JP2010202920A - Wire rod for high-strength steel wire, high-strength steel wire, and method for manufacturing them - Google Patents

Wire rod for high-strength steel wire, high-strength steel wire, and method for manufacturing them Download PDF

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JP2010202920A
JP2010202920A JP2009048278A JP2009048278A JP2010202920A JP 2010202920 A JP2010202920 A JP 2010202920A JP 2009048278 A JP2009048278 A JP 2009048278A JP 2009048278 A JP2009048278 A JP 2009048278A JP 2010202920 A JP2010202920 A JP 2010202920A
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steel wire
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JP5201000B2 (en
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Shingo Yamazaki
真吾 山崎
Makoto Okonogi
真 小此木
Yasutsugu Yoshimura
康嗣 吉村
Nariyasu Muroga
也康 室賀
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Nippon Steel Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a steel wire which can be manufactured without being subjected to patenting treatment in a wire-drawing process, and has superior mechanical properties such as strength and tensile strength; a wire rod to be used for manufacturing the steel wire; and a method for manufacturing them. <P>SOLUTION: The hot-rolled wire rod is made from a steel containing 0.30-0.50% C, 0.1-0.4% Si, 0.2-1.0% Mn, 0.01% or less Al, 0.01% or less Ti, 4-30 ppm B, 15-35 ppm N and 15-35 ppm O; includes pro-eutectoid ferrite and bainite of which the area rate FA(%) is in a range satisfying FA≤-35×(%C)+22, and pearlite which occupies 95% or more of the balance; and has a wire diameter of 3.6-7 mm. The steel wire is obtained by wire-drawing the wire rod at a true strain of 4 or more without subjecting the wire rod to the patenting treatment and bluing treatment, has a wire diameter D of 0.2-0.4 mm, has such a TS (MPa) as to satisfy 3,950-D×2,600≤TS, and does not cause the occurrence of the delamination in a twist test. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、強度、靭性、延性等に優れた極細鋼線を、伸線中にパテンティング処理およびブルーイング処理を施すこと無しに製造する技術に関する。   The present invention relates to a technique for manufacturing an ultrafine steel wire excellent in strength, toughness, ductility, and the like without performing patenting treatment and bluing treatment during drawing.

高強度鋼線の代表例であるスチールコード用鋼線を製造するには、通常、炭素含有量が0.7〜0.8%程度の高炭素鋼[JISG 3502(SWRS72A,SWRS82A)相当]を用い、それを熱間圧延した後、冷却条件を制御することにより直径:5.0〜6.4mm程度の鋼線材とし、次いで一次伸線加工、パテンティング処理、二次伸線加工、再度のパテンティング処理、Cu−Zn二相めっき、拡散処理を施した後、最終的に湿式伸線加工(仕上げ伸線)を行うことによって所定の線径になるように製造されている。   In order to manufacture steel wires for steel cords, which are typical examples of high-strength steel wires, usually high-carbon steel having a carbon content of about 0.7 to 0.8% [equivalent to JISG 3502 (SWRS72A, SWRS82A)] Use it, hot-roll it, and then control the cooling conditions to make a steel wire with a diameter of about 5.0 to 6.4 mm, then primary wire drawing, patenting treatment, secondary wire drawing, After a patenting treatment, Cu—Zn two-phase plating, and a diffusion treatment, it is manufactured to have a predetermined wire diameter by finally performing wet wire drawing (finish wire drawing).

この際、パテンティング処理は、伸線加工に適した均一微細なパーライト組織を得るために行われるが、高炭素鋼における伸線限界は、通常、真歪みで4以下と低いために、最終線径が細くなればなるほど最終パテンティング後の線径も細くなり、そのためパテンティング回数を増やす必要があるという問題があった。   At this time, the patenting process is performed in order to obtain a uniform fine pearlite structure suitable for wire drawing. However, since the wire drawing limit in high carbon steel is usually as low as 4 or less at the true strain, the final wire drawing is performed. As the diameter becomes thinner, the wire diameter after the final patenting also becomes thinner, so that there is a problem that the number of patenting needs to be increased.

そこで、伸線限界を向上させて線材の伸線加工性を高めることを目的として、種々の改良方法が提案されている。   Therefore, various improvement methods have been proposed for the purpose of improving the wire drawing limit and improving the wire drawing workability of the wire.

例えば特許文献1には、パテンティング処理時における冷却速度を制御することによって伸線に悪影響を及ぼす初析セメンタイトの析出を抑制する方法が、また、特許文献2には、熱間圧延線材の断面組織中の粗パーライト率を制御する技術が開示されている。
特許文献3および特許文献4には、鋼線組織を加工硬化の少ないベイナイト組織にすることによって、伸線による強度上昇を低く抑えて伸線限界を向上させる技術が開示されている。
特許文献5には、炭素含有量が0.30〜0.60%の中炭素鋼線材を用いて、最終パテンティング後の引張強さ、パーライト組織および初析フェライトを制御することにより伸線限界の向上を図る技術が開示されている。
For example, Patent Document 1 discloses a method for suppressing precipitation of pro-eutectoid cementite that adversely affects wire drawing by controlling a cooling rate during patenting, and Patent Document 2 discloses a cross section of a hot-rolled wire rod. A technique for controlling the coarse pearlite rate in the tissue is disclosed.
Patent Documents 3 and 4 disclose a technique for improving the wire drawing limit by suppressing the increase in strength due to wire drawing by making the steel wire structure a bainite structure with little work hardening.
Patent Document 5 discloses that a medium carbon steel wire having a carbon content of 0.30 to 0.60% is used to control the tensile strength after final patenting, the pearlite structure, and proeutectoid ferrite, thereby limiting the wire drawing. A technique for improving the above is disclosed.

これらの方法によれば、パテンティング回数を従来より少なくしても伸線加工性を高めることはできるが、いずれの方法においても、少なくとも伸線中に1回のパテンティング処理を必ず行う必要がある。   According to these methods, it is possible to improve the wire drawing workability even if the number of patenting is less than the conventional method, but in any method, it is necessary to perform at least one patenting process during the wire drawing. is there.

一方、特許文献6には、線径0.15mm以下の極細線を工業的に製造し得る方法が開示されている。具体的には、低炭素鋼線(C:0.01〜0.30%)に熱処理を施して、フェライトと、針状マルテンサイトまたはベイナイトの混合組織に調整した後に、主として伸線加工により高強度を得る方法が開示されているが、熱処理強度が70kgf/mm2程度と低く、かつ加工硬化率もパーライト鋼と比較して低いために、0.2mm程度の極細線に適用する場合、熱処理線径をかなり太くして伸線加工ひずみを大きく取らなければ所定の強度が得られないこと、5.5mm以上の太径熱処理では鋼線表層から中心部間の組織が不均一になり易く、わずかな塊状マルテンサイトの生成で、早期の伸線破断や機械的性質の劣化につながるという問題があった。   On the other hand, Patent Document 6 discloses a method capable of industrially producing an ultrafine wire having a wire diameter of 0.15 mm or less. Specifically, heat treatment is applied to a low carbon steel wire (C: 0.01 to 0.30%) to adjust to a mixed structure of ferrite and acicular martensite or bainite, and then the wire is processed mainly by wire drawing. Although a method for obtaining strength is disclosed, since the heat treatment strength is as low as about 70 kgf / mm 2 and the work hardening rate is also lower than that of pearlite steel, the heat treatment wire is applied when applied to an ultrafine wire of about 0.2 mm. The specified strength cannot be obtained unless the diameter is considerably increased and the wire drawing strain is increased, and in a large diameter heat treatment of 5.5 mm or more, the structure between the steel wire surface layer and the central portion tends to be non-uniform. There is a problem in that the formation of bulky martensite leads to early drawing breakage and deterioration of mechanical properties.

特許文献7には、中高炭素鋼線(C:0.35〜0.9%)の熱間圧延後冷却し、20%以下の面積率で初析フェライトを含有した組織に調整した後に、パテンティングすること無しに伸線によって0.15〜0.4mmの線径の高強度鋼線を得る方法が開示されているが、通常、スチールコード用フィラメントを製造するためには、伸線時の潤滑性とゴムとの密着性を保障するために、伸線工程の途中でCu-Zn二相めっき・加熱拡散処理(拡散黄銅めっき)を施す必要がある。このめっきの加熱拡散処理時(以後、この処理をブルーイング処理と称する。)に、伸線されて形成された伸長ラメラ組織が分断されるため、0.3〜0.4%程度のC量の線材では伸線後に所定の強度を得にくく、延性も劣化するという問題があった。   Patent Document 7 describes a method of cooling after hot rolling of a medium and high carbon steel wire (C: 0.35 to 0.9%), adjusting to a structure containing pro-eutectoid ferrite with an area ratio of 20% or less, and Although a method of obtaining a high strength steel wire having a wire diameter of 0.15 to 0.4 mm by wire drawing without drawing is usually disclosed, in order to produce a steel cord filament, To ensure lubricity and adhesion to rubber, it is necessary to perform Cu-Zn two-phase plating and heat diffusion treatment (diffusion brass plating) during the wire drawing process. During the heat diffusion treatment of this plating (hereinafter, this treatment is referred to as bluing treatment), the stretched lamella structure formed by drawing is divided, so that the C amount of about 0.3 to 0.4% However, it was difficult to obtain a predetermined strength after wire drawing, and the ductility deteriorated.

