CN107208241B - 将金属保护镀层施加到钢产品的表面上的方法 - Google Patents

将金属保护镀层施加到钢产品的表面上的方法 Download PDF

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CN107208241B
CN107208241B CN201580075062.1A CN201580075062A CN107208241B CN 107208241 B CN107208241 B CN 107208241B CN 201580075062 A CN201580075062 A CN 201580075062A CN 107208241 B CN107208241 B CN 107208241B
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coating
hot dip
steel product
protective coating
dip coating
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CN107208241A (zh
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马丁·诺登
英戈·克卢佩尔
米罗斯瓦夫·吉察
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ThyssenKrupp Steel Europe AG
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    • 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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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
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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
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    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
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    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
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Abstract

本发明涉及一种用于将金属保护镀层施加到钢产品的表面上的方法，在该方法中，至少一个其它表面没有该金属保护镀层，其中该金属保护镀层的施加通过热浸镀在热浸镀浴中进行并且在热浸镀之前在不需要金属保护镀层的表面上设置一层由SiO2组成的预涂层，该预涂层在进行热浸镀时阻止金属保护镀层附着在相关表面上。该根据本发明的方法实现了，在最小的成本和优化的资源保护下，在钢产品的至少一个特定表面上通过热浸镀设置一层金属保护镀层，并且保持该扁钢产品的至少一个其他表面没有该金属保护镀层。实现的方法是，由非结晶二氧化硅组成的厚度为0.5‑500nm的镀层作为预涂层从气相中沉积到钢产品的需要保持没有金属保护镀层的表面上。

Description

将金属保护镀层施加到钢产品的表面上的方法
技术领域
本发明涉及一种用于将金属保护镀层施加到钢产品的表面上的方法，在该方法中，至少一个其它表面没有该金属保护镀层，其中该金属保护镀层的施加通过在热浸镀浴中的热浸镀进行并且在热浸镀之前在没有金属保护镀层的表面上设置一层由SiO2组成的预涂层，该预涂层在进行热浸镀时阻止金属保护镀层附着在相关表面上。
背景技术
