CN110114501A - 点焊性及耐腐蚀性优异的多层镀锌合金钢材 - Google Patents

点焊性及耐腐蚀性优异的多层镀锌合金钢材 Download PDF

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Publication number
CN110114501A
CN110114501A CN201780080831.6A CN201780080831A CN110114501A CN 110114501 A CN110114501 A CN 110114501A CN 201780080831 A CN201780080831 A CN 201780080831A CN 110114501 A CN110114501 A CN 110114501A
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coating
phase
multilayer
alloy steel
alloy
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CN201780080831.6A
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CN110114501B (zh
Inventor
郭荣镇
金句和
严文钟
洪锡俊
高景弼
郑勇华
李东烈
金兑烨
曺庆勋
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Posco Holdings Inc
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Posco Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C18/00—Alloys based on zinc
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
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    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C2/36—Elongated material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C—CHEMISTRY; METALLURGY
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    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
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Abstract

本发明公开了一种多层镀锌合金钢材，所述多层镀锌合金钢材包含基材铁和所述基材铁上形成的多层镀层，所述多层镀层的每个镀层为Zn镀层、Mg镀层及Zn‑Mg合金镀层中的任何一个，相对于所述多层镀层的总重量，所述多层镀层中含有的Mg重量之比为0.13至0.24。

Description

点焊性及耐腐蚀性优异的多层镀锌合金钢材
技术领域
本发明涉及一种点焊性及耐腐蚀性优异的多层镀锌合金钢材，更具体地，涉及一种可以应用于汽车、家电产品及建筑材料等的点焊性及耐腐蚀性优异的多层镀锌合金钢材。
背景技术
通过阴极防蚀抑制铁的腐蚀的镀锌法具有优异的防腐蚀性能和经济性，因此广泛使用于制造具有高耐腐蚀特性的钢材，并且汽车、家电产品及建筑材料等的全部产业对镀覆有锌的镀锌钢材的需求正在增加。
这种镀锌钢材暴露在腐蚀环境中时，具有氧化还原电位比铁低的锌先被腐蚀而抑制钢材的腐蚀的牺牲防蚀(Sacrificial Corrosion Protection)的特性，另外，镀层的锌被氧化的同时在钢板表面形成致密的腐蚀生成物，将钢材与氧化气氛隔断，从而提升钢材的耐腐蚀性。
但是，随着产业的高度化大气污染逐渐增加，腐蚀环境恶化，并且由于对资源和节能的严格的管制，越来越需要开发具有比现有的镀锌钢材更优异的耐腐蚀性的钢材。作为其一个部分，进行了在镀层中添加镁(Mg)等的元素而提升钢材的耐腐蚀性的镀锌合金钢材制造技术相关的各种研究。
