CN107923024B - 用于从涂覆基于铝的金属涂层的钢板开始制造可磷酸盐化部件的方法 - Google Patents

用于从涂覆基于铝的金属涂层的钢板开始制造可磷酸盐化部件的方法 Download PDF

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CN107923024B
CN107923024B CN201680044153.3A CN201680044153A CN107923024B CN 107923024 B CN107923024 B CN 107923024B CN 201680044153 A CN201680044153 A CN 201680044153A CN 107923024 B CN107923024 B CN 107923024B
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metal coating
component
coating
equal
steel sheet
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CN107923024A (zh
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蒂亚戈·马沙多阿莫里姆
克里斯蒂安·阿勒利
格雷戈里·勒伊利耶
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ArcelorMittal SA
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Abstract

本发明涉及用于制造涂覆有可磷酸盐化涂层的硬化部件的方法，包括以下步骤：A)提供预涂覆金属涂层的钢板，所述金属涂层包含4.0重量％至20.0重量％的锌、1.0重量％至3.5重量％的硅、任选的1.0重量％至4.0重量％的镁、以及任选的选自Pb、Ni、Zr或Hf的另外的元素，每种另外的元素以重量计的含量小于0.3重量％，余量为铝和不可避免的杂质以及残留元素；B)切割经涂覆的钢板以获得坯件；C)在840℃至950℃的温度下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；D)将所述坯件转移至压制工具中；E)对所述坯件进行热成形以获得部件；F)使步骤E)中获得的部件冷却以在钢中获得这样的显微组织：所述显微组织为马氏体或马氏体‑贝氏体或由至少75％的等轴铁素体、5％至20％的马氏体和小于或等于10％的量的贝氏体构成。

Description

用于从涂覆基于铝的金属涂层的钢板开始制造可磷酸盐化部 件的方法
本发明涉及用于从涂覆有基于铝的涂层的钢板开始制造硬化部件的方法。所述部件在磷酸盐化方面具有良好的特性，因此表现出良好的涂料附着性和良好的耐腐蚀性。本发明特别适合用于制造机动车辆。
硬化部件可以涂覆有具有良好的耐腐蚀性和热性能的基于铝的涂层。通常，用于制造这些部件的方法包括提供钢板，切割板以获得坯件，对坯件进行热处理，热冲压随后冷却以获得通过马氏体转变或马氏体-贝氏体转变而硬化。
通常，将涂膜施加在硬化部件上，特别地e-涂层。先前，经常进行磷酸盐化。因此，磷酸盐晶体形成在待涂覆的部件表面上，增加了涂料附着性，特别是e-涂层。
涂覆有基于铝的金属合金的硬化部件不可磷酸盐化，即，几乎没有或没有磷酸盐晶体形成于涂层的表面上。因此，在没有预先磷酸盐化步骤的情况下直接实现涂膜的施加。涂覆有基于铝的合金的部件表面的微粗糙度允许涂料附着。然而，在一些情况下，涂料不均匀地分布在部件表面上，产生红锈区域。
专利申请US2012/0085466公开了用于生产设置有金属涂层的钢组件的方法，包括以下生产步骤：
a)用包含至少85重量％Al和任选的最高至15重量％Si的Al涂层涂覆由合金化热处理钢制成的钢扁材(steel flat)产品；
b)用包含至少85重量％Zn的Zn涂层涂覆设置有Al涂层的钢扁材产品；
c)用包含磷酸或焦磷酸的至少一种金属盐的主要成分的顶层涂覆设置有Al涂层和位于其上的Zn涂层的钢扁材产品；
d)在至少750℃的热处理温度下对所述钢扁材产品进行热处理；
