CN104024468B - 具有高抗变黑性和涂层粘附性的Zn‑Mg合金涂覆钢板及其制造方法 - Google Patents

具有高抗变黑性和涂层粘附性的Zn‑Mg合金涂覆钢板及其制造方法 Download PDF

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CN104024468B
CN104024468B CN201280065252.1A CN201280065252A CN104024468B CN 104024468 B CN104024468 B CN 104024468B CN 201280065252 A CN201280065252 A CN 201280065252A CN 104024468 B CN104024468 B CN 104024468B
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coatings
oxide
steel plate
film
alloy
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CN104024468A (zh
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李东烈
南庆勋
郑勇华
洪锡俊
金兑烨
郭荣镇
严文钟
郑宇城
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Posco Holdings Inc
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Posco Co Ltd
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Abstract

提供一种具有高抗变黑性和涂层粘附性的Zn‑Mg合金涂覆钢板及制造该Zn‑Mg合金涂覆钢板的方法，该Zn‑Mg合金涂覆钢板包括：基底钢板；形成于基底钢板上的Zn‑Fe金属间化合物层；形成于Zn‑Fe金属间化合物层上的第一Zn‑Mg涂层，其包含锌(Zn)含量为95重量％或更高的Zn‑Mg金属间化合物；形成于第一Zn‑Mg涂层上的第二Zn‑Mg涂层，其包含锌(Zn)含量为80重量％至95重量％的Zn‑Mg金属间化合物；以及形成于第二Zn‑Mg涂层上的氧化膜，其包含金属氧化物。

Description

具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板及其制 造方法
技术领域
本公开涉及一种在诸如汽车、家用电器和建筑的工业应用中的用作基体材料的Zn-Mg合金涂覆钢板，更具体而言，涉及一种具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板。
背景技术
钢板表面可通过诸如电镀锌(electrogalvanization)和热浸镀锌(hot-dipgalvanization)的方法进行镀锌，以提高该钢板的耐腐蚀性和耐久性。与未涂覆钢板相比，由于锌起到牺牲阳极的作用，镀覆钢板具有高耐腐蚀性，并因此广泛用作汽车、家用电器和建筑的材料。
然而，在这些工业领域中，除了需要高耐久性的涂覆钢板以外，也越来越需要相对质轻且经济性高的涂覆钢板。
同时，由于地下的锌矿数量有限以及对锌储藏消耗的关注，使用锌矿作为斗争工具(weapon)的趋势上升。此外，现有的电镀锌工艺和热浸镀锌工艺消耗大量能量且排放污染物，由于全球范围内对污染物的管制日益加强，因而上述污染物排放是不利的。
