Ti precipitates in the austenite region. This is to secure sufficient time.
The precipitation in the size region, which is important for improving the characteristics, is 750 to 6
Since it occurs at 50 ° C, the cooling rate in this region becomes particularly important. Cooling from the finishing temperature to 750 ° C. should be rapidly cooled to prevent coarsening of fine austenite crystal grains, but this region may also be gradually cooled to promote precipitation of Ti precipitates. The finish rolling temperature is the specified minimum 7
When rolled at 00 ° C, the temperature of the material rises up to about 750 ° C due to heat generated during processing. Also, if the temperature drops below 650 ° C,
Since more than half of the austenite finishes transformation, slow cooling may be discontinued.

【0038】以下本発明を実施例によって更に詳細に説
明するが、下記実施例は本発明を限定する性質のもので
はなく、前・後記の趣旨に徴して設計変更することはい
ずれも本発明の技術的範囲に含まれるものである。
The present invention will be described in more detail with reference to the following examples, but the following examples are not intended to limit the present invention, and any change in the design of the present invention can be made without departing from the spirit of the preceding and the following. It is included in the technical scope.

【0039】[0039]

【実施例】実施例1 下記表1に示す化学成分組成の供試材を準備し、直径:
13mmの線材に圧延した。ビレット再加熱温度を10
50℃、仕上げ圧延温度を800±30℃になるように
調整して圧延し、その後750℃の温度になるまで水冷
し、コンベアに搭載した。コンベア上で650℃までの
範囲を冷却速度が比較的速いコイル疎部での平均冷却速
度が0.8℃/sとなるように冷却した。この圧延後に
引張り試験を実施した。その結果(引張り強度TS)も
表1に併記する。
Example 1 A sample material having the chemical composition shown in Table 1 below was prepared, and the diameter:
It was rolled into a 13 mm wire. Billet reheat temperature 10
It was rolled at 50 ° C. and the finish rolling temperature was adjusted to 800 ± 30 ° C., then water-cooled to a temperature of 750 ° C., and mounted on a conveyor. The range up to 650 ° C. was cooled on the conveyor so that the average cooling rate in the coil sparse part where the cooling rate was relatively high was 0.8 ° C./s. A tensile test was performed after this rolling. The results (tensile strength TS) are also shown in Table 1.

【0040】[0040]

【表1】 [Table 1]

【0041】サンプルを遅れ破壊試験片に機械加工後、
870℃で30分間加熱して、油焼入れした。その後、
120分の焼戻し処理を行ったが、焼戻し温度は引張り
強度TSが135kgf/mm2 となるように調整し
た。焼入れ・焼戻し後の旧オーステナイト粒径をJIS
で規定される方法(JIS G 0551)で測定し
た。耐遅れ破壊性は、応力集中係数αが10の切り欠き
付き促進式の定荷重引張り試験を水中で行った。そし
て、100時間経過しても破断しない強度を遅れ破壊強
度とした。
After machining the sample into a delayed fracture test piece,
It was heated at 870 ° C. for 30 minutes and oil-quenched. afterwards,
Although tempering treatment was performed for 120 minutes, the tempering temperature was adjusted so that the tensile strength TS was 135 kgf / mm 2 . JIS the austenite grain size after quenching and tempering
It was measured by a method (JIS G 0551) specified by For the delayed fracture resistance, a notched acceleration constant load tensile test with a stress concentration factor α of 10 was performed in water. Then, the strength that does not fracture even after 100 hours has passed is defined as the delayed fracture strength.

【0042】その結果を、析出物の測定結果と共に下記
表2に示す。尚析出物のサイズや量の測定は熱間圧延ま
ま材で実施した。またTi系析出物中に含まれるTi量
の測定、析出物数の測定および析出物の観察は下記の方
法によった。
The results are shown in Table 2 below together with the measurement results of the precipitates. The size and amount of the precipitates were measured on the as-hot-rolled material. Further, the measurement of the amount of Ti contained in the Ti-based precipitate, the measurement of the number of precipitates, and the observation of the precipitates were carried out by the following methods.