e)将所述钢扁材产品加热至热成形温度；
f)对由经加热的钢扁材产品制成的钢组件进行热成形；以及
g)通过以足以形成回火或马氏体组织的冷却速率使热成形的钢组件冷却来形成精加工成形的钢组件。
热成形的钢组件包括：基础层，包含至少30重量％Al、至少20重量％Fe、至少3重量％Si、和至多30重量％Zn；中间层，包含至少60重量％Zn、至少5重量％Al、最高至10重量％F、和最高至10重量％Si；以及顶层，包含至少8重量％Zn，以及ZnO、P和Al，其中P含量为至多1重量％。顶层的主要组分是ZnO。顶层允许涂料附着。
然而，这个过程需要沉积三个层以形成金属涂层。Al涂层可以通过热浸镀沉积。Zn涂层可以通过热浸镀、物理气相沉积法或电解镀沉积。顶层可以通过喷涂、浸涂、气相沉积或通过凝胶/溶胶雾沉积。
因此，这种方法的持续时间非常长，导致生产力的损失和生产力成本的增加。此外，该专利申请公开了在实践中，顶层主要由焦磷酸盐和锌氧化物和/或铝氧化物组成。铝氧化物，也称作氧化铝，是不可磷酸盐化的。最后，该专利申请没有提及经涂覆的热成形钢上磷酸盐晶体的覆盖率。
本发明的目的是提供易于实施的用于从经涂覆的钢板开始制造可磷酸盐化并因此具有良好的涂料附着性的硬化部件的方法。特别地，其旨在使得可获得可以被磷酸盐化以获得部件表面上磷酸盐晶体的高覆盖率(即，大于或等于80％的比率)的硬化部件。
该目的通过提供根据权利要求1所述的用于制造可磷酸盐化硬化部件的方法来实现。所述方法还可以包含权利要求2至17的特征。
第二目的通过提供根据权利要求18所述的部件来实现。硬化部件还可以包含权利要求19至28的特征。
第四目的通过提供根据权利要求29所述的这样的部件用于制造机动车辆的用途来实现。
本发明的其他特征和优点将由本发明的以下详细描述变得明显。
为了说明本发明，将特别地参照以下附图描述多个实施方案和非限制性实施例的试验：
图1示出对应于规范VDA 233-102的168小时的一个腐蚀循环。
将定义以下术语：
-“磷酸盐晶体的覆盖率”由百分比定义。0％意指部件的表面完全没被磷酸盐晶体覆盖，100％意指部件的表面全部被磷酸盐晶体覆盖”。
名称“钢”或“钢板”意指用于压制硬化工艺的钢板，其具有允许部件实现大于或等于500MPa，优选大于或等于1000MPa，有利地大于或等于1500MPa的较高拉伸强度的组成。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％，余量为铁和来自钢制造的不可避免的杂质。
钢板可以为具有以下组成的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；碳、锰、铬和硅的含量满足：
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％，余量为铁和来自钢制造的不可避免的杂质。
例如，钢板为具有以下组成的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％，余量为铁和来自钢制造的不可避免的杂质。
钢板可以根据期望的厚度(其可以是例如0.7mm至3.0mm)通过热轧和任选地冷轧而获得。
本发明涉及用于制造涂覆有可磷酸盐化涂层的硬化部件的方法。首先，该方法包括提供预涂覆金属涂层的钢板，所述金属涂层包含4.0重量％至20.0重量％的锌、1.0重量％至3.5重量％的硅、任选的1.0重量％至4.0重量％的镁、以及任选的选自Pb、Ni、Zr或Hf的另外的元素，每种另外的元素以重量计的含量小于0.3重量％，余量为铝和不可避免的杂质以及残留元素，其中比率Zn/Si为3.2至8.0。
不希望受任何理论约束，看起来如果不满足这些条件，特别地如果硅的量大于3.5％，则存在锌在铝基体中局部化或形成金属间化合物Zn-Al的风险。因此，锌无法上升至经涂覆的钢板的表面。在经涂覆的钢板的表面上形成不可磷酸盐化的氧化铝层。
在大多数情况下，当磷酸盐晶体的覆盖率低时，存在涂料附着性差的风险。然而，在一些情况下，尽管磷酸盐晶体的覆盖率低，但涂料附着性好，但上涂料之后的耐腐蚀性差。事实上，经涂覆的部件表面的微粗糙度允许涂料附着。但是，涂料不均匀地分布在部件表面上。在这种情况下，磷酸盐晶体不能起到涂料和涂层之间粘合剂的作用。因此，在腐蚀性环境下，水容易渗入涂料下，产生红锈区域。
