CN110573335A - 用于制造抗液态金属脆化的镀锌扩散退火钢板的方法 - Google Patents

用于制造抗液态金属脆化的镀锌扩散退火钢板的方法 Download PDF

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CN110573335A
CN110573335A CN201880028753.XA CN201880028753A CN110573335A CN 110573335 A CN110573335 A CN 110573335A CN 201880028753 A CN201880028753 A CN 201880028753A CN 110573335 A CN110573335 A CN 110573335A
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克里斯蒂安·阿勒利
帕斯卡尔·贝尔托
阿尼尔班·查克拉博蒂
哈桑·卡西米-阿尔马基
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Abstract

本发明涉及用于制造镀锌扩散退火钢板的方法。

Description

用于制造抗液态金属脆化的镀锌扩散退火钢板的方法
本发明涉及用于制造镀锌扩散退火钢板的方法。本发明特别适用于机动车辆的制造。
基于锌的涂层因为其因屏障保护和阴极保护而能够实现抗腐蚀保护而被广泛使用。屏障作用通过在钢表面上施加金属或非金属涂层而获得。因此，涂层防止钢与腐蚀性气氛之间的接触。屏障作用与涂层和基材的性质无关。相反，牺牲阴极保护基于这样的事实：根据电化序，锌与钢相比是活泼金属。因此，如果发生腐蚀，则锌与钢相比被优先消耗。阴极保护在钢直接暴露于腐蚀性气氛的区域(例如切割边缘，其中周围的锌先于钢被消耗)中是必需的。
然而，当对这样的经锌涂覆的钢板进行加热步骤时，例如在热压制硬化或电阻点焊期间，在钢中观察到从钢/涂层界面萌生的裂纹。事实上，有时，由于以上操作之后在经涂覆的钢板中存在裂纹，因此存在机械特性的降低。这些裂纹随着以下条件出现：高于涂层材料的熔点的高温；除了存在拉伸应力之外，还与具有低熔点的液态金属(例如，锌)接触；熔融金属对基材钢晶粒和晶界的扩散和润湿。这种现象的名称被称为液态金属脆化(LME，liquid metal embrittlement)，并且也被称为液态金属辅助开裂(LMAC，liquid metalassisted cracking)。
专利US2016/0319415公开了对由液态金属脆化造成的开裂具有优异的抗性的热浸镀锌钢板，包括：
-具有其中奥氏体分数为90面积％或更大的显微组织的基础钢板；以及
-形成在基础钢板上的热浸镀锌层，
其中热浸镀锌层包括Fe-Zn合金层和形成在Fe-Zn合金层上的Zn层，并且Fe-Zn合金层的厚度为[(3.4×t)/6]μm或更大，其中t为热浸镀锌层的厚度。
在该专利中，提到了通过抑制用于抑制铁(Fe)和Fe-Al或Fe-Al-Zn合金层的扩散的表面氧化物的形成，并且通过在热浸镀锌层中形成具有足够厚度的Fe-Zn合金层，可以防止由LME引起的开裂的发生。
为了确保镀层附着力(plating adhesion)，优选在基础钢板的表面的刚好下方进一步包括Fe-Ni合金层。更特别地，Fe-Ni合金层可以确保优异的镀层附着力，原因是，以TWIP(孪晶诱导塑性)钢的方式，由于诸如Mn等的氧化性元素在Fe-Ni合金层的表面上富集，抑制了诸如MnO等的表面氧化物的形成，从而使得MnO等作为内部氧化物存在。为了确保以上效果，Fe-Ni合金层可以由于300mg/m2至1000mg/m2的Ni涂层而形成。然而，该专利申请公开了仅专用于TWIP钢的技术方案。
