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CN111315905A - Method for producing cold-drawn wire - Google Patents

Method for producing cold-drawn wire Download PDF

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Publication number
CN111315905A
CN111315905A CN201780096303.XA CN201780096303A CN111315905A CN 111315905 A CN111315905 A CN 111315905A CN 201780096303 A CN201780096303 A CN 201780096303A CN 111315905 A CN111315905 A CN 111315905A
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Prior art keywords
esr
wire
container
molten metal
melt
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Inventor
彼得·洛夫罗斯
大卫·桑莱布恩
扬·皮特斯
奥拉·埃里克松
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Suzuki Gafeton Co Ltd
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Suzuki Gafeton Co Ltd
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    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
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Abstract

本申请提供一种由颗粒冶金钢生产冷拔线材的方法,该方法包括以下步骤:‑制备大量的熔融金属,该熔融金属包含(按重量%计):C 0.03‑0.15,Si 0.01‑1.2,Mn 0.1‑1.5,Cr 15‑20,Ni 5‑10,A1 0.5‑1.5,任选地选自以下组中的最多2种元素:N、P、S、Cu、Co、W、Mo、Nb、Ti、Zr、Ta、B、Be、Bi、Se、Mg、Ca、Hf、V和REM,以及使用电渣精炼和雾化以提供金属粉末;‑用金属粉末填充容器并且将容器密封;‑将容器压实以提供全密度坯料;‑将坯料热加工并且通过线材轧制精加工;‑在减少至少30%面积的情况下冷拔退火的线材。The present application provides a method for producing cold drawn wire from granular metallurgical steel, the method comprising the steps of:-Preparing a large amount of molten metal comprising (by weight %): C 0.03-0.15, Si 0.01-1.2, Mn 0.1-1.5, Cr 15-20, Ni 5-10, A1 0.5-1.5, optionally up to 2 elements selected from the group: N, P, S, Cu, Co, W, Mo, Nb, Ti, Zr, Ta, B, Be, Bi, Se, Mg, Ca, Hf, V and REM, and using electroslag refining and atomization to provide metal powder; ‑fill the container with the metal powder and seal the container; Containers are compacted to provide full density billets; ‑ billets are hot worked and finished by wire rolling; ‑ annealed wire is cold drawn with at least 30% area reduction.

Description

生产冷拔线材的方法Method for producing cold drawn wire

技术领域technical field

本发明涉及一种用于制造可沉淀硬化的不锈钢(特别是被称为17-7PH型号的不锈钢)的冷拔线材和线材弹簧的方法。The present invention relates to a method for making cold drawn wire and wire springs of precipitation hardenable stainless steel, in particular of the type known as 17-7PH.

背景技术Background technique

在20世纪40年代,开发了含有约17%的Cr、约7%的Ni和任何沉淀硬化元素(通常为Al)的沉淀不锈钢。该沉淀不锈钢公开于1950年3月的《铁器时代(Iron Age)》第79-83页的一篇文章中。在该文章中已经提出了将钢作为弹簧材料的适合性。良好的弹簧特征与良好的耐腐蚀性相组合使钢广泛地用作腐蚀性环境中的弹簧材料。那种类型的环境是用于柴油发动机(更具体地为涡轮柴油发动机)的喷射泵。用于此目的的弹簧必须具有17-7PH钢所具有的良好的耐腐蚀性,以及很高的弹簧耐疲劳性。In the 1940s, precipitation stainless steels were developed containing about 17% Cr, about 7% Ni and any precipitation hardening elements (usually Al). This precipitated stainless steel is disclosed in an article in Iron Age, March 1950, pages 79-83. The suitability of steel as a spring material has been suggested in this article. Good spring characteristics combined with good corrosion resistance make steel widely used as a spring material in corrosive environments. An environment of that type is an injection pump for a diesel engine, more specifically a turbo diesel engine. Springs used for this purpose must have the good corrosion resistance of 17-7PH steel, as well as high spring fatigue resistance.

耐疲劳性在很大程度上取决于弹簧线材的表面。为使弹簧具有高耐疲劳性,线材不应具有可引起疲劳失效的任何可见的缺陷。表面层也不应包含也可引起失效的任何大的夹渣或包含较小夹渣的大累积物的大区域。Fatigue resistance largely depends on the surface of the spring wire. For the spring to have high fatigue resistance, the wire should not have any visible defects that could cause fatigue failure. The surface layer should also not contain any large slag inclusions or large areas containing large accumulations of smaller slag inclusions that could also cause failure.

