CN114555837A - 模压淬火方法 - Google Patents

模压淬火方法 Download PDF

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CN114555837A
CN114555837A CN202080071232.XA CN202080071232A CN114555837A CN 114555837 A CN114555837 A CN 114555837A CN 202080071232 A CN202080071232 A CN 202080071232A CN 114555837 A CN114555837 A CN 114555837A
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steel sheet
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aluminum
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CN114555837B (zh
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赖莎·格里戈里耶娃
佛罗林·杜米尼克
卜拉欣·纳比
帕斯卡尔·德里耶
蒂埃里·斯图雷尔
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ArcelorMittal SA
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Abstract

本发明涉及模压淬火方法,所述模压淬火方法包括以下步骤:A.提供用于热处理的钢板,所述钢板预涂覆有用于防腐蚀目的的基于锌或基于铝的预涂层,B.以10nm至550nm的厚度沉积氢屏障预涂层,C.在惰性气氛中对预涂覆钢板进行分批退火以获得预合金化钢板,D.切割预合金化钢板以获得坯件,E.对坯件进行热处理以在钢中获得完全奥氏体显微组织,F.将坯件转移到压制工具中,G.将坯件热加工成形以获得部件,H.将以步骤G)获得的部件冷却以在钢中获得以下显微组织:所述显微组织为马氏体或马氏体‑贝氏体,或者由以体积分数计至少75%的等轴铁素体、5体积%至20体积%的马氏体和量小于或等于10体积%的贝氏体构成。

Description

模压淬火方法
本发明涉及模压淬火方法,所述模压淬火方法包括提供涂覆有用于防腐蚀目的预涂层的钢板和具有优异的抗延迟开裂性的部件,所述预涂层的顶部被更好地抑制氢吸附的氢屏障预涂层直接覆盖。本发明特别适用于制造机动车辆。
用于模压淬火的涂覆钢板有时被称为“预涂覆的”,这个前缀表示预涂层性质的转变将在冲压之前的热处理期间发生。可以具有多于一种预涂层。本发明公开了两种预涂层。
已知某些应用(尤其在机动车领域中)要求金属结构在受到冲击的情况下进一步减轻和加强,并且还具有良好的可拉拔性。为此,通常使用具有改善的机械特性的钢,这样的钢通过冷冲压和热冲压来成形。
然而,已知对延迟开裂的敏感性随机械强度而增加,特别是在某些冷成形或热加工成形操作之后,因为在变形之后容易留存高残余应力。与可能存在于钢板中的原子氢结合,这些应力容易导致延迟开裂,也就是说在变形本身之后一定时间发生的开裂。氢可以通过扩散到晶格缺陷(例如基体/夹杂物界面、孪晶间界和晶界)中而逐渐地累积。在后面的缺陷中,当氢在一定时间之后达到临界浓度时其可能变得有害。该延迟由残余应力分布区域以及氢扩散的动力学造成,室温下的氢扩散系数低。此外,位于晶界处的氢削弱它们的内聚力并有利于延迟的晶间裂纹的出现。
一些部件通过对基于铝的涂覆钢板进行预合金化,然后通过将预合金化涂覆钢板热加工成形来生产。通常,这些部件在分批退火期间和在热冲压期间具有关于氢吸附非常差的性能。实际上,由于分批退火在数小时期间进行,因此特别是在分批退火期间可以吸附大量的氢。
