CN1883908A - 蜂窝结构体 - Google Patents

蜂窝结构体 Download PDF

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Publication number
CN1883908A
CN1883908A CNA2006100723701A CN200610072370A CN1883908A CN 1883908 A CN1883908 A CN 1883908A CN A2006100723701 A CNA2006100723701 A CN A2006100723701A CN 200610072370 A CN200610072370 A CN 200610072370A CN 1883908 A CN1883908 A CN 1883908A
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China
Prior art keywords
honeycomb structured
structured body
cellular unit
section
mentioned
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Granted
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CNA2006100723701A
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CN1883908B (zh
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大野一茂
国枝雅文
尾久和丈
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Ibiden Co Ltd
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Ibiden Co Ltd
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
    • B01J35/56—
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
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Abstract

本发明所提供的蜂窝结构体可以缓和由于蜂窝结构体发生局部温度变化而产生的热应力，不产生裂纹，强度和耐久性优异，对热冲击或振动的抗性强，而且，可以高度分散催化剂成分。本发明的蜂窝结构体是通过将多个柱状的蜂窝单元通过密封材料层结合成束而构成的，所述蜂窝单元中，多个小室隔着小室壁沿长度方向平行设置；其特征在于，所述蜂窝单元含有无机颗粒、无机纤维和/或晶须，所述蜂窝单元垂直于长度方向的截面的截面面积为5cm2～50cm2，所述密封材料层的热膨胀率αL与所述蜂窝单元的热膨胀率αF具有0.01≤|αL－αF|/αF≤1.0的关系。

Description

蜂窝结构体
技术领域
本发明涉及蜂窝结构体。
背景技术
以往，一般地，用于汽车的废气净化的蜂窝催化剂是通过在热膨胀性低的堇青石材质的蜂窝结构体的表面担载活性氧化铝等高比表面积材料和铂等催化剂金属来一体制造的。此外，为了在诸如贫燃发动机(leanbum engine)和柴油发动机等的氧气过剩氛围气下进行NOx处理，担载Ba等碱土金属作为NOx吸收剂。
但是，为了进一步提高净化性能，有必要提高废气与催化剂贵金属以及与NOx吸收剂的接触概率。所以，有必要进一步提高载体比表面积，减小贵金属颗粒的尺寸，并使贵金属颗粒高度分散。但是，若仅单纯地增加活性氧化铝等高比表面积材料的担载量，则只会导致氧化铝层的厚度增加，而不能提高接触概率，有可能产生压力损失过于增高等问题，所以针对小室(cell)形状、小室密度、小室壁的厚度等作出了改进(例如，参照特开平10-263416号公报)。
另一方面，作为由高比表面积材料形成的蜂窝结构体，已知有将高比表面积材料与无机纤维和无机粘合剂共同挤出成型的蜂窝结构体(例如，参照特开平5-213681号公报)。已知还有下述蜂窝结构体：为了将上述蜂窝结构体进行大型化，通过粘接层将蜂窝单元进行粘接而形成的蜂窝结构体(例如，参照DE4341159号公报)。
但是，上述现有技术存在下述问题：氧化铝等高比表面积材料由于热老化而产生烧结现象，比表面积减小；进一步，随着氧化铝等高比表面积材料比表面积的减小，所担载的铂等催化剂金属发生凝聚，粒径增大，比表面积减小。也就是说，为了在热老化后仍具有较高的比表面积，有必要在初期阶段提高其比表面积。此外，如上所述，为了进一步提高净化性能，有必要提高废气与催化剂金属以及与NOx吸收剂的接触概率。总之重点在于，使载体高比表面积化，减小催化剂金属的粒径，并使催化剂金属高度分散。但是，在诸如特开平10-263416号公报所公开的在堇青石材质的蜂窝结构体的表面担载活性氧化铝等高比表面积材料和铂等催化剂金属的蜂窝结构体中，为了提高与废气的接触概率，虽然对小室形状、小室密度和小室壁的厚度等进行了改进，使催化剂载体高比表面积化，但是还不够充分大。因此，存在催化剂金属未高度分散、热老化后废气净化性能不充分的问题。其中，上文所述的“热老化”包括下述两方面的含义：一方面是将蜂窝结构体作为催化剂载体使用时由于热所引起的热老化，另一方面是在进行加速试验等时由于其产热所致的热老化。