专利申请US2012100391公开了用于制造具有优异的镀层品质、镀层附着力和可点焊性的热浸镀锌钢板的方法，该方法包括：
-用涂覆量(CNi)为0.1g/m2至1.0g/m2(即约11nm至112nm)的Ni涂覆基础钢板；
-在还原性气氛中加热经Ni涂覆的钢板；
-将经加热的钢板冷却至钢板被进给至镀锌浴的温度(XS)；以及
-将经冷却的钢板进给并浸入有效Al浓度(CAl)为0.11重量％至0.14重量％且温度(Tp)为440℃至460℃的镀锌浴中，其中钢板被进给至镀锌浴的温度(XS)满足以下关系：CNi·(XS-TP)/2CAl＝5-100。
该专利申请还公开了在基础钢板与镀锌层之间的界面处形成有占镀锌层的截面面积的1％至20％的Fe-Ni-Zn合金相的热浸镀锌钢板。
所提及的是，在通过在镀覆在基础钢板上的Ni层上镀覆锌而获得的高强度镀锌钢板的情况下，如果将由形成在基础钢板与镀锌层之间的界面处的Fe-Ni-Zn合金相覆盖的面积的分数控制在特定水平，则会降低钢板的镀覆品质，并且将防止镀锌层在成形过程期间剥离，这表明钢板的镀层附着力将得到改善。此外，在从电极经由Fe-Ni合金层向基础钢板施加电流的点焊过程中，Fe将立即从钢板扩散以形成Fe-Ni-Zn合金相，使得电极与镀锌层之间的合金化将被延迟，因此提高了焊接电极的使用寿命。
然而，虽然点焊过程得到改善，但未提及LME的改善。
由于存在数个优点，镀锌扩散退火涂层被施加于钢。然而，在热压制硬化或电阻点焊期间，上述镀锌扩散退火涂覆钢板表现出LME裂纹。
因此，本发明的目的是提供不存在LME问题的镀锌扩散退火钢板。其目的是使可实现的尤其是易于实施的方法，以获得在热压制成形和/或焊接之后不存在LME问题的组合件。
该目的通过提供根据权利要求1所述的方法来实现。所述方法还可以包括根据权利要求2至12所述的任何特征。
另一个目的通过提供根据权利要求13所述的镀锌扩散退火钢板来实现。
又一个目的通过提供根据权利要求15所述的点焊接头来实现。所述点焊接头还可以包括根据权利要求14至17所述的特征。
最后，再一个目的通过提供根据权利要求18所述的钢板或组合件的用途来实现。
本发明的其他特征和优点将由以下对本发明的详细描述而变得明显。
表述“钢”或“钢板”意指具有允许零部件实现高达2500MPa并且更优选地高达2000MPa的拉伸强度的组成的钢板、卷材、板材。例如，所述拉伸强度高于或等于500MPa，优选地高于或等于980MPa，有利地高于或等于1180MPa并且甚至高于或等于1470MPa。
本发明涉及用于制造镀锌扩散退火钢板的方法，包括以下依次的步骤：
A.用由镍组成并且厚度为150nm至650nm的第一涂层涂覆钢板，按重量百分比计，所述钢板具有以下组成：
0.10％＜C＜0.40％，
1.5％＜Mn＜3.0％，
0.7％＜Si＜3.0％，
0.05％＜Al＜1.0％，
0.75％＜(Si+Al)＜3.0％，
以及在完全任选的基础上，诸如以下的一种或更多种元素：
Nb≤0.5％，
B≤0.010％，
Cr≤1.0％，
Mo≤0.50％，
Ni≤1.0％，
Ti≤0.5％，
所述组成的剩余部分由铁和由加工产生的不可避免的杂质构成，
B.使所述经涂覆的钢板在600℃至1200℃的温度下进行退火，
C.用基于锌的第二涂层涂覆步骤B)中获得的钢板，以及