【0043】〈析出物中に含まれるTi量の測定〉0.
1μm超の析出物中に含まれるTi量の測定には、抽出
残渣法を利用した。一般的に使用される電解抽出法によ
り、鋼材試料1.0gから析出物を抽出し、0.1μm
のフィルターで回収した。回収した析出物中のTi質量
{Ti}(g)をICP法により分析した。また鋼材中
に含まれる総Ti量[Ti](質量%)に対する割合A
(%)は、下記(1)式で評価した。 A(%)=〔(100/{Ti})/[Ti]〕×100 …(1)
<Measurement of Ti content in precipitate> 0.
The extraction residue method was used to measure the amount of Ti contained in the precipitates having a size of more than 1 μm. Precipitate was extracted from 1.0 g of a steel material sample by a commonly used electrolytic extraction method to obtain 0.1 μm
It was collected by the filter of. The Ti mass {Ti} (g) in the recovered precipitate was analyzed by the ICP method. Further, the ratio A to the total Ti amount [Ti] (mass%) contained in the steel material
(%) Was evaluated by the following formula (1). A (%) = [(100 / {Ti}) / [Ti]] × 100 (1)

【0044】〈析出物数の測定〉 Ti系析出物:視野25μm2 中に観察される0.01
〜0.2μmの大きさのTi系析出物の個数を測定し
た。
<Measurement of the number of precipitates> Ti-based precipitates: 0.01 observed in a visual field of 25 μm 2.
The number of Ti-based precipitates having a size of ˜0.2 μm was measured.

【0045】〈析出物の観察〉析出物の観察は、抽出レ
プリカ・電子顕微鏡によった。この方法は、例えば「鉄
鋼便覧IV:鉄鋼材料、試験・分析」(第3版、昭和5
6年、丸善発行、第395〜399頁)に記載されてい
る方法である。サンプルについては、その表層部が脱炭
等による析出物の形態変化の可能性があるので、それを
避ける為に表層部から0.3mmの位置から採取した。
電子顕微鏡観察は、加速電圧:200kVで観察すると
共に、EDX(エネルギー分散型半導体検出器)による
組織同定を行った。写真撮影は1500倍の倍率で行
い、写真上で大きさの測定を行った。このときTi以外
にも、Nb,Mo,V等が含まれる析出物においては、
EDXでの測定によってTiの強度が最も高いと認めら
れれば、Ti系析出物と判断した。
<Observation of Precipitates> Observation of the precipitates was performed by an extraction replica / electron microscope. This method is described, for example, in "Steel Manual IV: Steel Materials, Testing and Analysis" (3rd edition, Showa 5).
6th year, published by Maruzen, pp. 395-399). As for the sample, there is a possibility that the surface layer of the sample may change the morphology of the precipitate due to decarburization, so in order to avoid it, the sample was taken from a position 0.3 mm from the surface layer.
The electron microscope observation was performed at an accelerating voltage of 200 kV, and the tissue was identified by EDX (energy dispersive semiconductor detector). The photograph was taken at a magnification of 1500 times, and the size was measured on the photograph. At this time, in addition to Ti, in precipitates containing Nb, Mo, V, etc.,
If the strength of Ti was found to be the highest as measured by EDX, it was determined to be a Ti-based precipitate.

【0046】[0046]

【表2】 [Table 2]

【0047】これらの結果から、次の様に判断できる。
圧延まま材の引張り強度TSを前記表1に、熱処理後の
結晶粒度番号と遅れ破壊強度を表2に示したが、本発明
で規定する要件のいずれかを欠く比較鋼では全ての要求
特性を満足することができない。例えば、No.23,
24,27,28,31〜34のものは、圧延まま材の
引張り強度が高い(冷間加工性が悪い)。またNo.2
2,25,26,29,30〜34のものは、遅れ破壊
強度が不十分である。特に、No.25のものは、Bを
添加していないものであり、焼入れ性が不足しており、
熱処理後の強度も不十分であった。またNo.30のも
のは、焼入れ強度が135kgf/mm2 に到らない。
From these results, it can be judged as follows.
The tensile strength TS of the as-rolled material is shown in Table 1 above, and the grain size number and delayed fracture strength after heat treatment are shown in Table 2. However, in the comparative steel lacking any of the requirements specified in the present invention, all the required properties are shown. I can't be satisfied. For example, No. 23,
Those of 24, 27, 28, 31 to 34 have high tensile strength of the as-rolled material (poor cold workability). In addition, No. Two
Nos. 2, 25, 26, 29, and 30 to 34 have insufficient delayed fracture strength. In particular, No. No. 25 does not have B added and has insufficient hardenability,
The strength after heat treatment was also insufficient. In addition, No. The hardness of 30 is less than 135 kgf / mm 2 .