因此，为了弥补这种不足，可以通过大量地担载催化剂金属、或通过使催化剂载体本身大型化来解决此问题。但是铂等贵金属非常昂贵，是有限的贵重资源。此外，由于将蜂窝结构体设置于汽车时，其设置空间是非常有限的，因此上述方法都不适当。
进一步，对于特开平5-213681号公报所公开的将高比表面积材料与无机纤维以及无机粘合剂共同挤出成型的蜂窝结构体，由于基材本身由高比表面积的材料形成，因此其作为载体也具有高比表面积，并且可以充分地高度分散催化剂；但是为了保持基材氧化铝等的比表面积，不能充分进行烧结，基材的强度变得非常差。
进一步，如上所述，将蜂窝结构体用于汽车时，用于设置的空间是非常有限的。因此，为了提高单位体积载体的比表面积而使用了使小室壁变薄等方法，但是如此进一步降低了基材的强度。此外，氧化铝等的热膨胀率较大，烧制(预烧)时以及使用时，由于热应力容易生成裂纹。若考虑到这些问题，则将其用于汽车时，由于使用时会将温度急剧变化产生的热应力、以及大的振动等外力施加到该蜂窝结构体，使之容易破损，具有不能保持作为蜂窝结构体的形状、不能发挥作为催化剂载体的功能的问题。
进一步，在DE4341159号公报中所述的汽车用催化剂载体中，公开了使蜂窝单元的截面积大于等于200cm2以使蜂窝结构体大型化，但是由于受到了温度急剧变化导致的热应力、以及大的振动等，在这种情况下使用该蜂窝结构体时，如上所述，有容易破损、不能保持形状、不能发挥作为催化剂载体的功能的问题。
此外，例如，特开平8-28246号公报、特开2001-190916号公报等公开了将多个蜂窝单元通过粘接剂层结合成束而构成的蜂窝结构体。
而且，在具有这种结构的蜂窝结构体中，优选蜂窝单元的热膨胀率与粘接剂层的热膨胀率相等。
这是由于，上述蜂窝结构体在现实中例如在10℃～800℃的较宽的温度范围内进行使用，因而若蜂窝单元的热膨胀率和粘接剂层的热膨胀率不同，则由于它们的热膨胀率不同，会在蜂窝单元或粘接剂层上产生裂纹。
但是，若如此使蜂窝单元的热膨胀率与粘接剂层的热膨胀率完全相同，则所得到的蜂窝结构体与由单一的陶瓷部件所形成的蜂窝结构体实际上没有区别，在蜂窝结构体上担载催化剂时，由于催化剂量不均一，废气等所致的加热不均一，从而在蜂窝结构体上产生局部的温度变化，此时有可能在该局部的温度发生变化的部分和除此之外的部分之间产生较大的热应力，在蜂窝单元或粘接剂层上产生裂纹。
发明内容
本发明是为了解决上述问题而提出的，其目的在于提供蜂窝结构体，该蜂窝结构体可以缓和由于蜂窝结构体上发生局部温度变化而产生的热应力，不产生裂纹，对热冲击或振动的抗性强，耐久性优异，而且可以使催化剂成分高度分散。
本发明的蜂窝结构体是由将多个柱状的蜂窝单元通过密封材料层结合成束形成的陶瓷组件构成的蜂窝结构体，所述蜂窝单元中，多个小室隔着小室壁沿长度方向平行设置；其特征在于，所述蜂窝单元含有无机颗粒以及无机纤维和/或晶须，所述蜂窝单元垂直于长度方向的截面的截面面积为5cm2～50cm2，所述密封材料层的热膨胀率αL与所述蜂窝单元的热膨胀率αF具有0.01≤|αL-αF|/αF≤1.0的关系。
上述蜂窝结构体中，相对于所述蜂窝结构体垂直于长度方向的截面的截面面积，所述蜂窝单元垂直于长度方向的截面的截面面积的总和所占的比率优选大于等于85％，更优选大于等于90％。
对于上述蜂窝结构体，优选在其最外周形成涂覆材料层，所述涂覆材料层的热膨胀率αM与所述蜂窝单元的热膨胀率αF具有0.01≤|αM-αF|/αF≤1.0的关系。
上述蜂窝结构体中，所述无机颗粒优选为选自由氧化铝、氧化硅、氧化锆、氧化钛、氧化铈、莫来石和沸石组成的组中的至少1种。
此外，上述蜂窝结构体中，所述无机纤维和/或晶须优选为选自由氧化铝、氧化硅、碳化硅、氧化硅-氧化铝、玻璃、钛酸钾和硼酸铝组成的组中的至少1种。
上述蜂窝结构体中，所述蜂窝单元是使用含有所述无机颗粒、所述无机纤维和/或晶须、以及无机粘合剂的混合物来制造的，所述无机粘合剂优选为选自由氧化铝溶胶、氧化硅溶胶、氧化钛溶胶、水玻璃(waterglass)、海泡石和硅镁土组成的组中的至少1种。
上述蜂窝结构体优选担载有催化剂，所述催化剂优选含有选自由贵金属、碱金属、碱土金属和氧化物组成的组中的至少1种。
此外，上述蜂窝结构体优选用于车辆的废气净化。
本发明的蜂窝结构体，可以缓和由于蜂窝结构体局部发生温度变化而产生的热应力，对热冲击或振动的抗性强，耐久性优异，而且，可以高度分散催化剂成分。
此外，本发明的蜂窝结构体可以特别合适地用作催化剂转换器。
附图说明
图1(a)是说明构成本发明的蜂窝结构体的蜂窝单元的一个例子的示意立体图，图1(b)是说明本发明的蜂窝结构体的一个例子的示意立体图。
图2是实施例1涉及的蜂窝单元的小室壁的电子显微镜(SEM)照片。
图3是将多个蜂窝单元结合成束的实施例的说明图。
图4是将多个蜂窝单元结合成束的比较例的说明图。
图5(a)是振动试验使用的振动装置的正面图，图5(b)是振动装置的侧面图。
图6是压力损失测定装置的概略图。
符号说明
10蜂窝结构体
11蜂窝单元
12小室
14密封材料层
16涂覆材料层
具体实施方式
下文，参照附图对本发明的蜂窝结构体进行说明。
本发明的蜂窝结构体是将多个柱状蜂窝单元通过密封材料层结合成束而构成的蜂窝结构体，所述蜂窝单元中，多个小室隔着小室壁沿长度方向平行设置；其特征在于，所述蜂窝单元含有无机颗粒、无机纤维和/或晶须，所述蜂窝单元垂直于长度方向的截面的截面面积为5cm2～50cm2，所述密封材料层的热膨胀率αL与所述蜂窝单元的热膨胀率αF具有0.01≤|αL-αF|/αF≤1.0的关系。
