CN110139944A - 点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法 - Google Patents

点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法 Download PDF

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CN110139944A
CN110139944A CN201780080861.7A CN201780080861A CN110139944A CN 110139944 A CN110139944 A CN 110139944A CN 201780080861 A CN201780080861 A CN 201780080861A CN 110139944 A CN110139944 A CN 110139944A
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galvanized alloy
single layer
alloy steel
galvanized
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郭荣镇
金兑烨
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Posco Holdings Inc
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Abstract

本发明公开一种单层镀锌合金钢材及其制造方法，所述单层镀锌合金钢材包括基材铁和形成在所述基材铁上的镀锌合金层，所述镀锌合金层包含13～24重量％的Mg，所述镀锌合金层的附着量为40g/m2以下(0g/m2除外)。

Description

点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法
技术领域
本发明涉及一种点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法，更详细而言，涉及一种可应用于汽车，家电产品及建筑材料等的点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法。
背景技术
通过阴极防腐来抑制铁的腐蚀的镀锌法具有优异的防腐蚀性能及经济性，因此广泛用于制造具有高耐腐蚀特性的钢材，而且在汽车、家电产品及建筑材料等整体产业中对镀覆有锌的镀锌钢材的需求日益剧增。
这种镀锌钢材暴露在腐蚀环境时，具有氧化还原电位低于铁的锌先被腐蚀而抑制钢材的腐蚀的牺牲腐蚀保护(Sacrificial Corrosion Protection)特性，并且镀层的锌被氧化的同时在钢材表面上形成致密的腐蚀产物，使钢材与氧化气氛隔离，从而提高钢材的耐腐蚀性。
但是，随着产业的高度化，大气污染增加，腐蚀环境恶化，另外正在实施对于资源及节能的严格的管制，因此对于具有比现有的镀锌钢材更优异的耐腐蚀性的钢材的开发需求越来越高。作为其中的一部分，对于在镀层中添加镁(Mg)等元素来提高钢材的耐腐蚀性的镀锌合金钢材的制造技术正在进行各种研究。
另外，通常镀锌钢材或镀锌合金钢材(以下，称为“镀锌系钢材”)通过加工等被加工成部件，然后通过点焊等进行焊接并用作产品，将微细组织包含奥氏体或残余奥氏体的高强度钢材、高P添加高强度无间隙原子(Interstitial Free，IF)钢材等作为基材的镀锌系钢材的情况下，在点焊时熔融状态的锌沿着基材铁的晶界渗透，发生诱发脆性裂纹的又名为液态金属脆化(Liquid Metal Embrittlement，LME)的问题。
