CN106170580A - 多层基材及制造方法 - Google Patents

多层基材及制造方法 Download PDF

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Publication number
CN106170580A
CN106170580A CN201480077816.2A CN201480077816A CN106170580A CN 106170580 A CN106170580 A CN 106170580A CN 201480077816 A CN201480077816 A CN 201480077816A CN 106170580 A CN106170580 A CN 106170580A
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coating
weight
metal
metal coating
base material
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CN201480077816.2A
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CN106170580B (zh
Inventor
丹尼尔·沙莱
埃里克·西尔伯贝格
布鲁诺·施米茨
沙维尔·万登艾恩德
塞尔吉奥·帕切
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ArcelorMittal SA
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ArcelorMittal SA
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Priority to CN201911297141.3A priority Critical patent/CN111139477B/zh
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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
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C23C28/3225—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only with at least one zinc-based layer
    • 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
    • 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
    • B32B15/011—Layered products comprising a layer of metal all layers being exclusively metallic all layers being formed of iron alloys or steels
    • 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
    • B32B15/013—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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    • 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
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    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • C—CHEMISTRY; METALLURGY
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Abstract

设置有多个层的基材，其中至少一个层包含金属氧化物并且顶部上直接为金属涂层，所述金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，其中该金属涂层顶部上直接为抗腐蚀涂层。还提供了相应的制造方法。

Description

多层基材及制造方法
本发明涉及多层基材及其制造方法。
背景技术
钢板通常覆盖有金属涂层，所述金属涂层的组成根据钢板的最终用途而不同。例如，该涂层可以是锌、铝、镁或其合金，可以包括一个或更多个层，并且可以使用本领域技术人员已知的不同涂覆技术来施加，所述涂覆技术例如，如真空沉积方法、热浸涂覆或电沉积。在本说明书的剩余部分中，术语“金属涂层”还将用于指包含金属的涂层以及包含金属合金的涂层。
首先，可通过热浸涂覆来施加金属涂层，在此该工艺通常包括以下步骤：
-在惰性或还原性气氛下在钢板通过炉时对其进行退火以限制板表面的氧化；
-在板通过液态的金属浴或金属合金浴时，对其进行浸涂，以使当板离开浴时，其涂覆有金属/金属合金；
-在板离开液体浴之后，通过在表面上喷射气体来干燥金属/金属合金层以保证该层的厚度均匀且规则。
在退火步骤期间，在钢板进入金属浴(在本文的以下部分中，术语“金属浴”和“金属层”还用于指任何金属合金浴和对应的金属合金层)之前，通常将板在直焰式或辐射管式退火炉中加热。然而，尽管采取了大量措施(例如控制惰性气氛)，但是使用这些炉来加热钢板仍可导致在表面上形成金属氧化物，而所述金属氧化物随后必须被移除以确保钢板表面上液态金属的适当润湿性并防止在板表面上出现未经涂覆的区域。
当钢的组成包括显著量的易被氧化元素(例如Si、Mn、Al、Cr、B、P等)时尤其会遇到该问题。例如，含有0.2重量％Mn、0.02重量％Si和5ppm B的IF(无间隙)钢由于存在B而已遭受这些润湿性问题，B快速地扩散至板的表面并使Mn和Si的氧化物以连续膜的形式沉淀，导致差的润湿。
更一般地，在所有的高强度钢中也遇到液态金属的差润湿的风险，因为它们含有这些易被氧化元素中的至少一种，所述高强度钢例如双相钢(Dual Phase steel)、TRIP(相变诱发塑性(Transformation Induced Plasticity))钢、TWIP(孪生诱发塑性(TWinning-Induced Plasticity))钢、电工钢等。
对于双相钢，Mn的量通常小于3重量％，并且Cr、Si或Al的添加量通常小于1重量％。对于TRIP钢，Mn的量通常小于2重量％，与最多2重量％的Si或Al联合。对于TWIP钢，Mn的量可高达25重量％，与Al或Si(最大3重量％)组合。
还可通过电沉积来施加金属涂层。在该方法中，将待涂覆的钢板浸入其中还浸入有一个或更多个可溶性阳极的电解质浴中，所述阳极包含与待施加至板表面的涂层相一致的金属或金属合金。向电解质浴施加电流引起制成一个或更多个阳极的金属或金属合金溶解，并且由此形成的离子沉积在钢板的表面上以形成金属或金属合金涂层。在进入电解浴之前，钢板必需经历酸洗步骤以移除表面上存在的金属氧化物。事实上，为了使电解工艺有效，介质必须一定是导体，如果待涂覆钢板的表面上存在金属氧化物，则不是这种情况。此外，金属氧化物的存在可影响沉积物的萌发和生长，并且因此导致涂层的粘附和质量问题(显微组织、密度等)。
还可通过真空沉积来施加金属涂层。真空沉积技术主要需要三个组成部分：
-源材，其构成或者包含待沉积的材料。该源材可以是例如真空蒸镀器的坩埚或溅射靶材。待沉积的材料必须以离子、原子或者原子团或分子团的形式离开该源材；
-基材，其相当于待涂覆的部分。使来源于源材的材料附着至基材以形成胚核(成核)，其逐渐成长(生长)并且产生基本有序的涂层；
-介质，其使源材与基材分离，并且是以气相转移材料现象的位置。
除其他方面之外，还根据用于形成气相的方式进行不同类型的真空沉积的区别。如果气相由化学反应或分子分解产生，则将该工艺称为CVD或化学气相沉积。另一方面，如果该气相通过纯物理现象(例如热蒸镀或离子溅射)产生，则将该工艺为物理气相沉积或PVD。PVD沉积工艺包括溅射、离子注入和真空蒸镀。