本发明的蜂窝结构体中，由于将多个蜂窝单元通过密封材料层结合成束，因而对热冲击或振动的抗性强。这是因为，当由于温度的急剧变化等而在蜂窝结构体中产生温度分布时，该结构可以将在各个蜂窝单元上产生的温度差抑制在较低值，或者可以通过密封材料层来缓和热冲击、振动。此外，由于热应力等而使蜂窝单元产生裂纹时，该密封材料层可以抑制裂纹向蜂窝结构体的全体伸展，进一步发挥作为蜂窝结构体的框架的作用，使其保持作为蜂窝结构体的形状，不失去作为催化剂载体的功能。
对于所述蜂窝单元垂直于蜂窝结构体的长度方向的截面的截面面积(简称为截面面积，以下相同)，其下限为5cm2，上限为50cm2。截面面积小于5cm2时，由于将蜂窝单元彼此结合成束的密封材料层的截面面积增大，所以担载催化剂的比表面积相对减小，同时，压力损失相对增大；另一方面，若截面面积超过50cm2，则单元的尺寸过大，难以充分地抑制各个蜂窝单元所产生的热应力。
然而，若蜂窝单元的截面面积在5cm2～50cm2的范围内，则在蜂窝结构体中，可以调整密封材料层所占的比率，据此，可以保持较大的比表面积，结果，可以高度分散催化剂成分。
此外，即使对蜂窝结构体施加热冲击或振动等外力，也可以保持其作为蜂窝结构体的形状。进一步，可以减小压力损失。
因此，该蜂窝结构体可以高度分散催化剂成分，同时可提高其对于热冲击或振动的强度。
而且，可以根据下述式(1)来求得每单位体积的比表面积。
另外，当蜂窝结构体含有截面面积不同的多个蜂窝单元时，所谓蜂窝单元的截面面积是指作为构成蜂窝结构体的基本单元的蜂窝单元的截面面积，通常指的是蜂窝单元的最大截面面积。
上述截面面积的优选的下限为6cm2，更优选的下限为8cm2。另一方面，上述截面面积的优选的上限为40cm2，更优选的上限为30cm2。
此外，上述蜂窝结构体中，密封材料层的热膨胀率αL和蜂窝单元的热膨胀率αF的关系式|αL-αF|/αF的下限大于等于0.01，上限小于等于1.0。上述关系式中的各热膨胀率是在800℃测定的值。
在800℃下进行测定的原因在于800℃被认为大致是蜂窝结构体所需承受的上限温度。
即，构成本发明的蜂窝结构体的密封材料层的热膨胀率与蜂窝单元的热膨胀率并不相等，二者稍有不同。因此，上述蜂窝结构体中，即使由于担载催化剂时催化剂量的不均一或由于废气等所致加热的不均一而产生局部的燃烧，即发生局部的温度变化时，也可以合适地缓和在上述发生局部温度变化的部分和除此之外的部分之间所产生的热应力，不会在蜂窝单元或粘接剂层上产生裂纹，耐久性优异。
上述关系式|αL-αF|/αF小于0.01时，密封材料层的热膨胀率与蜂窝单元的热膨胀率基本相同，若由于担载催化剂时催化剂量的不均一或由于废气等所致加热的不均一而使蜂窝结构体局部发生燃烧时，不能充分地缓和在蜂窝结构体上由于局部发生燃烧而产生的局部热应力，有可能使蜂窝单元或密封材料层产生裂纹，甚至破坏蜂窝结构体。
另一方面，上述关系式|αL-αF|/αF超过1.0时，在蜂窝结构体通常的使用中，伴随着废气的温度差，密封材料层的热膨胀与蜂窝单元的热膨胀的差值过大，仍然可能使蜂窝单元或密封材料层产生裂纹，甚至破坏蜂窝结构体。
而且，上述关系式中，用于表示密封材料层的热膨胀率αL和蜂窝单元的热膨胀率αF的差αL-αF的分子部分是绝对值，这是由于，蜂窝单元的热膨胀率αF可以大于密封材料层的热膨胀率αL。
上述蜂窝结构体中，相对于上述蜂窝结构体垂直于长度方向的截面的截面面积，上述蜂窝单元的截面面积的总和所占的比率优选大于等于85％，更优选大于等于90％。
上述蜂窝单元的截面面积的总和所占的比率小于85％时，由于密封材料层的截面面积增大，蜂窝单元的总截面面积小，所以担载催化剂的比表面积相对减小，同时压力损失相对增大。
此外，上述比率大于等于90％时，可以进一步减小压力损失。
上述蜂窝结构体中，优选在其最外周形成涂覆材料层。
据此可以保护外周面，提高强度。
此外，形成涂覆材料层时，涂覆材料层的热膨胀率αM与蜂窝单元的热膨胀率αF的关系式|αM-αF|/αF的下限优选大于等于0.01，上限优选小于等于1.0。
上述关系式中的各热膨胀率是在800℃测定的值。
在800℃下进行测定的原因在于800℃被认为大致是蜂窝结构体所需承受的上限温度。
上述关系式|αM-αF|/αF小于0.01时，涂覆材料层的热膨胀率与蜂窝单元的热膨胀率基本相同，若由于担载催化剂时催化剂量的不均一或由于废气等所致加热的不均一而使蜂窝结构体局部产生燃烧时，不能充分地缓和由于局部发生燃烧而产生的局部热应力，有可能使蜂窝单元或涂覆材料层产生裂纹，甚至破坏蜂窝结构体。
另一方面，上述关系式|αM-αF|/αF超过1.0时，在蜂窝结构体的通常使用中，伴随着废气的温度差，涂覆材料层的热膨胀与蜂窝单元的热膨胀的差值过大，仍然可能使蜂窝单元或涂覆材料层产生裂纹，甚至破坏蜂窝结构体。
而且，上述关系式中，用于表示涂覆材料层的热膨胀率αM和蜂窝单元的热膨胀率αF的差αM-αF的分子部分是绝对值，这是由于蜂窝单元的热膨胀率αF可以大于涂覆材料层的热膨胀率αM。
此外，如后述所示，本发明的蜂窝结构体可以担载催化剂，此时，将担载催化剂后的密封材料层的热膨胀率设为αL，将担载催化剂后的蜂窝单元的热膨胀率设为αF，将担载催化剂后的涂覆材料层的热膨胀率设为αM。
对于将多个蜂窝单元结合成束而构成的蜂窝结构体的形状，不特别限定，可以举出例如，圆柱状、方柱状或椭圆柱状等。此外，对其尺寸也不特别限定。