用金属保护镀层进行涂覆是一种有效的保护由于其组成而有腐蚀危险的钢产品不受腐蚀的方法。对于许多应用目的来说，涉及经济和资源保护的生产和加工时，仅在实际使用中遭受腐蚀侵害的表面或者表面区段上设置保护层已经足够也是所期望的。
经济的，在大规模实践中有效的将金属保护层施加到钢产品上的方法是热浸镀。
进行热浸镀时，待涂覆的产品单件地或者连续通过热浸镀浴，该热浸镀浴由熔融的，组成该保护镀层的金属或者由熔融的金属合金构成。通常在经过热浸镀浴的流程之前设置热处理。其目的在于，将待涂覆的钢制基板分别如此预处理和活化其表面，使得一方面得到优化的材料特性，另一方面保证镀层在钢制基板上最优的浸润和附着。
尤其有效的是以锌或者铝为基的保护镀层，这些镀层除了其主组分以外分别还能含有其它的合金元素来分别得到想要的镀层特性。
扁钢产品典型地指由钢制基板形成的辊轧产品，如钢板或者带、由此得到的裁剪品或者扁条以及类似产品，这些扁钢产品上在大量生产的框架内能够通过在连续过程中进行的热浸镀工艺经济地设置防腐蚀的金属镀层。由扁钢产品形成的或者组成的、在其生产后需设置保护层的钢组件则与此相反地通常通过逐件浸入各个热浸镀浴中来进行热浸镀。在虽然应用热浸镀，但是只有钢产品的特定的面上需要设置保护层的情况下，就必须这样分别准备不需要镀层的面，即镀层金属在浸入到热浸镀浴中时不会附着在此处。
在DE2609968A1中为此建议，在对扁钢产品进行锌保护层热浸镀之前，在该扁钢产品不需要镀锌的面上涂覆硅树脂。在涂覆硅树脂之后，将该扁钢产品于氧化气氛中升温至300-800℃，以将该硅树脂层烧至钢制基板中。该烧制过程的目的是在无需镀层的面上构建二氧化硅覆盖层。然后将这样预涂层过的扁钢产品在还原气氛中进行热处理，然后引导至热浸锌镀浴中，此处对没有预涂层的表面进行镀锌。这里，成功的单面镀锌的决定条件是，在还原气氛中退火时在扁钢产品无需镀层的表面上涂覆足够厚的二氧化硅膜，该二氧化硅膜防止无需镀层的表面活化并同时构建无需镀层的表面和熔融的镀层金属接触的屏障。为了保证二氧化硅膜的足够厚度，将硅树脂涂覆到钢制基板上的涂覆重量在0.5-50g/m2范围内，其中在已知方法的实际测试中，涂覆重量设定在0.7-47g/m2。
因为尽管在已知的方法中采取了这些措施，在实际中依旧不能避免不需要镀层的面被熔融的镀层金属所浸润，已知方法设定，在离开锌浴之后刷净钢带涂有硅树脂层的面，以便一方面去除可能存在的镀层金属的积聚，另一方面去除该硅树脂镀层本身。
发明内容
在前述现有技术的背景下产生了目的，即开发一种方法，该方法能够在最小的成本和优化的资源保护下，在扁钢产品的至少一个特定表面上通过热浸镀设置一层金属保护镀层，并且保持扁钢产品的至少一个其他的表面没有该金属保护镀层。
该目的通过在权利要求1中给出的方法来解决。
本发明有利的设计方案在从属权利要求中给出并接下来与总体的发明思想进行细节说明。
与开始说明的现有技术一致，在根据本发明的方法中金属保护镀层到钢产品表面的涂覆也是通过在热浸镀浴中的热浸镀完成的，该方法中至少一个其它表面没有该金属保护镀层，并且在热浸镀之前在不需要金属保护镀层的表面上设置一层由二氧化硅组成的预涂层，该预涂层在进行热浸镀时阻止金属保护镀层附着在相关表面上。
根据本发明，由非结晶二氧化硅组成的厚度为0.5-500nm的镀层作为预涂层从气相中沉积到需要保持没有金属保护镀层的钢产品表面上。
由此，本发明提供了用于生产单面热浸镀防腐蚀的扁钢产品的方法，该方法中无需使用硅树脂，利用该树脂通过特殊的烧制和氧化步骤在钢产品不需要金属保护镀层的表面上形成相对较厚的二氧化硅膜。本发明取而代之设定，通过应用合适的沉积方法，无需中间载体，直接在需要保护而在热浸镀时不与镀层熔融物接触的钢产品表面上沉积一层薄的二氧化硅层。为了该目的可以在各个相应的沉积过程中使用硅有机化合物，然而这些硅有机化合物并不是在开始说明的现有技术中应用的硅树脂。
因为该含有硅的形成预涂层的化合物直接沉积在钢制基板上，在根据本发明的方法中省去了烧制步骤。此外，与二氧化硅层从液相中形成的镀层方式相比，根据本发明设定的有针对性的二氧化硅层从气相中的沉积具有以下优点，即从气相中的沉积不受限于复杂昂贵的过程池，需要明显更少的物质投入量并且实现了纳米范围内的最小化的层厚度。在使用本方法时，所有的这些都使得废料的产生明显减少并且由此使得对环境的负担与已知方法相比明显减轻。
