JP2006249458A - High strength steel with excellent delayed fracture resistance and method for producing the same - Google Patents
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Abstract
【課題】本発明は、自動車用や各種産業機械部品などに、好適な引張強さが1500MPa以上で耐遅れ破壊特性に優れる高強度鋼およびその製造方法を提供する。
【解決手段】質量%で、C:0.4超え〜0.6%、Si:0.2%未満、Mn:0.1〜1.0%、Ni:5超え〜12%、sol.Al:0.01〜0.1%、Ti:0.001〜0.1%、N:0.02%以下、P:0.01%以下、S:0.01%以下、更に、Cu:0.1〜1%、Cr:0.1〜1%、Mo:0.02〜1%、B:0.0001〜0.005%、Ca:0.0005〜0.005%、Mg:0.0005〜0.005%の一種または二種以上を含有し、残部がFe及び不可避的不純物からなり、好ましくは旧オーステナイト粒径が15μm以下とする。
【選択図】無し。The present invention provides a high-strength steel excellent in delayed fracture resistance with a suitable tensile strength of 1500 MPa or more for automobiles and various industrial machine parts, and a method for producing the same.
SOLUTION: In mass%, C: more than 0.4 to 0.6%, Si: less than 0.2%, Mn: 0.1 to 1.0%, Ni: more than 5 to 12%, sol.Al: 0.01 to 0.1%, Ti: 0.001 to 0.1%, N: 0.02% or less, P: 0.01% or less, S: 0.01% or less, Cu: 0.1-1%, Cr: 0.1-1%, Mo: 0.02-1%, B: 0.0001-0.005% , Ca: 0.0005 to 0.005%, Mg: 0.0005 to 0.005%, or one or more of them, the balance being Fe and inevitable impurities, preferably the prior austenite grain size is 15 μm or less.
[Selection figure] None.
Description
本発明は、高強度鋼およびその製造方法に関し、特に、引張強さが1500MPa以上で耐遅れ破壊特性に優れ、自動車用や、各種産業機械部品用として好適なものに関する。 The present invention relates to high-strength steel and a method for producing the same, and more particularly to a steel having a tensile strength of 1500 MPa or more and excellent delayed fracture resistance, and suitable for automobiles and various industrial machine parts.
自動車や各種産業機械の軽量化、高性能化のため高強度鋼のニーズが高まっているが、一方で鋼材の高強度化は遅れ破壊特性の劣化が懸念される。自動車用、各種産業機械用や橋梁用に使用されているボルトは1200MPa 以上の高強度になると遅れ破壊の危険性が増すために使用上の制約が設けられている。 There is a growing need for high-strength steel to reduce the weight and performance of automobiles and various industrial machines. On the other hand, increasing the strength of steel materials is a concern for delayed fracture characteristics. Bolts used for automobiles, various industrial machines, and bridges are restricted in use because the risk of delayed fracture increases when the strength becomes 1200 MPa or higher.
また、自動車用などの各種輸送機器に使用されている各種のばねにおいても輸送機器の燃費向上を達成するため、軽量化のための部品の高強度化が益々厳しく要求され、遅れ破壊特性の劣化が懸念されるようになっている。 In addition, various springs used in various transportation equipment such as automobiles are required to increase the strength of parts for weight reduction in order to achieve improved fuel efficiency of transportation equipment, resulting in deterioration of delayed fracture characteristics. Has become a concern.
一般的に遅れ破壊は、外部環境から、鋼中に侵入した水素が引張応力集中部の結晶粒界に集積し、粒界割れを助長するために発生すると考えられ、破壊に至るまでの過程は、腐食→水素の侵入→結晶粒界への水素の集積→粒界で亀裂発生→亀裂の伝播→破壊で、その破壊形態は粒界破壊である。 In general, delayed fracture is considered to occur because hydrogen that has entered the steel from the external environment accumulates at the grain boundaries of the tensile stress concentration part and promotes grain boundary cracking. Corrosion → Hydrogen penetration → Hydrogen accumulation at grain boundaries → Crack formation at grain boundaries → Propagation of cracks → Destruction.
この機構に基づいて種々の遅れ破壊特性を向上させる提案がなされており、例えば特許文献1では粒界強化を目的とした旧オーステナイト粒を微細化させること、特許文献2、特許文献3ではP、Sなど粒界脆化元素を低減させることが提案されている。 Various proposals for improving delayed fracture characteristics have been made based on this mechanism. For example, Patent Document 1 discloses refinement of prior austenite grains for the purpose of grain boundary strengthening, Patent Document 2 and Patent Document 3 indicate P, It has been proposed to reduce grain boundary embrittlement elements such as S.