构成本发明的蜂窝结构体的蜂窝单元含有无机颗粒以及无机纤维和/或晶须。
由此，通过无机颗粒来提高比表面积，通过无机纤维和/或晶须来提高多孔陶瓷的强度。
作为上述无机颗粒，优选为由氧化铝、氧化硅、氧化锆、氧化钛、氧化铈、莫来石和沸石等形成的颗粒。这些无机颗粒可以单独使用，也可以至少2种并用。其中，特别优选为氧化铝颗粒。
作为上述无机纤维或晶须，优选为由氧化铝、氧化硅、碳化硅、氧化硅-氧化铝、玻璃、钛酸钾、硼酸铝等形成的无机纤维或晶须。这些无机纤维或晶须可以单独使用，也可以至少2种并用。
对于上述无机纤维或上述晶须优选的长径比(长度/直径)，优选的下限为2，更优选的下限为5，进一步优选的下限为10。另一方面，优选的上限为1000，更优选的上限为800，进一步优选的上限为500。
而且，在长径比有差异时，上述无机纤维或晶须的长径比是其平均值。
对于上述蜂窝单元中所含有的上述无机颗粒的量，优选的下限为30重量％，更优选的下限为40重量％，进一步优选的下限为50重量％。
另一方面，优选的上限为97重量％，更优选的上限为90重量％，进一步优选的上限为80重量％，特别优选的上限为75重量％。
无机颗粒的含量小于30重量％时，有助于提高比表面积的无机颗粒的量相对减小，因而使蜂窝结构体的比表面积减小，担载催化剂成分时有时不能高度分散催化剂成分。另一方面，若超过97重量％，则有助于提高强度的无机纤维和/或晶须的量相对减小，蜂窝结构体的强度降低。
上述蜂窝单元所含有的上述无机纤维和/或晶须的合计量优选的下限为3重量％，更优选的下限为5重量％，进一步优选的下限为8重量％。另一方面，该合计量优选的上限为70重量％，更优选的上限为50重量％，进一步优选的上限为40重量％，特别优选的上限为30重量％。
无机纤维和/或晶须的合计量小于3重量％时，蜂窝结构体的强度降低；而超过50重量％时，则有助于提高比表面积的无机颗粒的量相对减小，所以作为蜂窝结构体的比表面积减小，担载催化剂成分时有时不能高度分散催化剂成分。
此外，上述蜂窝单元优选使用含有上述无机颗粒、上述无机纤维和/或晶须、以及无机粘合剂的混合物进行制造。
通过使用这种含有无机粘合剂的混合物，即使降低烧制生成型体的温度，也可以得到充分强度的蜂窝单元。
作为上述无机粘合剂，可以使用无机溶胶或粘土类粘合剂等。作为上述无机溶胶的具体例子，可以举出例如，氧化铝溶胶、氧化硅溶胶、氧化钛溶胶、水玻璃等。此外，作为粘土类粘合剂，可以举出例如陶土、高岭土、蒙脱土、海泡石、硅镁土等多链结构型粘土等。这些粘合剂可以单独使用，也可以至少2种并用。
其中，所述无机粘合剂优选为选自由氧化铝溶胶、氧化硅溶胶、氧化钛溶胶、水玻璃、海泡石和硅镁土组成的组中的至少1种。
上述无机粘合剂作为后述制造工序中所调制的原料糊的固体成分，其含量优选的下限为5重量％，更优选的下限为10重量％，进一步优选的下限为15重量％。另一方面，优选的上限为50重量％，更优选的上限为40重量％，进一步优选的上限为35重量％。
若上述无机粘合剂的含量超过50重量％，则成型性变差。
对上述蜂窝单元的形状不特别限定，优选为蜂窝单元彼此易于接合成束的形状，作为垂直于其长度方向的截面(下文仅称为截面)的形状，可以举出正方形、长方形、六边形或扇形等。
作为上述蜂窝单元的一个例子，截面为正方形的长方体的蜂窝单元如图所示。
图1(a)是说明构成本发明的蜂窝结构体的蜂窝单元的一个例子的示意立体图，图1(b)是说明本发明的蜂窝结构体的一个例子的示意立体图。
蜂窝单元11具有从近前侧走向后侧的多个小室12，还具有没有小室12的外表面13。
小室12之间的厚度(小室壁的厚度)不特别限定，优选的下限为0.05mm，更优选的下限为0.10mm，特别优选的下限为0.15mm。另一方面，优选的上限为0.35mm，更优选的上限为0.30mm，特别优选的上限为0.25mm。
小室壁的厚度小于0.05mm时，蜂窝单元的强度可能降低；另一方面，若小室壁的厚度超过0.35mm，则与废气的接触面积变小，气体不能充分渗透至深处，难以使小室壁内部所担载的催化剂与气体接触，因而可能降低催化剂性能。
此外，上述蜂窝单元的小室密度的优选的下限为15.5个/cm2(100cpsi)，更优选的下限为46.5个/cm2(300cpsi)，进一步优选的下限为62.0个/cm2(400cpsi)。另一方面，小室密度的优选的上限为186个/cm2(1200cpsi)，更优选的上限为170.5个/cm2(1100cpsi)，进一步优选的上限为155个/cm2(1000cpsi)。
小室密度小于15.5个/cm2时，与蜂窝单元内部的废气接触的壁的面积变小；若超过186个/cm2，则压力损失增大，同时，有可能难以制造蜂窝单元。
对形成于蜂窝单元的小室的截面形状不特别限定，除了如图1(a)所示的四边形以外，也可以大致为三角形、或大致为六边形。
接着，对本发明的蜂窝结构体的制造方法按照工序的顺序进行说明。
首先，使用以上述无机颗粒与上述无机纤维和/或晶须为主要成分的原料糊来进行挤出成型等，制造成型体。
在上述原料糊中，除了上述成分外，根据需要，还可以适当地添加上述无机粘合剂、有机粘合剂、分散介质和成型助剂以符合成型性要求。
作为上述有机粘合剂，不特别限定，可以举出例如，甲基纤维素、羧甲基纤维素、羟乙基纤维素、聚乙二醇、酚树脂和环氧树脂等。
这些有机粘合剂可以单独使用，也可以至少2种并用。
相对于上述无机颗粒、上述无机纤维、上述晶须、上述无机粘合剂的合计量100重量份，上述有机粘合剂的配合量优选为1重量份～10重量份。
