CN100337728C - 多层陶瓷复合物 - Google Patents

多层陶瓷复合物 Download PDF

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CN100337728C
CN100337728C CNB200380109361XA CN200380109361A CN100337728C CN 100337728 C CN100337728 C CN 100337728C CN B200380109361X A CNB200380109361X A CN B200380109361XA CN 200380109361 A CN200380109361 A CN 200380109361A CN 100337728 C CN100337728 C CN 100337728C
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sintering
layer
substrate
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particle
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CN1744941A (zh
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F·埃伦
O·宾克利
R·诺宁格
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Itn Nanovation AG
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Abstract

在一种制造多孔陶瓷复合物的方法中，向先前已经烧结的陶瓷衬底上应用未烧结层，并在500—1300℃的温度下，将其和先前已烧结的衬底一起烧结，其中，该未烧结层中专门包含有颗粒尺寸x≤100nm的陶瓷颗粒，并且该未烧结层在烧结后作为功能层所具有的层厚为s≤2.5μm。依据这种方法制得的功能层是无缺陷的，含有微细气孔，所以特别适合于用在过滤工艺中。

Description

多层陶瓷复合物
现有技术
本发明涉及一种通过烧结制造多层多孔陶瓷复合物的方法。
多层多孔陶瓷复合物可以用在例如过滤技术中，以及在电子学中用来制造条形导线结构。陶瓷多层过滤件可用于例如在芯片去除生产中分离油-水乳液，澄清啤酒，气体提纯，气体分离或者液-固混和物分离。陶瓷过滤件材料通常由烧结的颗粒和其间形成气孔的间隙构成。为了过滤目的，气孔体积部分必须尽可能高，且气孔的尺寸分布必须均匀并尽可能接近。因为这个原因，在制造陶瓷过滤材料时，优选采用的是具有窄分布的颗粒尺寸分布的陶瓷粉末。
陶瓷膜通常由具有不同气孔宽度的单个层的多孔陶瓷的多层体系构成。实际的过滤层(功能层)通常是该体系中具有最精细气孔的最薄层。其位于该体系的具有较大气孔结构的衬底上。该衬底同时具有整个体系的机械载体的功能，通常还构成用来收集过滤物的结构。多层过滤件通过最初成型，干燥，烧结衬底，然后施用功能层并将其烧结到衬底上而制得。包含陶瓷颗粒但还没有被烧结的层称为未烧结层(green layer)。相应的将由此材料制成的物体称为未烧结体(greenbody)。