对钢产品无需金属保护镀层的面的预涂层能够利用已知的并在实践当中证明有效的方法进行。根据各个初始产品和进行后续的加工步骤的方式，这里适宜的是，预涂层逐件地在不连续的工艺流程中沉积在钢产品上或者在连续的工艺流程中进行沉积。例如当钢产品是扁钢产品，尤其是钢带时，在连续工艺流程中将预涂层沉积在各个不需要镀层的面上。当预涂层整合到从预涂层到通过热浸镀浴都在连续过程中进行的热浸镀过程中时，这尤其适用。
根据本发明设定的预涂层沉积能够比如利用火焰裂解来进行。通过火焰裂解产生的层通常作为无机基板和有机镀层之间的增附剂，尤其是金属基板和有机镀层之间。如果根据本发明产生的预涂层利用火焰裂解涂覆到各个相应的钢制基板上，那么可以出乎意料地发现，尽管层厚度非常小，钢制基板各个无需保护镀层的面也没有被浸润。火焰裂解工艺比如在Bernhard Schinkinger博士发表在URLhttp://www-brs.ub.ruhr-uni-bochum.de/netahtml/HSS/Diss/SchinkingerBernhard/diss.pdf(也可参见URL：http://www-brs.ub.ruhr-uni-bochum.de/netahtml/HSS/Diss/SchinkingerBernhard/)之下的博士论文“对镀锌钢表面的薄二氧化硅和有机硅层沉积的层分析和电化学研究”中有详细的说明。
涉及到本发明，对于镀层能够利用火焰裂解将有机硅前驱物以10-5000ml/min的流量和-50℃至+100℃的蒸发器温度(比如六甲基二甲硅醚“HMDSO”)在可燃气体或气体混合物(比如空气/丙烷或者空气/丁烷)中进行火焰裂解，该气体由此沉积到引导通过火焰的板上。通过改变燃烧器间隔、镀层速度、气体混合和组成以及燃烧器的构造能够改变沉积层的厚度和特性，以获得最优的特性。为此，比如燃烧器间隔能够在0.5-10cm范围内，镀层速度能够在1-300m/min范围内变化。能够使用丙烷或者丁烷作为可燃气体。如果在应用了这些可燃气体中的一种的情况下使用由气体和空气组成的可燃气体混合物，那么该可燃气体在该气体混合物中的比例可以是10-100体积％。也就是说，只使用纯的气体而没有空气掺杂的可能性在本发明的意义中也包含在“可燃气体混合物”概念中。通过在火焰裂解中的燃烧器的构造和数量也能够对镀层效果产生积极影响。在流程中进行的火焰裂解当中，在待镀层的钢制基板流程的方向上在一列中连续设置最多10个燃烧器是有利的。由于良好的附着特性，没有必要对钢制基板进行预处理。
对于根据本发明所设定的预涂层的沉积，也可以使用已知的，现有技术中提供的化学沉积方法(CVD)或者物理沉积方法(PVD)(“CVD”＝化学气相沉积(Chemical VapourDeposition)；“PVD”＝物理气相沉积(Physical Vapour Deposition))。
在实际测试中有效的是利用空心阴极辉光放电沉积根据本发明设定的预涂层。通过这种在实际中也被称为“PE-CVD”的方法能够生产紧凑的含硅层-所谓的等离子体聚合物层(“PP”)。在SHC过程中，将由载体气体(比如氧气和氩气的混合物)和有机硅先驱物构成的混合物在低压等离子体中分解并沉积在板上以进行镀层。该过程的详细解释在KrasimirNikolov博士的博士论文“对高效率低压中在钢质薄板上依托等离子体的沉积的研究”，Shaker出版社有限责任公司，2008年3月，ISBN 978-3-8322-7068-1中能找到。这种处理方法的一个优点是由于降低的工作压力而明显更少的气体用量。这里可能的是，通过改变镀层参数，比如接入的电功率、气体组成、气体流速，来优化沉积层的厚度和特性。在实际应用的镀层设备中，接入电功率为0.3kW。将40sccm氩气混入400sccm氧气中作为载体气体并且将40sccm HMDSO混入这些载体气体中作为先驱物。
由于其高的热稳定性，该根据本发明沉积的预涂层在热浸镀之后依旧存在于钢产品不需要保护镀层的面上。根据钢产品的各个应用目的，该预涂层可以保留在不需要设置金属镀层的面上。该预涂层在其位置上也同样起到防腐蚀的作用并且在设置有根据本发明的预涂层的面需要喷漆或者以其它方式进行有机镀层的情况下构建附着基底，通过该附着基底各个镀层在钢制基板上的附着得到改善。