更に、特許文献4では旧オーステナイト粒界に析出した炭化物への応力集中を緩和するために550℃以上の高温で焼戻し処理し炭化物を球状化させることが有効であるとの技術が提案されている。
しかしながらいずれの提案も粒界強化に特化した内容であり、1500MPa以上の、例えば1800〜2000MPaなどの超高強度材においては、水素の侵入から亀裂伝播に至る個々の過程での対策が必要と考えられ、十分な耐遅れ破壊特性を発揮するには至らないと推測される。 However, both proposals are specialized for grain boundary strengthening. For ultra-high-strength materials of 1500MPa or more, for example, 1800-2000MPa, measures are required in each process from hydrogen penetration to crack propagation. It is thought that it does not reach sufficient delayed fracture resistance.
本発明は、上記のような状況に着目してなされたものであって、遅れ破壊特性が良好で特に強度が1500MPa以上の高強度鋼およびその製造方法を提供することを目的とする。 The present invention has been made paying attention to the above situation, and an object of the present invention is to provide a high-strength steel having good delayed fracture characteristics and particularly having a strength of 1500 MPa or more, and a method for producing the same.
本発明者等は、上記課題を達成するため、鋭意研究を重ねた結果、以下の知見を得た。
すなわち、鋼組成としては
a)侵入水素量を低減するための耐食性元素の添加(水素侵入抑制)
b)粒界脆化元素のP、Sの低減、およびこれらの元素の粒界への濃化を助長するMn、Siの低下
c)靭性の向上元素の添加(亀裂伝播抑制)
製造方法としては
a)低温焼戻しによる、粒界への炭化物析出を低減、かつ粒界脆化元素であるP、Sの濃化低減(亀裂発生抑制)、
d)焼入れ温度の低下、および/あるいは高周波急速加熱による、組織の微細化とP、Sの結晶粒界への濃化低減(亀裂発生。亀裂伝播抑制)
とすることで、優れた遅れ破壊特性の得られることを見出した。
本発明は得られた知見を基に更に検討を加えてなされたもので、すなわち、本発明は、
1 質量%で、C:0.4超え〜0.6%、Si:0.2%未満、Mn:0.1〜1.0%、Ni:5超え〜12%、sol.Al:0.01〜0.1%、Ti:0.001〜0.1%、N:0.02%以下、P:0.01%以下、S:0.01%以下、残部Fe及び不可避的不純物からなる耐遅れ破壊特性に優れた高強度鋼。
The present inventors obtained the following knowledge as a result of intensive studies to achieve the above-mentioned problems.
That is, as steel composition
a) Addition of corrosion-resistant elements to reduce the amount of intrusion hydrogen (suppression of hydrogen intrusion)
b) Reduction of P and S of grain boundary embrittlement elements, and reduction of Mn and Si to promote concentration of these elements at grain boundaries
c) Addition of elements to improve toughness (inhibition of crack propagation)
As a manufacturing method
a) Reduction of carbide precipitation at grain boundaries due to low-temperature tempering, and reduction of concentration of P and S, which are grain boundary embrittlement elements (inhibition of crack generation),
d) Reducing the microstructure and reducing the concentration of P and S at the crystal grain boundaries by lowering the quenching temperature and / or high-frequency rapid heating (crack generation, crack propagation suppression)
As a result, it was found that excellent delayed fracture characteristics can be obtained.
The present invention was made by further study based on the obtained knowledge, that is, the present invention is
1% by mass, C: more than 0.4 to 0.6%, Si: less than 0.2%, Mn: 0.1 to 1.0%, Ni: more than 5 to 12%, sol. Al: 0.01 to 0.1%, Ti: 0.001 to 0.1 %, N: 0.02% or less, P: 0.01% or less, S: 0.01% or less, high-strength steel excellent in delayed fracture resistance consisting of the balance Fe and inevitable impurities.
