CN104884666A - 铝镁镀层钢板及其制造方法 - Google Patents

铝镁镀层钢板及其制造方法 Download PDF

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Publication number
CN104884666A
CN104884666A CN201380068534.1A CN201380068534A CN104884666A CN 104884666 A CN104884666 A CN 104884666A CN 201380068534 A CN201380068534 A CN 201380068534A CN 104884666 A CN104884666 A CN 104884666A
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China
Prior art keywords
alloy layer
magnesium alloy
aluminum magnesium
steel plate
coating
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CN201380068534.1A
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CN104884666B (zh
CN104884666B9 (zh
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梁智勋
郑在仁
金兑烨
郑勇华
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Research Institute of Industrial Science and Technology RIST
Posco Holdings Inc
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Posco Co Ltd
Research Institute of Industrial Science and Technology RIST
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on 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
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • 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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    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of 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
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    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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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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    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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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
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    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • 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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    • 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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Abstract

本发明涉及一种利用真空镀膜来镀上铝镁的钢板，铝镁镀层包含1重量％至45重量％的镁，余量为铝和其他不可避免的杂质，通过对钢板进行热处理在铝镁镀层形成Al3Mg2合金相。

Description

铝镁镀层钢板及其制造方法
技术领域
本发明涉及一种铝镁镀层钢板及其制造方法，更具体地涉及一种具有为防止钢板腐蚀而通过真空镀膜形成的铝镁镀层的钢板及其制造方法。
背景技术
钢铁具有优秀的物理特性，是一种用于汽车、家电、建筑等各种工业领域的材料。然而，钢铁与氧气等反应容易产生腐蚀，为了防止这种腐蚀必须进行表面处理，例如镀保护膜等。
钢铁被加工成板、棒、管等各种形状，其中薄板形状的钢板是工业领域中使用最多的钢铁产品之一。为了防止这种钢板的腐蚀，最常用的方法是在钢板表面镀上金属保护膜，其与氧气的反应性高于铁，使得该保护膜起到牺牲阳极(sacrificial anode)的作用，藉以延缓钢板的腐蚀。
对这种钢板镀膜时所使用的金属中典型的是锌和铝，用于将这种金属镀在钢板上的方法例如有热镀、电镀等。镀金属的方法工艺简单费用也低，因此目前钢板表面处理工艺大都采用该方法。
利用镀锌法来镀钢板时，为了增加钢板的耐腐蚀性，可以考虑增加镀锌量。然而，为了增加镀锌量采用降低镀锌速度的方法，但这种方法会导致生产性下降。
另外，随着镀锌量的增加镀锌钢板的重量必然会增加，对于输送机械等而言，由于重量增加燃料效率随之降低。此外，近来锌的蕴藏量急剧减少，急需发掘出一种可替代锌的材料。
作为这种尝试的一个环节，正在开发一种不增加镀锌量而添加异种元素就能提高现有镀锌钢板的耐腐蚀性的方法。这种异种元素有铝、镁等。
发明内容
技术问题
本发明的目的在于提供一种铝镁镀层钢板及其制造方法，用铝和镁来替代用于防止钢板腐蚀的金属锌，而且镀层厚度薄于现有镀锌钢板的锌镀层，还能够显示出相同或者更高的性能。铝和镁可用作牺牲阳极，因此通过适当调节铝镁的组分，可实现具有优秀的耐腐蚀性的保护膜。
技术方案
为了达到所述目的，本发明一实施例提供一种形成有铝镁合金层的钢板，包括：ⅰ)钢板；ⅱ)形成于所述钢板上的铝铁合金层；ⅲ)形成于所述铝铁合金层上的铝镁合金层,其中所述铝镁合金层在整个合金层中镁含量为1重量％至45重量％。此时，所述铝镁合金层在整个合金层中镁含量优选为9重量％至45重量％。
优选地，所述铝铁合金层从所述钢板沿所述合金层方向形成且厚度为整个合金层厚度的1％至50％。
而且，所述铝铁合金层因钢板的铁成分扩散到镀层而形成AlxFey层，所述AlxFey层优选满足以下条件：AlxFey层中，x为1～3，y为0.5～1.5。
所述铝铁合金层的厚度优选为0.2μm～1μm。
另外，所述铝镁合金层优选由α相和β相(Al3Mg2)混杂的结晶相组成，所述铝镁合金层优选形成为晶粒形状。
所述铝镁合金层的厚度优选为0.5μm至30μm。
而且，所述铝镁合金层的晶粒是α相和β相(Al3Mg2)分别形成的晶粒，晶粒的平均粒径优选为0.1μm至2μm。
所述铝镁合金层中晶粒β相/α相的面积比优选为10％～70％。
优选地，所述铝镁合金层的α相和β相其XRD强度比即Iβ(880)/Iα(111)为0.01～1.5。
为了达到本发明的另一目的，本发明实施例提供一种钢板上形成铝镁合金层的方法，包括：ⅰ)准备钢板；ⅱ)在所述钢板上真空镀上铝镀层；ⅲ)在所述铝镀层上至少一次真空镀上镁镀层；ⅳ)在所述镁镀层上至少一次真空镀上第二铝镀层。
所述钢板上形成铝镁合金层的方法，还包括：在所述第二铝镀层上至少一次真空镀上第二镁镀层。