【0048】これらに対し、本発明で規定する要件の全
てを満足する本発明鋼(No.1〜21)では、いずれ
の特性も良好であることが分かる。
On the other hand, in the steels of the present invention (Nos. 1 to 21) satisfying all the requirements specified in the present invention, it is understood that all the properties are good.

【0049】実施例2 圧延条件の影響を調査する為の実験を行った。このとき
の実験条件を下記表3に示す。実施材としては、前記表
1のNo.1と同一チャージを行い、圧延条件のみを変
更した。また遅れ破壊性などの実験条件、析出物の測定
条件は実施例1と同様にした。
Example 2 An experiment was conducted to investigate the influence of rolling conditions. The experimental conditions at this time are shown in Table 3 below. As the working material, No. 1 in Table 1 was used. The same charge as 1 was performed, and only the rolling conditions were changed. The experimental conditions such as delayed fracture property and the measurement conditions of precipitates were the same as in Example 1.

【0050】その結果を下記表3に併記するが、本発明
方法で規定する製造条件を満足するものは、Ti系析出
物数が多く、熱処理後の結晶の微細化(粒度番号が大き
くなる)が達成され、遅れ破壊強度も高いことが分か
る。
The results are also shown in Table 3 below, and those satisfying the manufacturing conditions specified by the method of the present invention have a large number of Ti-based precipitates and have finer crystals after heat treatment (the particle size number increases). It can be seen that the delayed fracture strength is high.

【0051】[0051]

【表3】 [Table 3]

【0052】[0052]

【発明の効果】本発明は以上の様に構成されており、冷
間加工性と耐遅れ破壊性の両特性を満足することのでき
るB含有鋼が実現でき、このB含有鋼を用いれば上記両
特性に優れた高強度ボルトが実現できる。
EFFECTS OF THE INVENTION The present invention is constituted as described above, and it is possible to realize a B-containing steel which can satisfy both the characteristics of cold workability and delayed fracture resistance. A high-strength bolt with excellent properties can be realized.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 並村 裕一 神戸市灘区灘浜東町2番地 株式会社神 戸製鋼所 神戸製鉄所内 (56)参考文献 特開 平4−228519(JP,A) 特開 昭58−84960(JP,A) 特開 平11−92868(JP,A) 特開 平11−43737(JP,A) (58)調査した分野(Int.Cl.7,DB名) C22C 1/00 - 49/14 C21D 8/06 F16B 35/00 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Yuichi Namimura, 2 Nadahama Higashi-cho, Nada-ku, Kobe City Kamido Steel Works, Ltd. Inside the Kobe Steel Works (56) Reference JP-A-4-28519 (JP, A) 58-84960 (JP, A) JP-A-11-92868 (JP, A) JP-A-11-43737 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) C22C 1 / 00-49/14 C21D 8/06 F16B 35/00

