CN104011252A - 在超低温下具有优异粘合性的热浸镀锌钢板及其制造方法 - Google Patents
在超低温下具有优异粘合性的热浸镀锌钢板及其制造方法 Download PDFInfo
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- CN104011252A CN104011252A CN201280064126.4A CN201280064126A CN104011252A CN 104011252 A CN104011252 A CN 104011252A CN 201280064126 A CN201280064126 A CN 201280064126A CN 104011252 A CN104011252 A CN 104011252A
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- steel sheet
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- galvanized steel
- transition metal
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- 229910001335 Galvanized steel Inorganic materials 0.000 title claims abstract description 42
- 239000008397 galvanized steel Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 84
- 239000010959 steel Substances 0.000 claims abstract description 84
- 239000011701 zinc Substances 0.000 claims abstract description 54
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 38
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 31
- 150000003624 transition metals Chemical class 0.000 claims abstract description 31
- 229910000765 intermetallic Inorganic materials 0.000 claims abstract description 5
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010410 layer Substances 0.000 claims description 34
- 239000000758 substrate Substances 0.000 claims description 34
- 230000000903 blocking effect Effects 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 26
- 238000007747 plating Methods 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 239000011247 coating layer Substances 0.000 claims description 21
- 238000005246 galvanizing Methods 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010306 acid treatment Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000007669 thermal treatment Methods 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
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- 230000005764 inhibitory process Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
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- 239000000203 mixture Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005097 cold rolling Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 206010003591 Ataxia Diseases 0.000 description 1
