CN101500683A - 陶瓷壁流过滤器的制造 - Google Patents

陶瓷壁流过滤器的制造 Download PDF

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CN101500683A
CN101500683A CNA2006800195126A CN200680019512A CN101500683A CN 101500683 A CN101500683 A CN 101500683A CN A2006800195126 A CNA2006800195126 A CN A2006800195126A CN 200680019512 A CN200680019512 A CN 200680019512A CN 101500683 A CN101500683 A CN 101500683A
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mixture
shutoff
plug
flow filter
inorganic bond
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CN101500683B (zh
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B·S·基尔克
D·马达法利
S·B·奥古米
R·J·佩斯利
B·P·尤西安克
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Corning Inc
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Abstract

提供了整体或片段结构的多孔陶瓷壁流过滤器体，其中，蜂窝体孔道被封堵接合剂交替封堵。所述封堵接合剂中加入了低膨胀耐火填料和永久性无机粘合剂。该永久性无机粘合剂提供改进的封堵物完整性和封堵物与多孔陶瓷蜂窝体孔道粘合性。

Description

陶瓷壁流过滤器的制造
本申请要求由S.Ogunwumi等人于2005年6月1日提交的标题为“陶瓷壁流过滤器的制造”的美国临时申请No.60/686,497的权益。
发明背景
本发明涉及多孔陶瓷颗粒过滤器的制造，更具体地，涉及用于对多孔陶瓷蜂窝体的选定孔道进行密封以此形成壁流陶瓷过滤器的改进的材料以及方法。
发现陶瓷壁流过滤器的用途在不断扩大，可用于从柴油或其它内燃机的排气流中去除微粒污染物。已知有许多从由多孔陶瓷形成孔道蜂窝体结构制造这类过滤器的方法。最普遍采用的方法是将密封材料的固化封堵物置于这种结构的交替孔道的端部，可以堵塞流体不直接流过孔道，并迫使流体流通过蜂窝体的孔道壁，然后从该过滤器排出。这种方法在美国专利No.6,809,139中说明，该专利描述了使用包含能形成堇青石(MgO-Al2O3-SiO2)的陶瓷粉末混合物以及热固性或热塑性粘合剂体系的密封材料来形成这种封堵物。
在制造封堵的陶瓷过滤器产品时注意到的问题之一是确保封堵物的完整性和耐久性。许多已知的封堵方法涉及使用特定的封堵组合物，这种组合物必须在相对高温下烘焙，适当固化封堵材料，并使封堵材料牢固结合到该结构的多孔孔道壁上。其它方法涉及使用“冷固化”接合剂(cement)，而接合剂不是通过高温烘焙固化的，因此不能在内燃机排气系统中的高温和压力下提供足够的强度和耐久性。
对成功的封堵材料的其它要求包括为与填充材料物理相容性的相对低的热膨胀系数(CTE)，以及在内燃机排气流中填充存在的水蒸汽中的稳定性。要求低热膨胀，以使固化的封堵物能够抵抗封堵物或陶瓷蜂窝体孔道壁的热应力破裂，并能在反复的热循环下保持与孔道壁的结合。以前的某些封堵混合物产生的接合剂的热膨胀系数比焙烧后的孔道壁上陶瓷材料高得多。对于重复热循环，封堵孔道的CTE不匹配可能导致在封堵物/基质界面上的分离或者在过滤器面上的碎裂。
要求水分稳定性是为了避免封堵材料在发动机的排气环境中发生化学变化。所述的排气环境会使封堵物的物理和化学特性发生不希望的改变。当然，提供封堵材料和蜂窝体陶瓷之间长期的高粘合力的封堵物的物理和化学稳定性是为了壁流过滤器的寿命而保持封堵物-孔道密封完整性所必需的。
发明概述