さらに、特許文献8においては、セメンタイトが不連続なパーライト線材を、熱処理無しに伸線することによって鋼線を得る方法が示されているが、セメンタイトが不連続であるのは、冷却速度が遅いステルモア相当のパテンティングをしているために必然的に得られた組織であり、セメンタイトが不連続であるが故に強度が低いという問題があった。   Furthermore, Patent Document 8 discloses a method of obtaining a steel wire by drawing a pearlite wire rod with discontinuous cementite without heat treatment. However, discontinuous cementite has a slow cooling rate. This is a structure that is inevitably obtained because of patenting equivalent to stealmore, and has a problem that strength is low because cementite is discontinuous.

特開平5−98349号公報Japanese Patent Laid-Open No. 5-98349 特公平3−60900号公報Japanese Patent Publication No. 3-60900 特開平5−105965号公報JP-A-5-105965 特開平5−117764号公報Japanese Patent Laid-Open No. 5-117744 特開平6−2039号公報Japanese Patent Laid-Open No. 6-2039 特公平1−15563号公報Japanese Patent Publication No. 1-15563 特許第3499341号公報Japanese Patent No. 3499341 特許第3409055号公報Japanese Patent No. 3409005

そこで、本発明は、上記のような事情に鑑み、中炭素鋼を素材として用い、伸線工程中にパテンティング処理およびブルーイング処理などの熱処理を全く施さなくとも極細鋼線に伸線加工でき、かつ、高強度で撚り線時のデラミネーション(縦割れ)の発生のない極細鋼線が得られる線材を提供できるようにするとともに、その線材を用いて高強度の極細鋼線を提供できるようにすることを課題とするものである。   Therefore, in view of the circumstances as described above, the present invention uses medium carbon steel as a raw material, and can be drawn into an ultrafine steel wire without any heat treatment such as patenting treatment and bluing treatment during the drawing step. In addition, it is possible to provide a high-strength, ultra-fine steel wire that can be obtained from an ultra-fine steel wire that does not cause delamination (longitudinal cracking) at the time of stranded wire. It is a problem to make.

本発明者らは、炭素濃度0.5%以下の中炭素領域の鋼材を用い、まず種々の条件で圧延・冷却・パテンティングして、種々の組織、強度レベルの線材を作成し、その線材を用いて伸線を実施し、直径0.2〜0.4mmであるような極細鋼線を作製した。そして、これら鋼線の引張強度、ねじり特性等の機械的特性を調査した。そして、鋼線の機械的特性を向上させる鋼材成分、圧延条件、パテンティング条件、伸線条件の影響等について検討を重ねた。   The inventors of the present invention use a medium carbon region steel material having a carbon concentration of 0.5% or less, first rolling, cooling, and patenting under various conditions to create a wire material having various structures and strength levels, and the wire material. Was used to draw an ultrafine steel wire having a diameter of 0.2 to 0.4 mm. And, mechanical properties such as tensile strength and torsional properties of these steel wires were investigated. And the steel material component which improves the mechanical characteristic of a steel wire, the rolling condition, the patenting condition, the influence of the wire drawing condition, etc. were examined repeatedly.

この結果、軟質相である初析フェライト+ベイナイト組織の面積率を低下させるとともに、引張強度を線材のC量に応じて適正に管理した圧延線材を用いれば、伸線中に中間パテンティング処理およびブルーイング処理などの熱処理を全く施さなくとも極細鋼線の製造が可能であること、さらに、そのような線材を、最終的な真ひずみ4以上の伸線加工を施すことによって、最終線径に応じたより高強度でデラミネーションが発生しない鋼線を得ることができるという結論に達し、本発明をなしたものである。   As a result, while reducing the area ratio of proeutectoid ferrite + bainite structure which is a soft phase and using a rolled wire whose tensile strength is appropriately controlled according to the amount of C in the wire, intermediate patenting treatment and It is possible to produce ultra-fine steel wires without any heat treatment such as bluing treatment, and by applying such a wire to a final true strain of 4 or more, the final wire diameter can be reduced. The conclusion was reached that the steel wire with higher strength and no delamination can be obtained.

本発明は以上の知見に基づいてなされたものであって、その要旨とするところは、次の通りである。
(1) 質量%で、C :0.30〜0.50%、Si:0.10〜0.40%、Mn:0.20〜1.0%、B:4〜30ppm、N:15〜35ppm、O:15〜35ppm、Al:0.01%以下(0%を含む)、Ti:0.01%以下(0%を含む)を含有し、残部鉄および不可避的不純物よりなり、パテンティング後の引張強さTS(MPa)が、下記式1の範囲にあり、
1000×(%C)+350≦TS≦1000×(%C)+500
・・・ (式1)
かつ、初析フェライトとベイナイトの面積率FA(%)が下記式2の範囲にあり、
FA≦−35×(%C)+22 ・・・ (式2)
残部の95%以上がパーライト組織であり、該パーライト組織の平均ブロック粒径が20μm以下であることを特徴とする線径3.6〜7mmの高強度極細鋼線用線材。
(2) 更に、質量%で、Cr:0.5%以下、Ni:0.5%以下、Co:0.5%以下、Cu:0.2%以下、Mo:0.2%以下、W:0.2%以下よりなる群から選択される少なくとも1種以上を含有することを特徴とする上記(1)に記載の高強度極細鋼線用線材。
The present invention has been made on the basis of the above findings, and the gist thereof is as follows.
(1) By mass%, C: 0.30 to 0.50%, Si: 0.10 to 0.40%, Mn: 0.20 to 1.0%, B: 4 to 30 ppm, N: 15 Contains 35 ppm, O: 15-35 ppm, Al: 0.01% or less (including 0%), Ti: 0.01% or less (including 0%), and consists of the balance iron and unavoidable impurities, patenting Later tensile strength TS (MPa) is in the range of the following formula 1,
1000 × (% C) + 350 ≦ TS ≦ 1000 × (% C) +500
... (Formula 1)
And the area ratio FA (%) of pro-eutectoid ferrite and bainite is in the range of the following formula 2,
FA ≦ −35 × (% C) +22 (Formula 2)
95% or more of the balance is a pearlite structure, and the average block particle size of the pearlite structure is 20 μm or less, a high-strength ultrafine steel wire rod having a wire diameter of 3.6 to 7 mm.
(2) Further, in mass%, Cr: 0.5% or less, Ni: 0.5% or less, Co: 0.5% or less, Cu: 0.2% or less, Mo: 0.2% or less, W The wire for high-strength ultrafine steel wire according to (1) above, which contains at least one selected from the group consisting of 0.2% or less.

(3) (1)または(2)に記載の線材に、熱処理を施すことなしに伸線を行うことにより、直径D(mm)を0.2〜0.4mmとした鋼線であって、引張強度TS(MPa)が3000MPa以上で、かつ下記式3を満たすことを特徴とするデラミネーションの発生しない高強度極細鋼線。
3950−D×2600≦TS ・・・ (式3)
(3) A steel wire having a diameter D (mm) of 0.2 to 0.4 mm by drawing the wire according to (1) or (2) without performing heat treatment, A high-strength ultrafine steel wire that does not generate delamination and has a tensile strength TS (MPa) of 3000 MPa or more and satisfies the following formula 3.
3950−D × 2600 ≦ TS (Formula 3)

(4) (1)または(2)に記載の鋼成分の鋼片を熱間圧延し、仕上げ圧延温度を1000〜1200℃とし、次いで880〜960℃の温度にて巻き取った後に、520〜580℃の温度の溶融ソルトに30s以上浸漬する工程を含むパテンティング処理を施すことを特徴とする(1)または(2)に記載の高強度鋼線用線材の製造方法。
(5) (1)または(2)に記載の鋼成分の鋼片を熱間圧延し、仕上げ圧延温度を1000〜1200℃とし、次いで880〜960℃の温度にて巻き取った後に、800℃から600℃までの冷却速度を50〜200℃/sとし、その後、520〜580℃の温度域にて30s以上保持する工程を含むパテンティング処理を施すことを特徴とする(1)または(2)に記載の高強度鋼線用線材の製造方法。
(4) The steel slab of the steel component described in (1) or (2) is hot-rolled, the finish rolling temperature is 1000 to 1200 ° C, and then wound at a temperature of 880 to 960 ° C, and then 520 to The method for producing a high-strength steel wire according to (1) or (2), wherein a patenting treatment including a step of immersing in a molten salt at a temperature of 580 ° C. for 30 s or more is performed.
(5) The steel slab of the steel component described in (1) or (2) is hot-rolled, the finish rolling temperature is 1000 to 1200 ° C, and then wound at a temperature of 880 to 960 ° C, and then 800 ° C. (1) or (2), characterized in that a cooling rate from 1 to 600 ° C. is set to 50 to 200 ° C./s, and thereafter a patenting process including a step of holding for 30 seconds or more in a temperature range of 520 to 580 ° C. is performed. The manufacturing method of the wire material for high-strength steel wires as described in).