图1为将由于点焊产生LME裂纹的焊接部件的焊接部进行放大并观察的照片。图1中，在熔核(Nugget)的上部和下部产生的裂纹称为A型(Type A)裂纹，焊接肩部产生的裂纹称为B型(Type B)裂纹，焊接时由于电极的未对准(misalignment)而在钢板的内部产生的裂纹称为C型(Type C)裂纹。其中，B型裂纹及C型裂纹对材料的刚性产生很大的影响，因此焊接时防止裂纹的产生是本技术领域的核心要求事项。
发明内容
要解决的技术问题
本发明的多个目的之一在于，提供一种点焊性及耐腐蚀性优异的单层镀锌合金钢材及其制造方法。
技术方案
本发明的一个方面提供一种单层镀锌合金钢材，所述单层镀锌合金钢材包括基材铁和形成在所述基材铁上的镀锌合金层，所述镀锌合金层包含13～24重量％的Mg，所述镀锌合金层的附着量为40g/m2以下(0g/m2除外)。
本发明的另一个方面提供一种单层镀锌合金钢材的制造方法，所述制造方法包括以下步骤：准备基材铁；以及在真空腔室中通过电磁力使涂覆物质悬浮并对其进行加热以形成Zn和Mg合金沉积蒸气，向所述基材铁的表面诱导喷射所述Zn和Mg合金沉积蒸气以形成Mg沉积层；所述Zn和Mg合金沉积蒸气中的Mg的含量为13～24重量％，所述镀锌合金层的附着量为40g/m2以下(0g/m2除外)。
有益效果
作为本发明的多个效果之一，根据本发明的单层镀锌合金钢材的点焊性优异，因此将微细组织包含奥氏体或残余奥氏体的高强度钢材、高P添加高强度无间隙原子(Interstitial Free，IF)钢材等作为基材时，也能够有效地抑制液态金属脆化(LiquidMetal Embrittlement，LME)的发生。
并且，根据本发明的多层镀锌合金钢材即使以少的附着量也能够确保优异的耐腐蚀性，因此环保且经济性优异。
本发明的多个有益的优点和效果并不限定于上述内容，在对本发明的具体实施方式进行说明的过程中能够更加容易理解。
附图说明
图1为将由于点焊产生LME裂纹的焊接部件的焊接部进行放大并观察的照片。
图2为Mg-Zn二元系合金的相平衡图。
图3为示出镀覆钢材的腐蚀过程的模式图。
图4为电磁悬浮物理气相沉积装置的模式图。
图5为对发明例5的单层镀锌合金钢材进行点焊后观察焊接部的照片。
最佳实施方式
已知在Zn-Mg合金镀覆钢材中，随着Mg含量的增加，虽然在耐腐蚀性方面有利，但是在点焊性方面不利，因此通常将镀层中的Mg的含量控制在最大10重量％左右。这是因为Zn-Mg镀层中熔点低的Zn-Mg系金属间化合物容易溶解，诱发液态金属脆化。但是，根据本发明人的进一步的研究结果，发现即使镀层中Mg的含量超过10重量％的情况下，其平均含量属于一定范围内的同时镀层的宽度方向的Mg含量的偏差属于一定范围内时，点焊性反而显著提高，由此完成了本发明。
以下，对点焊性及耐腐蚀性优异的单层镀锌合金钢材进行详细说明。
本发明的单层镀锌合金钢材包括基材铁和形成在所述基材铁上的镀锌合金层。本发明中对所述基材铁的形状不作特别限定，例如可以为钢板或钢线材。
另外，本发明中对基材铁的合金组成也不作特别限定，作为一个例子，以重量％计，基材铁可以包含：C：0.10～1.0％、Si：0.5～3％、Mn：1.0～25％、Al：0.01～10％、P：0.1％以下(0％除外)、S：0.01％以下(0％除外)、余量的Fe和不可避免的杂质，在这种情况下，所述C、Si、Mn、P及S的含量可以满足以下关系式1。另外，具有如上所述的组成的基材铁的微细组织可以包含奥氏体或残余奥氏体。
[关系式1]
[C]+[Mn]/20+[Si]/30+2[P]+4[S]≥0.3