作为上述分散介质，不特别限定，可以举出例如，水、有机溶剂(苯等)、醇(甲醇等)等。
作为成型助剂，不特别限定，可以举出例如，乙二醇、糊精、脂肪酸、脂肪酸皂、多元醇等。
对上述原料糊的调制不特别限定，优选进行混合-混炼，例如，可以使用搅拌机、磨碎机等来进行混合，也可以使用混炼机等来充分地进行混炼。
上述原料糊的成型方法不特别限定，优选通过上述的挤出成型等来成型为具有小室的形状。
接着，根据需要，通过使用干燥机对得到的成型体进行干燥，得到干燥体。
作为上述干燥机，可以举出例如，微波干燥机、热风干燥机、电介质干燥机、减压干燥机、真空干燥机和冷冻干燥机等。
接着，将所得到的干燥体根据需要进行脱脂。
脱脂的条件不特别限定，可以根据成型体所含有的有机物的种类、含量来适当选择，优选在约400℃下脱脂2小时。
接着，对根据需要实施了干燥、脱脂处理的成型体进行烧制。
烧制条件不特别限定，优选为600℃～1200℃，更优选为600℃～1000℃。
选择上述烧制温度是由于，当烧制温度小于600℃时，陶瓷颗粒等有可能未进行烧结，降低作为蜂窝结构体的强度；若超过1200℃，则陶瓷颗粒等的烧结过度，单位体积的比表面积减小，有可能不能充分地将担载的催化剂成分高度分散。
经过这些工序，可以制造柱状的蜂窝单元，所述柱状蜂窝单元中，多个小室隔着小室壁沿长度方向平行设置。
另外，上述蜂窝单元的热膨胀率αF可以通过配合在混合组合物中的材料或烧制条件来确定。
接着，在得到的蜂窝单元上涂布用于形成密封材料层的密封材料糊，将蜂窝单元顺序地结合成束，然后进行干燥、固定化，制成通过密封材料层结合成束的规定大小的蜂窝单元接合体。
作为密封材料糊，不特别限定，可以使用例如，混合有无机粘合剂和陶瓷颗粒的密封材料糊、混合有无机粘合剂和无机纤维的密封材料糊、混合有无机粘合剂、陶瓷颗粒和无机纤维的密封材料糊等。
此外，可以在这些密封材料糊中加入有机粘合剂。
作为上述有机粘合剂，不特别限定，可以举出例如，聚乙烯醇、甲基纤维素、乙基纤维素、羧甲基纤维素等。
这些有机粘合剂可以单独使用，也可以至少2种。
上述密封材料层的厚度优选为0.5mm～2mm。
若密封材料层的厚度小于0.5mm，则有可能得不到充分的接合强度。此外，由于密封材料层是不发挥作为催化剂载体作用的部分，因此若其厚度超过2mm，则蜂窝结构体每单位体积的比表面积降低，担载催化剂成分时，有可能不能充分地将催化剂高度分散。
此外，若密封材料层的厚度超过2mm，则压力损失有可能增大。
此外，其中，在后述的热处理后，使密封材料层的热膨胀率αL和上述蜂窝单元的热膨胀率αF满足0.01≤|αL-αF|/αF≤1.0的关系来调制密封材料层的热膨胀率αL。
此外，可以按照蜂窝结构体的大小适当地确定结合成束的蜂窝单元的数目。此外，对通过密封材料层将蜂窝单元结合成束而构成的蜂窝单元接合体，可以根据需要进行适当的切断、研磨等，得到陶瓷组件。
接着，根据需要，在陶瓷组件的外周面涂布涂覆材料糊，通过干燥、固定化来形成涂覆材料层。
通过形成上述涂覆材料层，可以保护陶瓷组件的外周面，结果，可以提高蜂窝结构体的强度。
此外，在后述的热处理后，调制涂覆材料层的热膨胀率αM，使涂覆材料层的热膨胀率αM与上述蜂窝单元的热膨胀率αF满足0.01≤|αM-αF|/αF≤1.0的关系。
对于上述涂覆材料糊不特别限定，可以是含有与上述密封材料糊相同的材料的材料糊，也可以是含有与上述密封材料糊不同的材料的材料糊。
此外，上述涂覆材料糊是含有与上述密封材料糊相同的材料的材料糊时，两材料糊的构成成分的配合比可以相同，也可以不同。
对于上述涂覆材料层的厚度不特别限定，优选为0.1mm～2mm。小于0.1mm时，不能保护外周面，有可能不能提高强度；若超过2mm，则蜂窝结构体每单位体积的比表面积降低，担载催化剂成分时，有可能不能充分地将催化剂成分高度分散。
此外，利用本制造方法时，优选在通过密封材料层将多个蜂窝单元结合成束后(设置有涂覆材料层时，在形成涂覆材料层后)进行预烧制。
据此可以将密封材料层、涂覆材料层含有的有机粘合剂等通过预烧制脱脂除去。
预烧制的条件可以根据所含有的有机物的种类、含量来适当地确定，优选在约700℃下预烧制2小时。
其中，作为蜂窝结构体的一个例子，参照图1(b)对蜂窝结构体进行说明。图1(b)的蜂窝结构体是将多个截面为正方形的长方体的蜂窝单元结合成束而形成的外形为圆柱状的蜂窝结构体。
蜂窝结构体10中，通过密封材料层14将蜂窝单元11结合成束，切断成圆柱状后，通过涂覆材料层16覆盖陶瓷组件中没有形成小室12的外周面。
此外，利用上述制造方法，可以将蜂窝单元预先成型为截面为扇形的形状，或将其预先成型为截面为正方形的形状，将这些蜂窝单元通过密封材料层结合成束，制造具有规定形状的蜂窝结构体(例如，图1(b)中为圆柱状)。
此时，可以省略切断、研磨工序。
上述本发明蜂窝结构体的用途不特别限定，优选用作车辆的废气净化用的催化剂载体。
此外，用作柴油发动机的废气净化用的催化剂载体时，可以与具有碳化硅等陶瓷蜂窝结构并具有过滤废气中的粒状物质(PM)进行燃烧净化功能的柴油-颗粒-过滤器(DPF)并用。此时，对于本发明的蜂窝结构体和DPF的位置关系，本发明的蜂窝结构体可以在前侧或后侧。
这是因为，设置于前侧时，本发明的蜂窝结构体在发生伴随着产热的反应时，可以将热量传播到后侧的DPF，从而可促进DPF再生时的升温。此外，设置于后侧时，由于废气中的PM通过DPF进行过滤后，穿过本发明的蜂窝结构体的小室，因而不易引起堵塞；进一步，当利用DPF使PM燃烧时，对于不完全燃烧产生的气体成分，也可以使用本发明的蜂窝结构体来进行处理。
