CN114286869A - 热冲压成形体 - Google Patents

热冲压成形体 Download PDF

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Publication number
CN114286869A
CN114286869A CN202080059411.1A CN202080059411A CN114286869A CN 114286869 A CN114286869 A CN 114286869A CN 202080059411 A CN202080059411 A CN 202080059411A CN 114286869 A CN114286869 A CN 114286869A
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China
Prior art keywords
chemical conversion
hot
plating layer
conversion coating
coating
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CN202080059411.1A
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CN114286869B (zh
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光延卓哉
德田公平
高桥武宽
竹林浩史
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Nippon Steel Corp
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Nippon Steel and Sumitomo Metal Corp
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    • 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
    • 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
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/012—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 aluminium or an aluminium alloy
    • 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
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    • C22C18/04—Alloys based on zinc with aluminium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • 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
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    • 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
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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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/14—Removing excess of molten coatings; Controlling or regulating the coating thickness
    • C23C2/16—Removing excess of molten coatings; Controlling or regulating the coating thickness using fluids under pressure, e.g. air knives
    • C23C2/18—Removing excess of molten coatings from elongated material
    • C23C2/20—Strips; Plates
    • 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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    • 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

该热冲压成形体具备钢制母材、形成于所述母材表面的镀层以及形成于所述镀层表面的化学转化处理被膜，所述镀层的化学组成以质量％计含有Al：20.00～45.00％、Fe：10.00～45.00％、Mg：4.50～15.00％、Si：0.10～3.00％、Ca：0.05～3.00％、Sb：0～0.50％、Pb：0～0.50％、Cu：0～1.00％、Sn：0～1.00％、Ti：0～1.00％、Sr：0～0.50％、Cr：0～1.00％、Ni：0～1.00％、Mn：0～1.00％，余量为Zn和杂质，所述化学转化处理被膜包含磷酸锌晶体，所述磷酸锌晶体以质量％计含有Mg：5.0～50.0％和Ca：0.5～5.0％，所述化学转化处理被膜的单面附着量为0.1～10.0g/m2。

Description

热冲压成形体
技术领域
本发明涉及一种热冲压成形体。
本申请基于2019年8月29日在日本提出申请的专利申请2019-157205号主张优先权，将其内容引用于此。
背景技术
近年来，为了保护环境和防止地球温室化，要求抑制化学燃料的消耗。这种要求例如对于在日常生活和活动中作为移动手段不可欠缺的汽车也不例外。针对这种要求，汽车领域研究了通过减轻车身重量等来提高燃油效率等。汽车的结构大多是由铁、特别是由钢板形成的，所以减薄该钢板而降低重量对于减轻车身重量效果巨大。但是，如果简单地减薄钢板厚度而降低钢板重量，则作为结构物的强度降低，担心安全性降低。因此，为了减薄钢板厚度，需要提高所使用的钢板的机械强度，以免结构物强度降低。
因而，通过提高钢板的机械强度，对即使比以前使用的钢板薄也能维持或提高机械强度的钢板进行了研究开发。对这种钢板的需要不仅在汽车制造业，在各种制造业中也是同样的。
一般而言，机械强度高的材料在弯曲等成形加工中存在形状冻结性低的倾向，在加工成复杂形状的情况下，加工本身变困难。作为解决关于该成形性的问题的手段之一，可举出所谓的“热压法(热冲压法、高温压制法、模淬火法)”。该热压方法中，将作为成形对象的材料暂且加热到高温，对通过加热而软化了的材料进行压制加工而成形，然后或者在成形的同时进行冷却。
根据该热压方法，将材料暂且加热到高温而软化，在材料软化了的状态下进行压制加工，所以能够容易地对材料压制加工。因此，通过该热压加工，可得到兼具良好的形状冻结性和高机械强度的压制成形品。特别是在材料为钢的情况下，通过成形后的冷却带来的淬火效果，能够提高压制成形品的机械强度。
但是，在将该热压方法应用于钢板的情况下，由于加热到例如800℃以上的高温，表面的铁等氧化而产生氧化皮(氧化物)。因此，在进行热压加工后，需要除去氧化皮的工序(除氧化皮工序)，生产率降低。另外，对于需要耐蚀性的构件等，需要在加工后对构件表面进行防锈处理和/或金属被覆，所以需要表面清洁化工序、表面处理工序，这也会使生产率降低。
作为抑制这种生产率降低的方法的例子，考虑通过对热冲压前的钢板实施镀敷等被覆来提高耐蚀性并省略除氧化皮工序。
作为这种镀敷钢材，例如专利文献1公开了一种热压用镀敷钢板，其特征在于，在钢板表面具有Al-Zn系合金镀层，Al-Zn系合金镀层含有Al：20～95质量％、Ca+Mg：0.01～10质量％以及Si。根据专利文献1，公开了热压前的加热时可抑制氧化皮的生成，并且在热压时镀层不会在模具凝结，而且得到的热压构件的外观良好，具有优异的涂装密合性和耐蚀性。
另外，专利文献2公开了一种耐蚀性飞跃性地提高了的镀敷钢材，其在钢材表面具备含有Al-Fe合金层和Zn-Mg-Al合金层的镀层。