2 質量%で、C:0.4超え〜0.6%、Si:0.2%未満、Mn:0.1〜1.0%、Ni:5超え〜12%、sol.Al:0.01〜0.1%、Ti:0.001〜0.1%、N:0.02%以下、P:0.01%以下、S:0.01%以下、更にCu:0.1〜1%、Cr:0.1〜1%、Mo:0.02〜1%、B:0.0001〜0.005%、Ca:0.0005〜0.005%、Mg:0.0005〜0.005%の一種または二種以上を含有し、残部がFe及び不可避的不純物からなる耐遅れ破壊特性に優れた高強度鋼。 2% by mass, C: more than 0.4 to 0.6%, Si: less than 0.2%, Mn: 0.1 to 1.0%, Ni: more than 5 to 12%, sol. Al: 0.01 to 0.1%, Ti: 0.001 -0.1%, N: 0.02% or less, P: 0.01% or less, S: 0.01% or less, Cu: 0.1-1%, Cr: 0.1-1%, Mo: 0.02-1%, B: 0.00011- A high-strength steel excellent in delayed fracture resistance, containing one or more of 0.005%, Ca: 0.0005-0.005%, Mg: 0.0005-0.005%, the balance being Fe and inevitable impurities.
3 旧オーステナイト粒径が15μm以下である1または2記載の耐遅れ破壊特性に優れた高強度鋼。 3. A high strength steel excellent in delayed fracture resistance according to 1 or 2, wherein the prior austenite grain size is 15 μm or less.
4 1または2記載の成分組成の鋼を、焼入れ温度≦Ac3+60℃、焼戻し温度:400℃以下で焼入れ焼戻しすることを特徴とする耐遅れ破壊特性に優れた高強度鋼部品の製造方法。
5焼入れ焼戻し処理を高周波加熱で行うことを特徴とする4記載の耐遅れ破壊特性に優れた高強度鋼部品の製造方法。
61乃至3のいずれか一つの高強度鋼を用いた部品。
4. A method for producing a high strength steel part having excellent delayed fracture resistance, characterized by quenching and tempering a steel having the composition described in 1 or 2 at a quenching temperature ≦ Ac 3 + 60 ° C. and a tempering temperature: 400 ° C. or less. .
5. The method for producing a high-strength steel part having excellent delayed fracture resistance according to 4, wherein the quenching and tempering treatment is performed by high-frequency heating.
A part using high strength steel of any one of 61 to 3.
本発明によれば、水素の侵入から亀裂伝播に至る各段階において適切な対策を講じることで、1500MPa以上の高強度でも耐遅れ破壊特性に優れた高強度鋼およびその製造方法の提供が可能で、自動車用や、各種産業機械部品として好適な耐遅れ破壊特性に優れた高強度部品が得られ、産業上極めて有用である。 According to the present invention, by taking appropriate measures at each stage from hydrogen intrusion to crack propagation, it is possible to provide a high strength steel excellent in delayed fracture resistance even at a high strength of 1500 MPa or more and a method for producing the same. In addition, high strength parts excellent in delayed fracture resistance suitable for automobiles and various industrial machine parts can be obtained, which is extremely useful industrially.
以下、本発明の成分組成、ミクロ組織および焼入れ焼戻し処理について説明する。
1 成分組成(%は質量%)
C:0.4超え〜0.6%
Cは鋼の強度を確保するのに重要な元素であり、0.4%未満では所望の強度を得ることができない。
一方、0.6%を超えると加工性が悪くなるばかりでなく靭性の低下を招く。従って、0.4超え〜0.6%の範囲内に限定する。
Hereinafter, the component composition, microstructure and quenching / tempering treatment of the present invention will be described.
1 Component composition (% is% by mass)
C: 0.4 to 0.6%
C is an important element for securing the strength of steel, and if it is less than 0.4%, a desired strength cannot be obtained.
On the other hand, if it exceeds 0.6%, not only the workability is deteriorated but also the toughness is lowered. Therefore, it is limited within the range of more than 0.4 to 0.6%.
Si:0.2%未満
Siは鋼の脱酸材として重要な元素であるが、P、Sなどの不純物元素の粒界偏析を助長するため、0.2%未満にする。
Si: Less than 0.2% Si is an important element as a deoxidizing material for steel. However, in order to promote grain boundary segregation of impurity elements such as P and S, it is made less than 0.2%.
Mn:0.1〜1.0%
Mnは脱酸のために必要であるばかりでなく、焼入性を高めるために有効な元素であるが、0.1%未満ではその効果が得られず、一方多量に添加すると不純物元素の粒界偏析を助長する。従って0.1〜1.0%範囲内に限定する。
Mn: 0.1 to 1.0%
Mn is not only necessary for deoxidation but also an effective element for improving hardenability, but if it is less than 0.1%, the effect cannot be obtained. To help. Therefore, it is limited within the range of 0.1 to 1.0%.
