CN1139393A - 可用沸石涂层的金属箔 - Google Patents

可用沸石涂层的金属箔 Download PDF

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CN1139393A
CN1139393A CN95191367A CN95191367A CN1139393A CN 1139393 A CN1139393 A CN 1139393A CN 95191367 A CN95191367 A CN 95191367A CN 95191367 A CN95191367 A CN 95191367A CN 1139393 A CN1139393 A CN 1139393A
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H.伯德
H.普舍
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Vitesco Technologies Lohmar Verwaltungs GmbH
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Abstract

用沸石涂层的、尤其以蜂窝体形式存在的金属箔的制备方法，在此方法中：使含有铬和/或铝成分的钢箔氧化，以使在其表面形成细颗粒的氧化铝层；在此氧化物层上涂一层用作增粘层的陶瓷涂层；在陶瓷增粘层上涂一层沸石层。

Description

可用沸石涂层的金属箔
本发明涉及一种可用沸石涂层的金属箔以及涉及经过沸石涂层的金属箔的一种制备方法。
这些沸石是特别组成的和经过处理的陶瓷材料。这些陶瓷材料基于其组成和结构对某些物质具有特别的吸附性能。典型的是，这些沸石在低温范围内能贮存大量气体物质，在较高温度下又释放出这些气体物质。
为了贮存在低温起动阶段于汽车的废气系统中产生的烃，直到串接的催化转化器加热至足以使这些烃反应为止，例如有一些利用沸石这些性能的方案。对这种废气系统一定的加热之后来从沸石中放出这些烃，然后在后面的催化转化器中将它们氧化成水和二氧化碳。
为了这种和类似的应用，把这些沸石尤其作为涂层涂覆到废气可流过的蜂窝体上。基于这些沸石的陶瓷组成，首先把陶瓷蜂窝体用作载体，可是也努力将金属蜂窝体，例如将高级合金钢蜂窝体用作载体并用沸石涂层。在高的热交变负荷时，正如在汽车废气系统中所出现的那样，这种涂层的高附着强度当然是重要的，在此应考虑到这些金属材料和陶瓷材料的不同膨胀系数。
因此，本发明的任务是：制造一种可用沸石涂层的金属箔，任意厚度的沸石涂层都可牢固地固定在此金属箔上。用沸石涂层的金属箔的制备方法也是本发明的目的。为此尤其应创造这种可能性：将一种金属蜂窝体在其制成之后进行预处理，然后用沸石涂层。
用来解决此任务的是一种可用沸石涂层的金属箔，尤其是以蜂窝体形式存在的金属箔，这种蜂窝体形式的金属箔是由含有铬和/或铝的一种钢组成的，其表面覆盖一层氧化物层，而且在这种氧化物层上有一层用作增粘层的陶瓷涂层(Washcoat)，可用已知的方法在此陶瓷涂层上涂一层沸石层。具有氧化物层和增粘层的金属箔外面形成一种陶瓷结构，可用已知方法将这种陶瓷结构与陶瓷蜂窝体一样用沸石涂层，迄今这对金属载体和金属箔来说是不可能的。而且沸石层也可附加含有催化活性物质，尤其贵金属或者随后负载这些物质，而不随此带来不利情况。这样的一些复合层在废气纯化装置中甚至可能特别有效。
由高温耐腐蚀钢制成的箔特别适合于本发明的意图。这些钢箔最好含大于3.5％的铝和含大于15％的铬，尤其含约5％铝和含约20％铬。在这样的钢箔上可制成一种细粒氧化铝层，这种细粒氧化铝层不含或只含微量氧化铬和氧化铁，这借助于实施例和示意图还要更详细说明。这在大气中尤其通过长时间煅烧是可能的。在此情况下产生氧化物层，这种氧化物层具有平均表面糙度(平均糙度值Ra)为2～4μm，最好为3μm，其表面峰—谷平均高度Rz至少为0.2μm。
在这一氧化层上按溶胶凝胶浸渍法涂敷一层氧化铝基的陶瓷增粘层，它主要含γ—Al2O3。陶瓷增粘层的优选厚度为1—5μm，尤其是约2μm。而且该增粘层的比表面积为100—200米2/克，优选约180米2/克。