如上所述的镀敷钢材被热冲压而得到的构件大多适用于汽车部件，在作为汽车部件应用的情况下，一般对构件实施化学转化处理。但是，专利文献1和专利文献2中，对于形成化学转化处理被膜时的特性毫无研究。
本发明人研究的结果得知，作为对具有含Al和/或Zn的镀层的钢板进行热冲压而得到的构件，即使对该构件进行作为用于汽车的一般化学转化处理的磷酸锌处理，也难以形成磷酸锌被膜，或者即使形成，在其表面进一步形成电沉积涂膜等时的涂膜密合性也不足。
专利文献3公开了一种使用金属表面处理剂对锌-铝-镁合金镀敷钢板的表面进行处理的方法。专利文献3中，通过使化学转化处理液含有氟化合物，来通过化学转化处理在镀敷钢板的镀层表面形成含有Al和Mg的氟化物的反应层，能够更加提高化学转化处理膜与镀层表面的密合性。
但是，专利文献3中并未对在化学转化处理被膜上形成电沉积涂膜等时的涂膜密合性加以研究。
现有技术文献
专利文献1：日本特开2012-112010号公报
专利文献2：日本特开2017-66459号公报
专利文献3：日本特开2016-89232号公报
发明内容
本发明是鉴于上述课题而完成的。本发明的课题是提供一种热冲压成形体，其具有氧化皮被抑制且与涂膜密合性优异的化学转化处理被膜。
本发明人的见解如下：通过控制热浸镀Zn-Al-Mg钢板的镀层组成平衡和制造时的条件，来得到具有氧化皮被抑制且涂膜密合性优异的化学转化处理被膜的热冲压成形体。
本发明是基于上述见解而完成的，其主旨如下所述。
(1)本发明一方式的热冲压成形体，具备：钢制母材、形成于所述母材表面的镀层、以及形成于所述镀层表面的化学转化处理被膜，所述镀层的化学组成以质量％计含有Al：20.00～45.00％、Fe：10.00～45.00％、Mg：4.50～15.00％、Si：0.10～3.00％、Ca：0.05～3.00％、Sb：0～0.50％、Pb：0～0.50％、Cu：0～1.00％、Sn：0～1.00％、Ti：0～1.00％、Sr：0～0.50％、Cr：0～1.00％、Ni：0～1.00％、Mn：0～1.00％，余量为Zn和杂质，所述化学转化处理被膜包含磷酸锌晶体，所述磷酸锌晶体以质量％计含有Mg：5.0～50.0％和Ca：0.5～5.0％，所述化学转化处理被膜的单面附着量为0.1～10.0g/m2。
(2)根据上述(1)记载的热冲压成形体，所述镀层的所述化学组成可以以质量％计含有以下之中的1种或2种，Al：25.00～35.00％、Mg：6.00～10.00％。
(3)根据上述(1)或(2)记载的热冲压成形体，所述化学转化处理被膜的所述单面附着量可以为1.5～8.0g/m2。
根据本发明的上述方式，能够提供具有氧化皮被抑制且涂膜密合性优异的化学转化处理被膜的热冲压成形体。
附图说明
图1是表示本实施方式的热冲压成形体的示意图。
图2是表示本实施方式的热冲压成形体的化学转化处理被膜的组织一例的图。
图3是表示实施例No.12(比较例)的热冲压成形体的化学转化处理被膜的组织一例的图。
具体实施方式
参照附图对本发明一实施方式的热冲压成形体(本实施方式的热冲压体)进行说明。
参照图1，本实施方式的热冲压成形体1具备钢制母材2、形成于母材2表面的镀层3以及形成于镀层3表面的化学转化处理被膜4。图1中，镀层3和化学转化处理被膜4仅形成于母材2的单面，但也可以形成于两面。
<母材>
母材2由钢制成。母材2是例如通过热冲压钢板而得到的热冲压构件。因此，图1中，虽然是板形，但其形状没有限定。
另外，本实施方式的热冲压成形体1中，镀层3和化学转化处理被膜4很重要，对母材2的化学组成等没有特别限定。母材2根据适用的产品和要求的强度、板厚等确定供于热冲压和化学转化处理的钢即可。例如，作为母材，可以使用JIS G3193：2008中记载的热轧钢板或JIS G3141：2017中记载的冷轧钢板。
<镀层>
[化学组成]
以下，关于镀层、化学转化处理被膜的化学组成的％，只要没有特别说明就是质量％。
Al：20.00～45.00％
Al是用于提高镀层3的耐蚀性所必需的元素。另外，如果Al含量低于20.00％，则无法在镀层表面充分生成在热冲压的加热中抑制Zn和Mg的蒸发并且作为向化学转化处理层的Ca供给源的以Ca和Al为主体的金属间化合物。其结果，在镀层3上形成的化学转化处理被膜4的氧化皮变大。因此，将Al含量设为20.00％以上。优选为25.00％以上。
另一方面，即使Al含量超过45.00％，在热冲压的加热中也难以在镀层3表面生成以Ca和Al为主体的金属间化合物。其结果，化学转化处理被膜4的氧化皮变大。因此，将Al含量设为45.00％以下。优选为35.00％以下。