然而，不管所使用的真空沉积技术，其均需要准备表面以使待涂覆钢板的表面没有金属氧化物以保证金属涂层的适当粘附并且由此防止涂层层离的问题。
不管所使用的涂覆方法，钢带在涂覆之前的表面状况是最终涂层质量的重要因素。待涂覆钢板的表面上存在金属氧化物妨碍待施加涂层的适当粘附，并且可导致其中最终产品上没有涂层的区域或者与涂层层离有关的问题。这些金属氧化物在钢板表面上可以以连续膜的形式或者以不连续点的形式存在。金属氧化物还可在工艺的不同步骤期间形成，并且其组成根据制成所讨论板的钢的级别而变化。例如，该类氧化物包括铁氧化物FeO、Fe2O3，铝氧化物Al2O3以及MnSiOx或AlSiOx。
移除这些金属氧化物需要进行额外的加工步骤，即酸洗。在本说明书的剩余部分中，酸洗意指导致除去通过底层金属层氧化而形成的金属氧化物以使该金属层显现在表面上的任何方法，相比之下，例如擦亮方法尽管其也是除去金属氧化物的工艺，但是其仅旨在除去表面的金属氧化物层而不使下面的金属层暴露。
金属氧化物的这一移除可例如通过经由磁控破碎的真空酸洗(还称为蚀刻)来实现。该工艺包括在气体中在带材和辅助电极之间产生等离子体，使得可产生自由基和/或离子。在常规操作条件下，这些离子朝待酸洗带材的表面加速并将表面原子轰击掉，从而消除表面上存在的金属氧化物。该方法在很大程度上取决于待移除的金属氧化物层的厚度，并且取决于这些金属氧化物的组成，可产生电弧。因此，该工艺不稳定且不很稳健。此外，其为了获得良好结果而在生产线速度方面设置了严格限制，这造成生产率的问题。
还可通过使带材通过一个或更多个连续的强酸(例如盐酸或硫酸)浴来对其进行酸洗，所述强酸浴根据表面上金属氧化物的性质来选择并保持在约80℃至90℃的温度下。该工艺产生大量需要后续处理并且环境不友好的流出物。
此外，这种类型的酸洗造成控制所移除的金属氧化物的厚度以确保后续涂层的适当附着的问题。
最后，通过机械作用移除全部或部分的金属氧化物层是可能的，例如通过使用喷丸工艺，其中金属氧化物例如由于经充足动能喷射的小磨粒的多次冲击而得以移除。然而，这种类型的工艺直接冲击带材的表面并且还实施复杂。而且，这些工艺需要在特定条件(如惰性或还原性气氛)下工作例如以防止金属表面由于接触空气而再氧化。
发明内容
因此，本发明的一个目的是提供一种表面处理方法，该方法使能够改善后续涂层在基材上的附着并且不需要消除表面上存在的氧化物的步骤等。
为了这个目的，本发明提供了包括多个层的基材，其中至少一个层包含金属氧化物并且顶部上直接为金属涂层，所述金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述金属涂层自身顶部上直接为抗腐蚀涂层。
所述设置有多个层的基材还可具有下列特征，其单独或组合考虑：
所述基材还包括金属板，所述金属板的至少一个表面具有第一氧化物层，所述第一氧化物层顶部上直接为第一金属涂层，所述第一金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述第一金属涂层顶部上直接为第一抗腐蚀涂层，所述第一抗腐蚀涂层自身顶部上直接为第二氧化物层，所述第二氧化物层顶部上直接为第二金属涂层，所述第二金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述第二金属涂层自身顶部上直接为第二抗腐蚀涂层；
所述金属涂层由不锈钢组成，所述不锈钢含有10重量％至13重量％的镍、16重量％至18重量％的铬，剩余部分为铁和由制造工艺产生的可能杂质；
所述金属涂层由一个或更多个不锈钢层组成，所述不锈钢层含有0.02重量％碳、16重量％至18重量％铬、10.5重量％至13重量％镍、2重量％至2.5重量％钼、0.9重量％至1.3重量％硅、1.8重量％至2.2重量％锰，剩余部分为铁和由制造工艺产生的可能杂质；
所述金属涂层的厚度为2nm至15nm；
所述抗腐蚀涂层由选自锌、铝、铜、镁、钛、镍、铬、锰及其合金的金属组成；
所述抗腐蚀涂层由锌或锌合金组成；
所述抗腐蚀涂层由多个金属涂层子层组成；
至少一个抗腐蚀层位于氧化物层之下，并且与氧化物层直接接触；