另外，通常，镀锌钢材或者镀锌合金钢材(以下，称为‘镀锌系钢材’)通过加工等被加工成部件，然后通过点焊等被焊接而用作产品，对于微细组织包含奥氏体或者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)钢材等用作基材的镀锌系钢材而言，存在点焊时熔融状态的锌沿基材铁晶界渗透而诱发脆性裂纹的又名液态金属的脆化(Liquid Metal Embrittlement，LME)的问题。
图1是放大观察由于点焊而产生LME龟裂的焊接构件的焊接部的照片。图1中将在熔核(Nugget)上部和下部产生的裂纹称为A型(Type A)裂纹，将在焊接肩部产生的裂纹称为B型(Type B)裂纹，将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型裂纹和C型裂纹对材料的刚性产生大的影响，因此本技术领域中的核心要求事项为焊接时防止裂纹的产生。
发明内容
要解决的技术问题
本发明的多个目的之一是提供一种点焊性及耐腐蚀性优异的多层镀锌合金钢材。
技术方案
本发明的一个方面提供一种多层镀锌合金钢材，所述多层镀锌合金钢材包含基材铁和所述基材铁上形成的多层镀层，所述多层镀层的每个镀层为Zn镀层、Mg镀层及Zn-Mg合金镀层中的任何一个，相对于所述多层镀层的总重量，所述多层镀层中含有的Mg重量之比为0.13至0.24。
有益效果
作为本发明的多个效果之一，本发明的多层镀锌合金钢材具有优异的点焊性，因此即使将微细组织包含奥氏体或者残余奥氏体的高强度钢材、高P添加高强度IF(Interstitial Free)钢材等用作基材，也可以有效地抑制液态金属脆化(Liquid MetalEmbrittlement，LME)的发生。
另外，本发明的多层镀锌合金钢材即使在少量的附着量的情况下也可以确保优异的耐腐蚀性，因此环保并且具有优异的经济性。
另外，本发明的一个实施例的多层镀锌合金钢材具有优异的镀覆性。
另外，本发明的一个实施例的多层镀锌合金钢材具有优异的磷酸盐处理性。
本发明的多个有益的优点和效果并不限定于上述的内容，在说明过程中能够更容易理解本发明的具体的实施方式。
附图说明
图1是放大观察由于点焊而产生LME龟裂的焊接构件的焊接部的照片。
图2是Mg-Zn二元系合金的相平衡图。
图3是示出镀覆钢材的腐蚀过程的示意图。
图4是本发明的一个实施方式的多层镀锌合金钢材100的示意图。
图5是本发明的另一个实施方式的多层镀锌合金钢材200的示意图。
图6是本发明的另一个实施方式的多层镀锌合金钢材300的示意图。
图7是电磁悬浮物理气相沉积装置的示意图。
图8是对发明例18的多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
对于镀Zn-Mg合金钢材而言，已知随着Mg的含量的增加，虽然在耐腐蚀性方面有利，但是在点焊性方面不利，因此通常将镀层内的Mg含量控制在最大10重量％左右。这是因为，Zn-Mg镀层内熔点低的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，发现即使镀层内Mg含量超过10重量％的情况下所述含量属于特定含量范围内时，点焊性反而显著提升。尤其，这种点焊性改善的效果不仅可以适用于镀层形成为单层的情况，还可以同样地适用于镀层形成为两层以上的多层的情况，从而可以进一步实现改善镀覆性、改善磷酸盐处理性等的效果，并由此完成了本发明。
以下，对点焊性及耐腐蚀性优异的镀锌合金钢材进行详细的说明。本发明中可以根据载置状态随时改变钢板的上和下，因此需要注意的是，记载为‘上(on)’，例如记载为‘基材铁上’仅表示接触基材铁，而不表示在高度方向上位于上部。
本发明的镀锌合金钢材包含基材铁和形成在所述基材铁上的多层镀层。在本发明中对所述基材铁的形态不作特别限定，例如，所述基材铁可以是钢板或者钢线材。
另外，在本发明中对基材铁的合金组成不作特别限定，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。另一方面，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者残余奥氏体。
[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％))
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)可能会成为主要问题，其理由如下。即，与其它组织相比，奥氏体组织或者残余奥氏体组织的晶界脆弱，由于点焊而施加应力时，液态的熔融锌渗透到焊接部上的奥氏体组织或者残余奥氏体组织的晶界而产生裂纹，因此引发作为脆性断裂的液态金属脆化。
但是，在本发明中，如后面描述，由于将液态的熔融锌残留的时间最小化，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，也将有效地抑制液相金属脆化的发生。然而，基材铁的合金组成不满足所述范围时，当然也可以适用本发明。
