CN113195779A - 耐蚀性和表面质量优异的锌合金镀覆钢材及其制造方法 - Google Patents

耐蚀性和表面质量优异的锌合金镀覆钢材及其制造方法 Download PDF

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CN113195779A
CN113195779A CN201980084605.4A CN201980084605A CN113195779A CN 113195779 A CN113195779 A CN 113195779A CN 201980084605 A CN201980084605 A CN 201980084605A CN 113195779 A CN113195779 A CN 113195779A
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zinc alloy
corrosion resistance
plated steel
surface quality
alloy plated
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金兴润
韩到暻
金明守
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Posco Holdings Inc
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Posco Co Ltd
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Priority claimed from PCT/KR2019/017543 external-priority patent/WO2020130482A1/ko
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    • C23C2/06—Zinc or cadmium or alloys based thereon
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Abstract

本发明涉及一种用于汽车、建筑材料、家电产品等的锌合金镀覆钢材，更详细地，涉及一种耐蚀性和表面质量优异的锌合金镀覆钢材及其制造方法。

Description

耐蚀性和表面质量优异的锌合金镀覆钢材及其制造方法
技术领域
本发明涉及一种用于汽车、建筑材料、家电产品等的锌合金镀覆钢材，更详细地，涉及一种耐蚀性和表面质量优异的锌合金镀覆钢材及其制造方法。
背景技术
铁是工业上使用最多的材料，铁具有优异的物理特性和机械特性。但是，铁因容易被氧化而具有容易腐蚀的缺点。因此，作为防止铁的氧化的方法，已开发了一种通过在材料表面涂覆与氧的反应性比铁高的金属作为保护膜来延迟腐蚀的方法。代表性的有形成锌薄膜或锌系薄膜的镀锌钢材。
所述镀锌钢材通过氧化电位更高的锌比基材铁先被溶解的牺牲防蚀作用和致密的锌的腐蚀产物延迟腐蚀的腐蚀抑制作用等来保护铁免受腐蚀。
但是，近年来，腐蚀环境日益恶化，并且在节省资源和能源方面，为了高度地提高耐蚀性，正在做出很多努力。作为这种努力的一个方面，还正在研究具有优异的耐蚀性的锌-铝合金镀覆，但在碱性条件下铝比锌更容易被溶解，因此存在在长期耐久性方面不充分的缺点。
近年来，获得了通过利用镁(Mg)来大幅提高耐蚀性的成果。专利文献1的特征在于，具有由Mg：0.05-10.0重量％、Al：0.1-10.0重量％、余量的Zn和不可避免的杂质组成的Zn-Mg-Al合金镀层，但形成粗大的镀覆组织或集中形成特定组织时，存在发生择优腐蚀的问题。
另外，作为通过控制镀层的组织来提高耐蚀性的成果，专利文献2的特征在于，具有Zn-Al-Mg-Si镀层，这些镀层具有在Al/Zn/Zn2Mg的三元共晶组织中混合存在Mg2Si相、Zn2Mg相、Al相、Zn相等的金属组织，但问题点在于受限于含有Si的高强度钢，并且镀覆组织中必须包含Si成分，因此存在用于镀覆的钢锭的制造成本增加且难以操作管理的问题。此外，作为通过在Zn-Al-Mg主要成分中添加其它元素来提高耐蚀性的技术，专利文献3的特征在于，在镀层中添加铬(Cr)，从而在Al-Fe-Si系合金层中包含Cr，但由于添加Cr成分而存在形成过多的浮渣的问题，并且具有不利于控制镀浴的成分的缺点。