Fe：10.00～45.00％
热冲压时，如果加热镀敷钢板，则Fe从母材2向镀层3扩散，所以热冲压成形体1的镀层3中必然含有Fe。
在Fe含量低于10.0％的情况下，存在点焊性和焊接性恶化的倾向，所以将Fe含量设为10.00％以上。
另一方面，在Fe含量过高的情况下，存在耐蚀性恶化的倾向，所以将Fe含量设为45.00％以下。
Mg：4.50～15.00％
Mg是有助于提高镀层3的耐蚀性的元素。另外，Mg在热冲压的加热时，与镀层3中的Zn成分结合而防止液相Zn的产生，所以也具有抑制LME开裂的效果。另外，本实施方式的热冲压成形体1中，Mg是扩散到化学转化处理被膜4中，提高涂膜密合性的元素。为了获得这些效果，将Mg含量设为4.50％以上。如果Mg含量低于4.50％，则涂膜密合性降低。Mg含量优选为6.00％以上。
另一方面，如果Mg含量超过15.00％，则过度地出现牺牲防蚀作用，存在镀层3的耐蚀性降低的倾向。另外，镀层3中使化学转化处理性降低的Mg系金属间化合物大量形成，其结果，化学转化处理被膜4的氧化皮变大，并且涂膜密合性降低。因此，将Mg含量设为15.00％以下。优选为10.00％以下。
Si：0.10～3.00％
Si是与Mg一起形成化合物，有助于提高耐蚀性的元素。另外，Si在将镀层形成于钢板上时抑制钢板表面与镀层之间形成的合金层形成得过厚，也是具有提高钢板与镀层的密合性的效果的元素。Si含量低于0.10％时无法充分获得这些效果。因此，将Si含量设为0.10％以上。
另一方面，如果Si含量超过3.00％，则形成Mg2Si、Mg2Ca或(Mg,Ca)2Si，化学转化处理被膜4所含有的Mg含量和Ca含量不足，涂膜密合性降低。另外，如果Si相过剩地生成，则耐切屑性、耐烧结性降低。因此，将Si含量设为3.00％以下。
Ca：0.05～3.00％
本实施方式的热冲压成形体1中，Ca是扩散到化学转化处理被膜4中，提高涂膜密合性的元素。Ca含量低于0.05％时，化学转化处理被膜4的氧化皮变大。因此，将Ca含量设为0.05％以上。
另一方面，如果Ca含量超过3.00％，则形成以降低化学转化处理性的Ca为主体的金属间化合物，由此化学转化处理被膜的Mg含量、Ca含量不足，并且氧化皮变大，涂膜密合性降低。因此，将Ca含量设为3.00％以下。
本实施方式的热冲压成形体1的镀层3的基础是：含有上述元素，余量包含Zn和杂质。
但是，镀层3在上述元素之外，可以在下述范围含有Sb、Pb、Cu、Sn、Ti、Sr、Cr、Ni、Mn。由于这些元素并不必须含有，所以下限是0％。另外，这些元素的合计含量优选为5.00％以下。
Sb：0～0.50％
Pb：0～0.50％
Cu：0～1.00％
Sn：0～1.00％
Ti：0～1.00％
Sb、Pd、Cu、Sn和Ti在镀层3中与Zn置换，在MgZn2相内形成固溶体，但若在预定含量范围内，则不会对热冲压成形体1的特性造成不良影响。因而，这些元素也可以包含在镀层3中。但是，在各个元素的含量过剩的情况下，热冲压的加热时，这些元素的氧化物析出，存在热冲压成形体1的表面形状恶化，化学转化处理性降低的倾向。另外，在Pb、Sn的含量过剩的情况下，焊接性和耐LME性也会劣化。
因此，Sb和Pb的含量分别为0.50％以下，Cu、Sn和Ti的含量分别为1.00％以下。Sb和Pb的含量优选为0.20％以下。Cu、Sn和Ti的含量优选为0.80％以下，更优选为0.50％以下。
Sr：0～0.50％
Sr是对抑制制造时形成于镀浴上的顶渣生成有效的元素。另外，Sr在热冲压的热处理时抑制大气氧化，所以是抑制热处理后的镀敷钢板变色的元素。因此，可以含有Sr。为了获得上述效果，Sr含量优选为0.05％以上。
另一方面，在Sr含量过剩的情况下，在腐蚀试验中对涂膜膨胀幅度和流锈造成不良影响。因此，Sr含量为0.50％以下。Sr含量优选为0.30％以下，更优选为0.10％以下。
Cr：0～1.00％
Ni：0～1.00％
Mn：0～1.00％
Cr、Ni和Mn在镀敷钢板中在镀层与母材的界面附近变浓，具有使镀层表面的锌花消失等效果。因而，选自Cr、Ni和Mn中的一种以上可以在镀层中含有。在获得这些效果的情况下，Cr、Ni和Mn的含量分别优选为0.01％以上。