由于这些原因，通过真空沉积法形成的Zn-Mg合金涂覆钢板受到关注。根据所述真空沉积法，在真空中进行涂覆过程以生产Zn-Mg合金涂覆钢板。因此，污染物排放非常低，且随着蒸镀涂覆材料技术的发展，可得到高于现有镀覆工艺的生产率。此外，由于可制造出具有高抗腐蚀性且涂膜厚度薄的Zn-Mg合金涂覆钢板，因此Zn-Mg合金涂覆钢板作为具有经济性前景的钢板而受到关注。
尽管Zn-Mg涂层在制造工艺和产品性能方面具有上述优点，但Zn-Mg涂层比锌涂层更硬且更脆，因此难以提高Zn-Mg涂层的粘附性。
此外，由于镁(Mg)非常活跃，涂覆有Zn-Mg的产品表面会在潮湿环境中的与湿气反应，因此产品表面可能变黑且质量变差。
专利文献1公开了一种用于解决这一变黑问题的技术。根据专利文献1中公开的技术，防止Zn-Mg涂覆产品变黑通过以下方法进行：用0.01％至30％的磷酸钙溶液处理Zn-Mg涂覆产品以洗脱镁(Mg)，并将Zn-Mg涂覆产品表面的镁(Mg)含量调节至1重量％或更低。然而，根据专利文献1中公开的技术，对镁(Mg)的洗脱不均匀。因此，在用磷酸钙溶液处理的过程中，由于形成含有镁(Mg)的磷酸钙，Zn-Mg涂覆产品表面可能被污染或变黑。
(专利文献1)第1997-241828号日本专利申请公开出版物
发明内容
[技术问题]
本公开的几个方面可包括具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板，以及制造该Zn-Mg合金涂覆钢板的方法。
[技术方案]
根据本公开的一个方面，一种具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板可包括：基体钢板；形成于所述基体钢板上的Zn-Fe金属间化合物(intermetallic)层；形成于所述Zn-Fe金属间化合物层上的第一Zn-Mg涂层，其包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物；形成于所述第一Zn-Mg涂层上的第二Zn-Mg涂层，其包含锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物；以及形成于所述第二Zn-Mg涂层上的氧化膜，其包含金属氧化物。
根据本公开的另一方面，一种用于制造具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板的方法包括：在基体钢板上形成Zn-Mg涂层；实施一种燃烧化学气相沉积(CCVD)法以形成氧化膜。
[有益效果]
根据本公开，通过燃烧化学气相沉积(CCVD)法在Zn-Mg合金涂覆钢板上形成一种氧化膜以改善现有钢板的缺点，即提高涂层粘附性和抵抗湿气导致的变黑。因此，本公开的Zn-Mg合金涂覆钢板作为工业应用如汽车、家用电器和建筑中的经济型基础工业材料来提供。此外，所述Zn-Mg合金涂覆钢板可作为具有高耐久性和高质量表面的钢板进行商业化，并具有较大的市场份额。
附图说明
图1示出常规试样截面的S-TEM及TEM照片(a)和发明试样截面的S-TEM及TEM照片(b)。
图2示出摄于沸水测试之前和之后的发明试样的照片(a)和常规试样的照片(b)
图3示出对发明试样进行涂层粘附性测试(胶带测试)的结果(a)和对常规试样进行涂层粘附性测试(胶带测试)的结果(b)。
最佳实施方式
本公开的实施方案中使用的燃烧化学气相沉积(CCVD)法与传统物理气相沉积(PVD)法或传统化学气相沉积(CVD)法的不同之处在于，用作燃料的烃(如丙烷)与以前体(如HMDSO(原材料气体分子))饱和的空气混合，并将所述混合物(气体混合物)在大气压下燃烧所产生的热量用作前体进行蒸发、沉积和化学反应的能量来源，从而形成表面上的涂层。
在本公开的实施方式中，以有机硅烷作为CCVD法中的前体，从而在金属表面上形成因与来自空气中的氧偶联而具有交联键的金属氧化物(如二氧化硅)作为沉积涂层。
在下文中，将详细描述本公开的实施方案。
