CN101010266A - 陶瓷蜂窝结构体 - Google Patents

陶瓷蜂窝结构体 Download PDF

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Publication number
CN101010266A
CN101010266A CNA2006800007057A CN200680000705A CN101010266A CN 101010266 A CN101010266 A CN 101010266A CN A2006800007057 A CNA2006800007057 A CN A2006800007057A CN 200680000705 A CN200680000705 A CN 200680000705A CN 101010266 A CN101010266 A CN 101010266A
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China
Prior art keywords
structural body
ceramic
honeycomb structural
mentioned
ceramic honeycomb
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Pending
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CNA2006800007057A
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English (en)
Inventor
藤田祐基
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Ibiden Co Ltd
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Ibiden Co Ltd
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Application filed by Ibiden Co Ltd filed Critical Ibiden Co Ltd
Publication of CN101010266A publication Critical patent/CN101010266A/zh
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
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    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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    • B01D46/2455—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the whole honeycomb or segments
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Abstract

本发明提供一种陶瓷蜂窝结构体，该陶瓷蜂窝结构体防止容易产生的变形、或错位等的状态，耐久性优良；由组合并粘结了多个柱状的多孔蜂窝状陶瓷构件的单元而组成，该柱状的多孔蜂窝状陶瓷构件是用作气体通路的许多小室沿长度方向隔着小室壁并排设置而成的；使上述多孔蜂窝状陶瓷构件的两端部的、与构件的长度方向正交的截面的大小大于该构件的长度方向中心部分的截面的大小。

Description

陶瓷蜂窝结构体
相关申请的记载
本申请是将2005年2月4日申请的日本专利申请2005-28942号作为基础申请的、要求优先权的申请。
技术领域
本发明涉及一种陶瓷蜂窝结构体，该结构体可以作为用于捕获、除去从柴油机等内燃机排出的废气中所含有的粒子状物质(以下称作“微粒”)等的过滤器、及/或作为用于除去废气中的HC、CO或NOX等的有害成分的催化剂载体等而进行使用。