本发明的主要技术特征在于，多层镀层的每个镀层是Zn镀层、Mg镀层及Zn-Mg合金镀层中的任何一个，相对于所述多层镀层的总重量，所述多层镀层中含有的Mg重量之比为0.13至0.24。更优选的范围是0.157至0.20。
对于Zn-Mg合金镀层而言，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，多层镀层中含有的Mg含量控制在如上所述的范围时，点焊时焊接部上的多层镀层熔融而转变成包含90面积％以上(包括100面积％)的MgZn2合金相的单层合金层，在这种情况下，有效地抑制液态金属脆化(LME)。通过作为Mg-Zn二元系合金的相平衡图的图2可知，推测这是因为镀层的熔点高而使熔融的镀层以液态残留的时间最小化。另外，除了焊接部上的单层合金层中的MgZn2合金相之外，在本发明中对其余组织不作特别限定，但是根据一个非限制性的例子，除了MgZn2合金相之外，其余可以是Mg2Zn11合金相。
其中，对于相(phase)分数的测量，可以与利用通常的XRD的无标准里特菲尔德定量分析(standardless Rietveld quantitative analysis)方法一同利用更精确的基于TEM的晶体取向映射技术(TEM-bas ed crystal orientation mapping technique，TEM-ASTAR)进行分析和测量，但并不一定限定于此。另外，可以利用高温原位同步(in-situ)辐射光XRD分析Zn-Mg合金镀层的相转变过程。更具体而言，可以以1.3℃/sec、11.3℃/sec的加热速度、780℃的加热温度加热样品的同时在加热及冷却热循环期间以每秒一帧(frame)连续测量共900帧(frame)的XRD光谱(spectrum)，分析Zn-Mg合金镀层的相转变过程，但并不一定限定于此。
根据本发明人的进一步的研究结果，即使Mg的含量控制在如上所述范围，当在镀层的宽度方向(轧制方向的垂直方向)上Mg含量的偏差过大时，也可能难以实现改善点焊性的目的。考虑到这种情况，需要适当地控制镀层的宽度方向上的Mg含量的偏差的上限，在多层镀层的每个镀层的厚度方向上的中心部测量GDS分布时，优选地，将Mg含量的偏差控制在±5％以内。
根据本发明人的进一步的研究结果，组成多层镀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是示出镀覆钢材的腐蚀过程的示意图，图3的(a)是晶粒尺寸相对微细的情况的示意图，图3的(b)是晶粒尺寸相对粗大的情况的示意图。参照图3可知，晶粒尺寸微细时，进行腐蚀时形成相对致密且均匀的腐蚀生成物，从而相对地有助于延迟腐蚀。
另外，组成多层镀层的晶粒的平均粒径也对镀覆钢材的点焊性产生相当大的影响。晶粒的平均粒径为预定水平以下时，B型(Type B)裂纹的产生显著减少，推测为这是由于熔融的镀层内原子的移动活跃而有利于确保所需的组织。
如上所述，考虑镀覆钢材的耐腐蚀性和点焊性两个方面时，需要适当地控制组成多层镀层的晶粒的平均粒径的上限，组成多层镀层的晶粒的平均粒径优选控制在100nm以下(0nm除外)。其中，平均粒径表示观察镀层的厚度方向的剖面而检测的晶粒的平均长径。
根据一个例子，多层镀层的附着量的总和可以是40g/m2以下(0g/m2除外)。多层镀层的附着量的总和越大，在耐腐蚀性方面越有利，但是附着量增加可能会导致点焊时液态金属脆化(LME)，考虑焊接性方面，可以将其上限限定在所述的范围。另外，考虑耐腐蚀性和点焊性两个方面的多层镀层的附着量的总和的更优选的范围为10～35g/m2，再进一步优选的范围为15～30g/m2。
另外，如上所述，本发明的镀锌合金钢材的特征在于具有两层以上的多层镀层，由此除了上述的改善耐腐蚀性和焊接性的效果之外，可以进一步实现改善镀覆性、改善磷酸盐处理性等的效果，以下通过列举具体实施方式对此进行详细的说明。
图4是本发明的一个实施方式的多层镀锌合金钢材100的示意图。
根据本发明的一个实施方式，所述多层镀层包含所述基材铁上形成的第一镀层110和所述第一镀层110上形成的第二镀层120，所述第一镀层110可以由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量可以是7重量％以下，所述第二镀层120可以由Zn-Mg合金相组成。此时，各镀层中可以进一步包含除了Zn单相和Zn-Mg合金相之外的的附加的合金相。