因此，目前持续需要一种确保优异的耐蚀性的同时在浮渣等方面保护表面而具有优异的表面质量的镀覆钢材。
[现有技术文献]
(专利文献1)日本公开专利JP1999-158656号
(专利文献2)日本公开专利JP2001-295018号
(专利文献3)韩国公开专利第10-2011-0088573号
发明内容
要解决的技术问题
本发明的一个方面的目的在于提供一种通过优化镀层的组成和微细组织来确保优异的耐蚀性的同时具有优异的表面特性的锌合金镀覆钢材及其制造方法。
本发明的技术问题并不受限于上述内容。本发明的附加技术问题记载于说明书全文中，本发明所属技术领域中普通技术人员从本发明的说明书中记载的内容理解本发明的附加技术问题是没有任何困难的。
技术方案
本发明的一个实施方案提供一种耐蚀性和表面质量优异的锌合金镀覆钢材，所述锌合金镀覆钢材包括基材铁和形成在所述基材铁上的锌合金镀层，以重量％计，所述锌合金镀层包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质，在所述锌合金镀层的表面观察到的多边形凝固相所占的面积分数为20-90％。
本发明的另一个实施方案提供一种制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，所述方法包括以下步骤：准备基材铁；将准备的所述基材铁浸入镀浴中进行镀覆，以重量％计，所述镀浴包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质；对镀覆的所述基材铁进行擦拭；以及所述擦拭后，在热浸镀锌层表面形成多边形凝固相。
有益效果
根据本发明，可以提供一种具有优异的耐蚀性和表面特性的Zn-Al-Mg系锌合金镀覆钢材及其制造方法。特别地，所述锌合金镀覆钢材具有优异的耐蚀性和表面特性，因此具有可以扩大应用于现有的镀覆钢材未能被应用的新领域的优点。
附图说明
图1是示出观察本发明的实施例中的发明例1的镀层表面的照片。
图2是示出观察本发明的实施例中的比较例1的镀层表面的照片。
最佳实施方式
以下，对本发明进行详细说明。
本发明的锌合金镀覆钢材包括基材铁和形成在所述基材铁上的锌合金镀层。
对所述基材铁的种类不作特别限定，只要是可在本发明所属技术领域中应用的基材铁即可。例如，所述基材铁可以是热轧钢板、冷轧钢板、线材及钢线等。
所述锌合金镀层以锌(Zn)为基础包含镁(Mg)和铝(Al)。以重量％计，所述锌合金镀层优选包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质。此外，所述锌合金镀层可以进一步包含0.0005-0.009％的Be、Ca、Ce、Li、Sc、Sr、V和Y中的一种以上。以下，对各成分的组成范围进行详细说明。
铝(Al)：8-25重量％(以下，％)
所述Al在制造熔融金属时使Mg成分稳定化，并且在腐蚀环境中起到抑制初期腐蚀的腐蚀屏障的作用，Al含量可以根据Mg的含量而不同。当所述Al含量小于8％时，在制造熔融金属时无法使Mg稳定化，因此在熔融金属表面生成Mg氧化物而难以使用。另一方面，当所述Al含量超过25％时，镀覆温度上升，并且设置在镀浴中的各种设备发生严重的溶蚀，因此不优选。
镁(Mg)：4-12％
所述Mg是形成表现出耐蚀性的组织的主要成分，当所述Mg含量小于4％时，不能充分地表现出耐蚀性，当所述Mg含量超过12％时，存在形成大量的Mg氧化物的问题，从而可能会再次引起材质变差和成本上升等各种问题，因此，优选包含4-12％的所述Mg。更优选可以包含5％以上的所述Mg。
另外，优选地，所述Al和Mg满足以下关系式1。
[关系式1]
Mg≤-0.0186*Al2+1.0093*Al+4.5
其中，Al和Mg表示各成分的含量(重量％)。在本发明中，为了镀覆时使熔融金属稳定化并最大限度地抑制氧化物的形成，所述Al和Mg的含量优选满足关系式1的条件。