(其中，[C]、[Mn]、[Si]、[P]及[S]分别表示相应元素的含量(重量％)。)
在具有如上所述的合金组成和微细组织时，点焊时液态金属脆化(LME)成为主要问题，其理由如下：即，与其他组织相比，奥氏体组织或残余奥氏体组织的晶界脆弱，通过点焊施加应力时，液态的熔融锌渗透到焊接部上的奥氏体组织或残余奥氏体组织的晶界产生裂纹，因此引起作为脆性断裂的液态金属脆化。
但是，如下所述，本发明中使液态的熔融锌的滞留时间最小化，因此即使将具有如上所述的合金组成和微细组织的钢材作为基材制造镀锌合金钢材，也能够有效地抑制液态金属脆化的发生。但是，基材铁的合金组成不满足上述的范围时，当然也可以应用本发明。
镀锌合金层包含13～24重量％的Mg，余量由Zn和不可避免的杂质组成。更优选的Mg的含量为15.7～20重量％。
在Zn-Mg系锌合金镀层的情况下，镀覆组织可以由Zn单相、Mg单相、Mg2Zn11合金相、MgZn2合金相、MgZn合金相、Mg7Zn3合金相等组成，本发明人发现将镀锌合金层中含有的Mg的含量控制在如上所述的范围时，点焊时焊接部上的镀锌合金层熔融并转变成包含90面积％以上(包括100面积％)的MgZn2合金相的合金层，在这种情况下，有效地抑制液态金属脆化(LME)。通过图2的Mg-Zn二元系合金的相平衡图可以知道，推测这是因为镀层的熔点高而使得熔融的镀层以液态滞留的时间最小化。另外，本发明中对焊接部上的镀层中的除MgZn2合金相以外的余量的组织不作特别限定，根据不受限制的一个例子，除MgZn2合金相以外的余量可以为Mg2Zn11合金相。
其中，相(phase)分数的测量可以通过利用常规的XRD的无标准Rietveld定量分析(standardless Rietveld quantitative analysis)方法，同时利用更加精确的基于TEM的晶体取向映射技术(TEM-based crystal orientation mapping technique，TEM-ASTAR)进行分析和测量，但并不限定于此。另外，可以利用高温原位(in-situ)放射光XRD对Zn-Mg合金镀层的相变过程进行分析。更具体而言，可以以1.3℃/秒、11.3℃/秒的加热速度、780℃的加热温度对样品进行加热，同时在加热及冷却的热循环期间，对XRD光谱(spectrum)以每秒一帧(frame)连续测量共900帧(frame)，以此对Zn-Mg合金镀层的相变过程进行分析，但并不限定于此。
另外，虽然将Mg的含量控制在如上所述的范围，但是镀层的宽度方向的Mg含量的偏差过大时，难以实现改善点焊性的目的。考虑到这种情况，需要适当控制镀层的宽度方向的Mg含量偏差的上限，优选地，在镀锌合金层的厚度方向的中心部测量GDS分布时，Mg含量的偏差为±5％以内。
根据本发明人的进一步的研究结果，组成镀锌合金层的晶粒的平均粒径对镀覆钢材的耐腐蚀性产生相当大的影响。图3为示出镀覆钢材的腐蚀过程的模式图，图3的(a)为晶粒尺寸微细的情况的模式图，图3的(b)为晶粒尺寸粗大的情况的模式图。参照图3，可以知道晶粒尺寸微细的情况下，发生腐蚀时形成相对致密且均匀的腐蚀产物，因此相对地有助于延迟腐蚀。
另外，组成镀锌合金层的晶粒的平均粒径对镀覆钢材的点焊性也产生相当大的影响。晶粒的平均粒径为一定水平以下时，B型裂纹和C型裂纹的产生显著降低，推测这是因为熔融的镀层中的原子移动活跃而有利于确保期望的组织。
如上所述，考虑镀覆钢材的耐腐蚀性和点焊性两个方面时，需要适当控制组成镀锌合金层的晶粒的平均粒径的上限，组成镀锌合金层的晶粒的平均粒径优选控制在100nm以下(0nm除外)。其中，平均粒径是指对镀层的结晶进行观察时检测的晶粒的平均长径。