P:0.01%以下
Pはオーステナイト粒界に偏析して、粒界強度を弱め、遅れ破壊を助長する。従って、0.01%以下とする。
P: 0.01% or less P segregates at austenite grain boundaries, weakens grain boundary strength, and promotes delayed fracture. Therefore, it is 0.01% or less.
S:0.01%以下
SはP同様にオーステナイト粒界に偏析して、粒界強度を弱め、遅れ破壊を助長する。従って、0.01%以下とする。
S: 0.01% or less S, like P, segregates at austenite grain boundaries, weakens the grain boundary strength, and promotes delayed fracture. Therefore, it is 0.01% or less.
Ni:5超え〜12%
Niは鋼に焼入性を付与し静的強度を上昇させ、更に靭性と耐食性を向上させるのに有効な元素で、その効果を得るためには5%より多く必要である。しかし、多量に添加しても効果が飽和し、合金コストが増加する。従って、5超え〜12%とする。
Ni: More than 5 to 12%
Ni is an element effective for imparting hardenability to steel, increasing static strength, and further improving toughness and corrosion resistance, and more than 5% is necessary to obtain the effect. However, even if added in a large amount, the effect is saturated and the alloy cost increases. Therefore, it exceeds 5 to 12%.
sol.Al:0.01〜0.1%
Alは脱酸材として必要な元素であり、また熱処理時においてAlNを形成することによりオーステナイト粒の粗大化を防止する効果とともにNを固定する効果も有しているが、0.01%未満ではこれらの効果が発揮されず、0.1%を越えても効果が飽和するため0.01〜0.1%の範囲に限定する。
sol.Al: 0.01 to 0.1%
Al is an element necessary as a deoxidizing material, and also has the effect of fixing N as well as the effect of preventing coarsening of austenite grains by forming AlN during heat treatment. The effect is not exhibited, and even if it exceeds 0.1%, the effect is saturated, so it is limited to the range of 0.01 to 0.1%.
Ti:0.001〜0.1%
Tiは結晶粒の微細化効果を有し、更に鋼中Nを窒化物として固定し粒界脆化を緩和する。その効果を得るためには0.001%以上必要である。しかしながら、多量に添加すると逆に炭窒化物が増加しすぎて靭性や加工性が低下する他、合金コストも増加する。従って、0.001〜0.1%とする。
Ti: 0.001 to 0.1%
Ti has an effect of refining crystal grains, and further, N in steel is fixed as a nitride and mitigates grain boundary embrittlement. In order to obtain the effect, 0.001% or more is necessary. However, if added in a large amount, on the contrary, carbonitrides are excessively increased to reduce toughness and workability, and alloy costs also increase. Therefore, it is 0.001 to 0.1%.
N:0.02%以下
Nもオーステナイト粒界に偏析して粒界強度を弱め、粒界脆化の一因となる。従って0.02%以下にする。
N: 0.02% or less N also segregates at the austenite grain boundary to weaken the grain boundary strength and contribute to grain boundary embrittlement. Therefore, it is made 0.02% or less.
以上が本発明の基本成分組成であるが、更に、強度、靭性などの特性を向上させる場合、Cu、Cr、Mo、B、Ca、Mgの一種または二種以上を添加する。
Cu :0.1〜1%
Cuは鋼の焼入れ性を向上させ、鋼の強度を高め、更に耐食性を高めるのに有効な元素である。0.1%以下ではこの効果は十分発揮できず、一方、多量に添加すると熱間圧延時に表面疵が発生しやすくなり冷間加工性を低下させる。従って、添加する場合は、0.1〜1%とする。
The above is the basic component composition of the present invention, but when improving properties such as strength and toughness, one or more of Cu, Cr, Mo, B, Ca and Mg are added.
Cu: 0.1 to 1%
Cu is an element effective for improving the hardenability of steel, increasing the strength of the steel, and further improving the corrosion resistance. If the amount is less than 0.1%, this effect cannot be sufficiently exerted. On the other hand, if added in a large amount, surface flaws are likely to occur during hot rolling, and cold workability is lowered. Therefore, when adding, it is 0.1 to 1%.