专利申请EP3396010公开了制造用于热加工成形的Al-Fe合金涂覆钢板的方法,所述Al-Fe合金涂覆钢板具有高的抗氢延迟断裂性和抗涂层分离性以及高的可焊性,所述方法包括:
-在基础钢板的表面上形成Al-Si涂层,
-在存在露点低于-10℃的气氛的加热炉中以1℃/小时至500℃/小时的加热速率将Al-Si涂覆基础钢板加热至450℃至750℃范围内的热处理最高温度;以及
-通过将Al-Si涂覆基础钢板在热处理最高温度下保持1小时至100小时,在基础钢板的表面上形成Al-Fe合金涂层。
调节分批退火工艺的气氛和热处理条件以获得用于防止氢延迟断裂Al-Fe的特定显微组织和特性。
实际上,该专利申请公开了具有高的抗氢延迟断裂性和抗涂层分离性以及高的可焊性的用于热加工成形的铝-铁(Al-Fe)合金涂覆钢板,所述Al-Fe合金涂覆钢板包括基础钢板和形成在基础钢板与氧化物层之间的合金涂层,其中所述合金涂层包括:
Al-Fe合金层I,所述Al-Fe合金层I形成在基础钢板上并且其维氏硬度为200Hv至800Hv;
Al-Fe合金层III,所述Al-Fe合金层III形成在Al-Fe合金层I上并且其维氏硬度为700Hv至1200Hv;以及
Al-Fe合金层II,所述Al-Fe合金层II在钢板的长度方向上连续或不连续地形成在Al-Fe合金层III中,并且其维氏硬度为400Hv至900Hv,其中氧化物层的距表面0.1μm深度处的平均氧含量为20重量%或更少。
然而,在实践中,具有特定显微组织和特性的铝铁合金涂覆钢板非常难以获得。实际上,公开了宽范围的露点和加热速度。因此,存在无法在整个范围内获得特定Al-Fe合金涂层的风险,造成为找到正确参数而进行的重要的研究努力。
专利申请EP2312005公开了用于快速加热热冲压的镀铝钢板的生产方法,其特征在于,在箱式退火炉中对每单面镀铝沉积量为30g/m2至100g/m2的镀铝钢板原样在带卷的状态进行退火,在此期间通过在具有保留时间和退火温度作为其X轴和Y轴,并且其中X轴以对数表示的XY平面中具有坐标为(600℃,5小时)、(600℃,200小时)、(630℃,1小时)、(750℃,1小时)、和(750℃,4小时)的5个点为顶点的五边形的包含各边在内的内部区域中的保留时间和退火温度的组合进行退火。本专利申请还公开了通过以上方法获得的用于快速加热热冲压的镀铝钢板。
该专利建议在空气气氛中在600℃至750℃下进行分批退火的条件以降低钢中的氢。然而,在分批退火期间吸附的氢的量仍是高的。
因此,本发明的目的是提供易于实施的模压淬火方法,其中防止氢吸附到预合金化基于铝的钢板中并因此进入模压淬火部件中。其旨在使得可获得可通过包括热加工成形的所述模压淬火方法获得的具有优异的抗延迟开裂性的部件。
该目的通过提供包括以下步骤的模压淬火方法来实现:
A.提供用于热处理的钢板,所述钢板预涂覆有用于防腐蚀目的的基于锌或基于铝的预涂层,
B.以10nm至550nm的厚度沉积氢屏障预涂层,
C.在惰性气氛中对预涂覆钢板进行分批退火以获得预合金化钢板,
D.切割预合金化钢板以获得坯件,
E.对坯件进行热处理以在钢中获得完全奥氏体显微组织,
F.将坯件转移到压制工具中,
G.将坯件热加工成形以获得部件,
H.将以步骤G)中获得的部件冷却以在钢中获得以下显微组织:所述显微组织为马氏体或马氏体-贝氏体,或者由以体积分数计至少75%的等轴铁素体、5体积%至20体积%的马氏体和量小于或等于10体积%的贝氏体构成。
实际上,在不希望受任何理论束缚的情况下,本发明人出乎意料地发现,当钢板预涂覆有氢屏障预涂层时并且当在惰性气氛中进行分批退火时,吸附到钢板中的氢减少。实际上,认为由于氢屏障预涂层,热力学稳定的氧化物以低扩散动力学形成在氢屏障预涂层的表面上。这些热力学稳定的氧化物减少了H2吸附。此外,看来当分批退火的气氛是非氧化时,其允许进一步防止氢吸附,因为预涂层在预涂覆钢板的表面处扩散并氧化。因此,基于锌或基于铝的预涂层和氢屏障预涂层在预涂覆钢板的表面处氧化,二者均充当氢的屏障。