优选地，金属涂层不包含选自以下的元素：Cr、Mn、Ti、Ce、La、Nd、Pr、Ca、Bi、In、Sn和Sb、或其组合。在另一优选实施方案中，金属涂层不包含任意以下成分(compound)：Cr、Mn、Ti、Ce、La、Nd、Pr、Ca、Bi、In、Sn和Sb。事实上，不希望受任何理论约束，看起来当这些成分存在于涂层中时，存在涂层的特性(例如，电化学电位)改变的风险，原因是其与涂层的主要元素的可能相互作用。
有利地，金属涂层包含1.5重量％至3.5重量％的硅，优选1.5重量％至2.5重量％的硅。在另一优选实施方案中，涂层包含2.1重量％至3.5重量％的硅。
优选地，金属涂层包含10.0重量％至15.0重量％的锌。
在一个优选实施方案中，金属涂层中的比率Zn/Si为5至4至8，优选4.5至7.5，并且有利地5至7.5。
不希望受任何理论约束，已发现当比率Zn/Si不为3.2至8时，存在磷酸盐晶体的覆盖率降低的风险，原因是涂层表面处的Al和Fe的含量太高。
有利地，涂层包含1.1重量％至3.0重量％的镁。
有利地，涂层包含大于76重量％的铝。
涂层可以通过本领域技术人员已知的任何方法沉积，例如热浸镀工艺、电镀工艺、物理气相沉积例如射流气相沉积或磁控溅射。优选地，涂层通过热浸镀工艺沉积。在该工艺中，将通过轧制获得的钢板浸在熔融金属浴中。
浴包含锌、硅、铝和任选的镁。其可以包含选自Pb、Ni、Zr或Hf的另外的元素，每种另外的元素以重量计的含量小于0.3重量％。这些另外的元素可以改善钢板上的涂层附着性、延展性等。
浴还可以包含不可避免的杂质和残留元素，其来自供给锭或来自钢板在熔融浴中的通过。残留元素可以是含量最高至3.0重量％的铁。
金属涂层的厚度通常为5μm至50μm，优选10μm至35μm，有利地12μm至18μm或26μm至31μm。浴温度通常为580℃至660℃。
在涂层的沉积之后，通常用喷嘴在经涂覆的钢板两侧喷射气体来擦拭(wipe)钢板。然后使经涂覆的钢板冷却。优选地，凝固开始和凝固结束之间的冷却速率大于或等于15℃·秒-1。有利地，凝固开始和结束之间的冷却速率大于或等于20℃·秒-1。
然后，可以实现光整冷轧(skin-pass)，并允许对经涂覆的钢板进行加工硬化并给予其促进后续成形的粗糙度。可以施加脱脂和表面处理以改善例如附着结合或耐腐蚀性。
然后，切割经涂覆的钢板以获得坯件。在炉中在非保护气氛下在通常为840℃至950℃，优选880℃至930℃的奥氏体化温度Tm下对坯件施加热处理。有利地，在1分钟至12分钟，优选3分钟至9分钟的停留时间tm期间保持所述坯件。在热成形之前的热处理期间，涂层形成具有高耐腐蚀性、抗磨性(resistance to abration)、耐磨性(resistance to wear)和耐疲劳性的合金层。
在热处理之后，然后将坯件转移至热成形工具中并在600℃至830℃的温度下热成形。热成形包括热冲压和辊轧成形。优选地，对坯件进行热冲压。然后使部件在热成形工具中冷却或在转移至特定冷却工具之后冷却。
根据钢组成以如下方式控制冷却速率：使得在热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％的马氏体和小于或等于10％的量的贝氏体构成。
在一个优选实施方案中，部件是具有可变厚度的压制硬化的钢部件，即本发明的压制硬化钢部件可以具有不均匀但可以变化的厚度。事实上，可以在最经受外部应力的区域中实现期望的机械抗性水平，并且可以节省压制硬化的部件的另一些区域中的重量，从而有助于车辆重量减轻。特别地，具有不均匀厚度的部件可以通过连续柔性轧制来生产，即，通过如下过程：其中轧制后获得的板厚度在轧制方向上是可变的，这与在轧制过程期间通过辊施加至板的载荷有关。
因此，在本发明的条件下，可以有利地制造具有变化的厚度的车辆部件以获得例如不等厚轧制板(tailored rolled blank)。具体地，部件可以是前纵梁(front rail)、座椅横向构件、门框下边梁(side sill)构件、前围挡板(dash panel)横向构件、前底板(front floor)加强件、后底板(rear floor)横向构件、后纵梁(rear rail)、B柱、门框或shotgun。