根据一个例子，镀锌合金层的附着量可以为40g/m2以下(0g/m2除外)。镀锌合金层的附着量越大，在耐腐蚀性方面越有利，但是由于附着量的增加，在点焊时引起液态金属脆化(LME)，因此考虑焊接性方面，镀锌合金层的附着量的上限可以限定为上述的范围。另外，考虑耐腐蚀性和点焊性两个方面时的多层镀层的附着量之和的优选的范围为10～35g/m2，更优选的范围为15～30g/m2。
以上说明的本发明的单层镀锌合金钢材可以通过各种方法来制造，其制造方法不受特别限制。但是，作为一个具体实施例，可以通过如下所述的方法进行制造。
以下，对本发明的另一个方面的点焊性及耐腐蚀性优异的单层镀锌合金钢材的制造方法进行详细说明。
首先，准备基材铁，利用14重量％以上的HCl水溶液进行酸洗、冲洗及干燥后，利用等离子体及离子束等去除表面的异物及天然氧化膜，然后在基材铁的表面上形成镀锌合金层，以此能够制造本发明的单层镀锌合金钢材。
这时，在镀锌合金层的情况下，优选通过具有电磁搅拌(ElectromagneticStirring)效果的电磁悬浮物理气相沉积法形成。
其中，电磁悬浮物理气相沉积法是利用以下现象的沉积方法：对生成交流电磁场的一对电磁线圈施加高频电源来产生电磁力时，沉积物质(本发明中为Zn、Mg或Zn-Mg合金)在由交流电磁场包围的空间中在没有外部的帮助下悬浮在空中，如此悬浮的沉积物质形成大量的金属蒸气，图4示出用于这种电磁悬浮物理气相沉积的装置的模式图。如图4所示，通过如上所述的方法形成的大量的金属蒸气通过蒸气分配箱(vapor distribution box)的多个喷嘴高速喷射到基材铁的表面以形成镀层。
通常的真空沉积装置中，坩埚内部具备沉积物质，对具备沉积物质的坩埚进行加热而容易实现沉积物质的气化，在这种情况下，由于坩埚的熔融、坩埚引起的热损失等理由，难以向沉积物质本身供应充足的热能。因此，不仅沉积速度慢，而且在组成镀层的晶粒尺寸的微细化方面也存在一定的局限性。并且，如本发明使Zn-Mg合金蒸气沉积时，在确保镀层的均质性方面也存在一定的局限性。
但是，与此不同，通过电磁悬浮物理气相沉积法进行沉积时，与通常的真空沉积法不同，由于没有温度方面的约束条件，能够将沉积物质暴露在更高的温度下，因此不仅可以进行高速沉积，而且能够实现最终形成的镀层的晶粒尺寸的微细化，并且镀层中的合金元素均匀分布。
在沉积工序中，真空沉积腔室内部的真空度优选调节为1.0×10-3mbar至1.0×10-5mbar的条件，在这种情况下，可以有效地防止形成镀层的过程中由于氧化物的形成引起的脆性增加和物理性能的降低。
在沉积工序中，悬浮的涂覆物质的温度优选调节为700℃以上，更优选调节为800℃以上，进一步优选调节为1000℃以上。悬浮的涂覆物质的温度低于700℃时，有可能无法充分确保晶粒的微细化和镀层的均匀化效果。另外，悬浮的涂覆物质的温度越高，越有利于实现期望的技术效果，本发明中对该温度的上限不作特别限定，但是该温度为一定水平以上时，不仅其效果饱和，而且工序成本过高，考虑到这些情况，该温度的上限可以限定为1500℃。
沉积前后的基材铁的温度优选调节为100℃以下，基材铁的温度超过100℃时，由于钢板的宽度方向的温度不均匀度所引起的宽度方向上的弯曲，通过出口侧多级分级减压系统时妨碍保持真空度。
具体实施方式
以下，通过实施例对本发明进行更加详细的说明。但是，这些实施例的记载仅用于例示本发明的实施，本发明并不受限于实施例中记载的内容。这是因为本发明的权利范围由权利要求书中记载的事项及由此合理推导的事项所确定。
(实施例)