根据本发明，提供一类用于陶瓷壁流过滤器的封堵混合物，这类混合物解决了普通壁流过滤器材料的物理和化学稳定性差的问题，并且提供了在壁流发动机排气过滤器的潮湿、高应力环境中具有良好物理和化学稳定性的封堵物。因此，由这些混合物形成的封堵物提供了与壁流过滤器材料长期稳定的良好结合的密封。
本发明另一方面，提供了在过滤器体的选定孔道中加入固化的封堵物的多孔陶瓷壁流过滤器体，所述封堵物与壁流过滤器材料能达到良好的物理和化学匹配，与过滤器体的孔道壁形成永久的密封。
本发明提供的封堵混合物包含：(a)低膨胀的耐火填料；(b)永久性无机粘合剂；(c)液体赋形剂，和(d)可溶于赋形剂的临时粘合剂。低膨胀的耐火填料对确保与壁流过滤器材料的相容性很重要，而永久性无机粘合剂的作用是使密封固化和韧化，以及将耐火填料粘合到多孔孔道壁并密封。虽然优选的赋形剂是水，优选的临时粘合剂是可水溶的粘合剂，但是可以替代使用醇基、石油基的或其它类型的赋形剂，和溶于这些赋形剂的临时粘合剂。
因此，本发明的多孔陶瓷壁流过滤器体由孔道蜂窝体支承，其中，在选定的孔道中加入封堵物，以永久密封多孔孔道壁。封堵物显示改进了与壁流过滤器材料的化学和物理相容性。壁流过滤器材料包含低膨胀的耐火填料和永久性无机粘合剂，以便将耐火填料固结为整体封堵物并将封堵物密封在孔道孔道壁上。
发明详述
目前被用来制造壁流陶瓷过滤器的常规多孔陶瓷材料包括堇青石、碳化硅、氮化硅、钛酸铝、β-锂霞石和β-锂辉石之类的陶瓷。某些情况下，这些陶瓷是通过原位反应性烧结孔道蜂窝体的预制件形成的；其它情况下，陶瓷粉末本身简单地烧结在一起，产生所需孔隙度和强度的多孔蜂窝体。当壁流过滤器是低膨胀的过滤器时，即由低热膨胀的陶瓷如反应性烧结的堇青石和在1000℃测得的热膨胀系数小于约25 x 10-7/℃的钛酸铝形成的过滤器时，可以提供为单块蜂窝体结构，或者需要时，为粘合的蜂窝体组合件。当蜂窝体由碳化硅之类高热膨胀陶瓷形成时，一般需要粘合的蜂窝体组合件。
构成本发明的封堵混合物主体的低膨胀耐火填料可以采用任何方便的形式引入到封堵混合物中；所述的合适形式包括：粉末、小聚集物、陶瓷纤维等。在优选的接合剂实施方式中，低膨胀的耐火填料可以是预反应的无定形或结晶陶瓷粉末，在封堵物固化或过滤器的使用温度下其组成或结构不会发生明显的变化。这可以避免需要采用高固化温度来使封堵物组分化学反应，并确保耐火填料不会在固化或使用期间丧失其低热膨胀特性。
为了提高密封体与用于制造蜂窝体的多孔陶瓷材料的化学和物理相容性，应使用平均热膨胀系数不超过30 x 10-7/℃(25-800℃)的过滤器。蜂窝体的热膨胀系数与固化的密封体的热膨胀系数之差应优选不大于约20 x 10-7/℃(25-800℃)。此外，对与这些材料的化学相容性，填料或者在组成上与蜂窝体的组成相类似，或者在使用条件下，在与蜂窝体和与永久性无机粘合剂接触时是热稳定的和相对惰性的。
膨胀系数能与常规壁流过滤器材料的膨胀系数合理匹配的适当的耐火填料包括：碳化硅、氮化硅、堇青石、钛酸铝、铝酸钙、β-锂霞石和β-锂辉石的粉末，以及例如通过对硅铝酸盐粘土进行处理形成的硅铝酸盐的耐火纤维。
本发明的封堵混合物中的永久性无机粘合剂一般由胶体或细粉碎的氧化硅或硅酸盐材料组成，或源自这些材料，这些材料不含有机物或有机物含量很低。这些材料能简便地完全分散在本发明的封堵混合物中，提供对耐火填料的有效固结和对陶瓷蜂窝体结构的孔道壁的良好密封。
重要的一点是，氧化硅(silica)永久性无机粘合剂是细粉碎的氧化硅，以在相对较低的固化温度提供必要的粘合效力。为此目的，砂和其它粗的氧化硅材料不具有足够的反应性。细粉碎的氧化硅是指最大平均粒度不超过约0.5微米的氧化硅。
适合用作粘合剂的氧化硅或硅酸盐材料的例子包括：硅胶和粉末化氧化硅或硅酸盐玻璃。硅酸盐玻璃粘合的填料封堵物的一个潜在优点是，可以选择硅酸盐(玻璃)在再生的峰值温度时“软化”，因此“减轻”使用期间在封堵物或过滤器内形成的任何应力。
使用这些粘合剂对确保足够的封堵物强度和对陶瓷蜂窝体过滤器结构的多孔孔道壁的密封很重要。因此，封堵物不仅必须具有以下物理性质，包括接近于蜂窝体材料的热膨胀系数，而且封堵物的强度和与蜂窝体壁的粘合性必须足够高，能承受热排气流产生的压力梯度。当用于制造低膨胀的陶瓷蜂窝体过滤器时，对具备良好物理相容性和密封性能的封堵物的特定目标性质的例子如下：
 