另外，除了所述Al和Mg之外，为了使Mg成分进一步稳定化，还可以包含铍(Be)、钙(Ca)、铈(Ce)、锂(Li)、钪(Sc)、锶(Sr)、钒(V)和钇(Y)等，并且优选的含量为0.0005-0.009％。当所述含量小于0.0005％时，难以期待实质性的Mg稳定化效果，当所述含量超过0.009％时，在镀覆后期凝固，先发生腐蚀，从而可能会损害耐蚀性，并且存在成本上升的问题，因此不优选。
除了所述合金组成之外，余量包含锌(Zn)和不可避免的杂质。并不排除上述组成之外的有效成分的添加。
所述锌合金镀层的表面包含多边形凝固相，在表面观察到的多边形凝固相所占的面积分数优选为20-90％。
用扫描电子显微镜(Scanning Electron Microscope，SEM)和光学显微镜观察所述锌合金镀层的表面时，观察到多边形、圆形、椭圆形、砂状等各种形状的组织。本发明中所述多边形凝固相是在表面观察到的组织中的一种，其暴露在表层，并且在颜色和形状等方面与周围的其它凝固组织存在明显区别。即，如图1所示，与周围的其它组织的界限几乎是以直线区分，并且所述直线和直线交叉并形成一定的角度。此时，可以构成各种角度，因此对其不作特别限定。此外，所述多边形凝固相可以多重重叠地形成，并可以具有多个角度，并且所有多边形凝固组织内部可以不具有相同的颜色或相同的形状。一部分组织可能会重叠并变形而显示得不同，因此具有两个以上的所述角度时，将其作为多边形凝固相来包括。
所述多边形凝固相中检测出Zn、Al和Mg中的两种至三种成分，因此其可以是在单一金属间化合物或金属间化合物中包含用于稳定Zn和Al的附加元素等的合金相。其中，金属间化合物可以是MgZn2、Mg2Zn11等。
所述多边形凝固相在表面所占的面积优选为以面积分数计为20-90％。当所述多边形凝固相的面积小于20％时，耐蚀性和加工性不足，当所述多边形凝固相的面积超过90％时，反而会发生耐蚀性降低的问题。面积分数更优选为30-70％。所述多边形凝固相是在表面观察到的，因此以在表面积中所占的面积来表示。
所述多边形凝固相的长轴(b)与短轴(a)之比(b/a)的平均优选为1-3。如图1所示，多边形凝固相的形状可以由短轴(a)和长轴(b)来规定，包括一部分凝固相重叠而难以分离或变形的所有情况，并且可以以b/a之比来表示。当所述b/a比例为1以上时，加工性优异，但b/a之比变得过大而使得凝固相变得过长时，不利于加工。因此，当所述b/a之比超过3时，反而不利于加工性，因此所述b/a优选为1-3。
本发明的锌合金镀层可以包含各种相(phase)。例如，可以是MgZn2、Mg2Zn11、Al固溶相、Zn固溶相、Al/Zn/Mg共晶相等。其中，所述锌合金镀层的微细组织中所述MgZn2和Mg2Zn11中的一种以上的面积分数优选为20-45％。该面积分数优选为镀层的表面积的面积分数。
本发明中形成在所述锌合金镀层中的相实际上可以是在非平衡状态下形成的相。例如，MgZn2的情况下，以原子％计，计算Mg/Zn之比时，应由0.33构成，但实际上也有被计算为0.19-0.24的情况。此外，在非平衡状态下生成的所述相中可以检测出其它成分，这些其它成分通过综合研究成分分析和形状分析等来确定。
当所述MgZn2和Mg2Zn11中的一种以上少于20％时，在通常的水分环境和盐水环境中耐蚀性不充分，当所述MgZn2和Mg2Zn11中的一种以上超过45％时，耐蚀性增加，但所述MgZn2合金相和Mg2Zn11合金相为硬质相，因此产生镀层的裂纹的可能性增加。所述MgZn2和Mg2Zn11中的一种以上更优选为20-40％。
余量可以包含Zn固溶相、Al固溶相，Al/Zn/Mg共晶相和非化学计量组成等。
以下，对本发明的制造锌合金镀覆钢材的一个具体实施方案进行详细说明。
本发明中提出用于形成耐蚀性和表面外观优异的锌合金镀层的方法。
镀层的凝固过程通过成核和生长进行，冷却时生成凝固核，凝固核在热力学的吉布斯自由能最低的位置生成。与均匀成核相比，不均匀成核时，所述吉布斯自由能的差异成为有利于凝固的位置，不均匀成核位置的面积越大，则越有利于成核，并且实现大量成核。此时，不均匀成核位置是熔融金属的液相和固相接触的位置，具有代表性的不均匀成核位置是钢板的表面。另一种不均匀成核位置是熔融金属的液相与空气接触的位置，是熔融金属的表面。因此，本发明的发明人为了在镀层表面形成多边形凝固相，得出调节从镀浴中取出的钢材的凝固的方法。
本发明的制造锌合金镀覆钢材的方法包括以下步骤：准备基材铁，将准备的基材铁浸入镀浴中进行镀覆，然后进行擦拭以调节镀层厚度，并在热浸镀锌层表面形成多边形凝固相。以下，对各个步骤进行详细说明。