所述基材还包括位于氧化物层之下的钢板；和/或
所述钢板是强度大于或等于450MPa的钢。
本发明提供了一种用于制造设置有多个层的基材的方法，其中通过选自真空沉积工艺和电沉积工艺的工艺来沉积金属涂层。
所述制造工艺可包括为磁控阴极粉碎法(magnetron cathode pulverizationprocess)的沉积工艺。
所述制造工艺还可包括通过选自真空沉积工艺和电沉积工艺的工艺来沉积抗腐蚀层。
本发明还提供了一种用于制备基材表面的方法。所述方法包括在没有预先酸洗氧化物层的情况下在所述氧化物层上沉积至少一个金属氧化物层，其中金属涂层包含至少8重量％的镍和至少10重量％的铬，其余部分为铁和由制造方法产生的杂质。
所述表面制备方法还可包括在金属涂层上沉积抗腐蚀涂层。
在下文更详细地阐述本发明的其他特征和优势。
附图说明
为了说明本发明，已进行了测试并且将特别地参考附图以非限制性实例的方式对其进行描述，在附图中：
图1是本发明的第一实施方案中的基材的示意图。
图2是本发明的第二实施方案中的基材的示意图。
图3是本发明的第三实施方案中的基材的示意图。
具体实施方式
图1至图3说明了本发明的不同实施方案。所表示的层厚度仅用于说明目的，并且不可以被视为是不同层按比例的表示。
对于图1至图3的全部，此处所用的术语“钢”包括所有已知级别的钢，并且可以是例如下列THR钢(非常高强度，通常在450MPa至900MPa)或UHR钢(超高强度，通常大于900MPa)级别的含有大量可氧化元素的钢中的一种：
-无间隙元素的钢(IF-无间隙)，其可含有高达0.1重量％的Ti；
-双相钢，例如DP 500钢直到DP 1200钢，其可含有与高达1重量％的Si、Cr和/或Al联合的高达3重量％的Mn；
-TRIP(相变诱发塑性)钢，例如TRIP 780，其含有例如约1.6重量％的Mn和1.5重量％的Si；
-含磷的TRIP或双相钢；
-TWIP(孪生诱发塑性)钢，具有高含量的Mn(通常为17重量％至25重量％)的钢；
-低密度钢，例如Fe-Al钢，其可含有例如高达10重量％的Al；
-不锈钢，其具有与其他合金元素(Si、Mn、Al等)联合的高含量的铬(通常为13重量％至35重量％)。
图1说明了根据本发明的设置有数个层的基材的第一实施方案。该基材包括钢板1，钢板1在其至少一个表面上具有氧化物层2。该层2在所讨论的钢表面1上可以是连续的或不连续的，并且包含来自以下的金属氧化物：铁氧化物、铬氧化物、锰氧化物、铝氧化物、硅氧化物或者一种或更多种含有钢合金元素的混合氧化物，例如Mn-Si或者Al-Si混合氧化物。例如，该金属氧化物层2的厚度通常可在3nm至约60nm变化，并且优选在3nm至约20nm变化。
因此，该氧化物层2不通过酸洗移除并且被金属涂层3覆盖，所述金属涂层3含有至少8重量％的镍和至少10重量％的铬，剩余部分包括铁、附加元素(例如碳、钼、硅、锰、磷或硫)和由制造工艺产生的杂质。该涂层3可以是例如不锈钢并且优选316不锈钢(16重量％至18重量％的Cr、10重量％至14重量％的Ni)。其厚度可为例如大于或等于2nm。该金属涂层3可通过任何已知的涂覆方法并且特别地例如通过磁控阴极粉碎或者通过电沉积来施加。
通过磁控阴极粉碎(其通常称为“溅射”)在基材上形成涂层的方法是在其中已建立真空并且其中安装有靶材和基材的封闭室中进行的，所述基材位于靶材的对面并与后者相距一定的距离。所述靶材具有经调整朝向待在其上形成涂层的基材面的表面层。该表面层含有构成待通过溅射沉积在基材上的涂层的至少一种元素。
所述室含有惰性气体(例如氩)的等离子体。
在一种溅射方法中，原子从表面层的表面喷射出，并且以涂层的形式沉积在基材上。施加负电压至靶材并且因此至待喷射的表面层材料。结果产生生成由离子、电子和惰性气体离子形成的等离子体的放电。带正电荷的离子朝处于负电势的靶材加速，使得其以足够的能量到达靶材以引起原子从表面层喷射出。这些脱离的原子向基材移动，并以可再现且基本均匀的涂层的形式沉积在基材上，所述涂层良好地附着至基材面上。