诸如Mg2Zn11合金相、MgZn2合金相、MgZn合金相、Mg7Zn3合金相的Zn-Mg合金相是金属间化合物，不仅硬度高而且脆性高，从而阻碍镀覆性，并且加工镀锌合金钢材时诱发镀层脱落。因此，本发明人发现，向与基材铁邻接形成的第一镀层110赋予延展性，以补偿由于形成Zn-Mg合金相而导致的镀层的脆性增加，作为为此目的的一种手段，第一镀层110由Zn镀层或者Mg含量为7重量％以下(优选为6.3重量％以下，更优选为5.5重量％以下)的Zn-Mg合金镀层组成时，可以显著改善镀覆粘附性。
根据一个例子，第一镀层110可以由Zn单相和Mg2Zn11合金相的复合相组成，在这种情况下，第一镀层110可以包含20面积％以上的Zn单相。第一镀层110具有如上所述的组织时，显示出非常优异的压缩强度，因此第一镀层110可以吸收和缓冲由加工引起的应力而显示出非常优异的镀覆性。
根据一个例子，所述第一镀层110的镀覆附着量可以是3g/m2以上。在本实施方式中，将第一镀层110的附着量控制在如上所述的范围，从而可以充分确保所需的改善镀覆性的效果。本发明的一个具体实施例中3g/m2的镀覆附着量可以对应于0.6μm的厚度。
图5是本发明的另一个实施方式的多层镀锌合金钢材200的示意图。
本发明的一个具体实施例中，所述多层镀层包含基材上形成的第一镀层210和所述第一镀层210上形成的第二镀层220，所述第一镀层210可以由Zn-Mg合金相组成，所述第二镀层220可以由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量可以是2重量％以下。此时，各镀层中可以进一步包含除了Zn单相和Zn-Mg合金相之外的附加的合金相。
在镀锌合金钢材200的最表面存在预定水平以上的Zn-Mg合金相时，可能会使磷酸盐处理性变差。这是因为，磷酸盐处理溶液中含有的Ni离子与Zn-Mg合金相之间的腐蚀电位差异导致电化学腐蚀(Galvanic corrosion)而促进镀层的溶解，结果产生暴露基材铁的凹坑(pit)。考虑到这种情况，优选地，位于镀锌合金钢材的最表面的第二镀层220仅由Zn单相组成，或将Zn-Mg合金相的分数控制在预定水平以下，由此，可以有效地改善镀锌合金钢材200的磷酸盐处理性。
根据一个例子，第二镀层220的镀覆附着量可以是2g/m2以上。在本实施方式中，将第二镀层220的附着量控制在如上所述的范围时，可以充分确保所需的改善磷酸盐处理性的效果。
图6是本发明的另一个实施方式的多层镀锌合金钢材300的示意图。
根据本发明的一种实施方式，所述多层镀层包含所述基材铁上依次形成的第一镀层至第三镀层310、320、330，所述第一镀层310可以由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量可以是7重量％以下，所述第二镀层320可以由Zn-Mg合金相组成，所述第三镀层330可以由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量可以是2重量％以下。此时，各镀层中可以进一步包含除了Zn单相和Zn-Mg合金相之外的附加的合金相。
镀锌合金钢材依次包含如上所述第一镀层至第三镀层310、320、330时，具有可以综合地改善耐腐蚀性、点焊性、镀覆性及磷酸盐处理性的优点。
第一镀层310可以由Zn单相和Mg2Zn11合金相的复合相组成，在这种情况下，第一镀层310可以包含20面积％以上的Zn单相。第一镀层310具有如上所述的组织时，显示出非常优异的压缩强度，由此第一镀层310可以吸收和缓冲由加工引起的应力，因此显示出非常优异的镀覆性。
此时，第一镀层的附着量可以是3g/m2以上，第三镀层的附着量可以是2g/m2以上。
除了镀层由3层组成之外，还可以应用与上述的本发明的一个实施方式和另一个实施方式的镀锌合金钢材相关的组成重复的组成。
可以通过各种方法制造以上说明的本发明的镀锌合金钢材，对其制造方法不作特别限制。然而，作为其一个具体实施例，可以通过如下所述的方法制造。
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和离子束等去除表面的异物和天然氧化膜，然后依次形成多层镀层，从而可以制造本发明的镀锌合金钢材。
此时，多层镀层的每个镀层可以通过电镀法或通常的真空沉积法，例如，电子束法、溅射法、热蒸发法、感应加热蒸发法、离子电镀法等形成，但是对于其中的Mg镀层或Zn-Mg合金镀层，优选通过具有电磁搅拌(Electromagnetic Stirring)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(Electro-Magnetic Levitation PhysicalVapor Deposition)利用这样一种现象：将高频电源施加到生成交流电磁场的一对电磁线圈而产生电磁力时，涂敷物质(本发明中Zn、Mg或者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，如此悬浮的涂敷物质产生大量的沉积蒸气(金属蒸气)，图7示出用于这种电磁悬浮物理气相沉积的装置的示意图。参照图7，通过如上所述方法形成的大量的沉积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。