此外，优选在所述钢板上先真空镀上镁镀层用以替代铝镀层，接着依次真空镀上铝镀层和镁镀层且重复至少一次。
优选地，真空镀在所述钢板上的镁镀层以真空镀在所述镁镀层上的铝通过扩散能够与所述钢板上的铁进行反应而在所述镀层形成铁铝合金层的厚度来形成。
所述铝镁合金层在整个合金层中镁含量优选为1重量％至45重量％，镁含量更优选为9重量％至45重量％。
如上所述，由所述铝镀层和所述镁镀层组成的所述铝镁镀层其厚度优选为0.5μm至30μm。
此时，优选通过磁控溅镀来真空镀上所述镀层。
而且，优选通过将配置在铝源和镁源上方的所述钢板反复进行往返运动来真空镀上所述铝镁镀层。
此外，优选通过改变施加于所述铝源和镁源的电流来改变所述铝镁镀层的组分。
为了达到本发明的又一目的，本发明实施例提供一种将形成有所述铝镁镀层的钢板在热处理炉中进行热处理，以使所述铝镁镀层相变为铝镁合金层的方法。
优选地，这样的热处理是在惰性环境中温度范围为350℃～450℃、热处理时间为2分钟～10分钟的条件下进行。
通过这样的热处理将所述镀层形成为铁铝合金层或者铝镁合金层中的至少任何一种。
优选地，通过这样的热处理来形成的所述铝铁合金层因钢板的铁成分扩散到镀层而形成AlxFey层，所述AlxFey层满足以下条件：AlxFey层中，x为1～3，y为0.5～1.5。
此外，这样的所述铝铁合金层的厚度优选为0.2μm～1μm。
而且，通过所述热处理所述铝镁合金层会形成α相或者β相(Al3Mg2)中的至少任何一种。
有益效果
根据本发明的具有铝镁镀层的钢板其厚度薄于现有镀锌钢板的锌镀层，而且能够具有相同或者更高的耐腐蚀性。
改变镀在钢板上的铝镁组分并分别评价了腐蚀特性，确认到显示出较优秀的耐腐蚀性的铝镁组分。
此外，通过对镀有铝镁的钢板进行热处理后评价耐腐蚀性，比较了热处理前/后镀膜钢板的耐腐蚀性。确认到可使钢板具有热处理前/后铝镁镀层钢板的耐腐蚀性变化不大的稳定的镀层的镁含量。
附图说明
图1示出了本发明一实施例中使用的真空镀膜设备。
图2示出了基于热处理温度和热处理时间的镀层变化。
图3示出了针对图2所用试样的XRD(X-射线衍射分析，X-rayDiffraction Analysis)试验结果。
图4是针对图2所用试样示出基于热处理的组织变化的扫描电子显微镜(SEM)照片。
图5针对图2所用试样示出了基于热处理的GDLS(辉光放电光谱，Glow Discharge Light Spectroscopy)分析结果。
图6示出了针对从图2所用试样中抽出的部分试样进行盐水喷雾试验的结果，进行盐水喷雾试验是为了对形成有铝镁镀层的钢板评价其腐蚀特性。
图7示出了对具有铝镁合金层的钢板评价粘附力的结果。
图8a是示出形成于钢板上的铝镁合金层组织的透射电子显微镜(TEM)照片。
图8b是局部放大图8a的透射电子显微镜(TEM)照片。
具体实施方式
参照附图和下述实施例，就可以清楚地理解本发明的优点、特征及实现这些的方法。
然而，本发明能够以各种不同的方式实施，并不局限于下面公开的实施例。提供下述实施例的目的在于，充分公开本发明以使所属领域的技术人员对发明内容有整体和充分的了解，本发明的保护范围应以权利要求书为准。
下面，参照附图进一步详细说明本发明。
图1是示出用于将铝和镁镀在钢板上的真空镀膜设备的示意图。
根据本发明的一实施例，为了将铝和镁镀在钢板上，例如可以利用真空镀膜方法。这种真空镀膜方法与现有镀金属的方法相比，工艺费用虽高但能快速镀上厚度薄的镀层，因此在生产性方面具有竞争力。
图1中为了形成铝镁镀层采用磁控溅镀。同时启动铝源和镁源，使基板在溅镀源上方进行往返运动或者旋转运动以形成镀层。
作为根据本发明一实施例镀上铝和镁的基板，例如可使用冷轧钢板200。在这里，冷轧钢板优选碳含量为0.3重量％以下的低碳钢，而且优选用作车用钢板或家电用钢板或者建筑材料用钢板。
这种冷轧钢板200涂有防锈油，因此需要进行脱脂工艺以去除防锈油。
对于钢板200的脱脂工艺，例如可利用表面活性剂来进行。对钢板200进行脱脂后，例如用酒精和丙酮进行超声波清洗后，再装到真空镀膜设备上。
接着，对真空容器100进行排气，直至真空容器100内的压力达到约10-5torr以下。进行这种真空排气之后，将氩气注入真空容器100内，在真空度达到1*10-2torr时，向基板200施加约800V的直流电压使得产生辉光放电，从而可以清洗试样的表面。