获得根据本发明的可磷酸盐化的硬化部件。
优选地，部件的金属涂层的显微组织包含金属间化合物层Fe3Al、相互扩散层Fe-Si-Al、分布在涂层中的低量的硅、以及涂层表面处的ZnO层。当镁存在于涂层中时，显微组织还包含Zn2Mg相和/或Mg2Si相。有利地，显微组织不包含金属锌。
对于汽车应用，在磷酸盐化步骤之后，将部件脱脂和磷酸盐化以确保电泳的附着性。在磷酸盐化之后，获得部件表面上磷酸盐晶体的高覆盖率。部件表面上磷酸盐晶体的覆盖率大于或等于80％，优选大于或等于90％，有利地大于或等于99％。
然后，将部件浸在e-涂覆浴中。通常，磷酸盐层的厚度为1μm至2μm，e-涂层的厚度为15μm至25μm，优选小于或等于20μm。电泳层确保了另外的抗腐蚀保护。
在e-涂覆步骤之后，可以沉积另外的涂料层，例如涂料的底漆涂层、底涂层(basecoat layer)和顶涂层(top coat layer)。
现在将在仅用于提供信息而进行的试验中说明本发明。这些试验不是限制性的。
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％；V＝0.0284％。
所有涂层通过热浸镀工艺沉积。
实施例1：磷酸盐化测试：
可磷酸盐化性(phosphatability)测试用于通过评估部件表面上的覆盖率来确定硬化部件上磷酸盐晶体的附着性。
准备试验件1至10并使其经历磷酸盐化测试。
为此，切割经涂覆的试验件以获得坯件。然后在5分钟至10分钟不等的停留时间期间在900℃的温度下加热坯件。将坯件转移至压制工具中并热冲压以获得部件。最后，使部件冷却以通过马氏体转变获得硬化。
然后实现脱脂。随后通过在50℃下浸渍在包含24TA、Add H7141、H7102、Add H7257、Add H7101、Add H7155的溶液的浴中持续3分钟实现磷酸盐化步骤。然后用水擦拭部件并用热空气干燥。通过SEM观察部件表面。结果示于下表1中：
＊：根据本发明的实施例，ND：未进行。
以上结果显示试验件7至10具有硬化部件上磷酸盐晶体的高覆盖率。
实施例2：涂料附着性测试：
该测试用于确定硬化部件的涂料附着性。
在实施例1中制备的试验件1至5和7至10上沉积20μm的e-涂层。为此，将所有试验件在30℃下浸渍在包括包含PPG Industries的ResinW7911-N6和PigmentW9712-N6的水性溶液的浴中持续180秒。施加200V电流。然后，擦拭板并使其在180℃下在烘箱中固化35分钟。
然后，将上涂料的部件在50℃的温度下浸渍在包含软化水的密封盒中持续10天。在浸渍之后，用切割器实现网格。用胶带撕扯涂料。
通过肉眼评估除去的涂料：0表示优异，换言之，有少量或没有涂料被除去，5表示非常差，换言之，有大量涂料被除去。结果示于下表2中：
＊：根据本发明的实施例
如同试验件10和14，根据本发明的试验件15至18显示出良好的涂料附着性。
实施例3：分层测试：
该测试用于确定在硬化部件的上涂料之后的腐蚀性。
在实施例1制备的试验件1至5、8和10上沉积20μm的e-涂层。为此，将所有试验件在30℃下浸渍在包括包含PPG Industries的ResinW7911-N6和PigmentW9712-N6的水性溶液的浴中持续180秒。施加200V电流。然后，擦拭板并使其在180℃下在烘箱中固化35分钟。
然后，用切割器在e-涂层上实现划痕。
最后，根据规范VDA 233-102实现包括使板经受腐蚀循环的测试。将试验件放入室中，在所述室中1重量％的氯化钠的水溶液以3mL.小时-1的流量汽化在试验件上。温度从50℃变化至-15℃，湿度率从50％变化至100％。图1示出对应于168小时(即，一周)的一个循环。
通过肉眼观察分层的存在：0表示优异，换言之，没有分层，5表示非常差，换言之，存在大量的分层。结果示于下表3中：
＊：根据本发明的实施例，ND：未进行。
与试验件18至22相反，根据本发明的试验件(试验件23和24)在2周和5周的腐蚀循环后产生少量分层。

Claims (29)

1.一种用于制造硬化部件的方法，这样的部件是磷酸盐化的，所述方法包括以下步骤：