发明人发现，通过PVD法形成的Zn-Mg合金涂覆钢板的涂层具有不均匀分布的Zn-Mg、Zn和Mg结晶区，并且由于在所述涂层与Zn-Mg合金涂覆钢板之间形成精细的天然氧化层，所述涂层容易分离。此外，发明人发现，通过PVD法形成的Zn-Mg合金涂覆钢板由于与湿气反应在其上形成水合物而变黑。
因此，发明人通过采用CCVD法将Zn-Mg合金涂覆钢板暴露于高温火焰中。在这种情况下，Zn-Mg合金涂覆钢板的涂层变得均匀，并且所述涂层的粘附性提高。此外，氧化膜防止了所述涂层变黑。基于此知识，发明人发明了本公开的Zn-Mg合金涂覆钢板。
在CCVD法中，使烃(丙烷)和以原材料气体分子(前体)饱和的空气的气态混合物在大气压下燃烧，燃烧产生的热量用作能量来源，从而通过蒸发、沉积和氧化原材料气体分子形成具有交联结构的氧化膜。
首先，将根据本发明公开的一个实施方案详细描述一种Zn-Mg合金涂覆钢板。
所述实施方式中的Zn-Mg合金涂覆钢板包括：
基体钢板；
形成于所述基体钢板上的Zn-Fe金属间化合物层；
形成于所述Zn-Fe金属间化合物层上的第一Zn-Mg涂层，其包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物；
形成于所述第一Zn-Mg涂层上的第二Zn-Mg涂层，其包含锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物；以及
形成于所述第二Zn-Mg涂层上的氧化膜，其包含金属氧化物。
基体钢板的种类不受限制。换言之，本实施方案可应用任意种类的钢板，如热轧钢板、冷轧钢板和任意种类的金属板。
Zn-Fe金属间化合物层形成于基体钢板上。在CCVD法(将在下文中描述)中，存在于基体钢板与Zn-Mg涂层之间的精细氧化膜会扩散到Zn-Mg涂层中，因而可形成Zn-Fe金属间化合物层。所述Zn-Fe金属间化合物层改进基体钢板与Zn-Mg涂层之间的粘附性。
第一Zn-Mg涂层形成于Zn-Fe金属间化合物层上并包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物；第一Zn-Mg涂层为软富Zn区域。因此，第一Zn-Mg涂层具有高粘附性。
如第一Zn-Mg涂层中的锌(Zn)含量低于95重量％，则第一Zn-Mg涂层因Zn-Mg合金的影响会变脆，因而第一Zn-Mg涂层的粘附性可能不高。因此，较高含量的锌(Zn)可能是有利的。然而，为了形成Zn-Mg金属间化合物，锌(Zn)含量可优选低于100重量％。
第二Zn-Mg涂层形成于第一Zn-Mg涂层上并包含锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物。由于Zn-Mg合金的特性，第二Zn-Mg涂层与常规的锌涂层相比具有高耐腐蚀性。
Zn-Mg金属间化合物可优选具有80重量％至95重量％的锌(Zn)含量。如锌(Zn)含量低于80重量％，则第二Zn-Mg涂层的耐腐蚀性因具有不同的晶体形状的Zn-Mg合金涂层的影响而降低。
氧化膜形成于第二Zn-Mg涂层上。所述氧化膜包含有金属氧化物。所述氧化膜阻挡湿气的渗入，并因此防止变黑。
氧化膜包含通过CCVD法形成的金属氧化物(如二氧化硅，(SiO2))。此外，在实施CCVD法的过程中，通过高温空气的氧气形成氧化镁(MgO)作为天然氧化膜，且所述氧化镁与氧化膜共存。
氧化膜可优选具有10nm至40nm的厚度。如氧化膜的厚度小于10nm，则无法充分防止水蒸汽的渗入，由此可能无法实现充分的抗变黑性。另一方面，如氧化膜的厚度大于40nm，则氧化物颗粒(即氧化膜的SiO2颗粒)会变粗，因此所述氧化膜可能无法起到阻挡膜的作用。
在下文中，将根据本公开的一个实施方案详细描述一种制造Zn-Mg合金涂覆钢板的方法。
首先，在基体钢板上形成Zn-Mg涂层。此时，所述Zn-Mg涂层不是上述实施方案中描述的第一Zn-Mg涂层和第二Zn-Mg涂层。换言之，所述Zn-Mg涂层不是最终的Zn-Mg涂层。所述Zn-Mg涂层将通过随后的CCVD法来修饰。