(6) 請求項4または5に記載の方法によって製造された線材に、熱処理を施すことなしに、真ひずみ4%以上の条件で直径D(mm)が0.2〜0.4mmの範囲になるまで伸線を行うことを特徴とする(3)に記載の高強度極細鋼線の製造方法。   (6) The diameter D (mm) is in the range of 0.2 to 0.4 mm under the condition of true strain of 4% or more without subjecting the wire manufactured by the method according to claim 4 or 5 to heat treatment. The method for producing a high-strength ultrafine steel wire according to (3), wherein wire-drawing is performed until

伸線工程中にパテンティング処理およびブルーイング処理などの熱処理を全く施さなくとも極細鋼線に伸線加工できる線材を得ることができ、かつ、その線材を用いて、高強度で撚り線時のデラミネーション(縦割れ)の発生のない極細鋼線を得ることができる。   It is possible to obtain a wire that can be drawn into an ultrafine steel wire without performing any heat treatment such as patenting and bluing during the wire drawing process, and using the wire, high strength and twisted wire can be obtained. It is possible to obtain an ultra fine steel wire free from delamination (longitudinal cracking).

圧線線材の初析フェライト+ベイナイト組織の面積率と伸線後の引張強度TSの関係を示す図である。It is a figure which shows the relationship between the area ratio of the pro-eutectoid ferrite + bainite structure of a wire rod, and the tensile strength TS after wire drawing. 伸線後の鋼線の線径と引張強度の関係を示す図である。It is a figure which shows the relationship between the wire diameter of the steel wire after wire drawing, and tensile strength. 用いた鋼のC含有量と圧延線材の引張強度との関係を示す図である。It is a figure which shows the relationship between C content of the used steel, and the tensile strength of a rolled wire. 用いた鋼のC含有量と初析フェライト+ベイナイト組織の面積率との関係を示す図である。It is a figure which shows the relationship between C content of used steel, and the area ratio of pro-eutectoid ferrite + bainite structure. 本発明に係る鋼線の代表的なパーライト組織を示すSEM観察写真を用いた図である。It is the figure using the SEM observation photograph which shows the typical pearlite structure | tissue of the steel wire which concerns on this invention.

通常、スチールコード用鋼線を得るためには共析鋼に近い炭素濃度を有し、かつ0.2%程度のSiが含有する線材をオーステナイト化した後、450〜600℃で数〜数十秒保持するパテンティング処理を施し、ほぼ完全なパーライト組織にした後、伸線を実施する。しかしこの方法では、伸線前の線材強度が高く、伸線時の加工硬化係数も大きいため、3〜4程度の真ひずみで伸線時の破断あるいは伸線後のデラミネーションが発生する。   Usually, in order to obtain a steel wire for steel cord, after austenizing a wire having a carbon concentration close to that of eutectoid steel and containing about 0.2% of Si, it is several to several tens at 450 to 600 ° C. After performing a patenting process for holding for 2 seconds to obtain an almost complete pearlite structure, wire drawing is performed. However, in this method, since the wire strength before wire drawing is high and the work hardening coefficient at the time of wire drawing is large, breakage during wire drawing or delamination after wire drawing occurs with a true strain of about 3 to 4.

そこで、本発明者らは、炭素濃度0.5%以下の中炭素領域の鋼材を用い、まず種々の条件で圧延・冷却・パテンティング・一次伸線・ボンデ皮膜処理・仕上げ伸線を実施し、直径0.2〜0.4mmであるような種々の強度レベルの鋼線を作製し、これら鋼線の引張強度や鋼組織などを調査した。その結果、次のような知見を得た。   Therefore, the present inventors first performed rolling, cooling, patenting, primary wire drawing, bonder coating treatment, and finish wire drawing under various conditions using steel materials in the medium carbon region with a carbon concentration of 0.5% or less. Steel wires with various strength levels having a diameter of 0.2 to 0.4 mm were prepared, and the tensile strength and steel structure of these steel wires were investigated. As a result, the following knowledge was obtained.

(a)鋼中炭素量を0.3〜0.5%程度まで低減させた鋼素材を用いて、通常の圧延・ステルモア処理によるパテンティング処理を施しても、初析フェライトを抑制することは困難であり、線材の引張強度(TS)は低くなる。このような線材をパテンティング無しに伸線しても、真ひずみ4以上の伸線で所定のTSの高強度ワイヤを得ることは困難である。   (A) Using a steel material with the carbon content in the steel reduced to about 0.3 to 0.5%, suppressing the pro-eutectoid ferrite even if a patenting treatment is performed by a normal rolling / steelmore treatment. It is difficult and the tensile strength (TS) of the wire becomes low. Even if such a wire is drawn without patenting, it is difficult to obtain a high-strength wire having a predetermined TS with a true strain of 4 or more.

(b)鋼中炭素量を0.3〜0.5%程度まで低減させた鋼素材に通常の圧延を施し、ステルモアの風速を高める等して、500℃近傍までの線材の冷却速度を高めることによって、初析フェライトを抑制することが可能であるが、520℃未満まで急冷することによって過冷組織であるベイナイトが生成し、強度と延性が劣化する。このような線材を伸線しても、真ひずみ4以上の伸線で所定のTSの高強度ワイヤを得ることは困難である。   (B) The steel material whose carbon content in the steel is reduced to about 0.3 to 0.5% is subjected to normal rolling to increase the cooling speed of the wire to about 500 ° C. Thus, pro-eutectoid ferrite can be suppressed, but by rapidly cooling to less than 520 ° C., bainite which is a supercooled structure is generated, and strength and ductility deteriorate. Even if such a wire is drawn, it is difficult to obtain a high-strength wire of a predetermined TS by drawing with a true strain of 4 or more.

(c)鋼中炭素量を0.3〜0.5%程度まで低減させた鋼素材を用いて線材に圧延するに際して、仕上げ圧延温度を1000〜1200℃とし、次いで880℃以上960℃以下の温度にて巻き取った後に、520〜580℃の溶融ソルトに浸漬することにより、圧延γ粒径を粗大化させ、初析フェライトとベイナイトを共に抑制し、かつ残部の95%以上をパーライト組織とし、なおかつ、通常は20μmを超えるパーライトブロック粒径を20μm以下とすることが可能である。このような線材に真ひずみが4以上の伸線を施すことにより、高強度でかつデラミネーションの発生のない鋼線を得ることが可能になる。   (C) When rolling into a wire using a steel material whose carbon content in steel is reduced to about 0.3 to 0.5%, the finish rolling temperature is 1000 to 1200 ° C, and then 880 ° C to 960 ° C. After rolling up at a temperature, the rolled γ grain size is coarsened by dipping in a molten salt at 520 to 580 ° C., and both pro-eutectoid ferrite and bainite are suppressed, and the remaining 95% or more is a pearlite structure. In addition, the pearlite block particle size usually exceeding 20 μm can be made 20 μm or less. By applying a wire having a true strain of 4 or more to such a wire, it is possible to obtain a steel wire having high strength and no delamination.

そこで、鋼中炭素量:0.3〜0.5%の鋼を用い、圧延条件及び巻き取り後の冷却条件を変更して初析フェライトとベイナイトの量を種々に調節した圧延線材を作成し、さらに、その線材にパテンティング処理およびブルーイング処理なしに真ひずみが4以上の伸線を施すことにより、0.2〜0.4mmの線径の鋼線を作成した。   Therefore, using a steel with a carbon content of 0.3 to 0.5% in steel, the rolling condition and the cooling condition after winding were changed, and a rolled wire rod with various amounts of proeutectoid ferrite and bainite was prepared. Furthermore, a steel wire having a wire diameter of 0.2 to 0.4 mm was created by subjecting the wire to wire drawing with a true strain of 4 or more without patenting and bluing.

得られた圧延線材について、線材組織や引張強度を調べた。また、伸線後の鋼線について引張強度を調べるとともに、捻回試験を行ってデラミネーション発生の有無を調べた。
まず、高強度の鋼線を得るための条件について検討した。
The obtained rolled wire was examined for wire structure and tensile strength. In addition, the tensile strength of the steel wire after wire drawing was examined, and a twist test was conducted to examine whether delamination occurred.
First, the conditions for obtaining a high-strength steel wire were examined.