在通常的真空沉积装置中，坩埚内部具备涂敷物质，加热具备这种涂敷物质的坩埚而实现涂敷物质的气化，在这种情况下，由于坩埚的熔融、由坩埚引起的热损失等而难以向涂敷物质本身供应充足的热能。因此，不仅沉积速度慢，而且使组成镀层的晶粒尺寸微细化也存在一定局限性。另外，如本发明想要沉积Zn-Mg合金蒸气时，在确保镀层的均质性方面也存在一定局限性。
但是，与此不同，通过电磁悬浮物理气相沉积法执行沉积时，与通常的真空沉积法不同，由于没有温度的约束条件，因此可以将涂敷物质暴露在更高的温度下，因此，不仅可以进行高速沉积，而且可以实现组成最终形成的镀层的晶粒尺寸的微细化和镀层内合金元素分布的均质化。
沉积工艺时真空沉积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，可以有效地防止在镀层形成过程中形成氧化物而导致的脆性增加和物理性能降低。
沉积工艺时，悬浮的涂敷物质的温度优选调节为700℃以上，更优选调节为800℃以上，再进一步优选调节为1000℃以上。当悬浮的涂敷物质的温度低于700℃时，可能难以充分确保晶粒微细化和镀层均质化效果。另外，悬浮的涂敷物质的温度越高，越有利于实现所需的技术效果，在本发明中对其上限不作特别限定，其温度在预定水平时，不仅其效果将饱和，而且工艺成本过高，考虑到这种情况，可以将其上限限定在1500℃。
沉积前后基材铁的温度优选调节为100℃以下，当超过100℃时，由于钢板宽度方向的温度不均匀性，宽度方向上发生弯曲，从而通过出口侧多级分级减压系统时可能妨碍真空度的保持。
具体实施方式
以下，通过实施例对本发明进行更详细的说明。但是，这些实施例的记载仅用于例示本发明的实施，而并非用于限定本发明。这是因为本发明的权利要求范围由权利要求书中记载的事项和由此合理推导的事项确定。
(实施例)
准备厚度为1.4mm的车辆用高强度冷轧钢板，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：0.0029％、余量的Fe和不可避免的杂质，并且利用图7的装置(真空度为3.2×10-3mbar)制造具有以下表1中所示的组成的多层镀层的多层镀锌合金钢材。对于所有例子，在单独的真空室中通过单独的工艺获得各层的镀层，形成各层的镀层时，施加到一对电磁线圈的电流为1.2kA，以2kg的沉积物质为基准，施加到一对电磁线圈的频率为60kHz，悬浮的涂敷物质的温度为1000℃，蒸气分配箱的温度恒定在900℃。另外，各层的镀层沉积前后的基材铁的温度恒定在60℃。
接着，测量通过电感耦合等离子体(Inductively Coupled Plasma，ICP)法制造的多层镀锌合金钢材的附着量和Mg重量比。更具体而言，切割成80mm×80mm的尺寸的试片，并对其表面进行脱脂，然后利用高精度称进行一次评量(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，投入30cc的1：3HCl溶液，然后投入2～3滴抑制剂(inhibiter)。在表面产生H2气体的过程结束后，将溶液收集在100cc量瓶的烧瓶。此时，利用洗涤瓶以100cc以下收集全部的表面的余量。之后，将试片完全干燥，然后进行二次评量(W2)，将一次评量值与二次评量值之差除以单位面积的值作为总附着量。另外，将收集的溶液为对象通过ICP法测量Mg含量，并将其作为Mg重量比。
接着，在多层镀层的每个镀层的厚度方向上的中心部测量GDS分布，测量组成多层镀层的晶粒的平均粒径。测量结果，所有例子的Mg含量的偏差在±5％以内，平均粒径为100μm以下。
接着，评价制造的多层镀锌合金钢材的焊接性、耐腐蚀性、抗粉化性及磷酸盐处理性，其结果示于以下表2中。
更具体而言，对于焊接性，根据SEP1220-2标准切割成40mm×120mm的尺寸的试片，对各试片实施共100次的点焊，然后测量B型(Type B)裂纹的有无及其尺寸，然后以下述的标准进行评价。
1.非常优异：所有试片中没有产生B型(Type B)裂纹的情况