A)提供预涂覆金属涂层的钢板，所述金属涂层包含4.0重量％至20.0重量％的锌，1.0重量％至3.5重量％的硅，任选的1.0重量％至4.0重量％的镁，以及任选的选自Pb、Ni、Zr或Hf的另外的元素，每种另外的元素以重量计的含量小于0.3重量％，余量为铝和不可避免的杂质以及残留元素，其中比率Zn/Si为3.2至8.0；
B)切割经涂覆的钢板以获得坯件；
C)在840℃至950℃的温度下对所述坯件进行热处理以在所述钢中获得完全奥氏体显微组织；
D)将所述坯件转移至压制工具中；
E)使所述坯件热成形以获得部件；
F)使步骤E)中获得的部件冷却以在钢中获得这样的显微组织，所述显微组织为马氏体或马氏体-贝氏体或由至少75％的等轴铁素体、5％至20％的马氏体和小于或等于10％的量的贝氏体构成；以及
G)磷酸盐化步骤。
2.根据权利要求1所述的方法，其中所述金属涂层包含1.5重量％至3.5重量％的硅。
3.根据权利要求2所述的方法，其中所述金属涂层包含1.5重量％至2.5重量％的硅。
4.根据权利要求2所述的方法，其中所述金属涂层包含2.1重量％至3.5重量％的硅。
5.根据权利要求1至4中任一项所述的方法，其中所述金属涂层包含10.0重量％至15.0重量％的锌。
6.根据权利要求1至4中任一项所述的方法，其中所述钢板的所述金属涂层使得比率Zn/Si为4至8。
7.根据权利要求1至4中任一项所述的方法，其中所述钢板的所述金属涂层使得比率Zn/Si为4.5至7.5。
8.根据权利要求1至4中任一项所述的方法，其中所述钢板的所述金属涂层使得比率Zn/Si为5至7.5。
9.根据权利要求1至4中任一项所述的方法，其中所述钢板的所述金属涂层包含1.1重量％至3.0重量％的镁。
10.根据权利要求1至4中任一项所述的方法，其中所述金属涂层包含大于76重量％的铝。
11.根据权利要求1至4中任一项所述的方法，其中所述金属涂层的厚度为5μm至50μm。
12.根据权利要求11所述的方法，其中所述金属涂层的厚度为10μm至35μm。
13.根据权利要求12所述的方法，其中所述金属涂层的厚度为12μm至18μm。
14.根据权利要求12所述的方法，其中所述金属涂层的厚度为26μm至31μm。
15.根据权利要求1至4中任一项所述的方法，其中所述金属涂层不包含选自以下的元素：Cr、Mn、Ti、Ce、La、Nd、Pr、Ca、Bi、In、Sn和Sb、或其组合。
16.根据权利要求1至4中任一项所述的方法，其中步骤C)在惰性气氛或包含空气的气氛中在1分钟至12分钟的停留时间期间进行。
17.根据权利要求1至4中任一项所述的方法，其中在步骤E)期间在600℃至830℃的温度下进行所述坯件的热成形。
18.一种能够根据权利要求1至17中任一项所述的方法获得的涂覆有金属涂层的部件，包含所述金属涂层上的ZnO层和在所述ZnO层上的磷酸盐晶体层。
19.根据权利要求18所述的部件，其中所述部件表面上磷酸盐晶体的覆盖率等于或大于90％。
20.根据权利要求19所述的部件，其中所述部件表面上磷酸盐晶体的覆盖率等于或大于99％。
21.根据权利要求18至20中任一项所述的部件，另外包含在所述磷酸盐晶体层上的e-涂层。
22.根据权利要求18至20中任一项所述的部件，其中所述金属涂层包含金属间化合物层Fe3Al、相互扩散层Fe-Si-Al、分布在所述涂层中的低量的硅。
23.根据权利要求18至20中任一项所述的部件，其中所述金属涂层的显微组织包含Zn2Mg相或Mg2Si相或二者。
24.根据权利要求18至20中任一项所述的部件，其中所述金属涂层的显微组织不包含金属锌。
25.根据权利要求18至20中任一项所述的部件，所述部件为具有可变厚度的压制硬化的钢部件。
26.根据权利要求25所述的部件，其中所述可变厚度通过连续柔性轧制过程产生。
27.根据权利要求25所述的部件，所述部件为不等厚轧制板。
28.根据权利要求25所述的部件，所述部件为是前纵梁、座椅横向构件、门框下边梁构件、前围挡板横向构件、前底板加强件、后底板横向构件、后纵梁、B柱、门框或shotgun。
29.根据权利要求18至28中任一项所述的部件或能够根据权利要求1至17中任一项所述的方法获得的部件用于制造机动车辆的用途。
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