在该第一实施方案中，Fe-Ni-Cr金属涂层3被抗腐蚀金属涂层4覆盖。该抗腐蚀金属涂层4可包含例如纯锌(包含由制造工艺产生的可能杂质)，或者锌合金，例如Zn-Al、Zn-Al-Mg、Zn-Mg、Zn-Fe或Zn-Ni。例如，其还可包含铝、铜、镁、钛、镍、铬、纯锰(包含由制造方法产生的可能杂质)或其合金，例如Al-Si或Mg-Al。该抗腐蚀金属涂层4可通过任何已知的涂覆方法来施加，例如，如声速气相喷气沉积工艺(也称为JVD(喷气气相沉积，Jet VaporDeposition))、电子枪沉积法或等离子体辅助蒸发，其还称为SIP(自感应镀覆，Self-Induced Plating)并且特别地描述于专利EP 0780486中。
JVD法是真空沉积方法，其中通过在真空室中感应加热含有涂层金属浴的坩埚来产生金属蒸气。蒸气通过将其运输至出口孔的导管从坩埚逃选出(其为优选地经校准的)以形成指向待涂覆基材的表面的声速喷气。
图2说明了本发明的第二实施方案。在该实施方案中，基材如图1中包括钢板21。例如，该钢板21涂覆有基于铝的抗腐蚀涂层25，例如，如铝-硅涂层(10重量％至12重量％的Si)。例如，该铝基涂层25可通过热浸来沉积并且厚度可为10μm至30μm。该基于铝的涂层25顶部上为金属氧化物层22。该层22在所讨论的铝基涂层25的表面上可以是连续的或不连续的并且可包含铝氧化物和/或混合铝氧化物，例如Al-Si氧化物。该金属氧化物层22的厚度通常可在3nm至约60nm变化，优选地在3nm至约20nm变化。
因此，该氧化物层22不通过酸洗移除并且被金属涂层23覆盖，所述金属涂层23包含至少8重量％的镍和至少10重量％的铬，剩余部分包括铁、以上公开的附加元素和由制造工艺产生的杂质。该金属涂层23可为例如不锈钢并且优选地不锈钢316(16重量％至18重量％的Cr、10重量％至14重量％的Ni)。该金属涂层23可通过任何已知的涂覆方法施加，并且厚度可为例如大于或等于2nm。
在该第二实施方案中，该金属涂层23顶部上为抗腐蚀金属涂层24，所述抗腐蚀金属涂层24选自参照第一实施方案所描述的抗腐蚀金属涂层。例如，该抗腐蚀金属涂层24可通过任何已知的涂覆工艺(例如真空法或热浸法)来施加，任选地随后进行后扩散处理。
可考虑的涂层例如包括涂覆有基于Al-Si的涂层25的钢层21，在此该涂层25顶部上为由Al-Si混合氧化物构成的氧化物层22，氧化物层22涂覆有不锈钢316层23，该不锈钢层23涂覆有Zn-Mg合金抗腐蚀涂层24。
图3说明了本发明的第三实施方案。在该第三实施方案中，基材包括(如第一实施方案中)在其至少一个表面上具有第一氧化物层32的钢板31。该第一层32在钢31的表面上可以是连续的或不连续的并且例如含有来自以下的金属氧化物：例如，铁氧化物、铬氧化物、锰氧化物、铝氧化物、硅氧化物或者含有钢的合金元素的混合氧化物(例如Al-Si或Mn-Si混合氧化物)之一。该第一金属氧化物层32的厚度通常可在例如3nm至约60nm变化，并且优选地在3nm至约20nm变化。
因此，如在第一实施方案中，该氧化物层32不通过酸洗移除并且被金属涂层33覆盖，所述金属涂层33包含至少8重量％的镍和至少10重量％的铬，在此剩余部分包括铁、以上公开的附加元素和由制造工艺产生的杂质。例如，该涂层33可为不锈钢并且优选地不锈钢316(16重量％至18重量％的Cr、10重量％至14重量％的Ni)。例如，该金属涂层33的厚度可为大于或等于2nm。该金属涂层33可以通过任何已知的涂覆工艺施加，并且特别地例如通过磁控阴极粉碎或者通过电沉积施加。在该实施方案中，Fe-Ni-Cr金属涂层33被第一抗腐蚀金属涂层34覆盖。该第一抗腐蚀金属涂层34可包含例如纯锌(含有由制造工艺产生的可能杂质)，或者锌合金，例如Zn-Al、Zn-Al-Mg、Zn-Mg或Zn-Ni。例如，其还可包含铝、铜、镁、钛、镍、铬、纯锰(含有由制造工艺产生的可能杂质)或其合金，例如如Al-Si或Mg-Al。例如，该第一抗腐蚀金属涂层34可通过任何已知的涂覆方法例如在真空中进行的工艺或热浸法工艺。
在该第三实施方案中，该第一抗腐蚀金属涂层34顶部上为第二金属氧化物层36。该层36在抗腐蚀金属涂层34的表面上可以是连续的或不连续的并且可包含其组成取决于抗腐蚀金属涂层34的组成材料的氧化物。例如，这些氧化物可以是锌氧化物、铝氧化物或者Al-Si、Zn-Mg或Zn-Al混合氧化物。该金属氧化物层36的厚度通常可在例如3nm至约60nm变化，并且优选地在3nm至约20nm变化。