- 206010010947 Coordination abnormal Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000863032 Trieres Species 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
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- 239000010960 cold rolled steel Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 208000016290 incoordination Diseases 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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Classifications
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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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- C23C28/025—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 with at least one zinc-based layer
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- 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
- B32B15/015—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 the said other metal being copper or nickel or an alloy thereof
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
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- 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
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/20—Electroplating: Baths therefor from solutions of iron
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- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/12785—Group IIB metal-base component
- Y10T428/12792—Zn-base component
- Y10T428/12799—Next to Fe-base component [e.g., galvanized]
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Abstract
提供了一种在超低温下具有优异粘合性以及具有精细锌花的热浸镀锌钢板，以及其制造方法。根据本发明，所述在超低温下具有优异粘合性的热浸镀锌钢板包括：钢基板；形成于钢基板上的包括过渡金属的复合层；形成于复合层上的包括铁-铝(Fe-Al)基金属间化合物的阻挡层；以及形成于阻挡层上的镀锌(Zn)层，其中所述镀锌层中的锌花的平均直径为150μm以下，以及提供制造所述热浸镀锌钢板的方法。
Description
技术领域
本发明涉及一种热浸镀锌钢板，更具体而言，涉及一种在超低温下具有优异粘合性的热浸镀锌钢板及其制造方法。
背景技术
出于表面外观和耐腐蚀性的目的，通常将镀锌(Zn)钢板用作汽车用钢板。镀锌钢板可大致分类为热浸镀锌钢板(GI)钢板和电镀锌(EG)钢板。热浸镀锌钢板通过使用如下方法制造：通过浸渍于热浸镀锌浴中而镀覆钢板，而电镀锌钢板是通过使用电镀法镀覆。
热浸镀锌钢板比电镀钢板具有更好的价格竞争力，但由于在涂布后不良的图像清晰度和外观质量而因此限制了对其的需求。为了解决前述限制，已经开发出在镀覆层中精炼锌花(refining spangles)的技术，该技术通过在镀锌后在镀锌层上应用磷酸盐溶液静电雾化的技术(专利文件1)进行。如果使用该技术，可制造出在镀锌层中具有锌花直径为约50μm至约1000μm的热浸镀锌钢板(GI-ACE钢板)。通过在镀覆层中精炼锌花而得到的GI-ACE钢板具有优异的涂层表面特性，例如可涂布性、耐腐蚀性和表面外观，且由于与常规GI钢板相比在价格方面变化不显著而具有优异的经济因素。换言之，所述GI-ACE钢板与常规GI钢板相比更适于汽车用钢板的需求。
同时，在汽车的制造中，可使用结构粘合剂以增强碰撞性能，或者可用结构粘合剂替代焊接。为了使用结构粘合剂，需要优异的粘合性以确保在超低温度(约-4℃)下通过冲击剥离(impact peel)测试。