完成试样清洗后，对真空设备进行排气直至达到基本压力即约10-5torr，再利用磁控溅镀源300、400将铝和镁镀在钢板上。
通过溅镀在钢板上镀铝和镀镁时，依次镀铝和镀镁。此时，优选钢板上先镀铝，但钢板上也可以先镀镁再镀铝。只要通过后续热处理等将镁镀层的厚度控制得薄一点，使得镀在镁上方的铝能够通过扩散与钢板上的铁进行反应而在钢板上形成铁铝合金层，就可以在钢板上先镀镁再镀铝层。
而且，通过溅镀在钢板上镀铝和镀镁时，若依次镀铝和镀镁，则可以采用在初始铝层上方镀上镁层后再镀上镁层，其上镀上铝层后再镀上铝层的方式。也就是说，铝层上方还可以依次镀上两个镁层和两个铝层。
如上所述，在物质层上反复并依次镀上相同物质层时(例如，依照Al-Mg-Mg-Al-Al-Mg的次序镀膜时)，优选将配置在两种物质溅镀源300、400上方的基板即钢板200反复地进行往返运动。
而且，镀在钢板200上的铝镁保护膜的厚度优选为0.5μm至30μm。另外，通过改变施加于铝和镁溅镀源300、400的电流，使铝和镁的蒸发率产生差异，进而可以改变铝镁组分。
通过如上所述的溅镀方法在钢板200上形成铝镁镀层，并且形成在钢板上的铝镁镀层会形成多层结构。
此时，铝镁镀层中镁含量优选为1重量％～45重量％，更优选为9重量％～40重量％。
优选将如此形成有铝镁镀层的钢板在真空热处理炉中进行热处理。
真空热处理炉可以使用预热炉、热处理炉及均热炉连续连接而成的热处理炉。此时，预热炉、热处理炉及均热炉优选在各连接部分形成用于隔离各炉空间的隔离幕以及隔离幕上形成用于移动钢板的门。
对于这种热处理炉，排气形成真空状态后，可供应惰性气体(例如氮气)作为环境气体。
对于形成有铝镁镀层的钢板的热处理，先将所述钢板装入预热炉，再将所述钢板加热至热处理温度，在温度稳定的状态下移动至热处理炉进行热处理。
对于形成有镀层的钢板的热处理，优选在350℃～450℃下进行2分钟～10分钟。如果热处理是在350℃以下的温度下进行且时间为2分钟以内，则铝镁层不能形成铝镁合金，如果热处理是在450℃以上的温度下进行且时间为10分钟以上，则钢板的铁成分会扩散到镀层或者镁扩散到镀层表面，因此不可取。
这种热处理优选在350℃下进行10分钟或者在400℃下进行4分钟。
对形成有镀层的钢板进行热处理，则在钢板与镀层的界面钢板的铁成分会扩散到镀层而形成AlxFey层，并且铝镁镀层相变为铝镁合金层。
AlxFey层中x优选为1至3、y优选为0.5至1.5，并且这种AlxFey层的厚度优选为0.2μm～1μm。
AlxFey层中x值和y值范围是基于扩散的Al-Fe合金相中不会生成因显示脆性(brittle)而机械特性不佳的合金相(例如，FeAl2、Fe2Al5、FeAl3等)的范围，限制在该范围的理由是x为1至3且y为0.5至1.5的范围内的Al-Fe相(例如，Fe3Al、FeAl等)会提高钢板与铝镁合金层之间的粘附力。
另外，将Al-Fe合金相的层厚限制在0.2μm～1μm是因为Al-Fe层的厚度增加则Al相对有限而Fe含量增加，从而生成具有脆性的Al-Fe合金相，由此会导致镀层的机械特性降低。
此时，形成于钢板与镀层界面上的AlxFey层是含有微量镁的铝铁合金层，这种AlxFey层优选从钢板沿镀层方向形成且厚度为铝镁镀层厚度的1％～50％。
将AlxFey层的厚度限制在镀层厚度的1％～50％的理由是若AlxFey层的厚度超出镀层厚度的50％则Fe含量增加会生成机械特性不佳的合金相。
另外，因热处理而发生相变的铝镁合金层处于α相和β相混杂的状态，其中α相表示面心立方晶格(FCC)的铝相，β相表示面心立方晶格的Al3Mg2。在如此形成的铝镁合金层中，α相和β相之比以XRD强度比即Iβ(880)/Iα(111)计优选为0.01～1.5。
将铝镁合金层中α相和β相之比限制在以Iβ/Iα计为0.01～1.5是为了限制生成β相的Mg含量，因为对Al-Mg镀层进行热处理时，按照Mg含量所生成的Al-Mg合金相(β相)的XRD峰值强度会有所不同。
此外，因热处理而发生相变的铝镁合金层形成晶粒(grain)，这些晶粒优选为0.2μm～1μm。