该第二氧化物层36不通过酸洗消除并且被金属涂层37覆盖，所述金属涂层37包含至少8重量％的镍和至少10重量％的铬，剩余部分是铁、以上公开的附加元素和由制造工艺产生的杂质。该涂层37可以是例如不锈钢并且优选不锈钢316(16重量％至18重量％的Cr、10重量％至14重量％的Ni)。该金属涂层37可通过任何已知的涂覆工艺来施加，并且可以但并非必须与金属涂层33相同。该金属涂层37的厚度可为例如大于或等于2nm。
在该第三实施方案中，该金属涂层37顶部上为抗腐蚀金属涂层38，所述抗腐蚀金属涂层38选自参照第一实施方案所描述的抗腐蚀金属涂层。该抗腐蚀金属涂层38可通过任何已知的涂覆方法(例如，如真空法或热浸法)来施加，任选地随后进行后扩散处理。该抗腐蚀金属涂层38可以但并非必须与第一抗腐蚀金属涂层34相同。
例如，可以考虑：钢层31、第一铁氧化物层32、由不锈钢316组成的第一金属涂层33、由Al-Si合金组成的第一抗腐蚀金属涂层34、由Al-Si混合氧化物组成的第二氧化物层36、由不锈钢316组成的第二金属涂层37以及由Zn-Al-Mg合金组成的第二抗腐蚀金属涂层38。
现在，将基于测试对本发明进行阐述，所述测试仅仅是为了说明目的而进行并非旨在限制。
测试
验收标准
T-弯曲测试
该测试的目的是通过以180°的角度弯曲经涂覆板来确定涂层的附着。所施加的弯曲半径等于所使用基材的厚度的两倍(其相当于“2T”弯曲)。通过施加胶带来证明涂层的附着。如果在移除胶带之后涂层仍留在测试板上并且不出现在胶带上，则判断测试结果是肯定的。
用于在下述测试中进行该测试的胶带是商业化的胶带TESA4104。
杯测试
该方法由在形成杯期间进行冲压测试组成。材料以及金属涂层的这一变形确定与基材上金属沉积物的附着有关的潜在问题。附着的损失(或粉化)以在进行冲压前后称重的杯重量的减少来表示(以g/m2计)。
Daimler弯曲
该测试的第一阶段由对经涂覆的钢板施加冲头并测量观察到大于或等于30kN的强度减小时的弯曲角度组成。这一强度下降对应于基材的破裂。然后，金属涂层的附着力测试由以接近但小于该破裂点的角度来弯曲经涂覆板并通过施加粘合层来检测锌的附着组成。如果在移除胶带之后锌涂层仍留在板上并且不出现在胶带上，则判断测试结果是肯定的。
用于进行下述测试的胶带的粘合强度为400N/m至460N/m，例如3M595。
测试-1-附着力
对于所有的测试，使用的不锈钢316L的组成均为0.02％C、16％-18％Cr、10.5％-13％Ni、2％-2.5％Mo、1％Si、2％Mn、0.04％P、0.03％S。百分比是重量百分比，剩余部分为铁和由制造产生的可能杂质。
制备ArcelorMittal所出售类型的DP1180钢板的一系列8个试样。用于试样的钢的精确组成为0.15％C、1.9％Mn、0.2％Si、0.2％Cr和0.013％Ti。百分比是重量百分比，剩余部分为铁和由制造产生的可能杂质。
使所有的试样经受下述步骤：
-通过使钢板通过保持在50℃以下温度的含有甲酸HCOOH或硫酸H2SO4的浴来擦亮钢板。该步骤的目的是移除FeO型铁氧化物的上层，但其不移除下面的氧化物层；
-用水冲洗；
-干燥以移除在冲洗步骤期间吸附的水；
-将带材插入具有P＜10-3mbar压力的真空室中；
-真空蒸镀沉积5μm的锌层。
现有技术所述类型的试样2和6在该干燥步骤之后经受蚀刻步骤以移除钢板表面上存在的金属氧化物。
然后，根据本发明优选实施方案的试样1、5和9在插入到真空室中的步骤之后经受以下步骤：其中通过磁控阴极粉碎(参见上文对该方法的描述)对其涂覆10nm的不锈钢316L层。
试样4和8在插入到真空室中之后经受以下步骤：其中通过磁控阴极粉碎(参见上文对该方法的描述)对其涂覆10nm的钛层。
试样9不经受擦亮步骤。
各试样的特征示于下表中：
试样编号 擦亮 蚀刻 涂覆
1＊ H2SO4 否 不锈钢316
2 H2SO4 是 否
3 H2SO4 否 否
4 H2SO4 否 Ti
5＊ HCOOH 否 不锈钢316
6 HCOOH 是 否
7 HCOOH 否 否
8 HCOOH 否 Ti
9＊ 无 否 不锈钢316