図1に、圧線線材の初析フェライト+ベイナイト組織の面積率(分率)と伸線後の引張強度TSの関係を、図2に、伸線後の鋼線の線径とTSの関係を示す。これらの図中、比較例におけるオープンマークはデラミネーションが発生していることを示す。   Fig. 1 shows the relationship between the area ratio (fraction) of the proeutectoid ferrite + bainite structure of the wire rod and the tensile strength TS after wire drawing, and Fig. 2 shows the relationship between the wire diameter of the steel wire after wire drawing and TS. Indicates. In these figures, the open mark in the comparative example indicates that delamination has occurred.

図1より、圧延線材の初析フェライト+ベイナイト組織の面積率を、11、5%以下に低下させることで、引張強度が3000MPa以上の高強度でデラミネーションが発生しない鋼線の製造が可能であることがわかる。   From FIG. 1, by reducing the area ratio of the pro-eutectoid ferrite + bainite structure of the rolled wire to 11, 5% or less, it is possible to produce a steel wire having a tensile strength of 3000 MPa or more and no delamination. I know that there is.

また、図2より、鋼線の引張強度TS(MPa)と線径Dの関係が、次式を満たす範囲になるようにすれば、高強度でデラミネーションの発生のない鋼線を得ることが可能になることがわかる。
3950−D×2600≦TS
Further, from FIG. 2, if the relationship between the tensile strength TS (MPa) of the steel wire and the wire diameter D is in a range satisfying the following formula, a steel wire having high strength and no delamination can be obtained. You can see that it is possible.
3950-D × 2600 ≦ TS

ここで、初析フェライト+ベイナイト組織の面積率は、線材を湿式研磨した後、飽和ピクリン酸によって数秒腐食させ、光学顕微鏡にて×500の倍率で、表層、1/4D、1/2Dを各々5枚撮影し、初析フェライト+ベイナイト組織(白く見える)の面積分率を画像解析し、これらの平均値によって求めた。   Here, the area ratio of the pro-eutectoid ferrite + bainite structure was determined by corroding the wire material with wet picric acid, then corroding with saturated picric acid for several seconds, and using an optical microscope at a magnification of × 500, the surface layer, 1 / 4D, 1 / 2D, Five images were taken, and the area fraction of proeutectoid ferrite + bainite structure (which looks white) was image-analyzed, and the average value thereof was obtained.

次に、高強度で撚り線時にデラミネーションの発生しない鋼線を得るための圧延線材の引張強度及び初析フェライト+ベイナイト組織の面積率の条件について検討した。   Next, the conditions of the tensile strength of the rolled wire rod and the area ratio of pro-eutectoid ferrite + bainite structure to obtain a steel wire having high strength and no delamination when twisted were examined.

図1に示されたTSが2950MPa以上でデラミネーションが発生しない鋼線が得られた圧延線材について、図3に鋼のC含有量と引張強度との関係を示し、図4に鋼のC含有量と初析フェライト+ベイナイト組織の面積率との関係を示す。   FIG. 3 shows the relationship between the C content of steel and the tensile strength, and FIG. 4 shows the C content of steel, with respect to the rolled wire rod in which the steel wire shown in FIG. 1 has a TS of 2950 MPa or more and no delamination occurs. The relationship between the amount and the area ratio of proeutectoid ferrite + bainite structure is shown.

図3より、圧延線材の引張強度TS(MPa)を、C含有量%C(質量%)に応じて次式の関係を満たすようにすれば、高強度でデラミネーションの発生のない鋼線を得られることがわかる。
1000×(%C)+350≦TS≦1000×(%C)+500
From FIG. 3, if the tensile strength TS (MPa) of the rolled wire material satisfies the relationship of the following formula according to the C content% C (mass%), a steel wire having high strength and no occurrence of delamination can be obtained. It turns out that it is obtained.
1000 × (% C) + 350 ≦ TS ≦ 1000 × (% C) +500

また、図4より、初析フェライト+ベイナイト組織の面積率FA(%)を、C含有量%C(質量%)に応じて次式の関係を満たすようにすれば、同様の鋼線を得られることがわかる。
FA≦−35×(%C)+22
Further, from FIG. 4, if the area ratio FA (%) of the pro-eutectoid ferrite + bainite structure satisfies the relationship of the following formula according to the C content% C (mass%), a similar steel wire is obtained. I understand that
FA ≦ −35 × (% C) +22

本発明は、上記の検討結果に基づき、さらに、鋼の化学成分を最適なものにすることによりなされたものであり、以下、本発明についてさらに説明する。
なお、以下の説明で、成分の含有量の%、ppmは、それぞれ質量%、質量ppmを意味する。
まず、本発明に用いられる鋼線材の成分限定理由について説明する。
The present invention was made by further optimizing the chemical composition of steel based on the above examination results, and the present invention will be further described below.
In the following description,% and ppm of the component content mean mass% and mass ppm, respectively.
First, the reasons for limiting the components of the steel wire used in the present invention will be described.

C:0.30〜0.50%
Cは強度の上昇に有効で、且つ経済的な元素であり、C含有量の増加に伴って伸線時の加工硬化量、伸線後の強度が増大する。更に、C量が少ないと圧延線材の初析フェライト量を低減させることが困難となる。従って、本発明ではその下限を0.3%とすることが必要である。一方、C量が多くなり過ぎると線材の強度が高くなりすぎ、伸線中あるいは伸線後における鋼線の靭性・延性を劣化させるため、C量の上限を0.50%とする。好ましい上限は0.45%、より好ましくは0.40%である。
C: 0.30 to 0.50%
C is an effective and economical element for increasing the strength, and the amount of work hardening at the time of wire drawing and the strength after wire drawing increase as the C content increases. Furthermore, if the amount of C is small, it is difficult to reduce the amount of proeutectoid ferrite in the rolled wire rod. Therefore, in the present invention, the lower limit is required to be 0.3%. On the other hand, if the amount of C is too large, the strength of the wire becomes too high and the toughness and ductility of the steel wire during or after wire drawing is deteriorated, so the upper limit of the amount of C is made 0.50%. A preferable upper limit is 0.45%, more preferably 0.40%.

Si:0.10〜0.40%
Siは脱酸剤として有用な元素である。0.10%未満ではその効果が不十分となるため、0.10%以上とした。一方、Siはフェライト生成元素でありスケール剥離性を劣化させる働きがあるため、上限を0.40%とした。
Si: 0.10 to 0.40%
Si is an element useful as a deoxidizer. If the content is less than 0.10%, the effect becomes insufficient, so the content is made 0.10% or more. On the other hand, since Si is a ferrite-forming element and has a function of degrading scale peelability, the upper limit was made 0.40%.

Mn:0.20〜1.00%
MnもSiと同様、脱酸剤として有用な元素であり、その効果を十分なものとするためには0.20%以上が必要である。一方Mnは鋼の焼入性を高めて圧延材の初析フェライト量を低減させる効果がある。また偏析し易い元素でもあるため、過剰に添加するとMnの偏析部にマルテンサイト、ベイナイトなどの過冷組織が生成して伸線加工性が劣化する恐れがある。従って、Mn量の上限を1.00%とする。好ましい上限値は0.80%である。
Mn: 0.20 to 1.00%
Mn, like Si, is an element useful as a deoxidizing agent, and 0.20% or more is necessary to make its effect sufficient. On the other hand, Mn has the effect of increasing the hardenability of the steel and reducing the amount of proeutectoid ferrite in the rolled material. Further, since it is also an element that is easily segregated, if it is added excessively, a supercooled structure such as martensite or bainite may be generated in the segregated portion of Mn and the wire drawing workability may be deteriorated. Therefore, the upper limit of the amount of Mn is set to 1.00%. A preferable upper limit is 0.80%.

B:4〜30ppm
Bは固溶状態でオーステナイト中に存在する場合、粒界に濃化して初析フェライトの析出を抑制する効果がある。Bは窒化物を形成するため、その添加量は、固溶状態のB量を確保するため、N量とのバランスを考慮することが必要である。一方、Bを添加しすぎるとオーステナイト中で粗大なFe(CB)炭化物を生成し、伸線性を低下させる虞がある。これらの関係について、本発明者らが実験を重ね、Bの含有量の最適な範囲として4〜30質量ppmとした。好ましくは6〜20ppm、より好ましくは8〜12ppmである。
B: 4 to 30 ppm
When B exists in the austenite in a solid solution state, it has an effect of concentrating at the grain boundary and suppressing precipitation of proeutectoid ferrite. Since B forms a nitride, it is necessary to consider the balance with the N amount in order to secure the B amount in a solid solution state. On the other hand, when B is added too much, coarse Fe 3 (CB) 6 carbide is generated in austenite, and there is a possibility that the wire drawing property is lowered. About these relations, the present inventors repeated experiment and set it as 4-30 mass ppm as the optimal range of B content. Preferably it is 6-20 ppm, More preferably, it is 8-12 ppm.