本发明的一个主要优点在于：首先将金属箔预处理而生成一层很均匀的和细颗粒的氧化物层，该氧化物层基本上是氧化铝层。在此情况下自然只能将沸石层粘附强度不大地直接涂覆在这种氧化物层上，因为氧化物层和沸石层具有太不同的性能和结构。按照本发明，陶瓷涂层在这里可起增粘层作用。这种陶瓷涂层一方面特别牢固地粘附在已准备好的氧化物层上，另一方面对要涂覆的沸石层具有较大的相似性，因此沸石层对增粘层的粘附也满足这些高要求。为了改进以后要涂覆的沸石层的粘附状况，尤其还可通过煅烧来改变涂覆后的增粘层。
正如根据以下所述的处理步骤还加以说明那样，沸石涂层的厚度、表面特性以及组成对以后的粘附强度来说，尤其对热交变载荷下的粘附强度来说是重要的。薄氧化物层例如在金属层和陶瓷层之间产生良好的热传导。
制备涂沸石层金属箔的一种典型方法包括以下步骤：
—使含有铬和/或铝成分的钢箔氧化以在其表面产生一层细颗粒的氧化铝层；
—在此氧化物层上涂一层用作增粘层的陶瓷涂层；
—在此陶瓷增粘层上涂一层沸石层。
通过在大气中在约950℃的温度下处理数小时可在高温耐腐蚀钢上，例如在含有约5％铝和约20％铬的高温耐腐蚀钢上披上一层特别细颗粒的氧化铝层。图1a至1d这些图表示这样一种金属箔在初态(图1a)的，在950℃和标准大气压下的煅烧5小时后的(图1b)，煅烧24小时后的(图1c)和煅烧48小时后(图1d)的表面。基本上无铬成分或无铁成分的、几乎由纯氧化铝组成的一层膜逐渐形成。此表面变成非常细颗粒的表面，并具有平均表面糙度约为3μm和平均表面峰—谷高度至少为0.2μm。陶瓷涂层可以特别牢固地固定在这样一种表面上。
这一在氧化铝基础上的涂层是按照本来已知的溶胶—凝胶浸渍法涂覆的，而且尤其使用含固体成分约为10％(重量百分数)的一种氧化铝溶胶。在浸渍工艺之后把如此涂覆的增粘层在500～650℃，最好在550℃的温度下煅烧约三小时，此增粘层基本上由γAL2O3组成。
借助于溶胶—凝胶浸渍法也可涂上沸石层，而且特别有利的是：这种沸石层除了沸石材料之外还含有10％至30％(质量百分数)氧化铝，优选含有约20％氧化铝。在此情况下可用NH4 +或H+形式涂敷沸石，这种NH4 +或H+形式是用已知方法通过离子交换产生的。使待施用的沸石在胶体磨中通过数小时研磨混匀配料之后结合到陶瓷基体中，陶瓷基体最好由基于氧化铝的溶胶组成。
特别有意义的是将所述的这种方法应用到由钢箔制成的蜂窝体上，可用至少部份有纹理的钢箔进行叠层、卷绕或其它缠绕方式来制成这些蜂窝体。典型的是，这样一些蜂窝体由交替安置的光滑钢板和波形钢板组成，而且构成废气可通过的一些流体管道。如果按溶胶—凝胶方法将这些蜂窝体浸渍涂层，就有大量涂层物料在这些管道中侧面停留，因此必须清除这些涂层物料。现有技术对此应用压缩空气吹洗法，但按这种方法得到很均匀的涂层厚度是困难的。
按照本发明，特别有利的是，在涂层之后通过对蜂窝体的离心作用来清除多余的涂层物料。离心作用时流体管道应在相对于离心机轴的径向方向。为获得特别均匀的涂层厚度，应相继朝两个端面方向进行离心作用，为此必须把蜂窝体在第一次离心作用之后转动180°。
当对增粘层选择的层厚例如为2μm保持不变时，可以通过两次或多次重复用沸石涂层的操作，即重复涂层、离心操作和煅烧来增加沸石涂层的厚度。按此方法每重复涂层一次可涂上约15μm厚的沸石。
优选涂到蜂窝体上的沸石量为每平方米载体表面至少为30克。
显而易见的是，一些典型的加工步骤例如煅烧前烘干涂上的涂层对本发明来说为避免干燥裂纹以及诸如此类的问题也是有好处的。
附图也用来说明本发明，在此图中：图1a至d表示高级合金钢箔氧化过程中的不同阶段。
图2表示按本发明制成的用沸石涂层的钢箔，图3表示一个典型金属蜂窝体的横截面。
在不按正确比例的图1中，金属箔1带有氧化物层2、陶瓷增粘层3和沸石层4。如图示表明，增粘层3通过氧化物层2在某种意义上与金属箔1机械地夹合在一起，而通过它们很近似的材料组成和与此有联系的粘合力产生增粘层3和沸石层4之间的粘合。
图3表示由光滑钢板和波形钢板组成的一个典型蜂窝体5的截面，该蜂窝体在钢板的接触处用焊接点6连接。按此方法构成管道7。
按本发明方法有沸石涂层的蜂窝体特别适合于用内燃机的汽车在低温起动阶段的废气净化。

Claims (21)