在步骤A)中,所使用的钢板由如欧洲标准EN 10083中描述的热处理用钢制成。其在热处理之前或之后可以具有高于500MPa、有利地为500MPa至2000MPa的抗拉强度(tensile resistance)。
钢板的重量组成优选如下:0.03%≤C≤0.50%;0.3%≤Mn≤3.0%;0.05%≤Si≤0.8%;0.015%≤Ti≤0.2%;0.005%≤Al≤0.1%;0%≤Cr≤2.50%;0%≤S≤0.05%;0%≤P≤0.1%;0%≤B≤0.010%;0%≤Ni≤2.5%;0%≤Mo≤0.7%;0%≤Nb≤0.15%;0%≤N≤0.015%;0%≤Cu≤0.15%;0%≤Ca≤0.01%;0%≤W≤0.35%,余量为铁和来自钢的制造的不可避免的杂质。
例如,钢板为具有以下组成的22MnB5:0.20%≤C≤0.25%;0.15%≤Si≤0.35%;1.10%≤Mn≤1.40%;0%≤Cr≤0.30%;0%≤Mo≤0.35%;0%≤P≤0.025%;0%≤S≤0.005%;0.020%≤Ti≤0.060%;0.020%≤Al≤0.060%;0.002%≤B≤0.004%,余量为铁和来自钢的制造的不可避免的杂质。
钢板可以为具有以下组成的
Figure BDA0003589473590000043
0.24%≤C≤0.38%;0.40%≤Mn≤3%;0.10%≤Si≤0.70%;0.015%≤Al≤0.070%;0%≤Cr≤2%;0.25%≤Ni≤2%;0.020%≤Ti≤0.10%;0%≤Nb≤0.060%;0.0005%≤B≤0.0040%;0.003%≤N≤0.010%;0.0001%≤S≤0.005%;0.0001%≤P≤0.025%;应理解,钛和氮的含量满足Ti/N>3.42;以及碳、锰、铬和硅的含量满足:
Figure BDA0003589473590000041
组成任选地包含以下中的一者或更多者:0.05%≤Mo≤0.65%;0.001%≤W≤0.30%;0.0005%≤Ca≤0.005%,余量为铁和来自钢的制造的不可避免的杂质。
例如,钢板为具有以下组成的
Figure BDA0003589473590000042
0.040%≤C≤0.100%;0.80%≤Mn≤2.00%;0%≤Si≤0.30%;0%≤S≤0.005%;0%≤P≤0.030%;0.010%≤Al≤0.070%;0.015%≤Nb≤0.100%;0.030%≤Ti≤0.080%;0%≤N≤0.009%;0%≤Cu≤0.100%;0%≤Ni≤0.100%;0%≤Cr≤0.100%;0%≤Mo≤0.100%;0%≤Ca≤0.006%,余量为铁和来自钢的制造的不可避免的杂质。
钢板可以根据期望的厚度(其可以为例如0.7mm至3.0mm)通过热轧和任选地冷轧来获得。
任选地,在步骤A)中,氢屏障预涂层包含选自Sr、Sb、Pb、Ti、Ca、Mn、Sn、La、Ce、Cr、Zr或Bi的任选元素,每种附加的元素的含量按重量计低于0.3重量%。
优选地,在步骤A)中,所述氢屏障预涂层包含选自以下中的至少一种元素:镍、铬、铝、镁和钇。
优选地,在步骤A)中,氢屏障预涂层由镍和铬组成,即屏障预涂层包含镍、铬和不可避免的杂质。有利地,重量比Ni/Cr为1.5至9。实际上,不希望受任何理论束缚,认为该特定比率进一步降低了奥氏体化处理期间的氢吸附。
在另一个优选实施方案中,氢屏障预涂层由镍和铝组成,即氢屏障预涂层包含Ni、Al和不可避免的杂质。
在另一个优选实施方案中,氢屏障预涂层由以50重量%或75重量%或90重量%的铬组成。更优选地,其由铬组成,即氢屏障预涂层仅包含Cr和不可避免的杂质。
在另一个优选实施方案中,氢屏障预涂层由以50重量%或75重量%或90重量%的镁组成。更优选地,其由镁组成,即氢屏障预涂层仅包含Mg和不可避免的杂质。
在另一个优选实施方案中,氢屏障预涂层由镍、铝和钇组成,即氢屏障预涂层包含Ni、Al和Y以及不可避免的杂质。