Cr:0.1〜1%
Crは、焼入性を向上させ鋼の強度を高め、更に硫化物形成元素の1つで粒界に偏析するSを抑制させるのに有効な元素であるが、0.1%未満ではその効果が十分に発揮できず、一方、1%を超えて添加してもその効果は飽和する。従って、添加する場合は、0.1〜1%とする。
Cr: 0.1 to 1%
Cr is an element effective in improving hardenability and increasing the strength of steel, and further suppressing S segregating at the grain boundary as one of the sulfide-forming elements. However, the effect is saturated even if added over 1%. Therefore, when adding, it is 0.1 to 1%.
Mo:0.02〜1%
MoはPの粒界への偏析を防止し、粒界強度を高めるのに有効な元素であるが、0.02%未満ではその効果は十分に発揮できず、一方、1%を超えて添加してもその効果は飽和し、合金コスト増加を招く。従って、添加する場合は、0.02〜1%とする。
Mo: 0.02-1%
Mo is an element effective for preventing the segregation of P to the grain boundary and increasing the grain boundary strength. However, if it is less than 0.02%, the effect cannot be sufficiently exerted, while adding over 1%. Even so, the effect is saturated, resulting in an increase in alloy costs. Therefore, when adding, it is 0.02 to 1%.
B:0.0001〜0.005%
Bは微量の添加で焼入性を向上させ、鋼の強度を高めるとともに粒界脆化を緩和するが、0.0001%以下ではその効果が十分に発揮できず、一方、多量に添加してもその効果が飽和するだけである。従って、添加する場合は、0.0001〜0.005%とする。
B: 0.0001 to 0.005%
B improves hardenability with a small amount of addition, increases the strength of the steel and mitigates grain boundary embrittlement, but the effect cannot be fully exhibited at 0.0001% or less, while it is added in a large amount. The effect is only saturated. Therefore, when adding, it is 0.0001 to 0.005%.
Ca:0.0005〜0.005%、Mg:0.0005〜0.005%
Ca、Mgは硫化物形成元素でオーステナイト粒界に偏析するSを抑制し粒界強度を高める。その効果を十分発揮するには0.0005%以上必要であるが、一方で多量に添加してもその効果は飽和するばかりでなく鋳造性を阻害する。従って両元素とも添加する場合は、0.0005〜0.005%とする。
Ca: 0.0005 to 0.005%, Mg: 0.0005 to 0.005%
Ca and Mg are sulfide-forming elements that suppress S segregating at the austenite grain boundaries and increase the grain boundary strength. Although 0.0005% or more is necessary to fully exhibit the effect, on the other hand, even if added in a large amount, the effect is not only saturated but also castability is impaired. Therefore, when both elements are added, the content is made 0.0005 to 0.005%.
2 旧オーステナイト粒径:15μm以下
オーステナイト粒径を細粒にすることは、粒界強度を向上させ亀裂伝播速度を低下させる効果があるので遅れ破壊特性向上には有効な手段である。この効果を十分発揮させるため、焼入れ焼戻し後の旧オーステナイト粒径を15μm以下、より好ましくは10μm以下とする。
2 Prior austenite grain size: 15 μm or less Making the austenite grain size fine is an effective means for improving delayed fracture characteristics because it has the effect of improving the grain boundary strength and reducing the crack propagation rate. In order to sufficiently exhibit this effect, the prior austenite grain size after quenching and tempering is set to 15 μm or less, more preferably 10 μm or less.
3 焼入れ焼戻し処理
焼入れ温度≦Ac3+60℃、焼戻し温度:400℃以下
焼入れ温度が高すぎるとオーステナイト粒径が粗大化し、粒界強度が低下して、遅れ破壊特性が劣化するので、その上限をAc3温度+60℃に限定する。
3 Quenching and tempering treatment Quenching temperature ≦ Ac 3 + 60 ° C, tempering temperature: 400 ° C or less If the quenching temperature is too high, the austenite grain size becomes coarse, the grain boundary strength decreases, and the delayed fracture property deteriorates. Is limited to Ac 3 temperature + 60 ° C.
焼戻し温度はオーステナイト粒界へのセメンタイト析出を抑制し、更にオーステナイト粒界への不純物元素の濃化を低減し遅れ破壊特性を向上させるために400℃以下とする。 The tempering temperature is set to 400 ° C. or lower in order to suppress cementite precipitation on the austenite grain boundaries, further reduce the concentration of impurity elements on the austenite grain boundaries, and improve delayed fracture characteristics.