D.进行合金化热处理以形成镀锌扩散退火钢板。
不希望受任何理论的束缚，似乎在步骤B)的热处理期间，具有特定厚度的Ni向具有以上特定钢组成的钢板扩散而提供Fe-Ni合金层。另一方面，在钢与涂层之间的界面处仍然存在一定量的Ni，这防止在任何加热步骤例如焊接期间液态锌或锌合金渗入钢中。此外，在合金化处理即步骤D)期间，Ni还扩散入上覆的涂层中，从而防止LME。
由镍组成的第一涂层通过本领域技术人员已知的任何沉积方法来沉积。其可以通过真空沉积或电镀法来沉积。优选地，其通过电镀法沉积。
任选地，第一涂层可以包含选自Fe、Cu、Mn、Si、Al和P的杂质。例如，杂质的量低于5％、优选低于3％并且更优选低于1％。
由镍组成的第一涂层的厚度为150nm至650nm，优选为200nm至500nm，更优选为250nm至450nm，有利地为300nm至450nm，并且例如为350nm至450nm。例如，由镍组成的第一涂层的厚度为250nm至650nm。实际上，不希望受任何理论的束缚，本发明人出人意料地发现，关于第一涂层的厚度存在其中LME减少得到显著改善的最优值。认为该最优厚度允许减小焊接电流，并因此减少点焊期间输入的热量。因此，实现了由于LME而形成的裂纹的数量的显著减少。
有利地，在步骤B)中，热处理为连续退火。例如，连续退火包括加热、均热和冷却步骤。其还可以包括预热步骤。
优选地，热处理在露点为-60℃至-30℃的包含1％至10％的H2的气氛中进行。例如，气氛包含1％至10％的H2，露点为-40℃至-60℃。
在另一个优选实施方案中，在步骤B)中，热处理在露点为-30℃至+30℃的包含1％至10％的H2的气氛中进行。例如，气氛包含1％至10％的H2，露点为0℃至+20℃。
优选地，在步骤C)中，第二层包含大于50％的锌，更优选大于75％的锌，并且有利地大于90％的锌。第二层可以通过本领域技术人员已知的任何沉积方法来沉积。其可以通过热浸法、通过真空沉积或通过电镀锌过程来完成。
例如，基于锌的涂层包含0.01％至8.0％的Al，任选地0.2％至8.0％的Mg，剩余部分为Zn。
在另一个优选实施方案中，第二层由锌组成。当涂层通过热浸镀锌来沉积时，浴中的铝的百分比为0.10重量％至0.18重量％。
优选地，基于锌的涂层通过热浸镀锌方法来沉积。在该实施方案中，熔浴还可以包含不可避免的杂质和来自进给锭料或来自钢板通过熔浴的残留元素。例如，任选的杂质选自Sr、Sb、Pb、Ti、Ca、Mn、Sn、La、Ce、Cr、Zr或Bi，每种另外元素按重量计的含量低于0.3重量％。来自进给锭料或来自钢板通过熔浴的残留元素可以为含量最高至0.1重量％的铁。
有利地，在步骤C)中，第二层不包含镍。
优选地，在步骤D)中，通过在例如5秒至50秒期间，在470℃至550℃的温度下加热步骤C)中获得的经涂覆的钢板来进行合金化热处理。例如，步骤D在520℃下进行20秒。
利用根据本发明的方法，获得了这样的镀锌扩散退火钢板，所述镀锌扩散退火钢板涂覆有包含镍的第一层，所述第一层被基于锌的第二层直接覆盖，第一层和第二层通过扩散而合金化使得第二合金层包含8重量％至50重量％的铁、0重量％至25重量％的镍，余量为锌。优选地，镀锌扩散退火钢板涂覆有包含镍的第一层，所述第一层被基于锌的第二层直接覆盖，第一层和第二层通过扩散而合金化使得第二合金层包含12重量％至50重量％的铁、1重量％至25重量％的镍，余量为锌。有利地，镀锌扩散退火钢板涂覆有包含镍的第一层，所述第一层被基于锌的第二层直接覆盖，第一层和第二层通过扩散而合金化使得第二合金层包含13重量％至50重量％的铁、1重量％至25重量％的镍，余量为锌。