与此相反，如果需在热浸镀之后将该预涂层从钢产品保持没有镀层的面上去除，可以使用已知的机械方法，如刷去，或者化学方法，如利用液体酸根据传统酸洗实施的处理。
利用根据本发明的方法能够可靠地达到在预涂层最小厚度下阻止在热浸镀时不需要保护镀层的面被热浸镀浴的熔融物浸润。出乎意料地发现，根据本发明由气相沉积到钢制基板的预涂层虽然很薄，但是依旧非常致密，可靠地防止熔融物附着在不需要镀层的面上。当预涂层的厚度限制在200nm，尤其是100nm，这种效果甚至更加可以保证，其中已经证明，厚度为至少2nm，尤其是至少10nm时尤其有效。
根据本发明得到的并且由气相沉积在各个钢产品不需要金属保护镀层的面上的预涂层热稳定性好，通过其预涂覆的钢产品能够毫无问题地经过通常为准备热浸镀而设定的热处理步骤。
由此，在涂覆预涂层之后以及经过热浸镀浴之前，钢产品能够在700-900℃的退火温度下，在退火气氛中进行6-300s的连续退火，该退火气氛包含0.5-10体积％的H2，尤其是1-5体积％的H2，其余为氮气和不可避免的杂质，其露点为-50℃至-10℃，尤其是-45℃至-5℃。将该钢产品分别加热至退火温度的加热速率在这里通常为0.5-35K/s。
为了继续优化需设置镀层的面有关在接下来的热浸镀步骤中涂覆的镀层在钢制基板上的附着方面的性能，能够对各个钢产品在退火之后以及涂覆热浸镀层之前进行过时效处理，在该过时效处理中该钢产品在400-520℃温度范围内保持6-180s。
为了进入热浸镀浴，可以最后将该钢产品升温到入浴温度，该温度位于下限为热浸镀浴温度-30℃，上限温度为热浸镀浴温度+30℃的范围内。
通过热浸镀在各个钢制基板上产生的保护镀层的典型层厚度为7.5μm±3.5μm。
根据本发明的方法尤其适用于扁钢产品的加工，这些扁钢产品在连续过程中进行热浸镀。“扁钢产品”这一概念包括所有长度远大于厚度的辊轧产品。如前面提到的，这包括钢带和钢板以及由此得到的裁剪品或者扁条。这里，本发明的一个特殊优点在于，扁钢产品能够作为热带材或者在冷轧后在轧制状态下用根据本发明的方法进行处理。
根据本发明待设置有金属保护镀层的钢产品尤其能够来自于薄板。这里指的是能够在冷轧或者热轧状态下冷压成型为组件的厚度小于3mm的钢带或者钢板。关于通常设置作为用于冷压成型的薄板的、所讨论类型的扁钢产品钢产品的总览在DIN EN 10130中给出。特别地，适合作为根据本发明加工的钢产品的钢制基板的钢可以总结为一个合金配方，根据该配方，相关的钢组成为(以重量％表示)：最多16％的Mn，最多3％的Al，最多2％的Si，最多0.3％的C，最多0.5％的Ti，最多1％的Ni，最多0.5％的Nb和最多2％的Cr，其余为铁和不可避免的杂质。
尤其当需要通过热浸镀用由锌或者锌合金组成的保护涂层为钢产品镀层以防止腐蚀时，该效果会显现。通常这种Zn涂层包含最多5重量％的Al，最多2.0重量％的Mg，最多0.2重量％的Fe和总的最多10重量％的其它组分，如Mn，Si等，这些组分以已知方式添加至Zn涂层并且作用是调整该涂层特性，其余为锌和受限于生产而不可避免的杂质。
根据本发明涂覆的金属保护镀层的典型层厚度在3-30μm范围内。
若这里给出金属合金的含量数据，只要没有明确给出其它说明，那么这些数据分别都基于重量。这里，在可能情况下给出的关于某种气氛组成的数据分别基于该气氛的体积，只要没有明确给出其它说明。
具体实施方式
接下来借助于实施例进一步说明本发明。
一共给出了八种钢带试样P1-P8，这些试样由具有在表3中给出的组成的钢制成。
应分别在试样P1-P8的一个面的表面上设置Zn保护镀层。与此相对，这些试样上与该需要设置Zn保护镀层的面处于相对位置的面的表面则保持没有金属保护镀层。
通过火焰裂解在大气压下在试样P1-P4的不需要设置该保护镀层的表面上沉积一个SiO2预涂层。为此，在火焰裂解设备的硅烷蒸发器中，在40℃下蒸发六甲基二甲硅醚(“HMDSO”)作为前驱物。蒸发后的HMDSO以550ml/min的体积流量进入由燃烧器通过燃烧由丙烷和空气以1：10的体积比组成的气体混合物引发的，5cm宽的燃烧火焰中，通过燃烧热而热裂解并且沉积到试样P1-P4以30m/min的运输速度引导通过燃烧器平面之下的，待设置SiO2预涂层的表面上。
试样P1-P4进行的通过火焰裂解设备的流程的数量Z，各个由此得到的SiO2预涂层的层厚度SD和分别达到的SiO2预涂层的涂覆重量AG在表1中给出。