本発明では、焼入れ焼戻し処理方法は特に限定しないが、高周波誘導加熱を用いると、急速短時間加熱が可能で、オーステナイト粒の細粒化およびオーステナイト粒界への不純物元素の濃化が軽減でき、遅れ破壊特性を更に向上させるため、好ましい。 In the present invention, the quenching and tempering treatment method is not particularly limited, but when high-frequency induction heating is used, rapid and short-time heating is possible, and austenite grain refinement and concentration of impurity elements on the austenite grain boundary can be reduced. This is preferable because the delayed fracture characteristics are further improved.
以下、実施例に基づいて説明する。
表1に示した成分組成を有する鋼を真空溶解を行い(50kg)、熱間鍛造でΦ25材を作成した。表1において鋼No.1〜13は成分組成が本発明範囲内の本発明鋼、鋼No.14〜20は成分組成が本発明範囲外の比較鋼である。
Hereinafter, a description will be given based on examples.
Steel having the component composition shown in Table 1 was vacuum melted (50 kg), and a Φ25 material was prepared by hot forging. In Table 1, steel no. Nos. 1 to 13 are steels according to the present invention, steel Nos. 14-20 are comparative steels whose component composition is outside the scope of the present invention.
得られた鍛造素材を焼入れ焼戻し処理により、強度:1500〜1850MPaに調整し、遅れ破壊特性を評価した。焼入れ焼戻し処理は、高周波誘導加熱により、焼入れ温度:(Ac3+50℃)*30分→WQ、焼戻し温度:T℃*60分→WCとした。 The obtained forged material was adjusted to a strength of 1500 to 1850 MPa by quenching and tempering, and the delayed fracture characteristics were evaluated. The quenching and tempering treatment was performed by induction heating at a quenching temperature: (Ac 3 + 50 ° C.) * 30 minutes → WQ, and a tempering temperature: T ° C. * 60 minutes → WC.
遅れ破壊特性の評価方法は、材料の限界拡散性水素量(Hc)と環境侵入水素量(He/Hc)を測定し、He/Hc>1は不良(×)、He/Hc≦1は良好(○)と判定した。 Delayed fracture characteristics are evaluated by measuring the material's critical diffusible hydrogen content (Hc) and environmental intrusion hydrogen content (He / Hc). He / Hc> 1 is poor (×), and He / Hc ≦ 1 is good (○).
限界拡散性水素量(Hc)は、 図1に示す試験片を使用し、陰極チャージ法で水素を侵入させ、引張強度の0.9倍の静的引張応力を付与し破断までの時間を調べ、破断時間と拡散性水素量の関係から、破断しない限界の拡散性水素量をそれぞれ求めた。 For the critical diffusible hydrogen content (Hc), the test piece shown in Fig. 1 was used, hydrogen was infiltrated by the cathodic charging method, a static tensile stress 0.9 times the tensile strength was applied, the time until fracture was examined, From the relationship between time and the amount of diffusible hydrogen, the amount of diffusible hydrogen that does not break was determined.
尚、試験時間は100時間を最大とし、試験中に試験片からの水素放出をさけるために陰極チャージ後試験片にはメッキを施した。また、試験片への水素侵入量は陰極チャージ条件を種々変えて制御し、定荷重試験は、試験片内の水素分布を均一にするため、メッキ後24時間経過した時点から開始した。 The test time was 100 hours maximum, and the test piece was plated after cathodic charging in order to avoid hydrogen release from the test piece during the test. The amount of hydrogen intrusion into the test piece was controlled by changing the cathode charge conditions in various ways, and the constant load test was started from 24 hours after plating in order to make the hydrogen distribution in the test piece uniform.
水素の分析は、試験片をキャリアガス(Ar)中で一定の加熱速度で加熱し、そのガスをガスクロマトグラフィーで5分間隔で1分間分析を行い、300℃までに放出された水素の積算値を拡散性水素と定義し、破断時間との関係を整理した。 In the analysis of hydrogen, the test piece is heated in a carrier gas (Ar) at a constant heating rate, and the gas is analyzed by gas chromatography for 1 minute every 5 minutes, and the amount of hydrogen released up to 300 ° C is integrated. The value was defined as diffusible hydrogen, and the relationship with the fracture time was arranged.