断裂强度(棒弯曲)的模数 >500psi
线性热膨胀系数(x10-7/℃，800-25℃冷却) ≤30
封堵物推出破坏力 >6lbf
提供封堵混合物可流动的或糊料稠度的赋形剂优选是水，虽然如上所述可以使用其它对于合适的临时粘合剂显示溶剂作用的液体赋形剂。对优选加入水作为赋形剂的封堵混合物，适合用于这种封堵混合物的临时粘合剂包括：可水溶的纤维素粘合剂，一般为纤维素衍生物，如纤维素醚。具体例子包括甲基纤维素和羟丙基甲基纤维素。
本发明的封堵混合物中耐火填料和无机粘合剂的相对比例可依据填料的选择以及将填料固结成单块封堵物并将封堵物密封在过滤器的孔道内所采用的处理方法来改变。粘合剂与填料的重量比值一般在低至1:20至高达2:3的范围。粘合剂的比例较低可能导致封堵物固结不充分，或者对孔道壁的密封较差，而添加过量粘合剂可能降低封堵物的耐熔性，以及降低封堵物与多孔陶瓷孔道壁的物理和化学相容性。
本发明的封堵混合物可用于使用“冷固化”封堵物的封堵方法以及热固化封堵物的方法。在冷固化封堵中，要求只干燥封堵混合物，形成与蜂窝体的孔道壁的密封。加热封堵的蜂窝体至35-110℃温度范围对加速干燥有用。在某些冷固化封堵方法中，预期最后的封堵物固结，包括去除残余的临时粘合剂的副产物并对密封体增强，甚至可能发生在对过滤器进行随后处理过程(在催化或灌装过程中)或者在过滤器首次用于排气系统期间。
采用热固化封堵物时，固化温度一般在至少能有效去除临时粘合剂和任选的有机润滑剂和增塑剂的温度至较高的固化温度范围，所述固化温度下能达到粘合剂活化，使耐火过滤器固结并密封单块封堵物在蜂窝体的孔道壁中。最高至约1000℃的温度范围通常能更充分地热固化上面所述的封堵混合物的大多数耐火组分。
本发明的封堵混合物另外还包含少量任选添加的其它组分，以达到如提高临时粘合剂的效力或改进混合物的可塑性或润滑性，以提高与常规封堵方法的相容性。合适的任选添加剂的例子包括：增塑剂，如聚乙烯醇缩丁醛树脂增塑剂，润滑剂如矿物油。一般而言，这些任选添加剂的总比例不会超过最终封堵混合物重量的10％。
参见以下实施例可以更进一步的理解本发明，这些实施例意图进行说明，而不是构成限制。
实施例I-含纤维的封堵混合物和接合剂
适于对可组装成多孔壁流过滤器体的由碳化硅挤出的片段中选定的孔道进行封堵的封堵混合物是由以下组分的耐火填料混合物混合制成：硅铝酸盐纤维、钛酸铝粉末和铝酸钙粉末，该混合物的按重量％的组成列于下面表1A中：
Figure A200680019512D00071
将这些组分捏合成均质糊料，然后，将形成的糊料注入碳化硅蜂窝体片段中选定孔道的端部。还将同样的糊料施用于多个进行了选择封堵的片段之间，以形成由该糊料层连接的片段束。然后，对由此形成的选择封堵的片段束加热至110℃并保持一定的时间，足以干燥和部分固化封堵物和粘合的接合剂，从而提供粘合的选择封堵的碳化硅壁流过滤器体。
可以以相同的方式，使用组成与上述基本上相同，但碳化硅耐火填料粉末被同样重量的氮化硅粉末替代的类似的封堵混合物，形成粘合的选择封堵的壁流过滤器体，其中，氮化硅的挤出的蜂窝体片段形成了过滤器的蜂窝体结构。
可以使用类似组成但省略了碳化硅填料粉末的改进的封堵混合物，来选择封堵整体的陶瓷蜂窝体结构，该结构中，多孔陶瓷孔道是由钛酸铝形成的。合适的封堵混合物的代表例子列于下面表1B，组成按照混合物的重量份列出：
Figure A200680019512D00072
再次，对封堵的钛酸铝过滤器体只需要中等加热至约110℃的温度，以干燥和初始固化并且将封堵混合物粘合到该蜂窝体孔道的多孔陶瓷壁上。
实施例2-填充粉末的封堵混合物
对于需反复使用剧烈再生过程以通过燃烧从过滤器去除被捕集的含碳微粒的高温柴油机排气过滤应用，基于具有低热膨胀特性的预烧结(预反应)耐火陶瓷粉末的封堵混合物能提供改进的热相容性和化学稳定性。基于预反应的堇青石或钛酸铝粉末的封堵混合物提供了低热膨胀和高温稳定性的良好综合性能，并且在按照本发明与预合适的永久性粘合剂组合使用时，能提供具有优良强度和密封特性的封堵物。此外，这种封堵混合物可以与任何低膨胀的多孔陶瓷过滤器材料一起使用，包括例如堇青石和钛酸铝材料，不必特别考虑所使用的耐火粉末填料是否来自相同类或不同类陶瓷组合物。原因是这些粉末在过滤器实际使用的温度下基本上是惰性的。
用于封堵堇青石或钛酸铝陶瓷蜂窝体结构的三种封堵混合物的例子列于下面表2中。表2中的组成按照重量％列出，不包括添加在该混合物中的水赋形剂：
Figure A200680019512D00081
*Corning Code 7761硼硅酸盐玻璃粉末(78.56％SiO2，18.58％ B2O3，2.77％ K2O，0.09％ AL2O3)
这些混合物各自与水赋形剂掺混，形成糊料状稠度，可用于封堵钛酸铝陶瓷蜂窝体结构中选择的孔道，该蜂窝体结构被转化为钛酸铝组合物的陶瓷壁流过滤器体。在冷固化的封堵混合物情况，由上面的混合物A为例，将糊料混合物简便地引入钛酸铝蜂窝体的选择孔道中，该封堵体然后在约100℉烘箱内干燥2小时，去除封堵物中过量的水。用于该混合物的堇青石耐火填料的平均线性热膨胀系数在25-800℃温度范围约为15 x 10-7/℃，从膨胀匹配考虑，该封堵物与过滤器体的钛酸铝蜂窝体体微粒物理相容，并显示良好的高温组成稳定性。
类似地，用上面封堵混合物B或C通过添加适当的水转变为糊料，用其进行封堵的钛酸铝蜂窝体将显示良好的封堵物稳定性、强度和密封特性。例如，在混合物B的情况，该混合物是有用的热固化组合物，封堵体可以加热至干燥温度，如上面冷固化混合物A的情况，然后，加热到最高1000℃的固化温度。在此情况，固化会完全活化永久性粘合剂，因而立即固结，并将封堵物密封在该蜂窝体结构的多孔钛酸铝陶瓷壁中。
实施例3-填充混合粉末的封堵混合物
使用填充多种粉末的封堵混合物的另一些例子，来改进封堵物性质，这些混合物按照最终封堵混合物的重量份计列于下面表3。混合的耐火填料由两种不同粒度(40微米和12微米)的堇青石粉末组成。
*Corning Code 7740硼硅酸盐玻璃粉末
这些封堵混合物特别适合用于对钛酸铝蜂窝体进行封堵。样品E混合物显示改善了在降低封堵压力下对陶瓷蜂窝体进行封堵使的润滑性。