US 6,383,316公开了一种用于制造冷拔线材的方法,其中将铸钢重熔并使其经受ESR处理。将ESR铸锭热加工,通过线材轧制对其精加工。将轧制的线材酸洗并且冷拔。采用ESR处理以避免大夹渣和包含较小夹渣的大累积物的大区域。与以前的工艺相比,这是很大的改进。US 6,383,316 discloses a method for making cold drawn wire wherein cast steel is remelted and subjected to ESR treatment. The ESR ingot is hot worked and finished by wire rolling. The rolled wire is pickled and cold drawn. ESR treatment was used to avoid large slag inclusions and large areas containing large accumulations of smaller slag inclusions. This is a great improvement over the previous process.

具体实施方式Detailed ways

本发明提出了一种制造17-7PH弹簧线材和线材弹簧的新途径。该新途径包括铸造大量的熔融金属以提供铸锭;将铸锭电渣精炼以提供ESR熔体;将ESR熔体雾化以提供金属粉末;将粉末热等静压成坯料;以及将坯料加工成线材。该新程序进一步减小了夹杂物的尺寸。此外,它基本上去除了包含较小夹渣的大累积物的大区域。The present invention proposes a new way to manufacture 17-7PH spring wire and wire spring. The new approach includes casting large quantities of molten metal to provide ingots; electroslag refining the ingots to provide ESR melts; atomizing the ESR melts to provide metal powders; hot isostatic pressing of the powders into billets; and processing the billets into wire. The new procedure further reduces the size of the inclusions. Furthermore, it essentially removes large areas containing large accumulations of smaller slag inclusions.

更具体地,该方法包括制备大量的熔融金属,该熔融金属包含(按重量%计):More specifically, the method includes preparing a quantity of molten metal comprising (by weight %):

Figure BDA0002467251190000011
Figure BDA0002467251190000011

Figure BDA0002467251190000021
Figure BDA0002467251190000021

任选地optionally

选自以下组中的最多2种元素:N、P、S、Cu、Co、W、Mo、Nb、Ti、Zr、Ta、B、Be、Bi、Se、Mg、Ca、Hf、V、REM,和Up to 2 elements selected from the group: N, P, S, Cu, Co, W, Mo, Nb, Ti, Zr, Ta, B, Be, Bi, Se, Mg, Ca, Hf, V, REM ,and

除杂质外的余量Fe。The balance Fe excluding impurities.

根据本发明的一个实施例,有意地将钢与少量的N,优选地0.005重量%-0.15重量%,更优选地0.01重量%-0.15重量%的N合金化。还可有意地将钢与少量的Ti、V或Nb合金化。Ti、V或Nb优选地按重量%计为:According to one embodiment of the invention, the steel is intentionally alloyed with a small amount of N, preferably 0.005-0.15 wt%, more preferably 0.01-0.15 wt% N. Steel can also be intentionally alloyed with small amounts of Ti, V or Nb. Ti, V or Nb are preferably in % by weight:

Ti 0.01-0.1Ti 0.01-0.1

Nb 0.01-0.1Nb 0.01-0.1

V 0.01-0.1V 0.01-0.1

优选将将Ti、V或Nb的总量限制为0.01重量%-0.2重量%。The total amount of Ti, V or Nb is preferably limited to 0.01% by weight to 0.2% by weight.

优选地,将任选元素限制为(按重量%计):Preferably, the optional elements are limited to (by weight %):

Figure BDA0002467251190000022
Figure BDA0002467251190000022

Figure BDA0002467251190000031
Figure BDA0002467251190000031

REM包括元素Sc、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Y、Tb、Dy、Ho、Er、Tm、Yb和Lu中的至少一种。REM includes at least one of the elements Sc, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Y, Tb, Dy, Ho, Er, Tm, Yb, and Lu.

将大量的熔融金属铸造成铸锭的形状,或优选地铸造成被切断的线束。此后,将铸锭或切断的线束电渣精炼,即所谓的ESR重熔优选地在热加工成电极的形状之后。Large quantities of molten metal are cast into the shape of ingots, or preferably into severed strands. Thereafter, electroslag refining of the ingot or cut strands, so-called ESR remelting, is preferably followed by hot working into the shape of the electrode.