在对常规GI钢板进行冲击剥离测试的情况下，粘合剂中可能发生断裂。这表示镀锌层具有优异的粘合性。相比之下，对于GI-ACE钢板，断裂可能发生在镀锌层中。
一般而言，已知的是，在低温下锌的(0001)面和三个{10-10}面中发生脆性断裂，且锌断裂机制(fracture mechanism)的行为根据温度由在高温下的脆性+晶界+韧性断裂型变化至在低温下的脆性断裂型。还已知，镀覆层中的断裂发生在镀覆层的锌花边界处或钢基板和镀覆层之间的界面处。
锌花边界处或界面处发生的断裂可能是由于热浸镀锌后在锌花边界处产生孔隙的事实所造成，这是因为，锌在固化时由于发生收缩而使体积发生变化。此外，由于锌的热膨胀系数(约1.5至6.1×10-5/K)和铁的热膨胀系数(约1.18×10-5/K)之间存在差异，因此由于热不协调性(thermal misfit)而发生界面处断裂。此外，已知相对较大量的应力施加至锌花边界，所述锌花边界具有整合在(0001)面的镀覆层的择优取向，因此，断裂开始于钢基板和镀覆层之间的界面处。
因此，对于GI-ACE钢板，在镀覆层和钢基板之间的界面或具有整合在(0001)面的择优取向的锌花边界可起到裂痕起始位点的作用以产生断裂。为了解决GI-ACE钢板的前述限制，已经开发出提高镀覆层中锌花的平均直径的技术(专利文件2)。然而，表面品质例如图像清晰度、耐擦伤性和耐腐蚀性可能随锌花直径的增加而劣化。
(专利文件1)第2006-0076214号韩国专利申请公开出版物
(专利文件2)第2011-0075612号韩国专利申请公开出版物
发明内容
技术问题
本发明的一个方面提供一种热浸镀锌钢板，所述热浸镀锌钢板在超低温下具有优异的粘合性以及优异的表面品质例如图像品质和耐腐蚀性，以及涉及其制造方法。
技术方案
根据本发明的一个方面，提供了一种在超低温下具有优异粘合性的热浸镀锌钢板，所述钢板包括：钢基板；形成于钢基板上的包括过渡金属的复合层；形成于复合层上的包括铁-铝(Fe-Al)基金属间化合物(intermetallic compound)的阻挡层(inhibition layer)；以及形成于阻挡层上的镀锌(Zn)层，其中所述镀锌层中的锌花的平均直径为150μm以下。
根据本发明的另一个方面，提供了一种制造在超低温下具有优异粘合性的热浸镀锌钢板的方法，该方法包括：准备钢板；在钢板上镀覆过渡金属；对过渡金属涂覆钢板进行热处理以制造热处理钢板；冷却热处理钢板；将冷却钢板浸渍在热浸镀锌浴中以制造热浸镀锌钢板；以及冷却热浸镀锌钢板。
有益效果
本发明可提供一种在超低温下具有优异粘合性的热浸镀锌钢板，其中镀锌层中的锌花直径为150μm以下，且在-40℃的超低温下的冲击剥离强度为15N/mm以上。因此，可提供在超低温下具有优异粘合性以及优异镀覆特性的热浸镀锌钢板，因而其可广泛地用于汽车用钢板。
附图说明
由以下详细描述结合附图可更清楚地理解本发明的上述方面和其他方面、特征以及其他优势，在所述附图中：
图1为说明本发明的热浸镀锌钢板的横截面的示意图；
图2(a)和2(b)分别为示出了对比实施例2和发明实施例2中的镀覆层表面的显微照片；
图3为示出了在对比实施例1、2、4和5以及发明实施例1至4中根据铁(Fe)的涂布重量和冷却速率所测量的冲击剥离强度结果的图表；
图4分别为(a)对比实施例1和2以及(b)发明实施例3和4中的样品在冲击剥离测试后断裂面的照片；以及
图5(a)和5(b)分别为示出了对比实施例1和发明实施例1中的钢基板和镀覆层之间的界面的透射电子显微镜(TEM)照片。
最佳实施方式
在下文中，将详细描述本发明。
首先，将详细描述根据本发明的一个方面的热浸镀锌钢板。
本发明的热浸镀锌钢板包括钢基板；形成于钢基板上的包括过渡金属的复合层；形成于复合层上的包括铁-铝(Fe-Al)基金属间化合物的阻挡层；以及形成于阻挡层上的镀锌(Zn)层，其中所述镀锌层中的锌花的平均直径为150μm以下。
在本发明中，钢基板的类型无特别限制，只要所述钢基板可用于热浸镀锌钢板即可，例如热轧钢板、冷轧钢板和退火钢板。
本发明的热浸镀锌钢板包括位于钢基板上的包含过渡金属的复合层。所述复合层形成于钢基板和后文描述的阻挡层之间，并通过与阻挡层和钢基板的保形关系(conformal relationship)而起到改善界面粘附的作用。复合层的形成可确保优异的低温下的粘合性。
所述复合层包括过渡金属。在本发明中，过渡金属的类型无特别限制。例如，过渡金属可包括Fe、钴(Co)、镍(Ni)等。如下所述，可通过在热浸镀锌前镀覆过渡金属而纳入过渡金属。
所述复合层形成于钢基板和阻挡层之间，且用于确保界面粘附的复合层的组成可包括50重量％至90重量％的Fe和过渡金属的总量、10重量％至30重量％的Al，且剩余部分为其他不可避免的杂质。由于所述阻挡层的组成包括30重量％以上的Al和50重量％以下的Fe，且所述钢基板的组成包括90重量％以上的Fe，所述复合层中Fe和过渡金属的总和以及Al可分别在50重量％至90重量％的范围内和10重量％至30重量％的范围内，从而维持与阻挡层和钢基板的保形关系并确保界面粘附。
所述复合层可与阻挡层和钢基板呈保形关系。由于所述复合层与阻挡层和钢基板呈具有相同结晶取向(crystallographic orientation)的保形关系，因而阻挡层和钢基板之间的界面粘附(即粘合性)得到改善。所述复合层可包括立方结构。如上所述，所述复合层可具有立方结构以维持其与阻挡层和钢基板的保形关系。钢基板中的Fe具有立方结构，且复合层也可具有立方结构，从而通过在具有立方结构的钢基板上形成所述复合层而得到保形关系。所述复合层的厚度可为80nm以上。所述复合层的厚度的最小值可为80nm以上以确保界面粘附。所述复合层越厚，粘附会越好。然而，由于在复合层过厚的情况下可能会增加成本，复合层的厚度的最大值为500μm。