而且，该蜂窝结构体可以用于上述背景技术中所记载的用途等；进一步，也可用于不担载催化剂成分而进行使用的用途中(例如，吸附气体成分或液体成分的吸附材料等)，可以无特别限定地使用本发明的蜂窝结构体。
此外，可以在上述蜂窝结构体上担载催化剂，制成蜂窝催化剂。
作为上述催化剂，不特别限定，可以举出例如，贵金属、碱金属、碱土金属、氧化物等。
这些催化剂可以单独使用，也可以至少2种并用。
作为上述贵金属，可以举出例如，铂、钯、铑等；作为上述碱金属，可以举出例如，钾、钠等；作为上述碱土金属，可以举出例如钡等；作为上述氧化物，可以举出钙钛矿(La0.75K0.25MnO3等)、CeO2等。
担载有上述催化剂的蜂窝结构体(蜂窝催化剂)例如可以用作车辆的废气净化用的所谓三元催化剂、NOx吸收催化剂等，但不特别限定。
而且，对于担载催化剂的时期，不特别限定，可以在制成蜂窝结构体后担载催化剂，也可以在原料的陶瓷粒子的阶段担载催化剂。
此外，对于担载催化剂的方法，不特别限定，例如可以通过浸渗法来担载催化剂成分。
实施例
下文举出实施例来对本发明进行更详细的说明，但本发明并不限于这些实施例。
(糊料D的调制)
将29重量％的γ-氧化铝颗粒(平均粒径2μm)、7重量％的氧化硅-氧化铝纤维(平均纤维径为10μm，平均纤维长为100μm)、34重量％的氧化硅溶胶(固体浓度为30重量％)、5重量％的羧甲基纤维素(CMC)和25重量％的水混合，得到糊料D。
而且，糊料D固化后的热膨胀率(800℃)为6.00×10-6(1/K)。
(糊料A、B、C、E、F的调制)
改变配合物和配合量，使其分别如表1所示，除此以外，与糊料D同样地操作，调制各糊料。
而且，表1也表示了各糊料的热膨胀率(800℃)。
[表1]
                           糊料
  A   B   C   D   E   F
  γ-氧化铝颗粒(平均粒径为2μm)   -   -   -   29   29   29
  氧化硅颗粒(平均粒径为2μm)   -   -   29   -   -   -
  SiC颗粒(平均粒径为0.5μm)   29   29   -   -   -   -
  氧化硅-氧化铝纤维(平均纤维径为10μm，平均纤维长为100μm)   7   -   7   7   7   -
  氧化铝纤维(平均纤维径为10μm，平均纤维长为100μm)   -   7   -   -   -   7
  氧化硅溶胶(固体浓度为30重量％)   34   34   34   34   -   -
  氧化铝溶胶(固体浓度为30重量％)   -   -   -   -   34   34
  CMC   5   5   5   5   5   5
  水   25   25   25   25   25   25
  热膨胀率(800℃)(×10-6)(1/K)   3.8   3.85   3.0   6.0   7.6   7.8
(注)各配合量的单位为重量％。
(实施例1)
(1)将40重量％的γ-氧化铝颗粒(平均粒径为2μm)、10重量％的氧化硅-氧化铝纤维(平均纤维径为10μm，平均纤维长为100μm，长径比为10)、50重量％的氧化硅溶胶(固体浓度为30重量％)混合，得到混合物。相对于100重量份所得到的混合物，加入6重量份作为有机粘合剂的甲基纤维素，并加入少量的增塑剂和润滑剂，进一步进行混合-混炼来得到混合组合物。接着，通过挤出成型机来对该混合组合物进行挤出成型，得到生成型体。
(2)接着，使用微波干燥机和热风干燥机，对上述生成型体进行充分干燥，进一步，在400℃下保持2小时进行脱脂。
然后，在800℃下保持2小时进行烧制，得到方柱状(34.3mm×34.3mm×150mm)、小室密度为93个/cm2(600cpsi)、小室壁的厚度为0.2mm、小室的截面形状为四边形(正方形)的蜂窝单元11。
该蜂窝单元11的壁面的电子显微镜(SEM)照片如图2所示。
由该照片可知，该蜂窝单元11中，氧化硅-氧化铝纤维沿着原料糊的挤出方向进行定向。
此外，经过本工序来制造的蜂窝单元的热膨胀率αF(800℃)为3.8×10-6(1/K)。
(3)接着，使用上述糊料D作为密封材料糊，将多个蜂窝单元11结合成束，得到陶瓷组件。
从具有小室的一面(作为正面，以下相同)看到的将多个蜂窝单元11结合成束的陶瓷组件如图3(a)所示。
该陶瓷组件是如下形成的：在上述蜂窝单元11的外表面13涂布密封材料糊(糊料D)，使密封材料层14的厚度为1mm，以此将多个蜂窝单元11结合成束、固定在一起，形成该陶瓷组件。
(4)该陶瓷组件制造完成后，使用钻石刀将该陶瓷组件切断成圆柱状使陶瓷组件的正面大致为点对称，然后，在不具有小室的圆形的外表面(陶瓷组件的外周面)上涂布上述作为涂布材料糊的糊料D，使其厚度为0.5mm，对上述外表面进行涂布。
(5)接着，120℃下进行干燥，700℃下保持2小时，进行密封材料糊和涂覆材料糊的脱脂，得到圆柱状(直径143.8mm×高度150mm)的蜂窝结构体10。
对于由本实施例制造的蜂窝结构体，蜂窝单元的截面形状、蜂窝单元的截面面积、蜂窝单元的截面所占的比率(相对于蜂窝结构体的截面面积，蜂窝单元的截面面积的总和所占的比率)等各种数值如下述表2所示。
此外，对于由本实施例制造的蜂窝结构体，|αL-αF|/αF的值和|αM-αF|/αF的值如表2所示。
而且，表2也示出了其他实施例和比较例的各种数值。