优选地,在步骤A)中,氢屏障预涂层的厚度为10nm至90nm或150nm至250nm。例如,氢屏障预涂层的厚度为50nm、200nm或400nm。
不希望受任何理论束缚,看来当氢屏障预涂层低于10nm时,存在氢吸附到钢中的风险,因为氢屏障预涂层没有足够覆盖钢板。当氢屏障预涂层高于550nm时,看来存在氢屏障预涂层变得更脆以及由于屏障涂层脆性氢吸附开始发生的风险。
在一个优选实施方案中,基于锌或基于铝的预涂层基于铝并且包含小于15%的Si、小于5.0%的Fe、任选地0.1%至8.0%的Mg和任选地0.1%至30.0%的Zn,剩余部分为Al。例如,基于锌或基于铝的预涂层为
Figure BDA0003589473590000052
在另一个优选实施方案中,锌或铝预涂层基于锌并且包含小于6.0%的Al、小于6.0%的Mg,剩余部分为Zn。例如,基于锌或基于铝的预涂层为锌涂层,以获得以下产品:
Figure BDA0003589473590000051
GI。
基于锌或基于铝的预涂层还可以包含按重量计含量最高至5.0%,优选地为3.0%的残余元素例如铁和杂质。
优选地,步骤A)的预涂层通过物理气相沉积、通过电镀锌、热浸镀锌或辊涂来沉积。优选地,氢屏障预涂层通过电子束诱导沉积或辊涂来沉积。优选地,基于锌或基于铝的预涂层通过热浸镀锌来沉积。
任选地,在预涂层的沉积之后,可以实现光整冷轧并且其使预涂覆钢板加工硬化,并给予其便于后续成形的粗糙度。可以施加脱脂和表面处理以改善例如粘合剂粘结或耐腐蚀性。
优选地,在步骤C)中,分批退火在450℃至750℃,优选地550℃至750℃的温度下进行。
优选地,在步骤C)中,惰性气体选自氦(He)、氖(Ne)、氩(Ar)、氮气、氢气或其混合物。
有利地,在步骤C)中,分批退火的加热速率高于或等于5000℃.小时-1,更优选为10000℃.小时-1至15000℃.小时-1或20000℃.小时-1至35000℃.小时-1
优选地,步骤C)中,冷却速度低于或等于100℃.小时-1。优选地,冷却速度具有从1℃.小时-1到100℃.小时-1变化的三个冷却速率。
优选地,在步骤C)中,分批退火在1小时至100小时期间进行。
之后,切割预合金化钢板以获得坯件。
在具有惰性气氛的炉中对坯件施加热处理。
优选地,在步骤C)和/或E)中,露点低于或等于-10℃,更优选为-30℃至-60℃。实际上,不希望受任何理论束缚,认为当露点在上述范围内时,热力学稳定的氧化物的层在热处理期间减少甚至更多的H2吸附。
优选地,热处理在800℃至970℃的温度下进行。更优选地,热处理在通常为840℃至950℃,优选为880℃至930℃的奥氏体化温度Tm下进行。有利地,所述坯件在1分钟至12分钟、优选地3分钟至9分钟的停留时间tm期间保持。在热加工成形之前的热处理期间,预涂层形成具有高的耐腐蚀性、耐磨性、抗磨性和抗疲劳性的合金层。
在环境温度下,氢吸附到钢中的机理与高温(特别是奥氏体化处理)不同。实际上,通常在高温下,炉中的水在钢板的表面处离解成氢和氧。不希望受任何理论束缚,认为氢屏障预涂层和分批退火的惰性气氛可以防止水在氢屏障预涂层表面处离解,并且可以防止氢扩散通过两种预涂层。
在热处理之后,然后将坯件转移至热加工成形工具,并将其在600℃至830℃的温度下热加工成形。热加工成形可以为热冲压或辊轧成形。优选地,将坯件热冲压。然后将部件在热加工成形工具中冷却或者在转移至特定的冷却工具之后冷却。
根据钢组成以这样的方式控制冷却速率:使得热加工成形之后的最终显微组织主要包含马氏体,优选包含马氏体、或者马氏体和贝氏体,或者由至少75%的等轴铁素体、5%至20%的马氏体和量小于或等于10%的贝氏体构成。
由此通过热加工成形获得根据本发明的具有优异的抗延迟开裂性的硬化部件。
优选地,部件包含预涂覆有基于锌或基于铝的预涂层的钢板,该第一预涂层的顶部被氢屏障涂层和包含热力学稳定的氧化物的氧化物层直接覆盖,这样的氢屏障涂层通过扩散与基于锌或基于铝的预涂层合金化,基于锌或基于铝的预涂层与钢板合金化。实际上,不希望受任何理论束缚,看来在热处理期间,来自钢板的铁扩散至氢屏障预涂层的表面。