所述阻挡层起到提高关于镀Zn层的结合力的作用。在不含有阻挡层而形成镀锌层的情况下，由于加工过程中发生Zn的整体剥离，而阻挡层包括Fe-Al基化合物，因此阻挡层可包括具有Zn部分包含在Fe2Al5中的化合物。
所述镀锌层中锌花的平均直径可为150μm以下。需要锌花的平均直径尽可能小。这样做的原因是，在精炼锌花的情况下表面外观更佳。因此，本发明镀锌层中的锌花的平均直径的最大值为150μm。
在下文中，将详细描述根据本发明的另一个方面的制造热浸镀锌钢板的方法。
首先，准备钢板。如上所述，钢板的类型无特别限制，且可使用任意钢板，只要其用于通过热浸镀锌制造热浸镀锌钢板即可。
可进行表面清洗以除去外物或来自钢板表面的氧化层。表面清洗可通过除油和酸洗处理进行。除油和酸洗处理通过众所周知的方法进行。在表面清洗可能不充分的情况下，在下文将描述的镀Fe过程中镀覆可能不充分，且镀覆外观和粘附可能会劣化。
过渡金属镀覆是在钢板的表面上进行。如上所述，过渡金属的类型无特别限制。例如，过渡金属可包括Fe、Co、Ni等。任意镀覆方法可用于镀覆过渡金属。例如，可使用电镀Fe的方法。在电镀Fe的情况下，可使用包括FeSO4·7H2O和(NH4)2SO4的电解质。
过渡金属镀覆的涂布重量可为350mg/m2以上。在过渡金属涂布重量低于350mg/m2的情况下，由于复合层的相对较低的厚度而无法确保足够的表面粘附。在过渡金属涂布重量为350mg/m2以上的情况下，复合层的厚度可为80nm以上。在本发明中，过渡金属涂布重量的上限无特别限制，其上限可为10g/m2以下。
热处理在过渡金属镀覆钢板上进行。热处理可通过在还原气氛中以1.5℃/s至6℃/s的加热速率加热至750℃至900℃的温度范围并维持20秒以上而进行。在加热速率低于1.5℃/s的情况下，钢板的温度上升得相对较慢，因此经济因素可能会劣化，在加热速率高于6℃/s的情况下，钢板中残余应力的除去可能得不到促进，且回收和重结晶可能存在问题。因此，加热速率的上限可为6℃/s。此外，回收和重结晶可在前述750℃至900℃的温度范围内适当地进行。
还原气氛可为H2-N2气体气氛。H2-N2混合气可用于制备还原气氛，且为此作为混合比的一个实例，可使用5体积％至10体积％的氢气和余量的氮气。
维持时间可为20秒以上。在维持时间低于20秒的情况下，由于在钢基板和阻挡层之间的复合区域可能形成不充分，可能无法确保足够的表面粘附。维持时间的上限无特别限制，但维持时间可为100秒以下。在维持时间相对较长的情况下，锌花生长可能会过量，且因此材料可能会不均匀。
冷却热处理钢板。冷却可进行至450℃至500℃的温度范围。该温度至多高于热浸镀锌浴的温度50℃。在冷却温度低于450℃的情况下，后续的Zn镀覆可能无法适当进行，并且在冷却温度高于500℃的情况下，可能会发生诸如烟雾和浮渣的表面缺陷。
因此，冷却温度的上限可为500℃。
热浸镀锌通过将冷却钢板浸渍于热浸镀锌浴中进行。例如，热浸镀锌浴的温度可在430℃至480℃的范围内，且热浸镀锌浴中的Al含量可在0.1重量％至0.3重量％的范围内。在Al含量低于0.1重量％的情况下，Zn粘附可能会降低，并且在Al含量高于0.3重量％的情况下，诸如浮渣的缺陷可能会过度发生。在热浸镀锌浴中的浸渍时间可在2.5秒至8秒的范围内。在热浸镀锌之后可进一步进行空气擦拭(air wiping)以调节Zn的涂布重量。
冷却热浸镀锌钢板。冷却可以-20℃/s以下的冷却速率进行。在冷却速率高于-20℃/s的情况下，镀覆层中锌花的直径为200μm以上，由此可增加锌花的直径。在镀覆层中锌花的直径为200μm以上的情况下，可劣化涂层表面特性，即可涂布性、耐腐蚀性、耐擦伤性、图像清晰度和表面外观。在下文中，将详细描述本发明的实施例。提供以下实施例仅为更清楚地理解本发明，而不是限定其范围。
实施例
将常用的无间隙原子(IF)钢冷轧并通过碱性除油和酸洗处理进行表面清洗，随后，在60℃、pH为5的条件下施加20mA的电流，以在钢板表面上电镀铁——一种过渡金属。同时，如下表1中所述调节Fe的涂布重量。在镀覆Fe之后，进行退火处理并维持在露点温度为-40℃的5％H2-N2气氛中，随后将钢板冷却至500℃。
此后，在460℃的热浸镀锌浴中进行镀覆，随后进行擦拭以将涂布重量调节至约50g/m2。通过在-20℃/s或-65℃/s的冷却速率下冷却来制造热浸镀锌钢板。
同时，在不进行镀Fe的情况下，将IF钢进行冷轧和表面清洁。随后，进行退火处理并维持在露点温度为-40℃的5％H2-N2气氛中，随后将钢板冷却至500℃。此后，在460℃的热浸镀锌浴中进行镀覆，随后进行擦拭以将涂布重量调节至约50g/m2。通过在-20℃/s或-65℃/s的冷却速率下冷却来制造热浸镀锌钢板。
由此制备的热浸镀锌钢板在超低温下的粘附评价通过在-40℃下使用冲击剥离试验机进行，且其结果示于表1中。下表1示出了在每个发明实施例和对比实施例中的Fe涂布重量、热浸镀锌层的锌花直径、冲击剥离强度和冲击剥离测试后的断裂面的结果。
此外，通过前述实验得到的结果示于表2至表5中。
表1