＊根据本发明的试样
然后，使所有的这些试样经受上述T-弯曲测试和杯测试。
“杯测试”的结果表示为与杯的初始锌重量相比锌的损失百分比。
结果示于下表中。
现有技术所述的试样2和6对两种测试均取得肯定结果。该结果并不令人惊讶，因为现有技术的这两个试样经受了蚀刻步骤，蚀刻步骤使可能移除表面上存在的金属氧化物并且因此保证了在涂覆之前的良好表面状况以获得锌涂层的适当附着。
对于根据本发明的试样1、5和9，两种测试是确定的并且表明锌的良好附着，其等同于用蚀刻步骤可获得的附着，不管用于擦亮的酸并且甚至在无预擦亮步骤下也如此(试样9)。
此外，具有钛涂层替代不锈钢316涂层的试样4和8由于锌涂层的附着不足而在所进行的两种测试中未提供任何确定的结果。
测试-2
用不同级别的钢和不同的工艺参数制备了一系列12个试样。该组试样根据本发明制造并且经受以下加工步骤：
-碱脱脂以消除钢板表面上存在的潜在有机残留物。该脱脂通过将带材浸渍于保持在60℃的碱性溶液的浴中进行。浸渍时间以及用于各试样的浴特征示于下表中；
-用水冲洗；
-干燥以移除在冲洗步骤期间吸附的水；
-将带材插入P＜10-3mbar压力的真空室中；
-将带材预加热至约120℃的温度；
-通过磁控阴极粉碎(参见上文对该方法的描述)来沉积不锈钢316L层。该不锈钢316L层的厚度因试样而变化并且示于下表中；
-通过JVD(参见上文对该工艺的描述)来沉积锌层。
各试样的特征在下表中列出：
NovacleanTM和是Henkel出售的产品。Gardoclean S5183由Chemetall出售。
试样10至12以ArcelorMittal出售的DP1180钢板起始制备。用于试样的钢的精确组成为0.15％C、1.9％Mn、0.2％Si、0.2％Cr和0.013％Ti。百分比为重量百分比，剩余部分为铁和由制造产生的可能杂质。钢板表面上存在的大部分金属氧化物是铬氧化物和铁氧化物。被氧化的钢板涂覆有厚度因试样而变化的不锈钢316L层，并且然后涂覆有厚度为7.5μm至8μm的锌层。
试样13至15以ArcelorMittal出售的MS1500钢板起始来制备。MS代表马氏体钢。用于试样的钢的精确组成为0.225％C、1.75％Mn、0.25％Si、0.2％Cr、0.035％Ti。百分比为重量百分比，剩余部分为铁和由制造产生的可能杂质。钢板表面上存在的大部分金属氧化物是铁氧化物。被氧化的钢板涂覆有厚度因试样而变化的不锈钢316L层，并且然后涂覆有厚度为7.5μm至8μm的锌层。
试样16至18以ArcelorMittal出售的Trip Dual 1200钢板起始来制备。用于试样的钢的精确组成为0.2％C、2.2％Mn、1.5％Si和0.2％Cr。百分比为重量百分比，剩余部分为铁和由制造产生的可能杂质。钢板表面上存在的大部分金属氧化物是混合的锰和硅氧化物。被氧化的钢板涂覆有厚度因试样而变化的不锈钢316L层，并且然后涂覆有厚度为7.5μm至8μm的锌层。
试样19和20以AS150钢板起始来制备。所讨论的钢是涂覆有150g/m2的层(基于铝和硅的涂层)的钢。用于这些试样的涂层的精确组成为90％Al、10％Si。百分比表示为按重量计。钢板表面上存在的大部分金属氧化物是混合的铝和硅氧化物。被氧化的钢板涂覆有厚度因试样而变化的不锈钢316L层，接着是涂覆有厚度为4μm至5μm的锌层。
然后，使该组试样经受上述T-弯曲测试和Daimler弯曲测试。
结果示于下表中：
这些结果证明，对于根据本发明一个优选实施方案的基材，不管表面上存在的金属氧化物的组成或用于脱脂的溶液的pH，锌涂层是附着的。此外，以施加厚度为2.5nm的不锈钢316开始，锌涂层的附着力测试的结果是肯定的。
测试-3
以钢起始制备一系列2个试样。使这2个试样经受下列加工步骤：
-碱脱脂以移除钢板表面上可存在的任何潜在有机残留物。该脱脂通过将带材浸渍于保持在60℃的碱性溶液的浴中进行。浸渍时间以及用于各试样的浴的特征示于下表中；
-用水冲洗；
-干燥以移除在冲洗步骤期间吸附的水；
-将带材插入P＜10-3mbar压力的真空室中；
-沉积金属涂层。
现有技术所述的试样31在干燥步骤之后经受蚀刻步骤以移除钢板表面上存在的金属氧化物。