优选地,热力学稳定的氧化物可以分别包括Cr2O3;FeO;NiO;Fe2O3;Fe3O4、MgO、Y2O3或其混合物。
如果基于锌或基于铝的预涂层基于锌,则氧化物还可以包括ZnO。如果基于锌或基于铝的预涂层基于铝,则氧化物还可以包括Al2O3和/或MgAl2O4
优选地,氧化物层的厚度为10nm至550nm。
优选地,部件为前纵梁(front rail)、座椅横向构件、侧梁(side sill)构件、前围挡板(dash panel)横向构件、前底板加强件、后底板横向构件、后纵梁(rear rail)、B柱、门环(door ring)或霰弹枪(shotgun)。
对于机动车应用,在磷酸盐处理步骤之后,将部件浸入电涂覆浴中。通常,磷酸盐层的厚度为1μm至2μm,以及电涂覆层的厚度为15μm至25μm,优选小于或等于20μm。电泳层确保另外的抗腐蚀保护。在电涂覆步骤之后,可以沉积其他涂料层,例如,涂料的底漆涂层、底涂层和顶涂层。
在对部件施加电涂覆之前,将部件预先脱脂并进行磷酸盐处理以确保电泳的附着性。
现在将以仅用于信息性而进行的试验对本发明进行说明。所述试验不是限制性的。
实施例
对于所有样品,所使用的钢板为22MnB5。钢的组成如下:C=0.2252%;Mn=1.1735%;P=0.0126%;S=0.0009%;N=0.0037%;Si=0.2534%;Cu=0.0187%;Ni=0.0197%;Cr=0.180%;Sn=0.004%;Al=0.0371%;Nb=0.008%;Ti=0.0382%;B=0.0028%;Mo=0.0017%;As=0.0023%;以及V=0.0284%。
所有钢板都预涂覆有用于防腐蚀目的的下文中称为
Figure BDA0003589473590000081
的第一预涂层。该预涂层包含9重量%的硅、3重量%的铁,余量为铝。其通过热浸镀锌来沉积。
然后,两个试验品预涂覆有通过磁控溅射沉积的包含80%的Ni和20%的Cr的第二预涂层。
实施例1:氢测试:
该测试用于确定在模压淬火方法的奥氏体化热处理期间所吸附的氢的量。
试验品1为预涂覆有为
Figure BDA0003589473590000082
(25μm)的第一预涂层的钢板。然后,在5小时期间进行在650℃的温度下的分批退火。加热速率为10800℃.小时-1。分批退火的气氛为氮气。以在2小时20分钟期间85℃.小时-1、在17小时期间19℃.小时-1以及在8小时期间2.5℃.小时-1的速度进行在分批退火之后的冷却。
试验品2为预涂覆有为
Figure BDA0003589473590000083
(25μm)的第一预涂层和包含80%的Ni和20%的Cr的第二预涂层的钢板。然后,在5小时期间进行在650℃的温度下的分批退火。加热速率为10800℃.小时-1。分批退火的气氛为氮气。以在2小时20分钟期间85℃.小时-1、在17小时期间19℃.小时-1以及在8小时期间2.5℃.小时-1的速度进行在分批退火之后的冷却。
试验品3为预涂覆有为
Figure BDA0003589473590000084
(25μm)的第一预涂层的钢板。然后,在5小时期间进行在650℃的温度下的分批退火。加热速率为10800℃.小时-1。分批退火的气氛为空气。以在2小时20分钟期间85℃.小时-1、在17小时期间19℃.小时-1以及在8小时期间2.5℃.小时-1的速度进行在分批退火之后的冷却。
试验品4为预涂覆有为
Figure BDA0003589473590000085
(25μm)的第一预涂层和包含80%的Ni和20%的Cr的第二预涂层的钢板。然后,在5小时期间进行在650℃的温度下的分批退火。加热速率为10800℃.小时-1。分批退火的气氛为空气。以在2小时20分钟期间85℃.小时-1、在17小时期间19℃.小时-1以及在8小时期间2.5℃.小时-1的速度进行在分批退火之后的冷却。