2.优异：一部分或者所有试片中产生B型(Type B)裂纹，B型(Type B)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：一部分或者所有试片中产生B型(Type B)裂纹，B型(Type B)裂纹的平均长度为基材铁(冷轧钢板)厚度的0.1倍以上且0.2倍以下的情况
4.不良：一部分或者所有试片中产生B型(Type B)裂纹，B型(Type B)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，将各个多层镀锌合金钢材切割成75mm×150mm尺寸的试片，然后根据JISZ2371实施盐雾试验而测量初期红锈产生时间，并以下述的标准进行评价。
1.优异：与单面附着量为60g/m2的镀锌钢板(GI钢板)相比，红锈产生的时间为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，红锈产生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，红锈产生的时间短的情况
对于抗粉化性，将多层镀锌合金钢材切割成40mm×800mm的尺寸的试片，然后将试片安装在冲压试验机，实施60°弯曲试验，然后将试片从试验机取下，弯曲的部分贴上玻璃纸胶带并取下胶带，然后将取下的胶带贴在白纸上，从而测量剥离宽度，并以下述的标准进行评价。
1.优异：剥离宽度为6.0mm以下的情况
2.普通：剥离宽度为6.0mm以上8.0mm以下的情况
3.不良：剥离宽度超过8.0mm的情况
对于磷酸盐处理性，将多层镀锌合金钢材切割成75mm×150mm的尺寸的试片，然后根据通常的汽车公司标准进行表面调整和磷酸盐处理，然后评价磷酸盐均匀度。
1.良好：磷酸盐薄膜均匀形成
2.不良：磷酸盐薄膜不均匀形成
[表1]
[表2]
No. 焊接性 耐腐蚀性 抗粉化性 磷酸盐处理性 备注
1 4 1 1 2 比较例1
2 3 1 1 2 比较例2
3 2 1 1 2 发明例1
4 2 1 1 2 发明例2
5 2 1 1 2 发明例3
6 1 1 1 2 发明例4
7 1 1 1 2 发明例5
8 1 1 1 2 发明例6
9 1 1 1 2 发明例7
10 2 1 1 2 发明例8
11 2 1 1 2 发明例9
12 2 1 1 2 发明例10
13 3 1 1 2 比较例3
14 3 1 1 2 比较例4
15 1 1 1 2 发明例11
16 1 1 2 2 发明例12
17 3 1 3 1 比较例5
18 2 1 3 1 发明例13
19 1 1 3 1 发明例14
20 2 1 3 1 发明例15
21 3 1 3 1 比较例6
22 3 1 1 1 比较例7
23 1 1 1 1 发明例16
24 2 1 1 1 发明例17
25 1 1 1 1 发明例18
26 2 1 1 1 发明例19
27 2 1 1 1 发明例20
28 3 1 1 1 比较例8
参照表2，满足本发明中提出的所有条件的发明例1至20的情况下，可以确认，不仅显示出非常优异的耐腐蚀性，而且显示出非常优异的点焊性。另外，可以确认，为了确保更优异的点焊性，优选地，Mg重量比为0.157至0.20，多层镀层的附着量的总和控制在35g/m2以下。
与此相比，比较例1至8的情况下，可以确认，Mg重量比脱离本发明中提出的范围，点焊性差。
另外，参照表2，可以确认，为了改善镀覆性，最下部镀层优选为Zn镀层或者Mg含量为7重量％以下(0重量％除外)的Zn-Mg合金镀层，并且为了改善磷酸盐处理性，最上部镀层优选为Zn镀层或者Mg含量为2重量％以下(0重量％除外)的Zn-Mg合金镀层。
图8是对发明例18的多层镀锌合金钢材进行点焊后观察焊接部的照片。参照图8，本发明的多层镀锌合金钢材在焊接后转变成单层合金层，所述焊接部上的单层合金层中MgZn2合金相的比例为90面积％以上，并且可以通过视觉确认焊接部不仅没有产生B型(Type B)裂纹，而且完全没有产生C型(Type C)裂纹。
附图标记说明
100、200、300：多层镀锌合金钢材
110、210、310：第一镀层
120、220、320：第二镀层
330：第三镀层

Claims (25)

1.一种多层镀锌合金钢材，所述多层镀锌合金钢材包含基材铁和所述基材铁上形成的多层镀层，
相对于所述多层镀层的总重量，所述多层镀层中含有的Mg重量之比为0.13至0.24，
组成所述多层镀层的各镀层包含Zn单相、Mg单相及Zn-Mg合金相中的一个以上的相，并且与邻接的另一个镀层所包含的相的组成不同。
2.根据权利要求1所述的多层镀锌合金钢材，其中，
相对于所述多层镀层的总重量，所述多层镀层中含有的Mg重量之比为0.157至0.20。
3.根据权利要求1所述的多层镀锌合金钢材，其中，
在所述多层镀层的每个镀层的厚度方向上的中心部测量GDS分布时，Mg含量的偏差在±5％以内。