N:15〜35ppm
Nは、鋼中でAl、Bと窒化物を生成し、加熱時におけるオーステナイト粒度の粗大化を防止する作用があり、その効果は15ppm以上含有させることによって有効に発揮される。しかし、含有量が多くなり過ぎると、窒化物量が増大し過ぎて、オーステナイト中の固溶B量を低下させる。さらに固溶Nが伸線中の時効を促進する虞がある。従って、Nの含有量を、15〜35ppmの範囲内とした。
N: 15-35 ppm
N produces Al, B and nitride in the steel and has an effect of preventing coarsening of the austenite grain size at the time of heating, and the effect is effectively exhibited by containing 15 ppm or more. However, if the content becomes too large, the amount of nitride increases too much, and the amount of dissolved B in austenite is reduced. Further, solute N may promote aging during wire drawing. Therefore, the N content is within the range of 15 to 35 ppm.

O:15〜35ppm
Oは、Siその他と複合介在物を形成することで、伸線特性への悪影響を及ぼさない軟質介在物を形成させることが可能となる。このような軟質介在物は圧延後に微細分散させることが可能で、ピニング効果によりγ粒径の過度な粗大化を抑制し、パテンティング線材の延性を向上させる効果がある。そのため下限を15ppmより多い値とした。しかし、含有量が多くなり過ぎると、硬質な介在物を形成し、伸線特性が劣化するので、Oの上限を35ppmとした。
O: 15-35 ppm
O forms complex inclusions that do not adversely affect the wire drawing characteristics by forming complex inclusions with Si and others. Such a soft inclusion can be finely dispersed after rolling, and has an effect of suppressing the excessive coarsening of the γ grain size by the pinning effect and improving the ductility of the patenting wire. Therefore, the lower limit is set to a value greater than 15 ppm. However, if the content is too large, hard inclusions are formed and the wire drawing characteristics deteriorate, so the upper limit of O was set to 35 ppm.

Al:0.01%以下
Alの含有量は、硬質非変形のアルミナ系非金属介在物が生成して鋼線の延性劣化と伸線性劣化を招かないように0%を含む0.01%以下と規定した。
Al: 0.01% or less The Al content is 0.01% or less, including 0%, so that hard non-deformable alumina-based nonmetallic inclusions are generated and the steel wire is not ductile and drawn. Stipulated.

Ti:0.01%以下
Tiの含有量は、硬質非変形の酸化物が生成して鋼線の延性劣化と伸線性劣化を招かないように0%を含む0.01%以下と規定した。
Ti: 0.01% or less The content of Ti is specified to be 0.01% or less including 0% so that a hard non-deformable oxide is generated and the steel wire is not ductile and drawn.

なお、不純物であるPとSは特に規定しないが、従来の極細鋼線と同様に延性を確保する観点から、各々0.02%以下とすることが望ましい。   The impurities P and S are not particularly defined, but are each preferably 0.02% or less from the viewpoint of ensuring ductility as in the case of conventional ultra fine steel wires.

本発明に用いられる鋼線材は上記元素を基本成分とするものであるが、更に強度、靭性、延性等の機械的特性の向上を目的として、以下の様な選択的許容添加元素を1種または2種以上、積極的に含有してもよい。
Cr:0.5%以下,Ni:0.5%以下,Co:0.5%以下,Cu:0.2%以下、Mo:0.2%以下、W:0.2%以下。
以下、各元素について説明する。
The steel wire used in the present invention has the above-mentioned elements as basic components, but for the purpose of further improving mechanical properties such as strength, toughness, ductility, etc. Two or more kinds may be positively contained.
Cr: 0.5% or less, Ni: 0.5% or less, Co: 0.5% or less, Cu: 0.2% or less, Mo: 0.2% or less, W: 0.2% or less.
Hereinafter, each element will be described.

Cr:0.5%以下
Crはパーライトのラメラ間隔を微細化し、線材の強度や伸線加工性等を向上させるのに有効な元素である。この様な作用を有効に発揮させるには0.1%以上の添加が好ましい。 一方、Cr量が多過ぎると変態終了時間が長くなり、熱間圧延線材中にマルテンサイトやベイナイトなどの過冷組織が生じる恐れがあるほか、メカニカルでスケーリング性も悪くなるので、その上限を0.5%とした。
Cr: 0.5% or less Cr is an element effective for reducing the lamella spacing of pearlite and improving the strength of the wire and the wire drawing workability. Addition of 0.1% or more is preferable for effectively exhibiting such an action. On the other hand, if the amount of Cr is too large, the transformation end time becomes long, and there is a possibility that a supercooled structure such as martensite or bainite is generated in the hot-rolled wire, and the mechanical scaling property is also deteriorated. 0.5%.

Ni:0.5%以下
Niは線材の強度上昇にはあまり寄与しないが、伸線材の靭性を高める元素である。この様な、作用を有効に発揮させるには0.1%以上の添加が好ましい。 一方、Niを過剰に添加すると変態終了時間が長くなるので、上限値を0.5%とした。
Ni: 0.5% or less Ni does not contribute much to the strength increase of the wire, but is an element that increases the toughness of the wire. Addition of 0.1% or more is preferable for effectively exhibiting such action. On the other hand, if Ni is added excessively, the transformation end time becomes longer, so the upper limit was made 0.5%.

Co:1%以下
Coは、圧延材における初析セメンタイトの析出を抑制するのに有効な元素である。この様な作用を有効に発揮させるには0.1%以上の添加が好ましい。一方、Coを過剰に添加してもその効果は飽和して経済的に無駄であるので、その上限値を0.5%とした。
Co: 1% or less Co is an element effective for suppressing precipitation of pro-eutectoid cementite in the rolled material. Addition of 0.1% or more is preferable for effectively exhibiting such an action. On the other hand, even if Co is added excessively, the effect is saturated and economically useless, so the upper limit was set to 0.5%.

Cu:0.2%以下
Cuは、極細鋼線の耐食性を高める効果がある。この様な作用を有効に発揮させるには0.1%以上の添加が好ましい。しかし過剰に添加すると、Sと反応して粒界中にCuSを偏析するため、線材製造過程で鋼塊や線材などに疵を発生させる。この様な悪影響を防止するために、その上限を0.2%とした。
Cu: 0.2% or less Cu has an effect of increasing the corrosion resistance of the ultrafine steel wire. Addition of 0.1% or more is preferable for effectively exhibiting such an action. However, if added excessively, it reacts with S and segregates CuS in the grain boundaries, so that flaws are generated in the steel ingot, wire, etc. during the wire manufacturing process. In order to prevent such adverse effects, the upper limit was made 0.2%.

Mo:0.2%以下
Moは、極細鋼線の耐食性を高める効果がある。この様な作用を有効に発揮させるには0.1%以上の添加が好ましい。一方、Moを過剰に添加すると変態終了時間が長くなるので、上限値を0.2%とした。
Mo: 0.2% or less Mo has an effect of increasing the corrosion resistance of the ultrafine steel wire. Addition of 0.1% or more is preferable for effectively exhibiting such an action. On the other hand, if Mo is added excessively, the transformation end time becomes long, so the upper limit was made 0.2%.

W:0.2%以下
Wは、極細鋼線の耐食性を高める効果がある。この様な作用を有効に発揮させるには0.1%以上の添加が好ましい。一方、Wを過剰に添加すると変態終了時間が長くなるので、上限値を0.2%とした。
W: 0.2% or less W has an effect of enhancing the corrosion resistance of the ultrafine steel wire. Addition of 0.1% or more is preferable for effectively exhibiting such an action. On the other hand, if W is added excessively, the transformation end time becomes longer, so the upper limit was made 0.2%.

次に、圧延線材の線材の組織、強度及び製造条件について説明する。
上記のような成分からなる鋼のビレット(鋼片)を加熱後、熱間圧延により、最終製品径に応じた線径の圧延線材とする。本発明では、0.2〜0.4mmの範囲の極細鋼線を得るため、圧延線材の線径を3.6〜7mmとする。
Next, the structure, strength, and manufacturing conditions of the rolled wire will be described.
A steel billet (steel piece) composed of the above components is heated and then hot rolled to obtain a rolled wire having a wire diameter corresponding to the final product diameter. In this invention, in order to obtain the ultra fine steel wire in the range of 0.2 to 0.4 mm, the wire diameter of the rolled wire is set to 3.6 to 7 mm.

その際、熱間圧延条件や熱間圧延後の冷却条件を制御することによって、パテンティング後の圧延線材の引張強度TS(MPa)が、下記式1の範囲にあり、
1000×(%C)+350≦TS≦1000×(%C)+500 ・・・ (式1)
かつ、初析フェライトとベイナイトの合計の面積率FAが、下記式2の範囲にあり、
FA≦−35×(%C)+22 ・・・ (式2)
残部の95%以上がパーライト組織であり、該パーライト組織の平均ブロック粒径が20μm以下となるようにする。
At that time, by controlling the hot rolling conditions and the cooling conditions after hot rolling, the tensile strength TS (MPa) of the rolled wire after patenting is in the range of the following formula 1,
1000 × (% C) + 350 ≦ TS ≦ 1000 × (% C) +500 (Formula 1)
And the total area ratio FA of proeutectoid ferrite and bainite is in the range of the following formula 2,
FA ≦ −35 × (% C) +22 (Formula 2)
The remaining 95% or more is a pearlite structure, and the average block particle size of the pearlite structure is 20 μm or less.