之后,将所有试验品切割并在3分钟的停留时间期间在900℃的温度下加热。热处理期间的气氛为空气。将坯件转移到压制工具中并进行热冲压以获得具有可变的厚度的部件。然后,通过将试验品浸入温水中将部件冷却以通过马氏体转变获得硬化。
最后,使用TDA或热解吸分析仪通过热解吸来测量在热处理期间被试验品吸附的氢量。为此,将各试验品放置在石英室中并在氮气流下在红外炉中缓慢加热。通过检漏器拾取所释放的混合物氢气/氮气并通过质谱仪测量氢气浓度。结果示于下表1中:
试验 第二预涂层 气氛 比率Ni/Cr 第二预涂层厚度(nm) H<sub>2</sub>量(按质量计ppm)
1 - N<sub>2</sub> - - 0.6
2* Ni/Cr 80/20 N<sub>2</sub> 4 200 0.35
3 - 空气 - - 0.9
4 Ni/Cr 80/20 空气 4 200 0.6
*:根据本发明的实施例。
与比较例相比,根据本发明的试验品2释放显著少量的氢气。

Claims (14)

1.一种模压淬火方法,包括以下步骤:
A.提供用于热处理的钢板,所述钢板预涂覆有用于防腐蚀目的的基于锌或基于铝的预涂层,
B.以10nm至550nm的厚度沉积氢屏障预涂层,
C.在惰性气氛中对预涂覆钢板进行分批退火以获得预合金化钢板,
D.切割所述预合金化钢板以获得坯件,
E.对所述坯件进行热处理以在钢中获得完全奥氏体显微组织,
F.将所述坯件转移到压制工具中,
G.将所述坯件热加工成形以获得部件,
H.将以步骤G)获得的所述部件冷却以在钢中获得以下显微组织:所述显微组织为马氏体或马氏体-贝氏体,或者由以体积分数计至少75%的等轴铁素体、5体积%至20体积%的马氏体和量小于或等于10体积%的贝氏体构成。
2.根据权利要求1所述的模压淬火方法,其中在步骤B)中,所述氢屏障预涂层包含选自镍、铬、镁、铝和钇中的至少一种元素。
3.根据权利要求1或2所述的模压淬火方法,其中在步骤B)中,所述氢屏障预涂层由镍和铬;或者镍和铝;或者镁;或者铬;或者镍、铝和钇组成。
4.根据权利要求1至3中任一项所述的模压淬火方法,其中在步骤A)中,所述基于锌或基于铝的预涂层基于锌并且包含小于6.0%的Al、小于6.0%的Mg,剩余部分为Zn。
5.根据权利要求1至3中任一项所述的模压淬火方法,其中在步骤A)中,所述基于锌或基于铝的预涂层基于铝并且包含小于15%的Si、小于5.0%的Fe、任选地0.1%至8.0%的Mg和任选地0.1%至30.0%的Zn,剩余部分为Al。
6.根据权利要求1至5中任一项所述的模压淬火方法,其中在步骤C)中,所述分批退火在450℃至750℃的温度下进行。
7.根据权利要求1至6中任一项所述的模压淬火方法,其中在步骤C)中,所述分批退火的加热速率高于或等于5000℃.小时-1
8.根据权利要求1至7中任一项所述的模压淬火方法,其中在步骤C)中,冷却速度低于或等于100℃.小时-1
9.根据权利要求1至8中任一项所述的模压淬火方法,其中在步骤C)中,所述分批退火在1小时至100小时期间进行。
10.根据权利要求1至9中任一项所述的模压淬火方法,其中所述惰性气体选自氦(He)、氖(Ne)、氩(Ar)、氮气、氢气或其混合物。
11.根据权利要求1至权利要求10中任一项所述的模压淬火方法,其中彼此独立地在步骤E)中,气氛为惰性的或者其氧化力等于或高于由1体积%的氧气构成的气氛的氧化力且等于或小于由50体积%的氧气构成的气氛的氧化力。
12.根据权利要求1至11中任一项所述的方法,其中在步骤E)中,所述气氛的露点低于或等于-10℃。
13.根据权利要求1至12中任一项所述的模压淬火方法,其中在步骤E)中,所述热处理在800℃至970℃的温度下进行。
14.根据权利要求1至13中任一项所述的模压淬火方法,其中在步骤G)期间,将所述坯件在600℃至830℃的温度下热加工成形。
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