将晶粒大小限制在0.2μm～1μm是因为如果Al-Mg合金层的晶粒大小为0.2μm以下则难以通过控制热处理条件来形成，如果晶粒大小为1μm以上则会引起分离成为Al-Fe层和Mg层，因此不可取。
而且，如此形成的铝镁合金层的晶粒优选β相/α相的面积比为10％～70％。
将铝镁合金的晶粒中β相/α相的面积比限制在10％～70％的理由是如果超出该范围则不会形成Al-Mg合金相(β相)，因此不可取。
<实施例>
首先，作为用于试验的试样准备经热轧及冷轧的厚度为0.8mm的钢板，该钢板包含C：0.12重量％以下(但0％除外)、Mn：0.50重量％以下(但0％除外)、P：0.04重量％(但0％除外)、S：0.040重量％(但0％除外)，余量为Fe和其他不可避免的杂质。
将如此准备的钢板利用烯烃类表面活性剂进行脱脂,以去除防锈油。
将脱脂后的钢板用酒精进行超声波处理，再用丙酮进行超声波处理，以超声波进行清洗后，再装入真空镀膜设备。
之后，进行排气直至真空容器内的压力达到10-5torr以下，再将氩气注入真空容器内，当真空度达到1*10-2torr时，向钢板施加800V的直流电压，使得产生辉光放电以清洗试样的表面。
接着，将清洗完的钢板装入安装有铝源300和镁源400的磁控溅镀装置，并进行排气直至达到溅镀装置的基本压力即10-5torr。
然后，启动磁控溅镀装置在钢板上依次镀上铝和镁。此时，对于铝源和镁源，在固定状态下通过调节电压来控制溅镀量，而且将钢板反复进行左右往返运动，以在钢板上依照铝-镁-镁-铝-铝-镁的次序进行溅镀。
钢板上镀铝和镀镁的溅镀条件如下表1所示。
[表1]
对于镀在钢板上的铝镁镀层组分，铝源(靶材500)和镁源(靶材600)的溅镀率是通过控制输入电源的强度来控制的，而铝镁镀层的组分控制成在整个镀层中以镁含量计3.74重量％、5.69重量％、7.65重量％、12.25重量％、16.71重量％、20.97重量％、21.20重量％、27.72重量％及31.50重量％。而且，溅镀成整个镀层的厚度为5μm。
如此在钢板上镀上铝镁镀层后，将各试样装入热处理炉进行热处理。
为了镀层的热处理而使用的热处理炉是预热室与热处理室连接的真空热处理炉。
首先，预热炉中装入形成有镀层的钢板，再将所述钢板加热至热处理温度，在温度稳定的状态下移动至热处理炉进行热处理。预热炉和热处理炉均用氮气形成惰性环境，而且将形成有镀层的钢板在预热炉中充分预热至热处理温度后移送到热处理炉。
对于热处理炉中进行的镀层钢板的热处理，在350℃～450℃下热处理2分钟～10分钟并根据镀层的组分改变了热处理条件。
即，热处理温度较低时热处理时间控制得较长，而热处理温度较高时热处理时间控制得较短。
图2中示出了基于热处理温度和热处理时间的镀层变化。图2所用试样其镀层的镁组分为39.0重量％。
在图2的各图表中，左上方的红线(中间线)表示铝的浓度变化，左下方的蓝线(最左边的线)表示镁的浓度变化，而右边绿线表示铁的浓度变化。
从图2可知，对于镀层中各成分元素基于扩散的变化，温度越高显示相同效果的时间越短。例如，镀层的热处理在350℃下进行2分钟以上而450℃下进行10分钟以下时，镀层的成分元素相互扩散而形成铝镁合金层。
然而，镀层的热处理在350℃下进行2分钟时成分元素的扩散不充分，因此不会顺利地形成铝镁合金，而在450℃下进行10分钟时会产生镁的逆扩散。
图3中示出了对图2所用试样进行XRD(X-ray DiffractionAnalysis)试验的结果。图3中各图表的横轴是观察到峰值(peak)的角度(2θ)，而纵轴表示强度(intensity)，其单位是标准化的任意单位(arbitrary unit；a.u.)。
从图3可知，对镀层在350℃下热处理2分钟以上时会形成铝镁合金层(Mg或者Al12Mg17)，而在450℃下热处理10分钟时会在钢板界面形成铝铁合金，在这之间的温度和时间条件下铝镁合金层会适当地形成并处于α相(Al)和β相(Al3Mg2)混杂的状态。
在如此形成的铝镁合金层中，α相和β相之比以XRD强度比即Iβ(880)/Iα(111)计在0.01～1.5范围内。
图4中示出了针对图2所用试样观察基于热处理的电子显微镜(SEM)组织变化的结果。