所述Zn-Mg涂层可通过PVD法形成。例如，所述Zn-Mg涂层可通过相关领域中已知的常规PVD方法形成。
例如，在热PVD法或溅射法中，通过利用热能或离子碰撞能使大量的Zn-Mg或包含Zn和Mg的原始涂层材料在真空中蒸发，并且将蒸发的Zn-Mg或原始涂层材料引导至通过卷对卷(roll-to-roll)法连续进料至真空中的钢板或金属板的表面，从而在钢板或金属板的表面形成Zn-Mg合金涂层。热PVD法或溅射法可用于形成本公开的实施方案中的Zn-Mg涂层。特别地，在电磁PVD(EML-PVD)法中，即在一种利用电磁感应的热PVD方法中，通过电磁感应使Zn-Mg合金涂层材料在真空中悬浮并加热，从而快速产生大量的蒸汽并利用该蒸汽形成涂层。由于高生产率和经济效益，EML-PVD方法广泛地用于生产Zn-Mg涂覆产品。
在形成有Zn-Mg涂层的基体钢板上实施CCVD法，从而在所述Zn-Mg涂层上形成氧化膜。具体而言，通过CCVD法，在基体钢板上形成上述实施方案中描述的这种层(膜)。换言之，Zn-Fe金属间化合物层形成于基体钢板上；第一Zn-Mg涂层形成于所述Zn-Fe金属间化合物层上，所述第一Zn-Mg涂层包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物；第二Zn-Mg涂层形成于所述第一Zn-Mg涂层上，所述其中第二Zn-Mg涂层包含Zn-Mg锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物；氧化膜形成于所述第二Zn-Mg涂层上，所述氧化膜饱和金属氧化物。以这种方式，根据本公开的制造方法制造Zn-Mg合金涂覆钢板。
在CCVD法中，基体钢板可距离CCVD设备燃烧器10mm或更小的距离放置。另外，在CCVD法中，如根据以下比例提供空气和前体蒸汽，则可形成具有最佳特性的金属氧化物沉积膜。
前体流速:空气流速＝0.8:210至2.1:210(L/min)
如所述流速比小于0.8:210(L/min)，则由于形成膜的颗粒的量相对于空气量较小，而会形成未起到阻挡层作用的过薄或精细的膜。另一方面，如所述流速比大于2.1:210(L/min)，则由于前体粒子颗粒聚集在一起(粗颗粒)，而不会密集地形成膜(涂层)，并因此无法起到阻挡层的作用。
在CCVD法中，基体钢板可优选保持在330℃至450℃的温度范围内。如基体钢板保持在低于330℃的温度，则涂层不会具有原子扩散所必需的足够能量，因此所述涂层在CCVD过程期间不会变得均匀。另一方面，如所述基体钢板保持在高于450℃的温度，则在基体钢板与具有高密度的锌(Zn)的第一Zn-Mg涂层之间发生Zn-Fe合金的剧烈反应，因此Zn-Fe合金层可能过度形成，而不利地影响涂层粘附性。
[具体实施方式]
在下文中，将详细描述本公开的一个实施例。以下实施例用于说明性目的，并非旨在限制本公开的范围。
(实施例)
进行以下实验以评价钢板的抗变黑性和涂层粘附性随着钢板的氧化膜厚度和加热温度变化的变化情况。
制备常规的冷轧钢板(连续的带卷(strip coils))。然后，在该冷轧钢板上进行EML-PVD工序，一种利用电磁感应的热PVD法。具体而言，在EML-PVD过程中，通过电磁感应使Zn-Mg合金涂覆材料在真空中悬浮并加热，从而快速产生大量的蒸汽并将该蒸汽引导至通过卷对卷法连续进料至真空中的冷轧钢板表面。从而在冷轧钢板的表面形成Zn-Mg涂层。
随后，对形成Zn-Mg涂层的钢板进行CCVD工序，以通过使用有机硅烷在该钢板上形成二氧化硅膜。以这种方式，制造其上形成氧化膜的Zn-Mg合金涂覆钢板。在CCVD过程中，如表1所示，不同温度下，氧化膜在钢板上形成不同的厚度(处理循环)。
参照表1，对其上未形成氧化膜的对比试样7至10(钢板)进行不同温度下的测试，从而评价在CCVD过程中，随着对比试样7至10的温度变化的对比试样7至10的涂层粘附性。