陶瓷复合物的烧结是这样一种制造方法，在此过程中，将未烧结体转变成为多孔的无粘结剂的固体，或者转变成或多或少致密化的无粘结剂的固体，由此相应的提高了先前烧结体的机械牢固性或者密度。在理想情况下，用于烧结的最初物体可以看成是球状颗粒的紧密堆积，它们在接触点处松散的连接在一起，即，它们在称为“颈”的地方彼此接触并黏附在一起。颗粒之间的空间形成了最初物体中的气孔。最初的气孔具有几何上差别最大的复杂结构。烧结在高温下按两步进行。在第一步中，整体气孔率基本上保持不变。彼此的颗粒中心大体上保持相同的距离。然而，由于空隙即气孔的形状从最初状态的复杂结构转变成单一的球状模式，表面能提高，因而对应于给定的气孔率，得到最小的表面。颗粒在“颈”处彼此接触，在第一步烧结中，由于物质传输，“颈”变得越来越粗。由此，气孔变圆，得到最小的气孔表面。这种物质传输也叫做晶界扩散。在第二步中，气孔逐渐闭合。材料自身通过将孔洞传输到内外表面(体扩散)上而变致密。通过烧结体的致密化，整体气孔率降低。通过晶界扩散和体扩散，气孔被填充。在这步中，最初粉末颗粒的中心一起移动，由此烧结体致密化或者收缩。
发生晶界扩散的程度可以通过气孔中产生的毛细管压力来检测。不同的曲率半径导致物质传输，通过物质传输产生气孔形状的改变。物质发生传输，具体的，从颗粒的“腹部”传输到颗粒的“颈”上。平均而言，在向内弯曲的表面(凹面)上的原子结合的比在向外弯曲的表面(凸面)上的要强。颗粒“腹部”的毛细管压力是正的，颗粒“颈部”的是负的。这种压力的差异是物质传输的驱动力。这种导致陶瓷未烧结体烧结的毛细管压力除了依赖于温度和颗粒类型外，还依赖于所用颗粒的尺寸，因为凸面的曲率半径随着颗粒尺寸的降低而增加。由于这个原因，陶瓷未烧结体开始烧结的温度(在未烧结体的堆积密度是相同的前提条件下)随着最初颗粒的颗粒尺寸的减小而下降。
在传统的方法中，将颗粒层置于已烧结的衬底上，然后将整个的陶瓷复合物再次烧结，由于上面描述的过程，衬底和未烧结体的致密化不同。这在两种材料层之间产生应力，再一次在材料层和/或层间过渡区中引起缺陷。特别的，对于过滤层，这些有缺陷的区域是所不希望的。
发明目的
所以，本发明基本的目的就是提供一种在已烧结的陶瓷衬底上应用无缺陷陶瓷层的方法。
发明内容
依据本发明，这一目的是通过由烧结制造多层多孔陶瓷复合物的方法实现的，其中，在已烧结的衬底表面上应用一个层或多个层，其中，至少一层中含有颗粒尺寸为x≤100nm的纳米级颗粒，衬底表面的粗糙深度比应用在衬底表面上的纳米级颗粒的层厚s小，并且，应用的纳米级颗粒和衬底在500-1300℃的温度下的烧结过程结束后，具有的层厚s为s≤2.5μm。
本发明方法使得能够在已烧结的衬底上应用薄的无缺陷的功能层。尽管在通常的烧结过程中，未烧结体通过晶界扩散和/或体扩散致密化，依据本发明，通过选择颗粒尺寸x≤100nm，最大层厚s≤2.5μm，以引起晶界漂移(晶界流动或者迁移)，从而影响致密化过程，这在陶瓷体中还未曾观察到。晶界流动可以防止在已烧结的衬底和形成功能层的未烧结层之间产生应力。由此，功能层可以烧结到最高大约s＝2.5μm的厚度，致密化程度更高或更低，而不会引起缺陷。本发明使得可以制得无缺陷的功能层，并在功能层和用与功能层不同的材料的陶瓷颗粒制成的衬底之间得到无缺陷连接，其中，在烧结过程中或者之后，功能层不会从衬底上脱落。用该类型的功能层可以得到优异的过滤效果。
功能层的最小厚度由已烧结的衬底的粗糙深度决定。该粗糙深度一定不能超过功能层的层厚。
纳米级的颗粒可以具有不同的形状，例如，球状，板状或者纤维状。在每种情形下，颗粒尺寸指的都是这些颗粒的最长尺度，例如，如果颗粒是球状的，其是指直径。
所采用的陶瓷材料优选的来自(混和的)金属氧化物，以及金属和非金属的碳化物，氮化物，硼化物，硅化物和碳氮化物。其例子是Al2O3，部分或者完全稳定的ZrO2，莫来石，堇青石，钙钛矿，尖晶石，例如BaTiO3，PZT，PLZT以及SiC，Si3N4，B4C，BN，MoSi2，TiB2，TiN，TiC和Ti(C，N)。显然，这里列举的是不完全的。当然，也可以采用氧化物或者非氧化物的混和物，以及氧化物和非氧化物的混和物。