优选地，钢板具有包含1％至50％的残余奥氏体、1％至60％的马氏体以及任选地选自贝氏体、铁素体、渗碳体和珠光体中的至少一种成分的显微组织。
在一个优选实施方案中，钢板具有包含5％至25％的残余奥氏体的显微组织。
优选地，钢板具有包含1％至60％、并且更优选10％至60％的回火马氏体的显微组织。
有利地，钢板具有包含10％至40％的贝氏体的显微组织，这样的贝氏体包含10％至20％的下贝氏体、0％至15％的上贝氏体和0％至5％的无碳化物贝氏体。
优选地，钢板具有包含1％至25％的铁素体的显微组织。
优选地，钢板具有包含1％至15％的未回火马氏体的显微组织。
在制造钢板之后，为了制造车辆的某些零部件，已知通过对两个金属板进行点焊来进行组装。
为了制造根据本发明的点焊接头，在有效强度(effective intensity)为3kA至15kA并且施加在电极上的力为150daN至850daN(其中所述电极活性面(active face)直径为4mm至10mm)的情况下进行焊接。
因此，获得了包括根据本发明的经涂覆的钢板的至少两个金属板的点焊接头，这样的所述接头包含少于3个尺寸大于100μm的裂纹，并且其中最长的裂纹的长度小于300μm。
优选地，第二金属板为钢板或铝板。更优选地，第二金属板为根据本发明的钢板。
在另一个实施方案中，点焊接头包括第三金属板，所述第三金属板为钢板或铝板。例如，第三金属板为根据本发明的钢板。
根据本发明的钢板或点焊接头可以用于制造机动车辆用零部件。
现在将在仅用于提供信息而进行的试验中说明本发明。它们是非限制性的。
实施例
对于所有样品，按重量百分比计，所使用的钢板具有以下组成：C＝0.37％，Mn＝1.95％，Si＝1.95％，Cr＝0.35％和Mo＝0.12％。
在试验1中，使钢在露点为-45℃的包含5％的H2和95％的N2的气氛中进行退火。退火在900℃下进行132秒。在退火之后使钢板冷却至室温。通过电镀锌法在经退火的钢板上施加锌涂层。
在试验2至5中，在退火之前，首先通过电镀法在全硬化钢板(full hard steelsheet)上沉积厚度分别为150nm、400nm、650nm和900nm的Ni。此后，使经预涂覆的钢板在露点为-45℃的包含5％的H2和95％的N2的气氛中进行退火。退火在900℃下进行132秒。在退火结束时，将钢板冷却至210℃的淬火温度，并再次在410℃的配分温度下加热。进行配分88秒，然后再次加热直至460℃的镀锌温度，然后通过热浸涂覆法使用保持在460℃的包含0.12重量％的Al的液态锌浴来施加锌涂层。紧接在镀锌之后，在520℃下进行合金化热处理20秒。
通过电阻点焊法评估以上经涂覆的钢的LME敏感度。为此，对于每个试验，通过电阻点焊将两个经涂覆的钢板焊接在一起。电极类型为直径为16mm的ISO B型；电极的力为5kN，以及水的流速为1.5g/分钟。焊接周期记录于表1中：
表1.焊接制度
焊接时间 脉冲 脉冲(周波) 冷却时间(周波) 维持时间(周波)
周期 2 12 2 15
还使用三层堆叠条件评估了抗LME裂纹行为。对于每个试验，通过电阻点焊将三个经涂覆的钢板焊接在一起。然后使用光学显微镜评估100μm的裂纹的数量，如表2中所记录。
表2.点焊之后LME裂纹详情(三层堆叠条件)
*：根据本发明。
与试验1和5相比，根据本发明的试验2、3和4显示出优异的抗LME性。实际上，大于100μm的裂纹的数量小于3，并且最长的裂纹的长度小于300μm。此外，具有最优Ni涂层厚度的试验2至4使焊接电流减小。这使得点焊期间输入的热量减少，从而使得由于LME而形成的裂纹的数量显著减少。