首先，准备基材铁。如上所述，对所述基材铁的种类不作限制，只要是本发明所属技术领域中可应用的基材铁即可。在将所述基材铁浸入镀浴之前，可以包括去除存在于表面的氧化物和杂质等的工艺以及用于还原的热处理工艺等。
将所述基材铁浸入镀浴中以在基材铁表面形成锌合金镀层。以重量％计，所述镀浴的组成优选包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质，并且还可以包含0.0005-0.009％的选自Be、Ca、Ce、Li、Sc、Sr、V和Y中的一种以上。此外，所述Al和Mg的含量可以满足以下关系式1。所述镀浴的合金组成范围与上述锌合金镀层的合金组成范围相同。
[关系式1]
Mg≤-0.0186*Al2+1.0093*Al+4.5
所述镀浴的温度根据熔点而不同，所述熔点为依赖于镀浴的组成的物理化学特性。确定所述镀浴的温度的因素有多种，如操作的便利性、加热成本和镀覆质量等。综合考虑这些因素时，将所述镀浴的温度设为高于熔点，优选将镀浴的温度设为比熔点高20-100℃。
另外，浸入镀浴中的基材铁的温度是考虑操作的便利性、热平衡等来设置。优选地，将所述基材铁的温度设置为所述镀浴温度的-10℃至+10℃。
对从所述镀浴中取出的锌合金镀覆钢材进行擦拭处理，所述擦拭处理是通过镀浴上部的称为气刀(air knife)的擦拭喷嘴来调节镀层厚度。所述擦拭喷嘴通过喷射空气或惰性气体来调整镀层的厚度。
所述擦拭处理后，在镀层表面形成多边形凝固相。为此，首先，喷射以体积分数计的氮气浓度为78-99％的气体(一次气体喷射)，再次，依次喷射露点为-5℃至50℃的气体(二次气体喷射)。
所述一次气体喷射时，对除氮气之外的气体不作特别限制，但可以包含空气、氧气或氮气、氩气等惰性气体和它们的混合气体。另外，所述二次气体喷射中的露点是规定气体中包含的水分量的特定值，此时，二次气体喷射时，对气体的种类不作特别限制。作为一个实例，可以使用氮气浓度为89-99％的气体。
所述一次气体喷射时，当氮气浓度小于78％时，容易发生表面缺陷，当氮气浓度超过99％时，多边形凝固相的形成不足。此外，二次气体喷射时，露点上升时多边形凝固核的形成增加，当露点低于-5℃时，所述多边形凝固核的形成增加的不充分，当露点超过50℃时，存在产生大量表面缺陷的问题。
另外，进一步地，在二次气体喷射后，为了赋予有利于形成多边形凝固相的环境，可以施加100Hz-5MHz的振动。当所述振动小于100Hz时，在镀层表面的多边形凝固相的形成可能会不足，当所述振动超过5MHz时，可能会发生表面缺陷。
具体实施方式
以下，对本发明的实施例进行详细说明。以下实施例仅仅是用于理解本发明，并不用于限定本发明的权利范围。这是因为本发明的权利范围由权利要求书中记载的内容和由此合理推导的内容所确定。
(实施例)
作为基材铁准备厚度为0.8mm且包含0.03重量％的C、0.2重量％的Si、0.15重量％的Mn、0.01重量％的P和0.01重量％的S(余量为Fe和不可避免的杂质)的冷轧钢板，经过用于去除油等沾在钢板表面的杂质的脱脂工艺，然后经过在10体积％的氢气和90体积％的氮气的还原性气氛中以800℃进行热处理的工艺，然后浸入锌合金热浸镀浴中，从而制造具有下表1的镀层的组成的镀覆钢板。此时，所述锌热浸镀浴的温度设为493℃，所引入的钢板的温度也设为493℃。所述浸入后，通过气体擦拭，将镀层的厚度调节为约8-10μm。之后，进行表1的一次气体处理和二次气体处理，从而制造镀覆钢板。
对于所制造的锌合金镀覆钢材，通过EDS分析鉴定相，并通过XRD分析测量MgZn2相和Mg2Zn11相的分数。另外，利用图像分析仪(image analyzer)测量多边形凝固相的面积率，长轴(b)与短轴(a)之比(b/a)是分别测量长度来进行计算。
对于所述锌合金镀覆钢材，评价表面质量和耐蚀性，并将其结果一同示于表1中。
对于所述耐蚀性，进行盐水喷雾试验，测量红锈产生时间，并与比较样品进行比较来评价。此时，作为比较样品使用了镀层的组成为94重量％的Zn、3重量％的Al和3重量％的Mg的锌合金镀覆钢材，所述盐水喷雾试验是以5％的盐度、35℃的温度、6.8的pH、2ml/80cm2·1小时的盐水喷雾量来进行。