准备厚度为1.4mm的汽车用高强度冷轧钢板，以重量％计，所述冷轧钢板包含：C：0.16％、Si：1.43％、Mn：2.56％、Al：0.04％、P：0.006％、S：0.003％、余量的Fe和不可避免的杂质的，并且利用图4的装置(真空度为3.2×10-3mbar)制造具有如下表1所示的组成的镀锌合金层的单层镀锌合金钢材。在所有的例子中，在形成镀锌合金层时，条件恒定为：对一对电磁线圈施加的电流为1.2kA，以2kg的沉积物质为基准，对一对电磁线圈施加的频率为60kHz，悬浮的涂覆物质的温度为1000℃，蒸气分配箱的温度为900℃。并且，在沉积镀锌合金层前后的基材铁的温度保持在60℃。
然后，测量通过电感耦合等离子体(Inductively Coupled Plasma，ICP)法制造的镀锌合金层的附着量和Mg含量。更具体而言，切割成80mm×80mm尺寸的试片，对表面进行脱脂后，利用高精度称进行第一次评量(W1：0.0000g)。之后，利用夹具将O形(O-Ring)54.5mm直径(dia)的专用柱附着于正面部，并使其紧密结合以免漏出溶液。之后，加入30cc的1:3HCl溶液后，加入2～3滴抑制剂(inhibitor)。在表面产生H2气体的过程结束后，将溶液收集在100cc量瓶中。这时，利用洗涤瓶收集表面的所有余量，收集100cc以下。之后，使试片完全干燥后，进行第二次评量(W2)，将第一次评量值和第二次评量值之差除以单位面积的值作为镀锌合金层的附着量。另外，将收集的溶液作为对象，通过ICP法测量Mg的含量。
然后，在镀锌合金层的厚度方向的中心部测量GDS分布，并且测量组成镀锌合金层的晶粒的平均粒径。测量结果，所有例子的Mg含量的偏差为±5％以内，平均粒径为100nm以下。
然后，评价所制造的单层镀锌合金钢材的点焊性和耐腐蚀性，将其结果示于下表1中。
更具体而言，对于点焊性，根据SEP 1220-2标准，切割成40mm×120mm尺寸的试片，对各试片进行共100次点焊后，测量B型裂纹的有无及其尺寸，并以如下标准进行评价。
1.非常优异：所有试片中没有产生B型裂纹的情况
2.优异：一部分或所有试片中产生B型裂纹，并且B型裂纹的平均长度为基材铁(冷轧钢板)厚度的0.1倍以下的情况
3.普通：一部分或所有试片中产生B型裂纹，并且B型裂纹的平均长度超过基材铁(冷轧钢板)厚度的0.1倍且基材铁(冷轧钢板)厚度的0.2倍以下的情况
4.不良：一部分或所有试片中产生B型裂纹，并且B型裂纹的平均长度超过基材铁(冷轧钢板)厚度的0.2倍的情况
对于耐腐蚀性，将各个单层镀锌合金钢材切割成75mm×150mm尺寸的试片后，根据JIS Z2371进行盐雾试验，测量产生初期红锈的时间，并以如下标准进行评价。
1.优异：与单面附着量为60g/m2的镀锌钢板(GI钢板)相比，产生红锈的时间为2倍以上的情况
2.普通：与单面附着量为60g/m2的镀锌钢板(GI钢板)相比，产生红锈的时间为同等水平或小于2倍的情况
3.不良：与单面附着量为60g/m2的镀锌钢板(GI钢板)相比，产生红锈的时间更短的情况
[表1]
No. 镀层的种类(重量％) 附着量(g/m<sup>2</sup>) 点焊性 耐腐蚀性 备注
1 Zn-Mg(10％Mg) 20 4 1 比较例1
2 Zn-Mg(12％Mg) 20 4 1 比较例2
3 Zn-Mg(12.8％Mg) 20 3 1 比较例3
4 Zn-Mg(13％Mg) 20 2 1 发明例1
5 Zn-Mg(15％Mg) 20 2 1 发明例2
6 Zn-Mg(15.5％Mg) 20 2 1 发明例3
7 Zn-Mg(15.8％Mg) 20 1 1 发明例4
8 Zn-Mg(18％Mg) 20 1 1 发明例5
9 Zn-Mg(18％Mg) 25 1 1 发明例6
10 Zn-Mg(18％Mg) 30 1 1 发明例7
11 Zn-Mg(18％Mg) 34 1 1 发明例8
13 Zn-Mg(18％Mg) 40 2 1 发明例9
14 Zn-Mg(19.8％Mg) 20 1 1 发明例10