背景技术
在从巴士、卡车等的车辆或建筑机械等的内燃机排出的废气中，含有对环境或人体给予有害的影响的微粒或有害气体。为此，近年来，正在研究用于从废气中捕获、除去上述微粒的技术。在这样研究出的技术中的一项技术中，有一种用作废气净化用过滤器的陶瓷蜂窝结构体。该陶瓷蜂窝结构体由蜂窝结构的多孔质陶瓷构件而组成，作为从废气中捕获、除去微粒的陶瓷蜂窝过滤器而被具体化。
如图1所示的那样，在上述陶瓷蜂窝过滤器中使用了陶瓷蜂窝结构体10，而该陶瓷蜂窝结构体10是通过隔着密封材料层14而将多个棱柱状的多孔陶瓷构件(单元)11组合起来而做成陶瓷块，并在该陶瓷块的外周围上包覆废气泄漏防止用密封材料层16而组成的。该陶瓷蜂窝结构体10是将具有柱状的蜂窝结构的上述陶瓷构件(单元)11做成一个结构单位，将多个该结构单位粘结成截面呈圆形、椭圆形或多边形状而成的结构体。
如图1(a)所示的那样，在每个上述陶瓷构件11中，用作气体通路的许多小室12沿长度方向隔着小室壁13并排设置。并且，在将上述陶瓷蜂窝结构体10作为废气净化用过滤器使用时，主要是用密封材料对这些小室12的端面交替地进行封闭，在流入了小室12的废气通过上述小室壁13之中(壁流)时，废气中的微粒被小室壁13捕获。
如上述那样，将多个柱状的陶瓷构件粘结而构成陶瓷蜂窝结构体(过滤器)的理由如下述那样：即，由于陶瓷蜂窝结构体在将其一体成形而做成较大的结构时，作为陶瓷构件，即使使用了耐热性较高、机械特性优良、且热传导系数较大的碳化硅，也会因废气的温度变化或局部的发热而在陶瓷蜂窝结构体内产生温度差，由于该温度差而引起热膨胀差，从而在陶瓷蜂窝结构体上易于产生裂纹。因此，通过将该过滤器做成多个陶瓷构件(单元)的组合结构、且各陶瓷构件(单元)之间隔着密封材料层将各陶瓷构件相粘接而使之一体化，而可以缓和作用于过滤器的热应力。
但是，在将陶瓷蜂窝结构体做成柱状的陶瓷构件(单元)的组合结构时，存在这样的问题：当陶瓷构件的外壁平滑时，该构件相互间的粘接力变弱，由使用时的振动或废气的压力等的影响而导致陶瓷构件相互间的粘接部分剥离、陶瓷构件相互错位或破损等而使得耐久性差。为此，在日本特开2001-138416号公报所记载的技术中，提出了一种这样的方案：在成为各蜂窝模块(陶瓷构件)的粘接面的外壁上做出平面度为0.2mm～1.5mm左右的凹凸或起伏。
发明内容
以往的陶瓷蜂窝结构体是在相当于陶瓷构件(单元)的上述模块外壁面的整个面上，只是均匀地加工出外壁面的表面成为粗糙面的程度较小的凹凸或起伏的构造。为此，该蜂窝结构体存在当密封材料层的粘接力不大时容易产生变形、错位等的耐久性方面的问题。
本发明的目的在于解决以往技术所存在的这样的问题，特别是在于提供一种耐久性优良的陶瓷蜂窝结构体。
即，本发明是一种由组合并粘结多个柱状的多孔质蜂窝状陶瓷构件而成的陶瓷蜂窝结构体，该柱状的多孔蜂窝状陶瓷构件是用作气体通路的许多小室沿长度方向隔着小室壁并排设置而成的。该陶瓷蜂窝结构体的特征在于：使上述多孔质蜂窝状陶瓷构件的两端部上的、与构件的长度方向正交的截面的大小大于该构件的长度方向中心部分的截面的大小。
另外，对于本发明的陶瓷蜂窝结构体，最好为下述的状态：被设定得比上述中心部分的截面大的构件两端部的区域从各端面起在长度方向长度的0.5～25％的范围内；上述构件的两端部的截面的大小为该构件的长度方向中心部分的截面积的1.01～1.10倍；上述构件由从氮化铝、氮化硅、氮化硼、氮化钛、碳化硅、碳化锆、碳化钛、碳化钽、碳化钨、氧化铝、氧化锆、堇青石、多铝红柱石及钛酸铝中选取的、任何1种或1种以上的物质而构成；上述构件两端部的截面形状为三角形、四边形及六边形中的任一种形状；以及上述构件中心部分的截面形状与上述构件两端部的截面形状相同。
并且，本发明的陶瓷蜂窝结构体最好为这样的状态：将上述小室的任一端部封闭，并作为捕获、除去废气中所含有的粒子状物质的过滤器使用；或者是在上述小室壁表面上载有催化剂成分，而作为废气净化用催化剂载体使用。该催化剂成分由从Pt、Pd及Rh之中选取的任何1种或1种以上的贵金属或这些贵金属的合金而组成。
本发明的陶瓷蜂窝结构体通过使柱状的多孔质陶瓷构件的两端部的、与构件的长度方向正交的截面的大小大于该构件的长度方向中心部分的截面的大小，可以有效地防止在隔着密封材料层而组合多个陶瓷构件并将其一体化时产生的、陶瓷构件相互间的错位，可以期望提高作为过滤器及催化剂载体的耐久性。