与此相反，对于试样P5-P8则在PE-CVD设备中在不需要镀层的表面上沉积SiO2预涂层。为此，在60℃下蒸发的HMDSO以40标准立方厘米每分钟(“sccm”)的体积流量与作为载体气体的，同样也以40sccm体积流量引入的氩气混合，并且在添加以400sccm的体积流量引入的氧气的情况下在各个表面上沉积。该PE-CVD设备的电功率为0.3kW，频率为350kHz。能够达到4nm/s的最大沉积率。
各次进行镀层的时间TB，各个达到的SiO2预涂层的层厚度SD和分别达到的SiO2预涂层的涂覆重量AG在表2中给出。
在预涂层沉积后，试样P1-P8在连续过程中进行热处理，在该热处理中这些试样首先以10K/s±1K/s的加热速率加热到800℃±10℃的保持温度，在该保持温度下保持60s±1s。退火过程中的退火气氛由最多5体积％的H2和其余的N2以及技术上不能避免的杂质组成。该退火气氛的露点为-30℃。
然后试样P1-P8以7K/s±1K/s的降温速率降温到470℃±10℃的过时效温度，在此温度下这些试样保持30s±1s。
过时效温度对应入浴温度，在此温度下试样P1-P8接下来进入热浸锌镀浴，该热浸锌镀浴除不可避免的杂质外不含有其它组分。该热浸镀浴的温度为465℃±5℃。
对于通过热浸镀浴的过程来说所必需的时间为2s±1s。从热浸镀浴中出来后，这些试样需要设置保护镀层的表面上分别具有了Zn保护镀层，其厚度为所期望的7μm±3μm。
与此相反，设置有SiO2预涂层的表面上则完全没有Zn镀层。之后不需要去除附着的Zn。
Figure BDA0001365387500000091
表1
Figure BDA0001365387500000092
表2
Figure BDA0001365387500000101

Claims (13)

1.一种用于将金属保护镀层施加到钢产品的表面上的方法，在该方法中，至少一个其它表面没有该金属保护镀层，其中该金属保护镀层的施加通过热浸镀在热浸镀浴中进行并且在热浸镀之前在没有金属保护镀层的表面上设置一层由SiO2组成的预涂层，该预涂层在进行热浸镀时阻止金属保护镀层附着在相关表面上,其特征在于，由非结晶二氧化硅组成的、层厚度为0.5-100nm的镀层作为预涂层从气相中沉积到钢产品的需要保持没有金属保护镀层的表面上。
2.根据权利要求1所述的方法，其特征在于，所述预涂层通过火焰裂解沉积。
3.根据权利要求1所述的方法，其特征在于，所述预涂层利用物理或者化学气相沉积方法沉积。
4.根据权利要求1所述的方法，其特征在于，所述预涂层的厚度最小为2nm。
5.根据权利要求4所述的方法，其特征在于，所述预涂层的厚度最小为10nm。
6.根据权利要求1所述的方法，其特征在于，在涂覆预涂层之后以及经过热浸镀浴之前，钢产品能够在700-900℃的退火温度下，在退火气氛中进行6-300s的连续退火，该退火气氛包含0.5-10体积％的H2，其余为氮气和不可避免的杂质，其露点为-50℃至-10℃。
7.根据权利要求6所述的方法，其特征在于，各个钢产品在退火之后以及涂覆热浸镀层之前进行过时效处理，在该过时效处理中该钢产品在400-520℃温度范围内保持6-180s。
8.根据权利要求1所述的方法，其特征在于，为了进入到热浸镀浴中，该钢产品升温到入浴温度，该温度位于下限为热浸镀浴温度-30℃，上限温度为热浸镀浴温度+30℃的范围内。
9.根据权利要求1所述的方法，其特征在于，所述钢产品为基板由薄板构成的扁钢产品。
10.根据权利要求9所述的方法，其特征在于，扁钢产品在轧制状态下或者作为热轧带材提供用于热浸镀。
11.根据权利要求1所述的方法，其特征在于，其工作步骤在连续过程中进行。
12.根据权利要求1所述的方法，其特征在于，在热浸镀后将所述预涂层从钢产品的未镀层的表面上去除。
13.根据前述权利要求1至12中任意一项所述的方法，其特征在于，所述金属保护镀层由Zn和不可避免的杂质，以及可选地最多5重量％的Al，最多2.0重量％的Mg，最多0.2重量％的Fe和总的最多10重量％的“Mn，Si”中的一个或者多个元素组成。
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