ESR代表电渣精炼,也称为电渣重熔。在ESR处理中,可使用常规炉渣混合物,该常规炉渣混合物根据已知技术进行使用并且在ESR重熔过程中形成熔体,其中将要重熔的电极逐滴熔化,使得液滴将通过炉渣熔体下沉到下面的熔融金属(ESR熔体)池中。例如,可使用炉渣混合物,该炉渣混合物本身是已知的,并且含有各自为约30%的CaF2、CaO和Al2O3,并且通常含有一定量的石灰级分中的MgO以及百分之一或百分之几的SiO2ESR stands for Electroslag Refining, also known as Electroslag Remelting. In the ESR process, a conventional slag mixture can be used, which is used according to known techniques and forms a melt during the ESR remelting process, wherein the electrodes to be remelted are melted dropwise so that the droplets will pass through the slag melt Sink into the pool of molten metal (ESR melt) below. For example, a slag mixture can be used, which is known per se and contains approximately 30 % each of CaF2 , CaO, and Al2O3 , and typically contains some amount of MgO in the lime fraction and % One or a few percent of SiO 2 .

在根据本发明的熔化电极由包含不同尺寸的夹渣的不锈17-7PH钢组成的情况下,ESR熔体将获得与重熔操作之前不同的炉渣图像。在重熔操作之前,ESR炉渣似起到了筛查钢中存在的较大炉渣颗粒的作用。至少这对于已经证明对弹簧线材的疲劳强度具有有害影响的那些炉渣(即CaO、Al2O3和MgO类型的炉渣)似乎是正确的。尽管同时较小夹渣变得更均匀地分布,并且炉渣累积物的可能区域变得更小并且因此变得更加无害,但是重熔材料中这种类型的较小夹渣的量仅受到较小的影响。In the case where the melting electrode according to the invention consists of stainless 17-7PH steel containing slag inclusions of different sizes, the ESR melt will obtain a different slag image than before the remelting operation. The ESR slag appears to act as a screen for larger slag particles present in the steel prior to the remelting operation. At least this seems to be true for those slags that have been shown to have a detrimental effect on the fatigue strength of the spring wire (ie slags of the CaO, Al2O3 and MgO types ) . Although at the same time the smaller slag inclusions become more evenly distributed and the possible areas of slag accumulation become smaller and thus more harmless, the amount of this type of smaller slag inclusions in the remelted material is only limited by a greater small impact.

在ESR重熔操作期间,可损失一定量的在熔融金属的初始制备时添加的铝。因此,在ESR重熔操作时,应向熔池中供应更多的铝以弥补任何损失,使得在ESR重熔操作后获得的ESR熔体将含有0.5-1.5Al。During an ESR remelting operation, a certain amount of aluminum added during the initial preparation of the molten metal can be lost. Therefore, during the ESR remelting operation, more aluminum should be supplied to the molten pool to make up for any losses, so that the ESR melt obtained after the ESR remelting operation will contain 0.5-1.5 Al.

将ESR熔体雾化以提供金属粉末。雾化优选地通过气体雾化进行。可通过氮气和/或氩气的射流来实行气体雾化。The ESR melt is atomized to provide metal powder. The atomization is preferably carried out by gas atomization. Gas atomization can be carried out by a jet of nitrogen and/or argon.

优选地,在熔化炉中制备ESR熔体,在这种类型的熔化炉中,通过炉底部中的排放口将液态金属排放到炉下方的雾化腔室。例如,使用来自ALD真空技术有限责任公司(ALDVacuum technologies GMBH)的ESR-CIG,但进行雾化以提供金属粉末,而不是喷射成形。Preferably, the ESR melt is prepared in a melting furnace, in which the liquid metal is discharged through a discharge opening in the furnace bottom to an atomization chamber below the furnace. For example, ESR-CIG from ALD Vacuum Technologies GMBH is used, but atomized to provide metal powders instead of spray forming.

替代地,可在不将熔体暴露于空气的情况下将ESR熔体输送到在WO2013129996中描述的类型的熔化炉,该文献通过引用的方式在此并入。在这种类型的炉中,也通过炉底部中的排放口将液态金属排放到炉下方的雾化腔室。可通过惰性气体、真空或覆盖熔体表面的炉渣来保护炉中的ESR熔体。Alternatively, the ESR melt can be delivered to a melting furnace of the type described in WO2013129996, which is hereby incorporated by reference, without exposing the melt to air. In this type of furnace, the liquid metal is also discharged to the atomizing chamber below the furnace through a discharge opening in the furnace bottom. The ESR melt in the furnace can be protected by inert gas, vacuum or slag covering the melt surface.

一种替代方案是具有可倾动的ESR炉和单独的中间包,该可倾动的ESR炉和单独的中间包两者均布置在含有保护性气氛的包围腔室中。雾化腔室布置在中间包下方。此外,在该炉和中间包的组合中,熔融金属的氧气暴露得以最小化。An alternative is to have a tiltable ESR furnace and a separate tundish, both arranged in an enclosed chamber containing a protective atmosphere. The atomization chamber is arranged below the tundish. Furthermore, in this furnace and tundish combination, oxygen exposure of the molten metal is minimized.