1.可用沸石涂层的、尤其以蜂窝体形式存在的金属箔，具有以下特征：
—金属箔(1)由含有铬和/或铝的钢组成；
—表面被氧化物层(2)覆盖；
—在氧化物层(2)上有一层用作增粘层(3)的陶瓷涂层；
—在此陶瓷增粘层(3)上可用已知方法涂上沸石层(4)。
2.按权利要求1所述的金属箔，其特征在于：金属箔(1)由高温耐腐蚀钢组成，这种高温耐腐蚀钢优选含3.5％以上的铝和含15％以上的铬，尤其含约5％铝和含约20％铬。
3.按权利要求1或2所述的金属箔，其特征在于：氧化物层(2)是优选在大气中通过长时间煅烧制成的细颗粒氧化铝层，此细颗粒氧化铝层不含或只含少量氧化铬和氧化铁。
4.按权利要求3所述的金属箔，其特征在于：氧化物层(2)具有的平均表面糙度(平均糙度值Ra)为2至4μm，最好为3μm，平均表面峰—谷高度至少为0.2μm。
5.按权利要求1、2、3或4所述的金属箔，其特征在于：以氧化铝为基础的陶瓷增粘层(3)是按溶胶—凝胶浸渍方法涂上的，并且基本上含γ—AL2O3。
6.按权利要求5所述的金属箔，其特征在于：陶瓷增粘层(3)的层厚为1至5μm，最好约为2μm。
7.按权利要求5或6所述的金属箔，其特征在于：陶瓷增粘层(3)的比表面积为100～200米2/克，最好约为180米2/克。
8.按上述权利要求的一项所述的金属箔，其特征在于：把金属箔(1)在涂层之前制成蜂窝体(5)并将在此情况下产生的接触点(6)的至少一部份焊接上。
9.用沸石(4)涂层的、尤其以蜂窝体(5)的形式存在的金属箔(1)的制造方法，具有以下步骤：
—使含有铬和/或铝成分的钢箔(1)氧化，以使在其表面形成细颗粒的氧化铝层(2)；
—在此氧化铝层(2)上涂一层用作增粘层(3)的陶瓷涂层；
—在此陶瓷增粘层(3)上涂一层沸石层(4)。
10.按权利要求8所述的方法，其特征在于：金属箔(1)由高温耐腐蚀钢组成，该高温耐腐蚀钢优选含3.5％以上铝和含15％以上铬，尤其含约5％铝和含约20％铬。
11.按权利要求9或10的一项所述的方法，其特征在于：把金属箔(1)在涂层之前制成蜂窝体(5)并将在此情况下产生的接触点(6)的至少一部份进行焊接。
12.接权利要求9、10或11所述的方法，其特征在于：优选通过在大气中长时间煅烧在金属箔(1)上制成细颗粒的氧化铝层(2)，此细粒的氧化铝层只含有少量氧化铬和氧化铁。
13.按权利要求12所述的方法，其特征在于：氧化物层(2)是在大气中通过在900～1000℃，最好在950℃的温度下煅烧数小时生成的。
14.按权利要求9至13的一项所述的方法，其特征在于，按溶胶—凝胶方法涂上以氧化铝为基础的陶瓷增粘层(3)，此陶瓷增粘层(3)基本上由γAL2O3组成。
15.按权利要求14所述的方法，其特征在于：陶瓷增粘层(3)是以氧化铝溶胶形式，尤其以固体含量约为10％的氧化铝溶胶形式涂上的。
16.按权利要求14或15所述的方法，其特征在于：把按浸渍方法涂上的陶瓷增粘层(3)在500至650℃下，最好在550℃下煅烧约3小时。
17.按权利要求9至16的一项所述的方法，其特征在于：沸石层(4)是用溶胶—凝胶浸渍方法涂上的，沸石层(4)除了沸石材料以外还含有10％至30％(质量百分数)氧化铝，最好含有约20％氧化铝。
18.按权利要求11至17的一项所述的方法，其特征在于：在用增粘层(3)和/或沸石层(4)对蜂窝体(5)进行浸渍涂层之后通过对蜂窝体(5)的离心作用除去在其管道(7)中存在的多余涂层材料量。
19.按权利要求9至18的一项所述的方法，其特征在于：以NH4 +或H+形式涂敷沸石层(4)，这种NH4 +或H+形式是可用已知方法通过离子交换来制成的。
20.按权利要求9至19的一项所述的方法，其特征在于：使要涂敷的沸石(4)在胶体磨中通过数小时研磨之后结合到陶瓷基体中，该陶瓷基体最好由以氧化铝为基础的溶胶组成。
21.按权利要求9至20的一项所述的方法，其特征在于：在蜂窝体上涂覆沸石量为每米2载体表面至少30克。
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