Claims (10)

1.一种用于陶瓷壁流过滤器的封堵混合物，该混合物包含：
低膨胀的耐火填料；
永久性无机粘合剂；
液体赋形剂；和
可溶于赋形剂的临时粘合剂。
2.如权利要求1所述的封堵混合物，其特征在于，所述液体赋形剂是水，所述临时粘合剂是可水溶的纤维素粘合剂。
3.如权利要求1所述的封堵混合物，其特征在于，所述耐火填料选自以下：硅铝酸盐纤维，以及碳化硅、氮化硅、堇青石、钛酸铝、铝酸钙、β-锂霞石和β-锂辉石的粉末。
4.如权利要求2所述的封堵混合物，其特征在于，所述永久性无机粘合剂是粉末化的氧化硅或硅酸盐玻璃。
5.如权利要求1所述的封堵混合物，该混合物还包含润滑剂或增塑剂。
6.如权利要求1所述的封堵混合物，其特征在于，所述永久性无机粘合剂与所述耐火填料的重量比值在1∶20至2∶3范围。
7.一种多孔陶瓷壁流过滤器体，该过滤器体包括其中结合了多个由多孔陶瓷孔道壁限定的平行孔道的蜂窝体结构，选定的孔道中加入了对孔道壁永久密封的封堵物，其中，所述封堵物包含低膨胀的耐火填料和永久性无机粘合剂，所述永久性无机粘合剂使所述耐火填料固结成为封堵物并将封堵物密封在孔道壁中。
8.如权利要求7所述的多孔陶瓷壁流过滤器体，其特征在于，具有包含选择以下的陶瓷的组合物：堇青石、碳化硅、氮化硅、钛酸铝、β-锂霞石和β-锂辉石。
9.如权利要求8所述的多孔陶瓷壁流过滤器体，其特征在于，所述封堵物含有低膨胀的耐火陶瓷填料，还含有永久性无机粘合剂；所述填料选自：硅铝酸盐纤维，以及碳化硅、氮化硅、堇青石、钛酸铝、铝酸钙、β-锂霞石和β-锂辉石，所述永久性无机粘合剂选自粉末化氧化硅和硅酸盐玻璃。
10.如权利要求9所述的多孔陶瓷壁流过滤器体，其特征在于，所述永久性无机粘合剂与所述耐火填料的重量比值在1:20至2:3范围。
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