在雾化之后,将雾化的粉末优选地在保护性气氛中冷却以避免再氧化。任选地,可将雾化的粉末筛分到期望的粉末规格。例如,最大250μm。After atomization, the atomized powder is preferably cooled in a protective atmosphere to avoid re-oxidation. Optionally, the atomized powder can be sieved to the desired powder size. For example, up to 250 μm.

用金属粉末填充容器。在填充后,将容器密封。此后,任选地在冷等静压机(例如Asea QI 100)中以至少1000巴,优选地大约4000巴的压力将容器压实。此后,将容器任选地放置在预热炉中,在该预热炉中,在不经受任何外部施加的压力的情况下将温度逐步升高至900℃-1250℃(例如1130℃)的温度。此后,将容器转移至热等静压机(例如HIPen AseaQI 80),在该热等静压机中,在900℃-1250℃(例如1150℃)的温度下施加至少高于500巴(例如1000巴)的压力。在热等静压机中压实容器提供了全密度坯料。优选地,控制温度使得将材料在不存在液相的情况下固结。冷等静压步骤以及随后的预热步骤主要是出于工艺经济的原因而使用,并且很可能将密封的容器直接转移到热等静压机而无需事先进行冷压或预热。Fill the container with metal powder. After filling, the container is sealed. Thereafter, the vessel is optionally compacted in a cold isostatic press (eg Asea QI 100) at a pressure of at least 1000 bar, preferably about 4000 bar. Thereafter, the vessel is optionally placed in a preheated oven in which the temperature is gradually increased to a temperature of 900°C-1250°C (eg 1130°C) without being subjected to any externally applied pressure . Thereafter, the vessel is transferred to a hot isostatic press (eg HIPen AseaQI 80) in which at least more than 500 bar (eg 1000 bar) is applied at a temperature of 900°C-1250°C (eg 1150°C) bar) pressure. Compaction of the vessel in a hot isostatic press provides a full density billet. Preferably, the temperature is controlled such that the material is consolidated in the absence of a liquid phase. The cold isostatic pressing step followed by the preheating step is mainly used for reasons of process economy and it is possible to transfer the sealed vessel directly to the hot isostatic pressing without prior cold pressing or preheating.

此后,将来自热等静压机的坯料热加工成杆,然后将该杆磨削并热轧成线材。此后,通过机械除鳞和/或化学除鳞(酸洗)将热轧成线材的线材除鳞。Thereafter, the billets from the hot isostatic press are hot worked into rods, which are then ground and hot rolled into wire rods. Thereafter, the hot rolled wire rod is descaled by mechanical descaling and/or chemical descaling (pickling).

然后将除鳞的线材在900℃-1100℃范围内的温度下退火0.5小时-2小时。在减少至少30%面积的情况下冷拔退火的线材。The descaled wire is then annealed at temperatures ranging from 900°C to 1100°C for 0.5 hours to 2 hours. The annealed wire is cold drawn with at least a 30% area reduction.

可将冷拔线材旋转成弹簧,优选地为螺旋形状的弹簧。将弹簧在450℃-500℃的温度下适当地沉淀硬化0.5小时-2小时,然后在空气中冷却。The cold drawn wire can be rotated into a spring, preferably a coil-shaped spring. The springs are suitably precipitation hardened at a temperature of 450°C-500°C for 0.5 hours-2 hours and then cooled in air.

成品弹簧中的材料的结构包含50体积%-70体积%的回火马氏体(该回火马氏体在马氏体中含有铝和镍的沉淀相(优选地为AlNi3))、残余奥氏体和最大5%的δ-铁素体。The structure of the material in the finished spring contains 50-70 vol% of tempered martensite (which contains precipitation phases (preferably AlNi3 ) of aluminum and nickel in martensite), residual Austenite and max 5% delta-ferrite.

冷拔弹簧线材的横截面形状可以是圆形的。然而,本发明不唯一地限于具有此类横截面的线材,而是还可应用于具有其他形状的线材,即具有椭圆形横截面的线材,其可在旋转成形为螺旋形状的成品弹簧中提供更有利的张力分布。还可设想矩形横截面。The cross-sectional shape of the cold drawn spring wire may be circular. However, the present invention is not exclusively limited to wires having such a cross-section, but can also be applied to wires having other shapes, ie wires having an oval cross-section, which can be provided in a finished spring rotationally shaped into a helical shape More favorable tension distribution. A rectangular cross-section is also envisaged.