Claims (7)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 C:0.10〜0.45%(質量%の意
味、以下同じ)、B:0.0003〜0.0050%、
Ti:0.01〜0.1%、N:0.0025〜0.0
10%を含み、 更に他の成分として、Si:0.03〜0.5%、M
n:0.3〜1.5%およびAl:0.01〜0.10
%を含有し、 残部がFeおよび不可避不純物である、 熱間圧延材また
は熱間圧延後に冷間伸線された鋼材であって、下記
(1)および(2)の少なくともいずれかの要件を満足
するものであることを特徴とする冷間加工性と耐遅れ破
壊性に優れたB含有鋼。(1)抽出残渣法により抽出さ
れた粒径:0.1μm超の析出物に含まれるTi量が、 鋼材中に含まれる総Ti量の60%以上である。(2)
抽出レプリカ法による電子顕微鏡観察によって観察され
る粒径:0.01〜0.2μmのTi系析出物の平均個
数が、25μm2 の観察視野中において10〜500個
である。
1. C: 0.10 to 0.45% (meaning mass%; the same applies hereinafter), B: 0.0003 to 0.0050%,
Ti: 0.01 to 0.1%, N: 0.0025 to 0.0
10% saw including, as yet another component, Si: 0.03 to 0.5%, M
n: 0.3 to 1.5% and Al: 0.01 to 0.10.
%, With the balance being Fe and unavoidable impurities, a hot-rolled material or a steel material cold-drawn after hot-rolling, which satisfies at least one of the following requirements (1) and (2): A B-containing steel excellent in cold workability and delayed fracture resistance, which is characterized by being (1) The amount of Ti contained in the precipitates extracted by the extraction residue method and having a particle size of more than 0.1 μm is 60% or more of the total amount of Ti contained in the steel material. (2)
The average number of Ti-based precipitates having a grain size of 0.01 to 0.2 μm observed by an electron microscope observation by the extraction replica method is 10 to 500 in the observation visual field of 25 μm 2 .
【請求項2】 更に他の成分として、Cu:2%以下
(0%を含まない)、Ni:2%以下(0%を含まな
い)およびCr:2%以下(0%を含まない)よりなる
群から選ばれる1種以上を含有するものである請求項
記載のB含有鋼。
2. As other components, Cu: 2% or less (0% is not included), Ni: 2% or less (0% is not included) and Cr: 2% or less (0% is not included) claim 1 is intended to contain one or more selected from the group consisting of
B-containing steel according to.
【請求項3】 更に他の成分として、Mo:1%以下
(0%を含まない)を含有するものである請求項1又は
に記載のB含有鋼。
As claimed in claim 2, further other components, Mo: 1% or less (not including 0%) according to claim 1 or those containing
B-containing steel according to 2.
【請求項4】 更に他の成分として、Nb:0.005
〜0.1%および/またはV:0.005〜0.3%を
含有するものである請求項1〜のいずれかに記載のB
含有鋼。
4. Further, as another component, Nb: 0.005
To 0.1% and / or V: 0.005 to 0.3%, B according to any one of claims 1 to 5.
Containing steel.
【請求項5】 更に他の成分として、Caを0.000
3〜0.001%を含有するものである請求項1〜
いずれかに記載のB含有鋼。
5. As another component, Ca is 0.000.
B-containing steel according to any one of claims 1 to 4, those containing from 3 to 0.001%.
【請求項6】 請求項1〜のいずれかに記載のB含有
鋼によって製造されたものであるボルト。
6. those produced by B-containing steel according to any one of claims 1 to 5 volts.
【請求項7】 請求項1〜のいずれかに記載のB含有
鋼を製造する方法であって、下記(a)〜(c)の条件
を満足させつつ操業することを特徴とする冷間加工性と
耐遅れ破壊性に優れたB含有鋼の製造方法。 (a)ビレット再加熱温度:950℃以上 (b)仕上げ圧延温度(すなわち最終圧延パス前または
圧延ロール群前の放射温度計で測定可能な表面の平均温
度):700〜900℃ (c)仕上げ圧延後の750℃から650℃までの平均
冷却速度:1℃/秒以下
7. A method for producing a B-containing steel according to any one of claims 1 to 5 cold, characterized in that to operate while satisfying the following conditions (a) ~ (c) A method for producing a B-containing steel excellent in workability and delayed fracture resistance. (A) Billet reheating temperature: 950 ° C. or higher (b) Finish rolling temperature (that is, before the final rolling pass or
Mean surface temperature measurable with a radiation thermometer in front of rolling rolls
Degree) : 700 to 900 ° C (c) Average cooling rate from 750 ° C to 650 ° C after finish rolling: 1 ° C / sec or less
JP33781498A 1998-02-10 1998-11-27 B-containing steel excellent in cold workability and delayed fracture resistance, its manufacturing method and bolt Expired - Lifetime JP3535754B2 (en)

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WO2013145868A1 (en) 2012-03-26 2013-10-03 株式会社神戸製鋼所 Boron-added high strength bolt steel having excellent delayed fracture resistance and high strength bolt
US9845519B2 (en) 2012-03-26 2017-12-19 Kobe Steel, Ltd. Boron-added high strength steel for bolt and high strength bolt having excellent delayed fracture resistance

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