从图4可知，对镀层进行热处理之前，在铝镁镀层中镁含量为10重量％以下的条件下观察到柱状(columnar)结构，而在10重量％以上的条件下观察到组织致密的状态，但是对镀层进行热处理时，可以观察到镀层相变为铝镁合金层并形成晶粒(grain)。这种晶粒呈现出铝镁镀层中镁含量增加时大小减小的趋势，其大小在0.2μm～1μm范围内。
图5中示出了针对图2所用试样的基于热处理的GDLS(辉光放电光谱，Glow Discharge Light Spectroscopy)分析结果。
从图5可知，铝镁镀层在热处理前后，在钢板中沿镀层方向(图5的各图表中从左侧向右侧的方向)即镀层的深度方向镀层组分变化不大。这一事实表明由于热处理会产生镀层的相变但组分变化不大。也就是说，即使由于热处理产生镀层的相变，存在于产生相变之前和之后的Al-Mg镀层中的Al和Mg的总量也不会变。
以上，说明了对形成有铝镁镀层的钢板观察基于热处理的镀层变化的结果，以下说明对如此热处理的镀层进行腐蚀试验和评价镀层粘附力的结果。
首选，说明对热处理镀层的腐蚀试验。
图6示出了针对图2所用试样中抽出的部分试样进行盐水喷雾试验的结果，进行盐水喷雾试验是为了对形成有铝镁镀层的钢板评价其腐蚀特性。
盐水喷雾试验是按照ASTM B117规格在NaCl 5％、35℃的条件下进行的。图6的图表横轴表示镀层的镁含量(单位是重量％)，而纵轴表示产生红锈(red rust)的时间(单位是小时)。
图6中用斜线表示的图表是针对热处理前(non-heat treated)试样的结果，而用交叉线表示的图表是针对400℃下热处理10分钟的试样的结果。而且，用平行线表示的图表是为了对比而示出的具有5.6μm厚度的电镀锌钢板的盐水喷雾结果。
如图6所示，在热处理之前，形成有铝镁镀层的钢板呈现出随着镁含量的增加耐腐蚀性稍微提高的趋势。然而，将形成有铝镁镀层的钢板在400℃下热处理10分钟时，呈现出在大部分的范围内耐腐蚀性显著提高的结果。
如图6所示，形成有铝镁镀层的钢板中镁含量为21.2重量％时耐腐蚀性显著提高，但自27重量％以上起耐腐蚀性稍微降低，即使这样也比热处理前的试样耐腐蚀性得到提高。
如上所述，对形成有铝镁镀层的钢板进行热处理时，镀层的镁含量为7.6重量％至31.5重量％的情况下呈现出优秀的耐腐蚀性。耐腐蚀性提高是因为具有如下特性，即随着镁含量的增加镀层结构变得致密，并且由于热处理而生成的铝镁合金相中形成β相(Al3Mg2)。从该盐水喷雾试验结果可以确认到相对于电镀锌钢板性能提高了约10倍以上。
然而，当镀层的镁含量增加到45重量％以上时，铝镁镀层变得不稳定且耐腐蚀性降低。
图7示出了针对铝镁合金层钢板的粘附力评价结果。
这种粘附力试验是按ASTM D522规格进行的。
如图7所示，镀层的镁含量较低时，呈现出优秀的粘附力，但是镀层的镁含量越高粘附力越减小。镀层对钢板的粘附力增加是因为钢板的表面上形成铝铁合金层。
为了观察如此形成在钢板上的铝镁合金层的组织，用透射电子显微镜(TEM)调查了将镀层的镁含量为20.2重量％的试样在400℃下热处理10分钟的情形。
图8示出了这种TEM结果。
从图8a可知，镀层由于热处理在钢板与铝镁合金层之间形成了铝铁合金层，而且铝镁合金层形成晶粒并混杂有α相和β相(Al3Mg2)。
以上，参照附图对本发明的实施例进行了说明，但所属领域的技术人员会理解，在不改变技术思想或必要特征的情况下，本发明能够以其他方式实施。

Claims (27)

1.一种形成有铝镁合金层的钢板，包括：
钢板；
形成于所述钢板上的铝铁合金层；
形成于所述铝铁合金层上的铝镁合金层，
其中，所述铝镁合金层在整个合金层中镁含量为1重量％至45重量％。
2.根据权利要求1所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层在整个合金层中镁含量为9重量％至40重量％。
3.根据权利要求1所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层混杂有α相和β相(Al3Mg2)。
4.根据权利要求3所述的形成有铝镁合金层的钢板，其中，
所述铝铁合金层从所述钢板沿所述合金层方向形成且厚度为整个合金层厚度的1％至50％。
5.根据权利要求4所述的形成有铝镁合金层的钢板，其中，
所述铝铁合金层因钢板的铁成分扩散到镀层而形成AlxFey层，所述AlxFey层满足以下条件：
AlxFey层中，x为1～3，y为0.5～1.5。