附图说明
图1(a)是表示多孔质陶瓷构件的一个例子的立体图，图1(b)是表示集合型陶瓷蜂窝过滤器的一个例子的立体图。
图2(a)是表示本发明的、层叠了多个多孔质蜂窝状陶瓷构件的陶瓷蜂窝结构体的长度方向截面的立体图，图2(b)是表示以往的陶瓷蜂窝结构体的长度方向截面的立体图。
图3是本发明的陶瓷蜂窝结构体的立体图。
图4是用于本发明的实施例的多孔质蜂窝状陶瓷构件的概略图。
具体实施方式
图2(a)是沿构件的长度方向切断了多孔质蜂窝状陶瓷构件11(以下简称作“陶瓷构件”)时的剖视图。如该图所示的那样，本发明的陶瓷蜂窝结构体10，例如，做成使棱柱状的陶瓷构件11的两端部的、与构件的长度方向正交的截面的大小大于该构件的长度方向中心部分的截面的大小，且各陶瓷构件11之间对于两端部相邻的边相互密接的状态的构造。并且，主要在相邻的陶瓷构件11相互间的、构件长度方向的靠近中心的部分生成的空间里，通过设置给予了粘接作用的密封材料而形成密封材料层14。
作为构成上述密封材料层14的材料，例如，可以使用使由无机粘合剂、有机粘合剂、无机纤维及/或无机粒子而组成的材料干燥、固化并且按照需要在约700℃或700℃以上的温度烧结而成的材料等。
作为构成密封材料层14的上述无机粘合剂，可以使用例如硅溶胶、氧化铝溶胶等。这些溶胶等可以单独使用，也可以2种或2种以上并用。在上述无机粘合剂之中，最好是使用硅溶胶。
作为上述有机粘合剂，可以使用例如聚乙烯醇、甲基纤维素、乙基纤维素、羧甲基纤维素等。这些材料可以单独使用，也可以2种或2种以上并用。在上述有机粘合剂之中，最好是使用甲基纤维素。
作为上述无机纤维，可以使用例如硅酸铝、多铝红柱石、氧化铝、二氧化硅等的陶瓷纤维等。这些材料可以单独使用，也可以2种或2种以上并用。在上述无机纤维之中，最好是使用硅酸铝纤维。
作为上述无机粒子，可以使用例如碳化物、氮化物等，具体地说，可以使用由碳化硅、氮化硅、氮化硼等组成的无机粉末或者晶须等。这些成分可以单独使用，也可以2种或2种以上并用。在上述无机粒子之中，最好是使用导热性优良的碳化硅。
上述密封材料层14可以由致密体构成，也可以是可向其内部流入废气的多孔质体。
如图3所示的那样，组合了多个陶瓷构件11而成的蜂窝结构体10是并列配置了多个成为废气的通路的沿构件的长度方向的小室12的结构。在将该结构体作为过滤器使用时，该结构体成为这样的结构：上述小室12的废气入口侧或出口侧的任一侧的端部由密封材料15密封为例如西洋跳棋盘状(将这些小室12的端部开口隔一个堵一个的形状)，将这些小室12相互隔断的小室壁13作为过滤器而发挥作用。
在这种情况下，从小室12的废气入口侧端部流入的废气因该小室12的另一侧的端部成为被封堵住的结构而穿过小室壁13，此时，被小室壁13所捕获(捕捉)、除去了微粒的气体通过端部未被封堵的相邻小室12而被排出。
并且，在将本发明的陶瓷蜂窝结构体作为催化剂载体使用时，未必需要用密封材料对陶瓷构件11的各端部开口进行封堵。而且，使该小室壁的表面上承载有Pt、Pd或Rh等的贵金属催化剂。在这种情况下，从废气入口侧端部流入的废气被该贵金属催化剂改性，并作为清洁气体而从废气出口侧端部排出。
另外，图3所示的本发明的陶瓷蜂窝结构体10将组合了个陶瓷构件11(单元)而成的陶瓷块的外形表示为圆柱形的形状，但并不限定于圆柱形的形状，也可以做成例如椭圆柱形或多边柱形等的形状。并且，在本发明中，也可以在成为各陶瓷构件11的粘接面的外壁上施加凹凸或起伏。
本发明的陶瓷蜂窝结构体的特征在于：在与上述陶瓷构件的长度方向(气体通路方向)正交的截面中，使该陶瓷构件的两端部的大小大于该构件的长度方向的中心的大小。通过做成这样的构造，使端部与中心部之间的外壁上产生倾斜或台阶，并可以期望该倾斜部或台阶高差部上的卡定力变大而使陶瓷构件难以错位的这样的效果。
在本发明的陶瓷蜂窝结构体中，与中心部分相比，具有较大的截面的两端部最好是使其截面的大小分别从各端面向中心方向在构件的长度方向长度的0.5～25％的范围内连续地变小(倾斜部)、或台阶状地变小(台阶高差)。在该范围超过25％时，在陶瓷构件之间形成的密封材料层部分变小，变得难以得到充分的粘接强度。
并且，在该范围不足0.5％时，在上述倾斜部或台阶高差部存在应力易于集中、易于破损的隐患。