根据本发明的修改方案,该新途径包括将大量的熔融金属雾化以提供金属粉末;将粉末热等静压成坯料;以及将坯料加工成线材,从而提供一种由颗粒冶金钢生产冷拔线材的方法,该方法包括以下步骤:According to a modification of the present invention, the new approach includes atomizing a mass of molten metal to provide a metal powder; hot isostatic pressing the powder into a billet; and processing the billet into wire, thereby providing a cold-drawn production of metallurgical steel from pellets A method of wire, the method comprising the following steps:

-制备大量的熔融金属,该熔融金属包含(按重量%计):- producing a quantity of molten metal comprising (in % by weight):

Figure BDA0002467251190000051
Figure BDA0002467251190000051

任选地optionally

选自以下组中的最多2种元素:N、P、S、Cu、Co、W、Mo、Nb、Ti、Zr、Ta、B、Be、Bi、Se、Mg、Ca、Hf、V和REM,Up to 2 elements selected from the group: N, P, S, Cu, Co, W, Mo, Nb, Ti, Zr, Ta, B, Be, Bi, Se, Mg, Ca, Hf, V, and REM ,

以及,as well as,

除杂质外的余量Fe;The balance Fe except impurities;

-将熔融金属雾化,从而提供金属粉末;- Atomizing molten metal to provide metal powder;

-用金属粉末填充容器;- filling the container with metal powder;

-将容器密封;- seal the container;

-任选地在冷等静压机中将所述容器压实;- optionally compacting the container in a cold isostatic press;

-任选地将所述容器预热;- optionally preheating the container;

-在热等静压机中将容器压实以提供全密度坯料;- compaction of the container in a hot isostatic press to provide a full density billet;

-将坯料热加工并且通过线材轧制精加工;- hot working the billet and finishing by wire rolling;

-将所得的轧制线材除鳞;- descaling the resulting rolled wire;

-将除鳞的线材退火;以及- annealing the descaled wire; and

-在减少至少30%面积的情况下冷拔退火的线材。- Cold drawn annealed wire with at least 30% area reduction.

Claims (7)

1. A method of producing a cold drawn wire from a particulate metallurgical steel, the method comprising the steps of:
-preparing a quantity of molten metal comprising (in wt%):
Figure FDA0002467251180000011
optionally, optionally
Up to 2 elements selected from the group: n, P, S, Cu, Co, W, Mo, Nb, Ti, Zr, Ta, B, Be, Bi, Se, Mg, Ca, Hf, V and REM,
and the number of the first and second groups,
the balance Fe except impurities;
-casting the prepared molten metal into the shape of an ingot or, preferably, into a strand that is cut;
-electroslag refining (so-called ESR remelting) the ingot or the cut strand, preferably after hot working into the shape of an electrode, thereby providing an ESR melt or for forming and remelting an ESR ingot;
-atomizing the ESR melt, thereby providing a metal powder;
-filling a container with said metal powder;
-sealing the container;
-optionally compacting the container in a cold isostatic press;
-optionally preheating the vessel;
-compacting the container in a hot isostatic press to provide a full density billet;
-hot working and finishing the blank by wire rod rolling;
-descaling the obtained rolled wire;
-annealing the descaled wire; and
-cold drawing the annealed wire with at least a 30% area reduction.
2. The method of claim 1, wherein the quantity of molten metal comprises (in weight%):
n is 0.005-0.15, preferably 0.01-0.15.
3. The method of claim 1, wherein the quantity of molten metal comprises (in weight%):
Figure FDA0002467251180000021
4. the method of any one of claims 1 to 3, wherein the quantity of molten metal comprises at least one of the following elements:
Ti 0.01-0.1;
Nb 0.01-0.1;
V 0.01-0.1;
and satisfies the conditions
Ti+Nb+V 0.01-0.2。
5. The method of any of claims 1-4, wherein the method further comprises:
-atomizing the ESR melt in an atomization chamber below an ESR furnace.
6. The method of any of claims 1-4, wherein the method further comprises:
-protecting the remelted ESR ingot in an inert gas, in a vacuum or by slag covering the surface of the ESR melt;
-atomizing the remelted ESR ingot by discharging the liquid metal to an atomizing chamber through a discharge opening in the bottom of a furnace containing the melt.
7. A method for producing a spring, the method comprising the steps of:
-producing a cold drawn wire according to any one of claims 1 to 6;
-rotationally forming a spring, preferably a spiral shape, from the cold drawn wire;
-precipitation hardening the spring, preferably at a temperature of 450 ℃ -500 ℃ for 0.5-2 hours.
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