另一方面，在这些元素的含量过剩的情况下，涂膜膨胀幅度和流锈变大，存在耐蚀性劣化的倾向。因而，Cr、Ni和Mn的含量分别为1.00％以下。Cr、Ni和Mn的含量分别优选为0.50％以下，更优选为0.10％以下。
镀层的平均组成通过溶解镀层并剥离后，采用电感耦合等离子体发射(ICP)分析法分析剥离了的镀层所含的元素含量来测定。镀层的剥离例如可以将其浸渍在加入了抑制铁基体腐蚀的抑制剂(防酸洗抑制剂：朝日化学制)的10％盐酸中，将发泡停止时判断为溶解完成即可。
镀层的组织没有限定，例如包含Fe-Al相、Zn-Mg相、Zn-Al-Mg相。另外，镀层的附着量没有限定，但优选为10～120g/m2。镀层的附着量可以采用上述方法在室温下溶解镀层，根据溶解前后的重量变化来求得。
<化学转化处理被膜>
[包含以质量％计含有Mg：5.0～50.0％和Ca：0.5～5.0％的磷酸锌晶体]
通常，在将具有含Al镀层的钢材热冲压而得到的热冲压成形体的表面(镀层的表面)，形成主要由Al2O3构成的氧化物。形成于镀层表面的Al2O3会妨碍化学转化处理被膜的形成，所以对Al2O3形成于表面的镀敷钢材进行化学转化处理时，在热冲压成形体中，化学转化处理被膜的氧化皮比例变大。
对此，本实施方式的热冲压成形体中，通过采用如后所述的方法进行镀敷，来在供于化学转化处理的热冲压后的镀敷钢材表面，形成以Ca、Mg为主体的氧化物被膜。如果对该钢材料进行磷酸锌处理(化学转化处理)，则Mg和Ca扩散到化学转化处理被膜，形成包含磷酸锌晶体的化学转化处理被膜4，所述磷酸锌晶体以质量％计含有Mg：5.0～50.0％和Ca：0.5～5.0％。图2表示本实施方式的热冲压成形体1的化学转化处理被膜4的代表性组织照片。该化学转化处理被膜4包含磷酸锌晶体11，磷酸锌晶体11含有Mg：5.0～50.0％和Ca：0.5～5.0％，磷酸锌晶体11是晶体粒径为长径10μm以下且短径为5μm以下的鳞片状。另外，在形成这种磷酸锌晶体11的情况下，氧化皮的比例变为10％以下。另外，含有Mg的化学转化处理被膜本身的耐蚀性优异，所以与不含Mg的化学转化处理被膜相比有助于提高涂装后的密合性(涂膜密合性)。
如果在进行化学转化处理的钢材表面没有充分形成Mg、Ca的氧化物被膜，则生成Al氧化物，化学转化处理被膜4的氧化皮变大。如果化学转化处理被膜中的Mg、Ca含量少，则化学转化处理被膜的耐蚀性降低，所以涂膜密合性降低。
另一方面，如果Mg、Ca含量多，则化学转化处理被膜的耐蚀性反而降低，所以涂膜密合性降低。
根据热冲压条件和镀层厚度，通过合金化而扩散到镀层中的Fe存在于磷酸锌晶体的化学转化处理被膜中。
化学转化处理被膜的化学组成通过用镀层不溶解而仅使化学转化处理被膜溶解的试剂、例如20％铬酸溶解，对化学转化处理被膜溶解后的溶液进行ICP分析，并测定化学转化处理被膜的平均组成来得到。或者，也可以预先制作检测线，用荧光X射线定量分析来测定。
[单面附着量为0.1～10g/m2]
化学转化处理被膜4的单面附着量低于0.1g/m2时，无法充分得到涂膜密合性(在化学转化处理被膜的表面形成涂膜时的密合性)的提高效果。另一方面，如果单面附着量超过10g/m2，则受到弯曲加工等时化学转化处理被膜内容易产生龟裂，造成涂膜剥离。因此，将单面附着量设为0.1～10g/m2。优选为1.5～8.0g/m2。
在采用溶解单面附着量的方法求算的情况下，可以通过将进行测定的面以外的、相反侧的面和端面用胶带密封，并浸渍到溶液中，来得到仅测定面的剥离液，根据溶解前后的重量变化来求得。
在用X射线荧光测定的情况下，求得仅单面的附着量。
本实施方式的热冲压成形体1中，也可以在镀层3与化学转化处理被膜4之间进一步设置氧化物被膜。该氧化物被膜例如由氧化钙或氧化镁构成。
<制造方法>
本实施方式的热冲压成形体不取决于制造方法，只要具有上述特征即可获得其效果。但是，根据包括以下工序的制造方法能够稳定地制造，所以优选。
即，本实施方式的热冲压成形体可以采用以下制造方法得到，该制造方法具备：
(I)将钢材浸渍在镀浴中而得到具有镀层的镀敷钢材的镀敷工序、
(II)对镀敷工序后的镀敷钢材进行热冲压的热冲压工序、以及
(III)对热冲压后的镀敷钢材进行化学转化处理的化学转化处理工序，
(IV)在镀敷工序中，在镀浴浸渍后的冷却过程中，以将浴温～450℃的平均冷却速率设为10℃/秒以上、将450～350℃的平均冷却速率设为7℃/秒以下、并将350～150℃的平均冷却速率设为4℃/秒以下的方式冷却至室温。
<镀敷工序>
[向镀浴的浸渍]