本发明所要求保护的试样32在插入到真空室中的步骤之后随后经受其中通过磁控阴极粉碎(参见上文对该工艺的描述)对其涂覆不锈钢316L层的步骤。
该涂层的厚度为10nm。
在蚀刻步骤之后或者在沉积不锈钢316L层的步骤之后，通过磁控阴极粉碎对试样涂覆5nm的铝层。
各试样的特征示于下表中：
＊如本发明所要求保护的试样。
然后，通过向平面试样施加胶带并随后移除来测试各试样的顶部上金属涂层的附着力。使用的胶带的粘合强度为400N/m至460N/m，例如3M595。
如果当将胶带移除时涂层仍留在试样表面上且不出现在胶带上，则结果是肯定的。对于全部测试试样，胶带在测试之后均不含任何涂层，这意味着涂层是附着的。这一结果对于现有技术的试样31是期望的，因为其已经受了移除钢板表面上存在的金属氧化物的蚀刻步骤，而不论其是否经涂覆。另一方面，这些结果显示该移除氧化物的步骤可通过在被氧化表面上直接沉积不锈钢316L层来消除，因为对于本发明一个优选实施方案的结构，粘附测试的结果也是肯定的。

Claims (16)

1.一种设置有多个层的基材，其中至少一个层包含金属氧化物并且顶部上直接为金属涂层，所述金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述金属涂层自身顶部上直接为抗腐蚀涂层。
2.如权利要求1中所述的设置有多个层的基材，包括金属板，所述金属板的至少一个表面具有第一氧化物层，所述第一氧化物层顶部上直接为第一金属涂层，所述第一金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述第一金属涂层自身顶部上直接为第一抗腐蚀涂层，所述第一抗腐蚀涂层自身顶部上直接为第二氧化物层，所述第二氧化物层顶部上直接为第二金属涂层，所述第二金属涂层包含至少8重量％的镍和至少10重量％的铬，剩余部分为铁、附加元素和由制造工艺产生的杂质，所述第二金属涂层自身顶部上直接为第二抗腐蚀涂层。
3.如权利要求1或2中所述的设置有多个层的基材，其中所述金属涂层包含不锈钢，所述不锈钢包含10重量％至13重量％的镍、16重量％至18重量％的铬，剩余部分为铁和由制造工艺产生的可能杂质。
4.如权利要求1至3中所述的设置有多个层的基材，其中所述金属涂层包括一个或更多个不锈钢层，所述不锈钢层包含0.02重量％的碳、16重量％至18重量％的铬、10.5重量％至13重量％的镍、2重量％至2.5重量％的钼、0.9重量％至1.3重量％的硅、1.8重量％至2.2重量％的锰，剩余部分为铁和由制造工艺产生的可能杂质。
5.如前述权利要求中任一项所述的设置有多个层的基材，其中所述金属涂层的厚度为2nm至15nm。
6.如前述权利要求中任一项所述的设置有多个层的基材，其中所述抗腐蚀涂层包含选自以下的金属：锌、铝、铜、镁、钛、镍、铬、锰及其合金。
7.如权利要求6中所述的设置有多个层的基材，其中所述抗腐蚀涂层包含锌或锌合金。
8.如前述权利要求中任一项所述的设置有多个层的基材，其中所述抗腐蚀涂层包括多个金属涂层子层。
9.如前述权利要求中任一项所述的设置有多个层的基材，其中至少一个抗腐蚀层位于所述氧化物层之下并且直接接触所述氧化物层。
10.如前述权利要求中任一项所述的设置有多个层的基材，包括位于所述氧化物层之下的钢板。
11.如权利要求10中所述的设置有多个层的基材，其中所述钢板是强度大于或等于450MPa的钢。
12.一种用于制造如权利要求1至11中任一项所述的设置有多个层的基材的方法，其中通过选自真空沉积工艺和电沉积工艺的工艺来沉积金属涂层。
13.如权利要求12中所述的方法，其中沉积工艺是磁控阴极粉碎法。
14.如权利要求12或13中所述的用于制造设置有多个层的基材的方法，其中通过选自真空沉积工艺和电沉积工艺的工艺来沉积抗腐蚀层。
15.一种用于制备包括至少一个金属氧化物层的基材的表面的方法，其中在没有预先酸洗所述氧化物层的情况下在所述氧化物层上沉积金属涂层，所述金属涂层包含至少8重量％的镍和至少10重量％的铬，其余部分为铁和由制造方法产生的杂质。
16.如权利要求15中所述的方法，其中在所述金属涂层上沉积抗腐蚀涂层。
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