6.根据权利要求5所述的形成有铝镁合金层的钢板，其中，
所述铝铁合金层的厚度为0.2μm～1μm。
7.根据权利要求1至6中任何一项所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层形成为晶粒形状。
8.根据权利要求7所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层的厚度为0.5μm至30μm。
9.根据权利要求8所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层的晶粒是α相和β相(Al3Mg2)分别形成的晶粒，晶粒的平均粒径为0.1μm至2μm。
10.根据权利要求9所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层中所述晶粒β相/α相的面积比为10％～70％。
11.根据权利要求10所述的形成有铝镁合金层的钢板，其中，
所述铝镁合金层的α相和β相其XRD强度比即Iβ(880)/Iα(111)为0.01～1.5。
12.一种钢板上形成铝镁合金层的方法，包括：
准备钢板；
在所述钢板上真空镀上铝镀层；
在所述铝镀层上至少一次真空镀上镁镀层；
在所述镁镀层上至少一次真空镀上第二铝镀层。
13.根据权利要求12所述的钢板上形成铝镁合金层的方法，还包括：
在所述第二铝镀层上至少一次真空镀上第二镁镀层。
14.根据权利要求13所述的钢板上形成铝镁合金层的方法，其中，
在所述钢板上先真空镀上镁镀层用以替代铝镀层，接着依次真空镀上铝镀层和镁镀层且重复至少一次。
15.根据权利要求12所述的钢板上形成铝镁合金层的方法，其中，
真空镀在所述钢板上的镁镀层以真空镀在所述镁镀层上的铝通过扩散能够与所述钢板上的铁进行反应而在所述镀层形成铁铝合金层的厚度来形成。
16.根据权利要求12至15中任何一项所述的钢板上形成铝镁合金层的方法，其中，
所述铝镁合金层在整个合金层中镁含量为1重量％至45重量％。
17.根据权利要求16所述的钢板上形成铝镁合金层的方法，其中，
所述铝镁合金层在整个合金层中镁含量为9重量％至40重量％。
18.根据权利要求16所述的钢板上形成铝镁合金层的方法，其中，
由所述铝镀层和所述镁镀层组成的铝镁镀层其厚度为0.5μm至30μm。
19.根据权利要求18所述的钢板上形成铝镁合金层的方法，其通过磁控溅镀来真空镀上所述铝镁镀层。
20.根据权利要求19所述的钢板上形成铝镁合金层的方法，其通过将配置在铝源和镁源上方的所述钢板反复进行往返运动来真空镀上所述铝镁镀层。
21.根据权利要求20所述的钢板上形成铝镁合金层的方法，其通过改变施加于所述铝源和镁源的电流或者电压来改变所述铝镁镀层的组分。
22.根据权利要求18所述的钢板上形成铝镁合金层的方法，其将形成有所述铝镁镀层的钢板在热处理炉中进行热处理，以使所述铝镁镀层相变为铝镁合金层。
23.根据权利要求22所述的钢板上形成铝镁合金层的方法，其中，
所述热处理是在惰性环境中温度范围为350℃～450℃、热处理时间为2分钟～10分钟的条件下进行。
24.根据权利要求23所述的钢板上形成铝镁合金层的方法，其通过所述热处理将所述镀层形成为铁铝合金层或者铝镁合金层中的至少任何一种。
25.根据权利要求24所述的钢板上形成铝镁合金层的方法，其中，
钢板的铁成分扩散到镀层形成AlxFey层，所述AlxFey层满足以下条件：
AlxFey层中，x为1～3，y为0.5～1.5。
26.根据权利要求25所述的钢板上形成铝镁合金层的方法，其中，
所述铝铁合金层的厚度为0.2μm～1μm。
27.根据权利要求24所述的钢板上形成铝镁合金层的方法，其中，
通过所述热处理所述铝镁合金层形成α相或者β相(Al3Mg2)中的至少任何一种。
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US9689057B2 (en) 2017-06-27
WO2014104717A1 (ko) 2014-07-03
US20170253951A1 (en) 2017-09-07
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