圧延線材の引張強度TSを、C含有量に応じて上記のように規定するのは、上記図3に示されるように、式1の関係を満たすようにすれば、高強度でデラミネーションの発生のない鋼線を得ることができるようにするためである。   The tensile strength TS of the rolled wire is defined as described above in accordance with the C content. As shown in FIG. 3 above, if the relationship of Formula 1 is satisfied, delamination occurs with high strength. This is to make it possible to obtain a steel wire without any wire.

また、圧延線材の初析フェライトとベイナイトの面積率を上記のように規定するのは、上記図4に示されるように、伸線加工時に再度パテンティング処理を行わなくても高強度でデラミネーションの発生のない鋼線を得ることができるようにするためである。なお、初析フェライトとベイナイトの合計面積率は、0%であってもよいが、通常の製造条件では、それらの生成を避けることは困難である。   Moreover, the area ratio of pro-eutectoid ferrite and bainite of the rolled wire is defined as described above, as shown in FIG. 4 above, with high strength and delamination without performing patenting treatment again during wire drawing. This is to make it possible to obtain a steel wire that does not generate any of the above. The total area ratio of pro-eutectoid ferrite and bainite may be 0%, but it is difficult to avoid their generation under normal manufacturing conditions.

パーライト組織の面積率を残部の組織の95%以上としたのは、95%未満であると、必要な線材の強度が確保できず、かつ伸線時の延性が低下するためである。残部が100%パーライト組織でもかまわない。   The reason why the area ratio of the pearlite structure is 95% or more of the remaining structure is that if it is less than 95%, the strength of the necessary wire cannot be secured and the ductility at the time of drawing decreases. The balance may be 100% pearlite structure.

パーライト組織の平均ブロック粒径を20μm以下に制限するのは、線材の延性を確保するためである。通常、パーライトブロック粒径はγ粒径の粗大化に伴い大きくなるが、以下に説明するように、溶融ソルトに浸漬するか、急冷後保定することによって、パーライトブロック粒の核生成を促進させ、20μm以下とすることができる。   The reason why the average block particle size of the pearlite structure is limited to 20 μm or less is to ensure the ductility of the wire. Usually, the pearlite block particle size increases with the coarsening of the γ particle size, but as described below, by immersing in molten salt or holding after rapid cooling, promote nucleation of pearlite block particles, It can be 20 μm or less.

ここで、パーライトの平均ブロック粒径は、線材のL断面を、樹脂に埋め込み後切断研磨し、EBSP解析により倍率500倍で、方位差9°の界面で囲まれた領域を一つのブロック粒として解析し、その平均体積から平均粒径として求めた。   Here, the average block particle size of pearlite is that the L section of the wire is embedded in resin and cut and polished, and the region surrounded by the interface with a magnification of 500 times and an orientation difference of 9 ° is defined as one block particle by EBSP analysis. Analysis was performed and the average particle size was determined from the average volume.

この初析フェライトとベイナイトの面積率及びパーライト組織の平均ブロック粒径を以上のように制御するための手段としては、鋼片を、仕上圧延温度1000〜1200℃で熱間圧延し、次いで880℃以上960℃以下の温度にて巻き取った後に、520℃以上580℃以下の溶融ソルトに30s以上浸漬するパテンティング処理を行う方法、あるいは、上記条件で巻き取り後、局所衝風などの手段によって、800℃から600℃までの冷却速度が50℃/s以上200℃/s以下となるように冷却し、その後、520〜580℃の温度域にて30s以上保持するパテンティング処理を行う方法が採用される。   As means for controlling the area ratio of the pro-eutectoid ferrite and bainite and the average block particle size of the pearlite structure as described above, the steel slab is hot-rolled at a finish rolling temperature of 1000 to 1200 ° C, and then 880 ° C. After winding at a temperature of 960 ° C. or lower and after immersing in a molten salt of 520 ° C. or higher and 580 ° C. or lower for 30 seconds or more, or after winding under the above conditions, by means such as local blast , A method of performing a patenting treatment in which the cooling rate from 800 ° C. to 600 ° C. is 50 ° C./s or more and 200 ° C./s or less, and then maintained at a temperature range of 520 to 580 ° C. for 30 s or more. Adopted.

熱延及び巻取条件を上記の範囲とするのは、圧延γ粒径を粗大化させるとともに、Bを固溶状態でオーステナイト中に存在させ、そのようなBが粒界に濃化して初析フェライトの析出を抑制する効果を発揮させるためである。   The hot rolling and coiling conditions are within the above range because the rolled γ grain size is increased and B is present in the austenite in a solid solution state, and such B is concentrated at the grain boundary and is first precipitated. This is because the effect of suppressing the precipitation of ferrite is exhibited.

熱間圧延の仕上げ温度が1000℃未満であると圧延反力が大きくなり、またγ粒径が微細化するため焼入れ性が低下し、初析フェライトの面積率が高くなる。一方、1200℃を超えると巻き取り温度を規定の温度に制御しにくくなる。そのため、1000℃以上1200℃以下と規定した。   When the finishing temperature of hot rolling is less than 1000 ° C., the rolling reaction force increases, and the γ grain size becomes finer, so that the hardenability is lowered and the area ratio of pro-eutectoid ferrite is increased. On the other hand, when it exceeds 1200 ° C., it becomes difficult to control the winding temperature to a specified temperature. Therefore, it is defined as 1000 ° C. or more and 1200 ° C. or less.

また、巻き取り温度が880℃未満であると、Bが炭化物として析出し、初析フェライトの析出を抑制する効果が不十分となり、960℃を超えるとγ粒径が過度に粗大化する。   When the coiling temperature is less than 880 ° C., B precipitates as carbides, and the effect of suppressing the precipitation of pro-eutectoid ferrite becomes insufficient, and when it exceeds 960 ° C., the γ particle size becomes excessively coarse.

溶融ソルトの温度あるいは冷却途中の保持温度を、520〜580℃の温度域に限定したのは、初析フェライトとベイナイトの面積率を上記式2で規定する範囲にするためであり、520℃未満では上部ベイナイト量が急増し、580℃より高ければ初析フェライト量が急増するためである。
また、溶融ソルトに浸漬しない場合、800℃から600℃までの冷却速度が50℃/s以上200℃/s以下となるように冷却するのは、溶融ソルトに浸漬した場合の冷却速度と同様の冷却速度にするためである。
The reason why the temperature of the molten salt or the holding temperature during cooling is limited to the temperature range of 520 to 580 ° C. is to make the area ratio of proeutectoid ferrite and bainite within the range defined by the above formula 2, and less than 520 ° C. Then, the amount of upper bainite increases rapidly, and if it is higher than 580 ° C., the amount of proeutectoid ferrite increases rapidly.
In addition, when not immersed in the molten salt, cooling is performed so that the cooling rate from 800 ° C. to 600 ° C. is 50 ° C./s or more and 200 ° C./s or less, similar to the cooling rate when immersed in the molten salt. This is to achieve a cooling rate.

以上によって、初析フェライトとベイナイトを共に抑制し、かつ残部の95%以上をパーライト組織とし、かつ、巻き取り後の急冷による核生成の促進に起因して、通常は20μmを超えるパーライトブロック粒径を20μm以下と微細化することが可能となる。
なお、図5に本発明による圧延線材の代表的なパーライト組織のSEM観察写真を示す。
As a result, both the pro-eutectoid ferrite and bainite are suppressed, and the remaining 95% or more has a pearlite structure, and the pearlite block particle size usually exceeds 20 μm due to the promotion of nucleation by rapid cooling after winding. Can be reduced to 20 μm or less.
FIG. 5 shows a SEM observation photograph of a typical pearlite structure of the rolled wire rod according to the present invention.

パーライトのラメラ間隔は、変態時の温度に依存し、温度変動が大きいと、ラメラが連続したパーライトを得にくくなる。0.3〜0.5%Cの中炭素鋼においては特にこの傾向が顕著である。通常のステルモアでは、衝風するのみであり、パーライト変態が進行する際の変態潜熱による復熱を抑制できないため、変態中の温度を一定に保つことは難しい。   The lamella spacing of pearlite depends on the temperature at the time of transformation, and if the temperature fluctuation is large, it becomes difficult to obtain pearlite with continuous lamellae. This tendency is particularly remarkable in the medium carbon steel of 0.3 to 0.5% C. In normal stealmore, only a breeze is produced and recuperation due to the latent heat of transformation when pearlite transformation proceeds cannot be suppressed, so it is difficult to keep the temperature during transformation constant.