另外，在本发明的陶瓷蜂窝结构体中，将陶瓷构件的外形尺寸设为，例如，10～50mm×10～50mm×100～400mmL。该陶瓷构件的两端部的、与该构件的长度方向正交的截面的大小最好设为该构件的长度方向中心部分的截面积的1.01～1.10倍。这是因为，在两端部的截面积大于中心部分的截面积的1.10倍时，由于在陶瓷构件之间形成的密封材料层的中心部分的厚度比端部的厚度厚，因而过滤面积变小，存在由陶瓷构件与密封材料层的热膨胀差而使陶瓷构件及/或密封材料层破损的隐患。并且，在陶瓷构件的两端部的截面积不足中间部分的截面积的1.01倍的情况下，由于陶瓷构件端部与中心部的倾斜或台阶高差较小而使卡定力较小，陶瓷构件易于错位。
另外，在本发明的陶瓷蜂窝结构体中，作为多孔质陶瓷构件，可以使用由氮化铝、氮化硅、氮化硼、氮化钛等的氮化物陶瓷、碳化硅、碳化锆、碳化钛、碳化钽、碳化钨等的碳化物陶瓷、氧化铝、氧化锆、堇青石、多铝红柱石等的氧化物陶瓷、或钛酸铝等的、2种或2种以上的材料而形成的构件。本说明书中的碳化硅陶瓷是把碳化硅的含有量为60质量％以上的物质称作碳化硅陶瓷，也包括硅与碳化硅的复合体。在这些物质当中，由于碳化硅陶瓷的耐热性较强，机械特性优良，且热传导系数也较大，所以也最好是使用碳化硅陶瓷。
本发明的构成上述陶瓷蜂窝结构体的陶瓷构件的两端部的、与构件长度方向正交的截面的形状最好为三角形、四边形及六边形中的任一种形状，且都形成为柱状。设为这样的截面形状的理由是因为有效地提高了陶瓷构件的开口率，可以抑制压力损失的上升。
实施例
下面，列举实施例而进一步详细地说明本发明，但本发明并不仅限定于这些实施例。
该实施例是为了确认两端部长度(21)相对于陶瓷构件整个长度(L)的比率(21/L)、及两端部截面积(A)与中心部分截面积(a)的比率(A/a)对陶瓷构件的抗冲压强度给予的作用效果而进行的。图4表示使用于本实施例的陶瓷构件的概略图。并且，将实施例1～6、及比较例1、2的制法归纳于表1中予以表示。另外，陶瓷构件的制法依据以下形式。
首先，对于由70重量份的平均粒子直径约为22μm的碳化硅原料粉末与30重量份的平均粒子直径约为0.5μm的碳化硅原料粉末而组成的原料，添加并混合了5.7重量份的作为成形辅助剂的甲基纤维素。并且，在含有该甲基纤维素的混合粉末中添加并混匀了22.5重量份的由有机溶剂及水组成的分散溶剂之后，使用成为目标的陶瓷形状那样的金属模具进行挤压成形，制作出具有许多个通孔(小室)的蜂窝成形体。另外，使用密封材料而将上述通孔(小室)的任一侧的端部封堵成西洋跳棋盘状(隔一个通孔封堵一个通孔地交替地封堵通孔的任一侧端部开口)，获得了生坯成形体。
其次，将该生坯成形体以150℃进行干燥并以300℃进行脱脂之后，通过在惰性气体环境下、以2200℃进行烧结，获得了由碳化硅烧结体组成的陶瓷构件的试样(No.1～8)。
由于上述陶瓷构件在烧结时会有些许收缩，因此作为使用于上述陶瓷构件两端的封堵部的密封材料，使用了其收缩率小于陶瓷构件(单元)的收缩率的材料，从而抑制了烧结时的两端部的收缩，可以使两端部的截面积大于中心部截面积。另外，通过调整混合了坯土的有机溶剂的比例、粒子直径、碳化硅原料粉末的粗粉和细粉的混合比率、造孔材料的混入量等，可以改变密封材料与陶瓷构件的收缩率。例如，由于在将使用于封固部的密封材料所用的有机溶剂的比例设为小于使用于基体材料的量时，封堵部的收缩率较小，因此使两端部的截面积大于中心部截面积。
对于用这8种陶瓷构件试样制作成的陶瓷蜂窝结构体(实施例1～6、比较例1、2)，使用内向式万能材料试验机(MODEL5582型：インストロン社制)测定了陶瓷构件的抗冲压性。具体地说，组合9根陶瓷构件(单元)并使用含有30质量％的纤维长为20μm的氧化铝纤维、21质量％的平均粒子直径为0.6μm的氮化硅粒子、15质量％的硅溶胶、5.6质量％的羧甲基纤维素、28.4质量％的水的粘接剂胶而将该9根陶瓷构件一体化，并将其以700℃干燥2小时，从而制作出陶瓷蜂窝结构体。在做好的陶瓷蜂窝结构体中，只在中央的1根陶瓷构件上放置夹具并施加压力，将该陶瓷构件被冲压时的压力作为抗冲压载荷而进行了测定。将其结果一并表示于表1中。
表1