镀敷工序中，通过将作为原板的钢板等钢材浸渍到镀浴中，来在表面形成镀层。
关于向镀浴的浸渍条件没有特别限定。例如在600～940℃对镀敷原板表面进行加热还原处理，用N2气空冷使钢材温度达到浴温+20℃，然后在500～750℃的浴温的镀浴中浸渍约0.2～6秒。
浸渍时间低于0.2秒时，无法充分形成镀层。另一方面，浸渍时间超过6秒时，镀层与钢材过剩地合金化，镀层中会含有大量Fe。在镀层中含有过剩铁的情况下，难以在热冲压的加热中抑制Zn和Mg的蒸发。因此，在浸渍时间超过6秒的情况下，无法通过其后的化学转化处理工序来得到具有预定组成的化学转化处理被膜，热冲压成形体的涂膜密合性降低。
镀浴根据作为目标的镀层3的组成，以含有Zn、Al、Mg和其他元素的方式设定即可。镀浴的组成例如含有Al：30.00～75.00％、Mg：4.00～17.00％、Si：0.20～2.00％，且根据需要含有希望在镀层中含有的任选元素，余量为Zn和杂质。
[冷却]
浴温～450℃的平均冷却速度：10℃/秒以上
本实施方式的热冲压成形体的制造方法中，将镀敷钢材从镀浴中提拉后，以直到450℃为止的温度范围的平均冷却速度为10℃/秒以上的方式进行冷却。通过将该温度范围的平均冷却速度设为10℃/秒以上，能够抑制在镀敷钢材表面形成Al氧化物。
450～350℃的平均冷却速度：7℃/秒以下
接着上述冷却，以450℃～350℃的温度范围的平均冷却速度为7℃/秒以下的方式进行冷却。
通过降低在该温度范围的冷却速度而控制凝固组织，来在接下来实行的热冲压工序中，在表面形成Al含量少(例如10原子％以下)的Mg、Ca的氧化物。其结果，在进行化学转化处理的情况下，可得到氧化皮少且含有Mg、Ca的化学转化处理被膜。
另外，在锌系镀层的情况下，担心Zn(锌)由于热冲压而蒸发，但在如上所述地控制的凝固组织中，尽管详细机制尚不完全清楚，但通过在镀层的表面附近优先地生成含有具有抑制蒸气压高的元素即Zn和Mg的蒸发的效果的Al、Zn、Ca和/或Si的金属间化合物，能够抑制在接下来进行的热冲压的加热时Zn和Mg的蒸发。
350～150℃的平均冷却速度：4℃/秒以下
接着上述冷却，如果将350℃～150℃的平均冷却速度设为4℃/秒以下，则凝固组织所含有的Al与Zn的固溶体分离为Al相和Zn相，由此镀层的熔点降低，含有Al、Zn、Ca和/或Si的金属间化合物容易在热冲压加热中向处于熔融状态的镀层表面移动。作为其结果，能够更有效地抑制Zn和Mg的蒸发，能够形成含有Mg和Ca的化学转化处理被膜。
不过，即使350℃～150℃的平均冷却速度为4℃/秒以下，部分的温度范围的冷却速度快时也得不到合适的金属组织。因此，优选350℃～150℃的平均冷却速度为4℃/秒以下，350℃～250℃的平均冷却速度为4℃/秒以下，并且250～150℃的平均冷却速度为4℃/秒以下。
<热冲压工序>
对镀敷工序后的镀敷钢材(具有母材和形成于其表面上的镀层的钢材)实行热冲压。
热冲压的条件没有限定，例如可举出将镀敷钢板加热至750～1200℃，保持0～8分钟，然后用处于室温左右的温度的平板模具夹持镀敷钢板进行急冷的方法。
<化学转化处理工序>
对热冲压后的成形体进行化学转化处理。对化学转化处理没有限定，可以是公知的磷酸锌处理。
根据上述制造方法，能够得到本实施方式的热冲压成形体。
实施例
以下，通过实施例更具体地说明本发明，但本发明并不限定于这些实施例。
表1～表3表示本发明中公开的实施例。制作各种Zn-Al-Mg系镀浴并供于热冲压加热。作为镀敷原板，使用了板厚1.6mm的钢板(含有C：0.2％和Mn：1.3％)。将原板切断为100mm×200mm后，使用本公司制的间歇式热浸镀试验装置实施镀敷。使用在镀敷原板中心部点焊了的热电偶测定板温度。
在镀浴浸渍前，将镀敷原板表面在氧浓度20ppm以下的炉内在N2-5％H2气体气氛下以800℃进行加热还原处理，并用N2气进行空冷而使浸渍板温度达到浴温+20℃，然后在表2所示浴温的镀浴中浸渍约3秒。镀浴浸渍后，以20～200mm/秒的提拉速度提拉。
提拉时，用N2擦拭气体如表2所示地控制镀敷附着量。将钢板从镀浴中提拉后，在表2所示条件下将其从镀浴温度冷却至室温。
对制成的镀敷钢板实施热冲压加热和模具急冷。加热条件是将镀敷钢板插入900℃的加热炉中，镀敷钢板温度达到炉内温度-10℃后，保持0～8分钟，然后用处于室温左右的温度的平板模具夹持镀敷钢板进行急冷，由此制作成形品。