これに対して、直接溶融塩に浸漬した場合では、抜熱能が高いため、変態時の線材温度をソルト温度に近い温度で一定温度に保つことが可能であり、図5に示したように、ラメラ組織がほぼ連続したパーライト組織を得ることができる。また、強制的に冷却した後、一定温度に保定する場合でも同様である。   In contrast, when directly immersed in the molten salt, the heat removal ability is high, so the wire temperature at the time of transformation can be kept constant at a temperature close to the salt temperature, as shown in FIG. A pearlite structure in which the lamella structure is almost continuous can be obtained. The same applies to the case where the temperature is kept constant after forcibly cooling.

さらに、線材の伸線条件及び、伸線後の鋼線の条件について説明する。
上記のような製造条件で製造され、上記のような成分組成、組織及び強度の条件を満足するインラインパテンティングを施した圧延線材を、その後パテンティング処理およびブルーイング処理などの熱処理を全く施さないで、直径Dが0.2mm以上0.4mm以下になるように、真ひずみが4以上の冷間伸線を施すことにより、引張り強さTS(MPa)が3000MPa以上で、かつ下記式3を満たす極細鋼線にする。
3950−D×2600≦TS ・・・ (式3)
Furthermore, the wire drawing conditions and the steel wire conditions after drawing will be described.
Rolled wire that has been manufactured under the above manufacturing conditions and has been subjected to in-line patenting that satisfies the above-described component composition, structure, and strength conditions, and thereafter is not subjected to any heat treatment such as patenting or blueing. Thus, by performing cold wire drawing with a true strain of 4 or more so that the diameter D is 0.2 mm or more and 0.4 mm or less, the tensile strength TS (MPa) is 3000 MPa or more and Use ultra fine steel wire to satisfy.
3950−D × 2600 ≦ TS (Formula 3)

なお、昨今の燃費向上のための高強度材への要求を考慮すると、望ましいTSは、下記式4を満たすレベルである。
4100−D×2600≦TS ・・・ (式4)
このようにすることにより、図2に示されるように、高強度でデラミネーションの発生のない鋼線を得ることが可能になる。
In consideration of the recent demand for high-strength materials for improving fuel efficiency, desirable TS is a level that satisfies the following formula 4.
4100−D × 2600 ≦ TS (Formula 4)
By doing in this way, as shown in FIG. 2, it becomes possible to obtain a steel wire having high strength and no occurrence of delamination.

ここで、真ひずみを4以上としたのは、本発明の圧延線材径から目的とする0.2〜0.4mmの線径の鋼線を得るためには、4以上の真ひずみが必要なためである。
なお、真ひずみ4以上の伸線を実施するためには一度もしくは複数回の潤滑処理が必要となる。このため、シアン浴による電気黄銅めっきや黄銅の粉体塗装、ボンデ処理などのブルーイングを必要としない潤滑皮膜処理の実施を行うとよい。
Here, the true strain was set to 4 or more in order to obtain a steel wire having a target wire diameter of 0.2 to 0.4 mm from the rolled wire diameter of the present invention. Because.
Note that one or more lubrication treatments are required to perform drawing with a true strain of 4 or more. For this reason, it is advisable to carry out a lubricating film treatment that does not require bluing such as electric brass plating using a cyan bath, powder coating of brass, and a bond treatment.

表1に示す化学組成を有する供試材を熱間圧延した後、種々の巻き取り温度で巻き取り、直ちに種々の温度の溶融ソルトに浸漬するパテンティング、あるいは、局所衝風により、800℃から600℃までの冷却速度が50℃/s以上200℃/s以下となるように強制的に冷却し、一定温度で保持するパテンティング(供試鋼No.8)を行い、直径3.8〜6.7mmの線材を得た。なお、供試鋼No.16では、巻き取り後徐冷した。その後、これらの線材を再パテンティングおよびブルーイング処理をすることなしに直径0.2〜0.4mmまで伸線して鋼線を得た。
得られた線材及び鋼線について引張試験によって引張強さを、鋼線について捻回試験によってデラミネーション特性を調べた。その結果を表2に示す。
After hot rolling the test material having the chemical composition shown in Table 1, it was wound at various winding temperatures and immediately immersed in molten salt at various temperatures, or by local blast from 800 ° C. Forcibly cooled so that the cooling rate to 600 ° C. is 50 ° C./s or more and 200 ° C./s or less, and patenting (test steel No. 8) is held at a constant temperature, and the diameter is 3.8 to A 6.7 mm wire was obtained. The test steel No. No. 16 was gradually cooled after winding. Thereafter, these wires were drawn to a diameter of 0.2 to 0.4 mm without re-patenting and bluing to obtain steel wires.
The tensile strength of the obtained wire and steel wire was examined by a tensile test, and the delamination characteristics of the steel wire were examined by a twist test. The results are shown in Table 2.

表1、2の1〜15が本発明例で、その他は比較例である。同表に見られるように本発明例はいずれも圧延線材のTSが次の式1
1000×(%C)+350≦TS(MPa)≦1000×(%C)+500
の範囲にあり、かつ初析フェライトとベイナイトの面積率FA(%)が次の式2
0≦FA≦−35×(%C)+22
の範囲にあり、4以上の真ひずみにて直径0.2〜0.4mmまで伸線した場合に、引張り強さが次の式3
3950−D×2600≦TS(MPa)
を満たし、かつデラミネーションが発生していない。
1 to 15 in Tables 1 and 2 are examples of the present invention, and others are comparative examples. As can be seen from the table, all the examples of the present invention have the TS of the rolled wire rod as the following formula 1
1000 × (% C) + 350 ≦ TS (MPa) ≦ 1000 × (% C) +500
The area ratio FA (%) of pro-eutectoid ferrite and bainite is expressed by the following formula 2.
0 ≦ FA ≦ −35 × (% C) +22
When the wire is drawn to a diameter of 0.2 to 0.4 mm with a true strain of 4 or more, the tensile strength is expressed by the following formula 3
3950-D × 2600 ≦ TS (MPa)
And delamination does not occur.

これに対し、比較例では、次のような問題があった。
16は、圧延後のインライン熱処理をステルモアによる衝風冷却により実施したことでフェライト+ベイナイト分率を抑制できなかったため、圧延線材のTSが低く、伸線後に狙いのTSを確保できなかった例である。
In contrast, the comparative example has the following problems.
No. 16 was an example in which the TS of the rolled wire rod was low and the target TS could not be secured after wire drawing because the inline heat treatment after rolling was performed by blast cooling with stealmore, and the ferrite + bainite fraction could not be suppressed. is there.

17、18は各々、最終圧延温度と巻き取り温度が低かったために、圧延γ粒径が微細化し、フェライト+ベイナイト分率を抑制できなかった例である。
19と20はC量が高すぎたために圧延線材のTSが高く、伸線中に延性が劣化して断線した例であり、21と22はC量が低いため、圧延線材のTSが低く、伸線後に狙いのTSを確保できなかった例である。
Examples 17 and 18 are examples where the final rolling temperature and the coiling temperature were low, so that the rolled γ grain size was reduced and the ferrite + bainite fraction could not be suppressed.
19 and 20 are examples in which the TS of the rolled wire is high because the amount of C is too high, and the ductility deteriorates during wire drawing, and 21 and 22 are examples in which the TS of the rolled wire is low because the C amount is low. This is an example in which the target TS could not be secured after wire drawing.

23は溶融ソルト処理時のソルト温度が低すぎたためベイナイトが多量に発生した例である。24はB量が少なすぎたため、フェライト+ベイナイト分率が高かった例、25はB量が多すぎたため、B炭窒化物の析出が多く、B添加の効果(フェライト+ベイナイト分率の低減)を得られなかった例である。   No. 23 is an example in which a large amount of bainite was generated because the salt temperature during the melted salt treatment was too low. No. 24 is an example in which the B content was too small, and the ferrite + bainite fraction was high, and 25 was an excessive amount of B, so there was much precipitation of B carbonitride, and the effect of B addition (reduction of the ferrite + bainite fraction) This is an example that could not be obtained.

伸線工程中にパテンティングおよびブルーイング処理を施さなくとも製造可能な、強度・引張強さ等の機械的特性に優れた鋼線および同鋼線を製造するための線材、およびこれらの製造方法を提供するものであり、産業上の効果は極めて顕著なものがある。   A steel wire excellent in mechanical properties such as strength and tensile strength that can be produced without performing patenting and bluing treatment during the wire drawing process, and a wire for producing the steel wire, and methods for producing the same The industrial effect is extremely remarkable.