同时，对比实施例1和发明实施例1的钢基板和镀覆层的界面通过使用透射电子显微镜(TEM)来观察，其结果分别示于图5(a)和5(b)中。在图5(a)所示的对比实施例1中，热浸镀锌钢板的横截面由钢基板、阻挡层和镀覆层组成。然而，在图5(b)所示的发明实施例1中，可证实在钢基板和阻挡层之间形成了具有黑带形状的层(复合层)。
对于在复合层上进行的选择区域衍射图(SADP)分析的结果，可证实，复合层的SADP与钢基板和阻挡层的SADP相匹配。因此，可证实，复合层为与钢基板和阻挡层具有保形关系并且钢基板和阻挡层之间具有高度粘附的区域。因此，可以理解，本发明可通过形成复合层而增加钢基板和阻挡层之间的界面粘附，并且可改善超低温下的粘合性。
同时，观察对比实施例2和发明实施例2中的镀覆层表面，其结果分别示于图2(a)和2(b)中。如表1和图2所示，对比实施例2的镀覆层中的锌花直径约为62.9μm，对于发明实施例2而言，锌花直径约为46.8μm。因此，可以理解，当在热浸镀锌之后将冷却速率控制在-60℃/s时，可获得精细的镀覆结构。
此外，测量对比实施例1、2、4和5和发明实施例1至4的冲击剥离强度，其结果示于图3中。如表1和图3所示，对于发明实施例1至4而言，可确保本发明所要求的强度(约15N/mm以上)。然而，对于对比实施例而言，可理解为强度达不到本发明所要求的强度，并且在镀覆层中发生断裂。
同时，将对比实施例1和2中未镀覆Fe的钢板和发明实施例3和4中Fe涂布重量为500mg/m2的钢板进行冲击剥离测试，其断裂面分别示于图4(a)和4(b)中。对于图4(a)中所示的对比实施例而言，可证实，在镀覆层中发生断裂。然而，对于图4(b)中所示的发明实施例而言，可证实，在镀覆层中未发生断裂，因此在低温下的粘合性极佳。
虽然已经结合示例性的实施方案示出和描述了本发明，但是对本领域技术人员显而易见的是，可以在不偏离所附权利要求书限定的本发明的主旨和范围下做出改进和变化。
Claims (16)
1.一种在超低温下具有优异粘合性的热浸镀锌钢板，所述钢板包括：
钢基板；
形成于钢基板上的包括过渡金属的复合层；
形成于复合层上的包括铁-铝(Fe-Al)基金属间化合物的阻挡层；以及
形成于阻挡层上的镀锌(Zn)层，
其中所述镀锌层中的锌花的平均直径为150μm以下。
2.权利要求1的在超低温下具有优异粘合性的热浸镀锌钢板，其中所述复合层包含50重量％至90重量％的Fe和过渡金属的总量、10重量％至30重量％的Al，且剩余部分为其他不可避免的杂质。
3.权利要求1的在超低温下具有优异粘合性的热浸镀锌钢板，其中所述复合层与阻挡层和钢基板呈保形关系。
4.权利要求1的在超低温下具有优异粘合性的热浸镀锌钢板，其中所述复合层具有立方结构。
5.权利要求1的在超低温下具有优异粘合性的热浸镀锌钢板，其中所述复合层的厚度为80nm以上。
6.一种制造在超低温下具有优异粘合性的热浸镀锌钢板的方法，所述方法包括：
准备钢板；
在钢板上镀覆过渡金属；
对过渡金属镀覆的钢板进行热处理以制造热处理钢板；
冷却热处理钢板；
将冷却钢板浸渍在热浸镀锌浴中以制造热浸镀锌钢板；以及
冷却热浸镀锌钢板。
7.权利要求6的方法，其中钢板的准备包括进行除油和酸洗处理。
8.权利要求6的方法，其中过渡金属为Fe、钴(Co)、镍(Ni)中的一种或多种。
9.权利要求8的方法，其中在镀覆作为过渡金属的Fe的情况下，通过使用包括FeSO4·7H2O和(NH4)2SO4的电解质进行电镀。
10.权利要求6的方法，其中进行过渡金属镀覆以具有350mg/m2以上的涂布重量。
11.权利要求6的方法，其中热处理通过在还原气氛中以1.5℃/s至6℃/s的加热速率加热至750℃至900℃的温度范围并维持20秒以上而进行。
12.权利要求6的方法，其中热处理钢板的冷却进行至450℃至500℃的温度范围。
13.权利要求6的方法，其中热浸镀锌通过将钢板在430℃至480℃的温度下浸渍于热浸镀锌浴中2.5秒至8秒而进行，所述热浸镀锌浴包括0.1重量％至0.3重量％的Al。
14.权利要求6的方法，其中热浸镀锌钢板的冷却以-20℃/s以下的冷却速率进行。
15.权利要求6的方法，其中镀覆过渡金属以在热浸镀锌钢板的钢基板和阻挡层之间形成具有优异界面粘附的复合层。
16.权利要求6的方法，其中冷却热浸镀锌钢板以使其镀覆层中的锌花的平均直径为150μm以下。
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| KR10-2011-0141257 | 2011-12-23 | ||
| PCT/KR2012/011172 WO2013095007A1 (en) | 2011-12-23 | 2012-12-20 | Hot-dip galvanized steel sheet having excellent adhesiveness at ultra-low temperatures and method of manufacturing the same |
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| CN104011252B (zh) | 2017-07-18 |
| KR101353701B1 (ko) | 2014-01-21 |
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