采用上述方法调查的结果，热冲压后的镀层的化学组成如表1所示。
No.31中对市售的合金化热浸镀锌钢板进行了热冲压。
然后，从热冲压后的钢材制取50×100mm(×板厚)的试样，依据(SD5350系统：日本涂料工业编码公司制标准)对该试样实施磷酸锌处理，形成化学转化处理被膜。
表1
Figure BDA0003514944510000131
表2
Figure BDA0003514944510000141
<化学转化处理被膜的评价>
为了调查化学转化处理被膜，将制成的样品用20％铬酸溶解，对溶解了化学转化处理被膜的溶液进行ICP分析，测定了化学转化处理被膜的平均组成。另外，根据溶解前后重量变化测定了每单面的附着量。
另外，通过对形成有化学转化处理被膜的镀敷钢板表面进行SEM观察，由此测定了化学转化处理被膜的氧化皮比例(面积％)。此时，在SEM观察视场中，将钢板露出的区域的面积率定义为氧化皮的比例。氧化皮的比例若为10面积％以下，则判断为氧化皮得到抑制。
再者，将化学转化处理后的样品切断为25mm(C方向)×15mm(L方向)，得到样品表面的SEM像。基于该SEM像，观察磷酸锌晶体的形状。其结果，发明例中，确认到磷酸锌晶体的、晶体粒径为长径10μm以下且短径5μm以下的鳞片状。
<涂膜密合性(耐SDT性)>
热冲压成形体的涂膜密合性如上所述，依据(SD5350系统：日本涂料工业编码公司制标准)对样品50×100mm实施磷酸锌处理，然后实施电沉积涂装(PN110パワーニクスグレー：日本涂料工业编码公司制标准)以使得涂膜厚度为20μm，在烧结温度150℃进行20分钟烧结，然后将带有到达铁基体的横切划痕(40×√2mm 2条)的涂装镀敷钢板在55℃的5％NaCl盐水中浸渍1000小时，然后通过胶带剥离使电沉积涂膜剥离，根据发生剥离的部分的面积率和红锈发生状况来进行评价。
剥离面积为5％以下的情况为“AA”，剥离面积超过5％～10％的情况为“A”，剥离面积超过10％或发生红锈的情况为“B”。
将结果示于表3。
表3
Figure BDA0003514944510000161
在作为本发明例的No.3、5～10、17～20、23～26、28和29中，在合适的制造条件下制作镀敷钢板并热冲压，由此在镀层上形成了含有Mg和Ca的化学转化处理被膜。其结果，具有优异的涂膜密合性。
图2是表1～表3中No.10的SEM像(BSE像)。在样品表面形成磷酸锌晶体，没有发现磷酸锌晶体未形成的氧化皮。作为ICP分析的结果，磷酸锌晶体含有33.5％的Mg和2.6％的Ca。
另一方面，镀层的化学组成在本发明的范围外或制造方法不合适的比较例中，化学转化处理被膜的组成和/或氧化皮的面积率变大，涂膜密合性低。例如，No.12中，如图3所示，磷酸锌膜13不含Ca、Mg，并且发现许多氧化皮12。
另外，对市售的合金化热镀锌钢板进行热冲压的No.28中，涂膜密合性也差。
附图标记说明
1 热冲压成形体
2 母材
3 镀层
4 化学转化处理被膜
11 含有Mg和Ca的磷酸锌晶体
12 氧化皮
13 不含Mg和Ca的磷酸锌晶体

Claims (3)

1.一种热冲压成形体，其特征在于，具备：
钢制母材、
形成于所述母材表面的镀层、以及
形成于所述镀层表面的化学转化处理被膜，
所述镀层的化学组成以质量％计含有
Al：20.00～45.00％、
Fe：10.00～45.00％、
Mg：4.50～15.00％、
Si：0.10～3.00％、
Ca：0.05～3.00％、
Sb：0～0.50％、
Pb：0～0.50％、
Cu：0～1.00％、
Sn：0～1.00％、
Ti：0～1.00％、
Sr：0～0.50％、
Cr：0～1.00％、
Ni：0～1.00％、
Mn：0～1.00％，
余量为Zn和杂质，
所述化学转化处理被膜包含磷酸锌晶体，所述磷酸锌晶体以质量％计含有Mg：5.0～50.0％和Ca：0.5～5.0％，
所述化学转化处理被膜的单面附着量为0.1～10.0g/m2。
2.根据权利要求1所述的热冲压成形体，其特征在于，
所述镀层的所述化学组成以质量％计含有以下之中的1种或2种，
Al：25.00～35.00％、
Mg：6.00～10.00％。
3.根据权利要求1或2所述的热冲压成形体，其特征在于，
所述化学转化处理被膜的所述单面附着量为1.5～8.0g/m2。
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