Claims (6)

質量%、質量ppmで、C :0.30〜0.50%、Si:0.10〜0.40%、Mn:0.20〜1.0%、B:4〜30ppm、N:15〜35ppm、O:15〜35ppm、Al:0.01%以下(0%を含む)、Ti:0.01%以下(0%を含む)を含有し、残部鉄および不可避的不純物よりなり、パテンティング後の引張強さTS(MPa)が、下記式1の範囲にあり、
1000×(%C)+350≦TS≦1000×(%C)+500
・・・ (式1)
かつ、初析フェライトとベイナイトの面積率FA(%)が下記式2の範囲にあり、
FA≦−35×(%C)+22 ・・・ (式2)
残部の95%以上がパーライト組織であり、該パーライト組織の平均ブロック粒径が20μm以下であることを特徴とする線径3.6〜7mmの高強度鋼線用線材。
% By mass, ppm by mass, C: 0.30 to 0.50%, Si: 0.10 to 0.40%, Mn: 0.20 to 1.0%, B: 4 to 30 ppm, N: 15 Contains 35 ppm, O: 15-35 ppm, Al: 0.01% or less (including 0%), Ti: 0.01% or less (including 0%), and consists of the balance iron and unavoidable impurities, patenting Later tensile strength TS (MPa) is in the range of the following formula 1,
1000 × (% C) + 350 ≦ TS ≦ 1000 × (% C) +500
... (Formula 1)
And the area ratio FA (%) of pro-eutectoid ferrite and bainite is in the range of the following formula 2,
FA ≦ −35 × (% C) +22 (Formula 2)
95% or more of the balance is a pearlite structure, and the average block particle size of the pearlite structure is 20 μm or less, a wire rod for high strength steel wire having a wire diameter of 3.6 to 7 mm.
更に、質量%で、Cr:0.5%以下、Ni:0.5%以下、Co:0.5%以下、Cu:0.2%以下、Mo:0.2%以下、W:0.2%以下よりなる群から選択される少なくとも1種以上を含有することを特徴とする請求項1に記載の高強度鋼線用線材。   Furthermore, in mass%, Cr: 0.5% or less, Ni: 0.5% or less, Co: 0.5% or less, Cu: 0.2% or less, Mo: 0.2% or less, W: 0.0. The wire for high-strength steel wire according to claim 1, comprising at least one selected from the group consisting of 2% or less. 請求項1または2に記載の線材に、熱処理を施すことなしに伸線を行うことにより、直径D(mm)を0.2〜0.4mmとした鋼線であって、引張強度TS(MPa)が3000MPa以上で、かつ下記式3を満たすことを特徴とするデラミネーションの発生しない高強度極細鋼線。
3950−D×2600≦TS ・・・ (式3)
A steel wire having a diameter D (mm) of 0.2 to 0.4 mm by drawing the wire according to claim 1 or 2 without performing a heat treatment, wherein the tensile strength TS (MPa ) Is 3000 MPa or more, and satisfies the following formula 3. A high-strength ultrafine steel wire free from delamination.
3950−D × 2600 ≦ TS (Formula 3)
請求項1または2に記載の鋼成分の鋼片を熱間圧延し、仕上げ圧延温度を1000〜1200℃とし、次いで880〜960℃の温度にて巻き取った後に、520〜580℃の温度の溶融ソルトに30s以上浸漬する工程を含むパテンティング処理を施すことを特徴とする請求項1または2に記載の高強度鋼線用線材の製造方法。   The steel slab of the steel component according to claim 1 or 2 is hot-rolled, the finish rolling temperature is 1000 to 1200 ° C, and then wound at a temperature of 880 to 960 ° C. The method for producing a high-strength steel wire according to claim 1 or 2, wherein a patenting treatment including a step of immersing in a molten salt for 30 seconds or more is performed. 請求項1または2に記載の鋼成分の鋼片を熱間圧延し、仕上げ圧延温度を1000〜1200℃とし、次いで880〜960℃の温度にて巻き取った後に、800℃から600℃までの冷却速度を50〜200℃/sとし、その後、520〜580℃の温度域にて30s以上保持する工程を含むパテンティング処理を施すことを特徴とする請求項1または2に記載の高強度鋼線用線材の製造方法。   The steel slab of the steel component according to claim 1 or 2 is hot-rolled, the finish rolling temperature is 1000 to 1200 ° C, and then wound at a temperature of 880 to 960 ° C, and then 800 ° C to 600 ° C. The high-strength steel according to claim 1 or 2, wherein the cooling rate is set to 50 to 200 ° C / s, and thereafter a patenting process including a step of holding at a temperature range of 520 to 580 ° C for 30 s or more is performed. A method for manufacturing a wire rod. 請求項4または5に記載の方法によって製造された線材に、熱処理を施すことなしに、真ひずみ4%以上の条件で直径D(mm)が0.2〜0.4mmの範囲になるまで伸線を行うことを特徴とする請求項3に記載の高強度極細鋼線の製造方法。   The wire rod manufactured by the method according to claim 4 or 5 is stretched until the diameter D (mm) is in a range of 0.2 to 0.4 mm under a condition of a true strain of 4% or more without performing heat treatment. The method for producing a high-strength ultrafine steel wire according to claim 3, wherein the wire is formed.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014037162A1 (en) * 2012-09-07 2014-03-13 Compagnie Generale Des Etablissements Michelin High-drawability steel wire with a proportion by mass of carbon of a value which is greater than or equal to 0.4 % and less than or equal to 0.5 %
JP2014055316A (en) * 2012-09-11 2014-03-27 Kobe Steel Ltd Wire material for high strength steel wire
JP2017193732A (en) * 2016-04-18 2017-10-26 新日鐵住金株式会社 Hot-rolled wire rod for high strength steel wire and production method therefor
US9884356B2 (en) 2012-09-07 2018-02-06 Compagnie Generale Des Establissements Michelin Wire drawing method
CN108699650A (en) * 2016-07-05 2018-10-23 新日铁住金株式会社 Rolled wire

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7205324B2 (en) 2019-03-19 2023-01-17 株式会社リコー Head module, head unit, head for ejecting liquid, device for ejecting liquid

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11302743A (en) * 1998-04-16 1999-11-02 Nippon Steel Corp Production of high strength steel wire
JP2000119756A (en) * 1998-10-16 2000-04-25 Pohang Iron & Steel Co Ltd Wire rod for high strength steel wire excellent in wire drawability and production of high strength steel wire
WO2001075186A1 (en) * 2000-04-04 2001-10-11 Nippon Steel Corporation Hot rolled wire or steel bar for machine structural use capable of dispensing with annealing, and method for producing the same
JP2002061085A (en) * 2000-08-10 2002-02-28 Kobe Steel Ltd Wire rope having excellent wear resistance and fatigue characteristics, steel wire and steel material
JP2004359992A (en) * 2003-06-03 2004-12-24 Nippon Steel Corp Wire rod for high strength steel wire, high strength steel wire, and their production method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11302743A (en) * 1998-04-16 1999-11-02 Nippon Steel Corp Production of high strength steel wire
JP2000119756A (en) * 1998-10-16 2000-04-25 Pohang Iron & Steel Co Ltd Wire rod for high strength steel wire excellent in wire drawability and production of high strength steel wire
WO2001075186A1 (en) * 2000-04-04 2001-10-11 Nippon Steel Corporation Hot rolled wire or steel bar for machine structural use capable of dispensing with annealing, and method for producing the same
JP2002061085A (en) * 2000-08-10 2002-02-28 Kobe Steel Ltd Wire rope having excellent wear resistance and fatigue characteristics, steel wire and steel material
JP2004359992A (en) * 2003-06-03 2004-12-24 Nippon Steel Corp Wire rod for high strength steel wire, high strength steel wire, and their production method

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014037162A1 (en) * 2012-09-07 2014-03-13 Compagnie Generale Des Etablissements Michelin High-drawability steel wire with a proportion by mass of carbon of a value which is greater than or equal to 0.4 % and less than or equal to 0.5 %
FR2995248A1 (en) * 2012-09-07 2014-03-14 Michelin & Cie HIGH TREFILABILITY STEEL WIRE INCLUDING A MASS CARBON RATE INCLUDED BETWEEN 0.4% AND 0.5% TERMINALS INCLUDED
CN104641035A (en) * 2012-09-07 2015-05-20 米其林集团总公司 High-drawability steel wire with a proportion by mass of carbon of a value which is greater than or equal to 0.4 % and less than or equal to 0.5 %
US9884356B2 (en) 2012-09-07 2018-02-06 Compagnie Generale Des Establissements Michelin Wire drawing method
CN104641035B (en) * 2012-09-07 2018-12-14 米其林集团总公司 The tire of vehicle for heavy duty vehicle type
JP2014055316A (en) * 2012-09-11 2014-03-27 Kobe Steel Ltd Wire material for high strength steel wire
JP2017193732A (en) * 2016-04-18 2017-10-26 新日鐵住金株式会社 Hot-rolled wire rod for high strength steel wire and production method therefor
CN108699650A (en) * 2016-07-05 2018-10-23 新日铁住金株式会社 Rolled wire

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