如表1所示，测试了每一个Zn-Mg合金涂覆钢板的抗变黑性和涂层粘附性。通过以下方法评价每一个Zn-Mg合金涂覆钢板的涂层粘附性：将胶带粘附于钢板(试样)、弯曲钢板、分离胶带和观察胶带，从而根据涂层从钢板的分离情况来确定该涂层粘附性是好还是坏。通过以下方法评价每一个Zn-Mg合金涂覆钢板的抗变黑性：将钢板浸在沸水中并观察钢板的颜色，从而根据钢板颜色的变化来确定其抗变黑性是是好还是坏。
[表1]
满足本公开实施方案的条件的发明试样具有高抗变黑能力和涂层粘附性。图1示出常规试样的结构(a)和发明试样的结构(b)。参照图1，在常规试样中，Zn-Mg合金涂层作为混合层形成于基体钢板上。然而，在发明试样中，金属间化合物层、富Zn层、Zn-Mg合金层和最外层氧化膜形成于基体钢板上。因此，根据本公开的实施方案形成的发明试样具有高抗变黑性和涂层粘附性。
不满足本公开实施方案的氧化膜厚度条件的对比试样1和6具有较差的抗变黑性。满足本公开实施方案的氧化膜厚度条件，但不满足本公开实施方案的温度条件的对比试样2至5具有良好的抗变黑性和较差的涂层粘附性。
对比试样8和9，满足本公开实施方案的温度条件，具有良好的涂层粘附性。然而，由于氧化膜未形成于对比试样8和9上，对比试样8和9具有较差的抗变黑性能。对比试样7和10，不满足本公开实施方案的温度条件，具有较差的涂层粘附性。
图2示出摄于沸水测试之前和之后的发明试样的照片(a)和常规试样的照片(b)。参照图2，发明试样的颜色未改变。换言之，发明试样具有高抗变黑性。然而，常规试样完全变黑。
图3示出对发明试样进行的胶带测试结果(a)和对常规试样进行的胶带测试结果(b)。参照图3，该发明试样具有比常规试样更高的涂层粘附性。

Claims (4)

1.一种具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板，所述Zn-Mg合金涂覆钢板包括：
基体钢板；
形成于所述基体钢板上的Zn-Fe金属间化合物层；
形成于所述Zn-Fe金属间化合物层上的第一Zn-Mg涂层，其包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物；
形成于所述第一Zn-Mg涂层上的第二Zn-Mg涂层，其包含锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物；以及
形成于所述第二Zn-Mg涂层上的氧化膜，其中所述氧化膜包含二氧化硅(SiO2)，且氧化镁(MgO)作为氧化膜的一部分包括在内，并且所述氧化膜具有11nm到40nm的厚度。
2.一种用于制造具有高抗变黑性和涂层粘附性的Zn-Mg合金涂覆钢板的方法，所述方法包括：
在基体钢板上形成Zn-Mg涂层；
实施燃烧化学气相沉积(CCVD)法以形成氧化膜，从而所述Zn-Mg涂层包含第一Zn-Mg涂层和形成于所述第一Zn-Mg涂层上的第二Zn-Mg涂层，所述第一Zn-Mg涂层包含锌(Zn)含量为95重量％或更高的Zn-Mg金属间化合物，所述第二Zn-Mg涂层包含锌(Zn)含量为80重量％至95重量％的Zn-Mg金属间化合物，
其中所述氧化膜包含二氧化硅(SiO2)，且氧化镁(MgO)作为氧化膜的一部分包括在内，并且所述氧化膜具有11nm到40nm的厚度，
其中在CCVD过程中，所述基体钢板保持在330℃至450℃的温度范围内。
3.权利要求2的方法，其中，所述Zn-Mg涂层的形成通过物理气相沉积(PVD)方法进行。
4.权利要求2的方法，其中，在CCVD过程中，根据以下比例提供空气和前体蒸汽：
前体流速:空气流速＝0.8:210至2.1:210，以L/min计。
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