陶瓷构件长度方向产度L(mm) 端部长度I(mm) 21/L×100(％) 端面纵长度D(mm) 端面截面积A(mm2) 中心部分纵长度d(mm) 中心部分截面积a(mm2) 端部/中心部分截面积比率A/a 冲压载荷(kgf)
实施例1     306     2     1.3    3.42     11.7     3.38     11.5     1.02     1081
实施例2     305     5     3.3    3.42     11.7     3.33     11.1     1.05     1217
实施例3     254     10     7.9    3.41     11.6     3.24     10.5     1.10     1183
实施例4     256     15     11.7    3.42     11.7     3.38     11.4     1.03     1208
实施例5     151     18     23.8    3.41     11.6     3.27     10.7     1.08     1195
实施例6     149     1     1.3    3.41     11.6     3.32     11.0     1.05     1053
比较例1     304     0     0    3.42     11.7     3.42     11.7     1.00     824
比较例2     151     21.2     28.1    3.42     11.7     3.13     9.8     1.20     312
依据试验结果，在实施例1～6中，由于两端部长度与整个长度的比例(21/L)都在0.5～25％的范围，并且端面截面积与中心部分截面积的比率(A/a)都在1.01～1.10的范围内，所以可以得到1053kgf以上的较高的抗冲压强度。另一方面，由于在比较例1中，端面截面积与中心部分截面积的比率(A/a)小到1.00，在比较例2中，端部长度(1)较大，并且端面截面积与中心部分截面积的比率(A/a)大到1.2，因此抗冲压强度都小到824kgf或824kgf以下。并且，在比较例2中，由于抗冲压强度小到312kgf，密封材料层的中心部分的厚度较厚，所以在制作成陶瓷蜂窝结构体时，由于陶瓷构件与密封材料层的热膨胀差而在密封材料层上产生裂痕，可以推测出抗冲压强度变小了。
产业上的可利用性
本发明的陶瓷蜂窝结构体作为用于捕获、除去从柴油机等的内燃机排出的废气中所含有的微粒等的过滤器、或作为用于除去排气中的有害成分的催化剂载体而使用。

Claims (7)

1.一种陶瓷蜂窝结构体，是由组合并粘结了多个柱状的多孔质蜂窝状陶瓷构件而成的单元组成的，该柱状的多孔质蜂窝状陶瓷构件是用作气体通路的许多小室沿长度方向隔着小室壁并排设置而成的，其特征在于，上述多孔质蜂窝状陶瓷构件的两端部的、与构件长度方向正交的截面的大小大于该构件长度方向中心部分的截面的大小。
2.根据权利要求1所述的陶瓷蜂窝结构体，其特征在于，截面比上述中心部分的截面大的构件两端部的区域从各端面起在长度方向长度的0.5～25％的范围内。
3.根据权利要求1或2所述的陶瓷蜂窝结构体，其特征在于，上述构件的两端部的截面的大小为该构件的长度方向中心部分的截面积的1.01～1.10倍。
4.根据权利要求1～3中任一项所述的陶瓷蜂窝结构体，其特征在于，上述构件由从氮化铝、氮化硅、氮化硼、氮化钛、碳化硅、碳化锆、碳化钛、碳化钽、碳化钨、氧化铝、氧化锆、堇青石、多铝红柱石及钛酸铝中选取的任何1种或1种以上的物质构成。
5.根据权利要求1～4中任一项所述的陶瓷蜂窝结构体，其特征在于，上述构件两端部的截面形状为三角形、四边形及六边形中的任一种形状。
6.根据权利要求1～5中任一项所述的陶瓷蜂窝结构体，其特征在于，将上述小室的任一侧的端部封堵住，用作捕获、除去废气中所含有的粒子状物质的过滤器。
7.根据权利要求1～5中任一项所述的陶瓷蜂窝结构体，其特征在于，在上述小室壁表面上承载有催化剂成分，用作废气净化用催化剂载体，该催化剂成分由从Pt、Pd及Rh之中选取的任何1种或1种以上的贵金属或这些贵金属的合金构成。
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