(实施例2、3)
将蜂窝单元制成如表2所示形状，除此以外，与实施例1同样地操作来制造蜂窝结构体。
而且，对于实施例2、3涉及的陶瓷组件，从正面看到的示意图分别如图3(b)、图3(c)所示。
(实施例4)
分别使用上述糊料B作为密封材料糊和涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(实施例5)
分别使用上述糊料C作为密封材料糊和涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(实施例6)
分别使用上述糊料E作为密封材料糊和涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(实施例7)
使用上述糊料D作为密封材料糊，使用上述糊料A作为涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(实施例8)
使用上述糊料D作为密封材料糊，使用上述糊料F作为涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(比较例1、2)
将蜂窝单元制成如表2所示的形状，除此以外，与实施例1同样地操作来制造蜂窝结构体。
而且，对于比较例1、2涉及的陶瓷组件，从正面看到的示意图分别如图4(a)、(b)所示。
(比较例3)
分别使用上述糊料A作为密封材料糊和涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
(比较例4)
分别使用上述糊料F作为密封材料糊和涂覆材料糊，除此以外，与实施例1同样地操作来制造蜂窝结构体。
[表2]
                蜂窝单元              密封材料层                涂覆层
截面形状 截面面积 截面所占比率 厚度   糊料 |αL-αF|/αF 厚度   糊料 |αM-αF|/αF
 实施例1   3.43cm方   11.8cm2   93.5％   1mm   D   0.579   0.5mm   D   0.579
 实施例2   2.24cm方   5.0cm2   90.2％   1mm   D   0.579   0.5mm   D   0.579
 实施例3   7.10cm方   50.0cm2   95.5％   1mm   D   0.579   0.5mm   D   0.579
 实施例4   3.43cm方   11.8cm2   93.5％   1mm   B   0.013   0.5mm   B   0.013
 实施例5   3.43cm方   11.8cm2   93.5％   1mm   C   0.211   0.5mm   C   0.211
 实施例6   3.43cm方   11.8cm2   93.5％   1mm   E   1.000   0.5mm   E   1.000
 实施例7   3.43cm方   11.8cm2   93.5％   1mm   D   0.579   0.5mm   A   0
 实施例8   3.43cm方   11.8cm2   93.5％   1mm   D   0.579   0.5mm   F   1.053
 比较例1   2.00cm方   4.0cm2   89.7％   1mm   D   0.579   0.5mm   D   0.579
 比较例2   7.41cm方   55.0cm2   95.6％   1mm   D   0.579   0.5mm   D   0.579
 比较例3   3.43cm方   11.8cm2   93.5％   1mm   A   0   0.5mm   A   0
 比较例4   3.43cm方   11.8cm2   93.5％   1mm   F   1.053   0.5mm   F   1.053
(评价)
通过下述方法，测定所制造的蜂窝结构体的特性。
[比表面积测定]
首先，实测蜂窝单元和密封材料层的体积，计算相对于蜂窝结构体的体积，蜂窝单元所占的比率A(体积％)。接着，测定蜂窝单元的每单位重量的BET比表面积B(m2/g)。BET比表面积是使用BET测定装置(岛津制作所社制，Micromeritics FlowSorbII-2300)、根据用日本工业标准规定的JIS-R-1626(1996)通过1点法进行测定的。测定时，使用切成圆柱状小片(直径15mm×高度15mm)的样品。接着由蜂窝单元的重量和外形的体积计算蜂窝单元的表观密度C(g/L)，由下式(1)求得蜂窝结构体的比表面积S(m2/L)，而且其中的蜂窝结构体的比表面积是蜂窝结构体相对于每表观体积的比表面积。
S(m2/L)＝(A/100)×B×C               (1)
[热冲击-振动重复试验]
热冲击试验中，在蜂窝结构体的外周面缠绕氧化铝衬垫(三菱化学社制MAFTEC，46.5cm×15cm，厚度为6mm，该氧化铝衬垫为由氧化铝纤维形成的绝热材料)，以放入金属外壳21的状态投入设定为600℃的烧制炉中，加热10分钟，从烧制炉取出，急剧冷却至室温。接着，以将蜂窝结构体放入该金属外壳的方式，直接进行振动试验。图5(a)表示振动试验使用的振动装置20的正面图，图5(b)表示振动装置20的侧面图。将放有蜂窝结构体的金属外壳21置于底座22之上，通过螺丝24拧紧略呈U字形的固定设备23，以此来固定金属外壳21。于是，金属外壳21以与底座22和固定设备23成为一体的状态进行振动。进行振动试验的条件如下：频率为160Hz，加速度为30G，振幅为0.58mm，保持时间为10小时，室温下，振动方向为Z轴方向(上下方向)。各自10次交替反复进行该热冲击试验和振动试验，测定试验前的蜂窝结构体的重量T0和试验后的重量Ti，使用下式(2)求得重量减少率G。