100時間未満で破断した条件は、再度同条件で水素を侵入させメッキを行い、24時間放置後、更に、メッキを剥離して水素分析を行い、一方、100時間まで未破断の場合は、そのままメッキを剥離し水素分析を行った。 For conditions that broke in less than 100 hours, infiltrate hydrogen again under the same conditions and perform plating.After leaving for 24 hours, further, peel off the plating and perform hydrogen analysis. The plating was peeled off and hydrogen analysis was performed.
環境侵入水素量(He)は、5%NaCl塩水噴霧→乾燥の促進試験により測定した。促進試験の腐食条件は塩水噴霧(5%NaCl、25℃)を16時間実施し、その後大気放置(湿度60%、25℃)を8時間実施する工程を1サイクルとして7サイクル実施した。7サイクル実施後、表面の錆をショットブラストで除去し、上記と同様の水素分析を行い,拡散性水素量を測定した。 The amount of hydrogen penetrating into the environment (He) was measured by a 5% NaCl salt spray-> drying acceleration test. Corrosion conditions for the accelerated test were 7 cycles of a process in which salt spray (5% NaCl, 25 ° C.) was performed for 16 hours and then left in the atmosphere (humidity 60%, 25 ° C.) for 8 hours. After 7 cycles, the surface rust was removed by shot blasting, hydrogen analysis was performed in the same manner as described above, and the amount of diffusible hydrogen was measured.
表2に得られた結果を示す。鋼No.1〜13の本発明鋼はいずれもHe/Hc≦1で良好であった。一方、鋼No.14はC量が本発明範囲の上限を超えて高いために粒界にセメンタイトが多数析出し靭性が低下し、Hcが低く遅れ破壊特性が悪い。 Table 2 shows the results obtained. Steel No. The steels of the present invention of 1 to 13 were all good with He / Hc ≦ 1. On the other hand, Steel No. No. 14 has a high C content exceeding the upper limit of the range of the present invention, so that a large amount of cementite precipitates at the grain boundaries, lowering toughness, Hc is low, and delayed fracture characteristics are poor.
鋼No.15はSi、Mn量が本発明範囲の上限を超えて高いために、靭性が低下し、Hcが低く遅れ破壊特性が悪い。鋼No.16,17はそれぞれP、S量が本発明範囲の上限を超えて高いために、靭性が低下し、Hcが低く遅れ破壊特性が悪い。 Steel No. No. 15 has high amounts of Si and Mn exceeding the upper limit of the range of the present invention, so that toughness is lowered, Hc is low, and delayed fracture characteristics are poor. Steel No. Nos. 16 and 17 have high amounts of P and S exceeding the upper limit of the range of the present invention, respectively, so that toughness is reduced, Hc is low, and delayed fracture characteristics are poor.
鋼No.18はNi量が本発明範囲の下限をより低いために、靭性が低下し遅れ破壊特性が悪い。
鋼No.19はAlが本発明範囲の下限をより低いため脱酸不足によって清浄性が悪く、その結果靭性が劣化し、遅れ破壊特性が悪い。
Steel No. In No. 18, since the Ni content is lower than the lower limit of the range of the present invention, the toughness is lowered and the delayed fracture characteristics are poor.
Steel No. In No. 19, since Al is lower than the lower limit of the range of the present invention, cleanliness is poor due to insufficient deoxidation. As a result, toughness is deteriorated and delayed fracture characteristics are poor.
鋼No.20はTi量が本発明範囲の下限をより低く、更にN量が本発明範囲の上限を超えて高いために靭性が低下し、遅れ破壊特性が悪い。 Steel No. In No. 20, the Ti content is lower than the lower limit of the range of the present invention, and the N amount is higher than the upper limit of the range of the present invention.
★ ★
★
[遅れ破壊特性に及ぼす旧オーステナイト粒径の影響]
表1に示した鋼No.3により、遅れ破壊特性に及ぼす旧オーステナイト粒径の影響を調査した。遅れ破壊特性の評価は前記同様にHcとHeを測定してHe/Hcの値により評価した。
★
[Effect of prior austenite grain size on delayed fracture characteristics]
Steel No. shown in Table 1 3 was used to investigate the effect of prior austenite grain size on delayed fracture characteristics. The delayed fracture characteristics were evaluated by measuring Hc and He in the same manner as described above and using the value of He / Hc.