4.根据权利要求1所述的多层镀锌合金钢材，其中，
组成所述多层镀层的晶粒的平均粒径为100nm以下(0nm除外)。
5.根据权利要求1所述的多层镀锌合金钢材，其中，
所述多层镀层的附着量的总和为40g/m2以下(0g/m2除外)。
6.根据权利要求1所述的多层镀锌合金钢材，其中，
所述多层镀层的附着量的总和为10～35g/m2。
7.根据权利要求1所述的多层镀锌合金钢材，其中，
对所述镀锌合金钢材进行点焊时，焊接部上的多层镀层转变成单层合金层，
所述焊接部上的单层合金层包含90面积％以上(包括100面积％)的MgZn2合金相。
8.根据权利要求1所述的多层镀锌合金钢材，其中，
根据SEP1220-2标准实施点焊时，B型裂纹的平均长度为基材铁厚度的0.1倍以下。
9.根据权利要求1所述的多层镀锌合金钢材，其中，
在真空室内通过电磁力使涂敷物质悬浮及加热而生成沉积蒸气，将所述沉积蒸气诱导喷出到基材铁的表面以形成所述多层的各个镀层。
10.根据权利要求9所述的多层镀锌合金钢材，其中，
悬浮的所述涂敷物质的温度为700℃以上。
11.根据权利要求1所述的多层镀锌合金钢材，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(0％除外)、S：0.01％以下(0％除外)、余量的Fe和不可避免的杂质。
12.根据权利要求11所述的多层镀锌合金钢材，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％)。
13.根据权利要求11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。
14.根据权利要求1所述的多层镀锌合金钢材，其中，
所述多层镀层包含所述基材铁上形成的第一镀层和所述第一镀层上形成的第二镀层，所述第一镀层由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量是7重量％以下，所述第二镀层由Zn-Mg合金相组成。
15.根据权利要求14所述的多层镀锌合金钢材，其中，
所述第一镀层或者所述第二镀层中进一步包含除了Zn单相、Mg单相及Zn-Mg合金相之外的附加的合金相。
16.根据权利要求15所述的多层镀锌合金钢材，其中，
所述第一镀层和所述第二镀层的附着量的总和为40g/m2以下(0g/m2除外)，所述第一镀层的附着量为3g/m2以上。
17.根据权利要求15所述的多层镀锌合金钢材，其中，
所述第一镀层为Zn-Mg合金镀层，并且由Zn单相和Mg2Zn11合金相的复合相组成。
18.根据权利要求17所述的多层镀锌合金钢材，其中，
所述第一镀层包含20面积％以上的Zn单相。
19.根据权利要求1所述的多层镀锌合金钢材，其中，
所述多层镀层包含基材上形成的第一镀层和所述第一镀层上形成的第二镀层，所述第一镀层由Zn-Mg合金相组成，所述第二镀层由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量为2重量％以下。
20.根据权利要求19所述的多层镀锌合金钢材，其中，
所述第一镀层或者所述第二镀层中进一步包含除了Zn单相、Mg单相及Zn-Mg合金相之外的附加的合金相。
21.根据权利要求18所述的多层镀锌合金钢材，其中，
所述第一镀层和所述第二镀层的附着量的总和为40g/m2以下(0g/m2除外)，所述第二镀层的附着量为2g/m2以上。
22.根据权利要求1所述的多层镀锌合金钢材，其中，
所述多层镀层包含所述基材铁上依次形成的第一镀层至第三镀层，所述第一镀层由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量为7重量％以下，所述第二镀层由Zn-Mg合金相组成，所述第三镀层由Zn单相或者Zn单相与Zn-Mg合金相组成，镀层中的Mg含量为2重量％以下。
23.根据权利要求21所述的多层镀锌合金钢材，其中，
所述第一镀层至所述第三镀层中的一个以上的镀层中进一步包含除了Zn单相、Mg单相及Zn-Mg合金相之外的附加的的合金相。
24.根据权利要求22所述的多层镀锌合金钢材，其中，
所述第一镀层至所述第三镀层的附着量的总和为40g/m2以下(0g/m2除外)，所述第一镀层的附着量为3g/m2以上，所述第三镀层的附着量为2g/m2以上。
25.根据权利要求22所述的多层镀锌合金钢材，其中，
所述第一镀层为Zn-Mg合金镀层，由Zn单相和Mg2Zn11合金相的复合相组成，并且包含20面积％以上的Zn单相。
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