在本方法的一个有利实施方案中，在已烧结的衬底上应用两个层，其中，至少一个层中含有纳米级颗粒。通过提供具有不同气孔率的几个层，可以精确控制多孔陶瓷复合物的过滤性能。特别的，如果这些层中有一个没有缺陷，可以得到特别好的过滤效果。
在一个可供选择的方法变化中，在已烧结的衬底上应用两个以上的层，其中，至少有两层中含有纳米级颗粒。由此制得了具有好的过滤性能的多层多孔陶瓷复合物。
如果纳米级颗粒的颗粒尺寸为x≤20nm，优选的x≤10nm，小的活化能即可诱发晶界流动。这使得可以采用低的烧结温度，伴有的烧结应力大约为200MPa。
在一个有利的方法变体中，通过喷涂，浸渍，溢流或者箔片(foil)浇注在已烧结的衬底上应用纳米级颗粒。如果纳米级颗粒含在悬浮体中，采用上述方法步骤向已烧结的衬底上的应用是尤其便利的。具体的，这使得可以对应用在已烧结衬底上的未烧结层的层厚进行良好的控制和调节，相应的控制了烧结的功能层。
在一个尤其优选的方式中，在应用纳米级颗粒之前，向已烧结的衬底上应用中间层，特别是有机中间层。有机粘结剂平整了已烧结衬底的不平整表面并且/或者有机粘结剂防止了形成功能层的纳米颗粒向含有粗大气孔的衬底表面内渗透。有机粘结剂可以阻塞或者抹去衬底表面上的气孔，防止所不希望的形成功能层的纳米颗粒向衬底表面内的渗透。特别的，可以用有机粘结剂处理衬底，形成合适的载体结构。在烧结过程中，有机中间层消失，这样最终陶瓷复合物的过滤性能不受有机粘结剂的影响。
这一目的还可以通过包括已烧结的衬底和无缺陷功能层的多层多孔陶瓷复合物实现，该无缺陷功能层由纳米级颗粒烧结而成且具有的层厚为s≤2.5μm。由于没有缺陷，这种类型的多孔陶瓷复合物具有尤其高性能的过滤层。
在一个优选的实施方案中，该陶瓷复合物具有三个层，其中一层中含有纳米级颗粒。这些层的材料性能可以相互匹配，使得至少一个过滤层是无缺陷的，由此得到高性能的过滤件。
在一个可供选择的实施方案中，该陶瓷复合物具有三个以上的层，其中至少两层中包含纳米级颗粒。这种情况下，陶瓷复合物中的过滤效果可以逐步提高，其中提供至少两个具有特别精细的气孔并且没有缺陷的层。此外，其还可以制备多层条形导体结构，其中由纳米级颗粒制成的无缺陷层是绝缘体，这使得可以用小的相互隔离来以电绝缘的方式布置条形导线。
在制造多孔陶瓷复合物的一种方法中，未烧结层应用在先前已烧结的陶瓷衬底上，并和先前已烧结的衬底一起在500-1300℃的温度下烧结，其中，未烧结层中专门包括颗粒尺寸为x≤100nm的陶瓷颗粒，且未烧结层烧结后具有的层厚为s≤2.5μm。用这种方法制得的层是无缺陷的，具有精细气孔，所以特别适合用在过滤工艺中，并可以用作催化转化器。
本发明的进一步的特征和优点可以从权利要求中得到。在本发明的变体中，各个特征可以单独实现或者以任意组合的方式集中实现。

Claims (5)

1.通过烧结制造多层多孔陶瓷复合物的方法，其中，向已烧结的陶瓷衬底上应用无缺陷陶瓷层，其中将未烧结层直接应用在烧结的衬底的表面上，其中该未烧结层含有颗粒尺寸为x≤100nm的纳米级颗粒，将该含有纳米级颗粒的层应用在衬底上，其中层的厚度s大于衬底表面的粗糙深度，在与衬底一起在500-1300℃下烧结后，所应用的该含有纳米级颗粒的层厚为s≤2.5μm。
2.依据权利要求1的方法，其特征在于使用颗粒尺寸为x≤20nm的纳米级颗粒。
3.依据权利要求1的方法，其特征在于使用颗粒尺寸为x≤10nm的纳米级颗粒。
4.依据前述任意权利要求之一中的方法，其特征在于通过喷涂，浸渍或者溢流将纳米级颗粒应用到已烧结的衬底上。
5.由前述任意权利要求之一中的方法制得的多层多孔陶瓷复合物，其包括已烧结的衬底和由纳米级颗粒烧结而成的且具有的层厚为s≤2.5μm的无缺陷功能层。
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