表3に結果を示す。旧オーステナイト粒径が小さくなるにつれ、He/Hcが低くなり、遅れ破壊特性が良好となる。特性例-1は旧γ粒の微細化により粒界強度の向上によりHe/Hcが低くなり最も良好な結果となった。特性例-2は最も旧γ粒が大きく、その結果、主にHcが低下し、遅れ破壊特性は若干劣化した。尚、特性例-1、2、3のHe/Hcはいずれも1以下であった。 Table 3 shows the results. As the prior austenite grain size becomes smaller, the He / Hc becomes lower and the delayed fracture property becomes better. The characteristic example-1 shows the best results because the grain boundary strength is improved by refinement of the old γ grains and the He / Hc is lowered. In the characteristic example-2, the oldest γ grains were the largest, and as a result, Hc mainly decreased and the delayed fracture characteristics slightly deteriorated. In addition, the He / Hc of the characteristic examples-1, 2, and 3 were all 1 or less.
★
[熱処理条件]
表1に示した鋼No.3を用いて、遅れ破壊特性に及ぼす焼入れ温度、焼戻し温度、高周波熱処理の影響を調査した。表4に結果を示す。遅れ破壊特性の評価はHc、Heを測定し、He/Hcの大小関係で評価した。
★
[Heat treatment conditions]
Steel No. shown in Table 1 3 was used to investigate the effects of quenching temperature, tempering temperature, and induction heat treatment on delayed fracture characteristics. Table 4 shows the results. Delayed fracture characteristics were evaluated by measuring Hc and He, and evaluating the magnitude relationship of He / Hc.
製造例1、3、5、6は、焼入れ温度がAC3+60℃以下、焼戻し温度が400℃以下と本発明範囲内であり、焼入れ温度が本発明範囲外である製造例2、焼戻し温度が本発明範囲外である製造例4と比較してHe/Hcが低く、遅れ破壊特性は良好である。 Production Examples 1, 3, 5, and 6 have a quenching temperature of AC3 + 60 ° C. or less and a tempering temperature of 400 ° C. or less within the scope of the present invention, and the quenching temperature is outside the scope of the present invention. Compared with Production Example 4 which is outside the scope of the present invention, He / Hc is low, and delayed fracture characteristics are good.
特に、製造例5は高周波加熱により焼入れ焼戻しを行ったもので、製造例1、3、6より旧γ粒界が細粒で、遅れ破壊特性が良好になった。尚、いずれの場合のHe/Hcも1以下であった。 In particular, Production Example 5 was obtained by quenching and tempering by high-frequency heating, and the old γ grain boundaries were finer than Production Examples 1, 3, and 6, and delayed fracture characteristics were improved. In all cases, He / Hc was 1 or less.
★ ★
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| JPH03243744A (en) * | 1990-02-20 | 1991-10-30 | Sumitomo Metal Ind Ltd | Steel for machine structural use excellent in delayed fracture resistance |
| JPH09235658A (en) * | 1996-02-27 | 1997-09-09 | Nkk Corp | Steel for high strength bolts with excellent cold forgeability and delayed fracture resistance |
| JPH1180903A (en) * | 1997-09-08 | 1999-03-26 | Nkk Corp | High strength steel member excellent in delayed fracture characteristics and method of manufacturing the same |
| JP2000144245A (en) * | 1998-11-10 | 2000-05-26 | Nkk Corp | Manufacturing method of high-strength steel with excellent delayed fracture resistance |
| JP2001288538A (en) * | 2000-04-04 | 2001-10-19 | Nippon Steel Corp | Steel for high-strength bolts having excellent delayed fracture resistance, bolts, and method of manufacturing the bolts |
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| JPH03243744A (en) * | 1990-02-20 | 1991-10-30 | Sumitomo Metal Ind Ltd | Steel for machine structural use excellent in delayed fracture resistance |
| JPH09235658A (en) * | 1996-02-27 | 1997-09-09 | Nkk Corp | Steel for high strength bolts with excellent cold forgeability and delayed fracture resistance |
| JPH1180903A (en) * | 1997-09-08 | 1999-03-26 | Nkk Corp | High strength steel member excellent in delayed fracture characteristics and method of manufacturing the same |
| JP2000144245A (en) * | 1998-11-10 | 2000-05-26 | Nkk Corp | Manufacturing method of high-strength steel with excellent delayed fracture resistance |
| JP2001288538A (en) * | 2000-04-04 | 2001-10-19 | Nippon Steel Corp | Steel for high-strength bolts having excellent delayed fracture resistance, bolts, and method of manufacturing the bolts |
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