Claims (18)

1.一种用于制造镀锌扩散退火钢板的方法，包括以下依次的步骤：
A.用由镍组成并且厚度为150nm至650nm的第一涂层涂覆所述钢板，按重量百分比计，所述钢板具有以下组成：
0.10％＜C＜0.40％，
1.5％＜Mn＜3.0％，
0.7％＜Si＜3.0％，
0.05％＜Al＜1.0％，
0.75％＜(Si+Al)＜3.0％，
以及在完全任选的基础上，诸如以下的一种或更多种元素：
Nb≤0.5％，
B≤0.010％，
Cr≤1.0％，
Mo≤0.50％，
Ni≤1.0％，
Ti≤0.5％，
所述组成的剩余部分由铁和由加工产生的不可避免的杂质构成，
B.在600℃至1200℃的温度下进行所述经涂覆的钢板的退火的退火步骤，
C.用基于锌的第二涂层涂覆步骤B)中获得的所述钢板，以及
D.进行合金化热处理以形成镀锌扩散退火钢板。
2.根据权利要求1所述的方法，其中在步骤A)中，所述第一涂层的厚度为200nm至500nm。
3.根据权利要求2所述的方法，其中在步骤A)中，所述第一涂层的厚度为250nm至450nm。
4.根据权利要求1至3中任一项所述的方法，其中在步骤B)中，所述热处理为连续退火。
5.根据权利要求1至4中任一项所述的方法，其中在步骤B)中，所述热处理在露点为-60℃至-30℃的包含1％至10％的H2的气氛中进行。
6.根据权利要求1至5中任一项所述的方法，其中在步骤B)中，所述热处理在露点为-30℃至+30℃的包含1％至10％的H2的气氛中进行。
7.根据权利要求1至6中任一项所述的方法，其中在步骤C)中，所述第二层包含大于50％的锌。
8.根据权利要求7所述的方法，其中在步骤C)中，所述第二层包含大于75％的锌。
9.根据权利要求8所述的方法，其中在步骤C)中，所述第二层包含大于90％的锌。
10.根据权利要求1至9中任一项所述的方法，其中所述第二涂层不包含镍。
11.根据权利要求10所述的方法，其中在步骤C)中，所述第二层由锌组成。
12.根据权利要求1至11中任一项所述的方法，其中在步骤D)中，所述合金化处理通过在470℃至550℃的温度下加热步骤C)中获得的经涂覆的钢板来进行。
13.一种能够由根据权利要求1至12中任一项所述的方法获得的镀锌扩散退火钢板，所述镀锌扩散退火钢板涂覆有包含镍的第一层，所述第一层被基于锌的第二层直接覆盖，所述第一层和所述第二层通过扩散而合金化使得所述第二合金层包含8重量％至50重量％的铁、0重量％至25重量％的镍，余量为锌。
14.一种至少两个金属板的点焊接头，所述至少两个金属板至少包括根据权利要求13所述的钢板、或者能够由根据权利要求1至12中任一项所述的方法获得的钢板，所述接头包含少于3个尺寸大于100μm的裂纹，并且其中最长的裂纹的长度小于300μm。
15.根据权利要求14所述的点焊接头，其中所述第二金属板为钢板或铝板。
16.根据权利要求15所述的点焊接头，其中所述第二金属板为根据权利要求13所述的钢板、或者能够由根据权利要求1至12所述的方法获得的钢板。
17.根据权利要求14至16中任一项所述的点焊接头，包括第三金属板，所述第三金属板为钢板或铝板。
18.根据权利要求13所述的镀锌扩散退火钢板或根据权利要求14至17中任一项所述的点焊接头用于制造机动车辆的用途。
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