G(重量％)＝100×(T0-Ti)/T0           (2)
[压力损失测定]
压力损失测定的装置40如图6所示。测定方法如下：将缠绕氧化铝衬垫的蜂窝结构体放入金属外壳中，将上述放入金属外壳的蜂窝结构体配置于2L的共轨式柴油发动机的排气管中，在蜂窝结构体的前后安装压力计来进行测定。而且，设定的测定条件如下，发动机旋转数为1500rpm，扭矩为50Nm。测定运转开始5分钟后的压差。
[表3]
     比表面积(m2/L)   热冲击-振动试验的减少率G(重量％)   压力损失(kPa)
  蜂窝单元   蜂窝结构体
 实施例1   42000   39270   0   2.4
 实施例2   42000   37884   0   2.5
 实施例3   42000   40110   3   2.3
 实施例4   42000   39270   3   2.4
 实施例5   42000   39270   0   2.4
 实施例6   42000   39270   4   2.4
 实施例7   42000   39270   6   2.4
 实施例8   42000   39270   9   2.4
 比较例1   42000   37674   0   2.8
 比较例2   42000   40152   52   2.3
 比较例3   42000   39270   24   2.4
 比较例4   42000   39270   32   2.4
由上述结果可知，对于实施例1～实施例6涉及的蜂窝结构体，热冲击-振动试验中的重量减少率G为0重量％～4重量％，对热冲击和振动的抗性强，耐久性优异。
与此相对，对于比较例1涉及的蜂窝结构体，虽然热冲击-振动试验中的重量减少率G小，但是与实施例涉及的蜂窝结构体相比，在压力损失方面变差。这是由于蜂窝单元的截面面积小，因而蜂窝单元的截面所占有的比率必然随之减小，结果，压力损失增高。此外，对于比较例2～比较例4涉及的蜂窝结构体，热冲击-振动试验中的重量减少率G大，强度或耐久性差。推测其原因是由于蜂窝单元的截面面积不在5.0cm2～50.0cm2的范围内(比较例1、2)、或不满足0.01≤|αL-αF|/αF≤1.0的关系(比较例3、4)而造成的。
而且，对于实施例7和实施例8涉及的蜂窝结构体，与实施例1～实施例6涉及的蜂窝结构体相比，其热冲击-振动试验中的重量减少率G在容许的范围内，但是稍差。这是由于，实施例7和实施例8涉及的蜂窝结构体中，虽然密封材料层的热膨胀率αL和蜂窝单元的热膨胀率αF之间满足0.01≤|αL-αF|/αF≤1.0的关系，但是涂覆层的热膨胀率αM和蜂窝单元的热膨胀率αF之间不满足0.01≤|αM-αF|/αF≤1.0的关系。根据这种结果可知，优选涂覆层的热膨胀率αM和蜂窝单元的热膨胀率αF之间满足0.01≤|αM-αF|/αF≤1.0的关系。
此外，实施例涉及的蜂窝结构体具有较高的比表面积。

Claims (10)

1.蜂窝结构体，其是将多个柱状的蜂窝单元通过密封材料层结合成束而构成的蜂窝结构体，所述蜂窝单元中，多个小室隔着小室壁沿长度方向平行设置；其特征在于，所述蜂窝单元含有无机颗粒以及无机纤维和/或晶须，所述蜂窝单元垂直于长度方向的截面的截面面积为5cm2～50cm2，所述密封材料层的热膨胀率αL与所述蜂窝单元的热膨胀率αF具有0.01≤|αL-αF|/αF≤1.0的关系。
2.如权利要求1所述的蜂窝结构体，其中，相对于蜂窝结构体垂直于长度方向的截面的截面面积，所述蜂窝单元垂直于长度方向的截面的截面面积的总和所占的比率大于等于85％。
3.如权利要求1所述的蜂窝结构体，其中，相对于蜂窝结构体垂直于长度方向的截面的截面面积，所述蜂窝单元垂直于长度方向的截面的截面面积的总和所占的比率大于等于90％。
4.如权利要求1～3任意一项所述的蜂窝结构体，其中，在其最外周形成有涂覆材料层，所述涂覆材料层的热膨胀率αM与所述蜂窝单元的热膨胀率αF具有0.01≤|αM-αF|/αF≤1.0的关系。
5.如权利要求1～4任意一项所述的蜂窝结构体，其中，所述无机颗粒为选自由氧化铝、氧化硅、氧化锆、氧化钛、氧化铈、莫来石和沸石组成的组中的至少1种。
6.如权利要求1～5任意一项所述的蜂窝结构体，其中，所述无机纤维和/或晶须为选自由氧化铝、氧化硅、碳化硅、氧化硅-氧化铝、玻璃、钛酸钾和硼酸铝组成的组中的至少1种。
7.如权利要求1～6任意一项所述的蜂窝结构体，其中，所述蜂窝单元是使用含有所述无机颗粒、所述无机纤维和/或晶须、以及无机粘合剂的混合物进行制造的，所述无机粘合剂为选自由氧化铝溶胶、氧化硅溶胶、氧化钛溶胶、水玻璃、海泡石和硅镁土组成的组中的至少1种。
8.如权利要求1～7任意一项所述的蜂窝结构体，其担载有催化剂。
9.如权利要求8所述的蜂窝结构体，其中，所述催化剂含有选自由贵金属、碱金属、碱土金属和氧化物组成的组中的至少1种。
10.如权利要求1～9任意一项所述的蜂窝结构体，其用于车辆的废气净化。
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