15 Zn-Mg(20.1％Mg) 20 2 1 发明例11
16 Zn-Mg(21.5％Mg) 20 2 1 发明例12
17 Zn-Mg(22.8％Mg) 20 2 1 发明例13
18 Zn-Mg(23.2％Mg) 20 3 1 比较例4
19 Zn-Mg(25％Mg) 20 4 1 比较例5
参照表1，可以确认满足本发明中提出的所有条件的发明例1至13中，不仅耐腐蚀性优异，而且点焊性也非常优异。尤其，可以确认为了确保更优异的点焊性，优选地，Mg的重量比为0.157至0.20，多层镀层的附着量之和控制在35g/m2以下。
另一方面，比较例1至5中，可以确认Mg的重量比脱离本发明中提出的范围，因此与期望的目标相比，点焊性差。
图5为对发明例5的单层镀锌合金钢材进行点焊后观察焊接部的照片。参照图5，可以在视觉上确认根据本发明的单层镀锌合金钢材的焊接部不仅没有产生B型裂纹，而且完全没有产生C型裂纹。

Claims (14)

1.一种单层镀锌合金钢材，包括基材铁和形成在所述基材铁上的镀锌合金层，所述镀锌合金层包含13～24重量％的Mg，所述镀锌合金层的附着量为40g/m2以下且0g/m2除外。
2.根据权利要求1所述的单层镀锌合金钢材，其中，所述镀锌合金层包含15.7～20重量％的Mg。
3.根据权利要求1所述的单层镀锌合金钢材，其中，所述镀锌合金层的附着量为10～35g/m2。
4.根据权利要求1所述的单层镀锌合金钢材，其中，组成所述镀锌合金层的晶粒的平均粒径为100nm以下且0nm除外。
5.根据权利要求1所述的单层镀锌合金钢材，其中，在所述镀锌合金层的厚度方向的中心部测量GDS分布时，Mg含量的偏差为±5％以内。
6.根据权利要求1所述的单层镀锌合金钢材，其中，对所述单层镀锌合金钢材进行点焊时，焊接部上的镀锌合金层包含90面积％以上且包括100面积％的MgZn2合金相。
7.根据权利要求1所述的多层镀锌合金钢材，其中，根据SEP1220-2标准进行点焊时，B型裂纹的平均长度为基材铁厚度的0.1倍以下。
8.根据权利要求1所述的单层镀锌合金钢材，其中，以重量％计，所述基材铁包含：C：0.10～1.0％、Si：0.5～3％、Mn：1.0～25％、Al：0.01～10％、P：0.1％以下且0％除外、S：0.01％以下且0％除外、余量的Fe和不可避免的杂质。
9.根据权利要求8所述的单层镀锌合金钢材，其中，所述基材铁中包含的C、Si、Mn、P及S的含量满足以下关系式1，
[关系式1]
[C]+[Mn]/20+[Si]/30+2[P]+4[S]≥0.3
其中，[C]、[Mn]、[Si]、[P]及[S]分别表示相应元素的含量(重量％)。
10.根据权利要求8所述的多层镀锌合金钢材，其中，所述基材铁的微细组织包含奥氏体和残余奥氏体中的一种以上。
11.一种单层镀锌合金钢材的制造方法，包括以下步骤：
准备基材铁；以及
在真空腔室中通过电磁力使涂覆物质悬浮并对其进行加热以形成Zn和Mg合金沉积蒸气，向所述基材铁的表面诱导喷射所述Zn和Mg合金沉积蒸气以形成Mg沉积层，
所述Zn和Mg合金沉积蒸气中的Mg的含量为13～24重量％，所述镀锌合金层的附着量为40g/m2以下且0g/m2除外。
12.权利要求11所述的单层镀锌合金钢材的制造方法，其中，所述Zn和Mg合金沉积蒸气中的Mg的含量为15.7～20重量％。
13.权利要求11所述的单层镀锌合金钢材的制造方法，其中，悬浮的所述涂覆物质的温度为700℃以上。
14.权利要求11所述的单层镀锌合金钢材的制造方法，其中，沉积前后的基材铁的温度为100℃以下。
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