就评价结果而言，与比较样品相比，当红锈产生时间为1.5倍以上时，评价为良好(○)，当红锈产生时间小于1.5倍时，评价为不良(×)。
另外，表面质量是在所制造的样品中通过观察样品的外观来评价是否发生浮渣等表面缺陷。其结果如下。
良好(○)：表面没有发生浮渣、斑点等缺陷
不良(×)：表面发生浮渣、斑点等缺陷
[表1]
Figure BDA0003122183570000091
Figure BDA0003122183570000101
如所述表1所示，可知满足本发明的条件的发明例均具有优异的表面质量和耐蚀性。
特别地，图1是示出观察所述发明例1的表面的照片，观察所述图1时，可知形成有适当分数的直线交叉而形成一定角度的多边形凝固相。另一方面，图2是示出观察所述比较例1的表面的照片，可知与图1比较时，难以在表面观察到多边形凝固相。
比较例1和比较例2是提出的作为镀层的必要成分的Al和Mg的含量不在本发明中提出的范围的情况，比较例1的Al和Mg的含量过少，在表面观察到的多边形凝固相不充分，因此无法确保耐蚀性，比较例2的镀层的Al和Mg的含量过多，并且表面上的多边形凝固相过多，因此可知表面质量和耐蚀性均差。
比较例3是镀层中包含过多的为了进一步的效果而添加的Be的情况，可知表面质量和耐蚀性差。比较例4和比较例5不满足本发明中提出的气体喷射条件，因此可以确认镀层的表面耐蚀性或表面特性差。

Claims (10)

1.一种耐蚀性和表面质量优异的锌合金镀覆钢材，其包括基材铁和形成在所述基材铁上的锌合金镀层，
以重量％计，所述锌合金镀层包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质，
在所述锌合金镀层的表面观察到的多边形凝固相所占的面积分数为20-90％。
2.根据权利要求1所述的耐蚀性和表面质量优异的锌合金镀覆钢材，其中，所述多边形凝固相的长轴(b)与短轴(a)之比(b/a)为1-3。
3.根据权利要求1所述的耐蚀性和表面质量优异的锌合金镀覆钢材，其中，所述锌合金镀层的微细组织中MgZn2和Mg2Zn11中的一种以上的面积分数为20-45％。
4.根据权利要求1所述的耐蚀性和表面质量优异的锌合金镀覆钢材，其中，所述Al和Mg满足以下关系式1，
[关系式1]
Mg≤-0.0186*Al2+1.0093*Al+4.5
其中，所述Al和Mg表示各成分的含量(重量％)。
5.根据权利要求1所述的耐蚀性和表面质量优异的锌合金镀覆钢材，其中，所述锌合金镀层还包含0.0005-0.009％的选自Be、Ca、Ce、Li、Sc、Sr、V和Y中的一种以上。
6.一种制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，其包括以下步骤：
准备基材铁；
将准备的所述基材铁浸入镀浴中进行镀覆，以重量％计，所述镀浴包含：Al：8-25％、Mg：4-12％、余量的Zn和不可避免的杂质；
对镀覆的所述基材铁进行擦拭；以及
所述擦拭后，在热浸镀锌层表面形成多边形凝固相。
7.根据权利要求6所述的制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，其中，将包含以体积分数计为78-99％的氮气的气体喷射在热浸镀锌层表面(一次气体喷射)，然后喷射露点为-5℃至50℃的气体(二次气体喷射)，从而形成所述多边形凝固相。
8.根据权利要求7所述的制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，其中，在喷射所述气体后，还包括施加100Hz-5MHz的振动。
9.根据权利要求6所述的制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，其中，所述Al和Mg满足以下关系式1，
[关系式1]
Mg≤-0.0186*Al2+1.0093*Al+4.5
其中，所述Al和Mg表示各成分的含量(重量％)。
10.根据权利要求6所述的制造耐蚀性和表面质量优异的锌合金镀覆钢材的方法，其中，所述镀浴还包含0.0005-0.009％的选自Be、Ca、Ce、Li、Sc、Sr、V和Y中的一种以上。
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