CN101240728A - 陶瓷蜂巢式结构件 - Google Patents

陶瓷蜂巢式结构件 Download PDF

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Publication number
CN101240728A
CN101240728A CNA2007101928879A CN200710192887A CN101240728A CN 101240728 A CN101240728 A CN 101240728A CN A2007101928879 A CNA2007101928879 A CN A2007101928879A CN 200710192887 A CN200710192887 A CN 200710192887A CN 101240728 A CN101240728 A CN 101240728A
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China
Prior art keywords
next door
structural components
pore
ceramic honeycomb
honeycomb structural
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CNA2007101928879A
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CN101240728B (zh
Inventor
諏访部博久
冈崎俊二
德留修
大坪康彦
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Proterial Ltd
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Hitachi Metals Ltd
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Priority claimed from JP2002068189A external-priority patent/JP4161292B2/ja
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    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2418—Honeycomb filters
    • B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
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    • B01D46/247—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the cells
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    • B01D46/2429—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material of the honeycomb walls or cells
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Abstract

一种具有分割成多个流路的多孔质隔壁的陶瓷蜂巢式结构件，其特征在于：形成所述流路的所述隔壁的厚度是不均匀的，构成隔壁交叉部的各流路的隔壁厚度不同。

Description

陶瓷蜂巢式结构件
本申请是分案申请，其母案申请的申请号：02152473.4，申请日：2002.12.3，发明名称：陶瓷蜂巢式过滤器及其结构件
技术领域
本发明涉及一种对汽车废气、尤其是对包含在从柴油发动机排出的废气中的微粒子进行收集的陶瓷蜂巢式过滤器以及用于它的陶瓷蜂巢式结构件。
背景技术
为了除去在从柴油发动机排出的废气中的以碳为主要成分的微粒子，使用有把多孔质陶瓷蜂巢式结构件的两端交替封住的陶瓷蜂巢式过滤器。
如图1所示，陶瓷蜂巢式结构件1为接近圆筒形(包括截面为椭圆形)，并在外周壁2的内侧具有隔壁3，而且还具有由隔壁围出的多个单元(流路)4。另外，如图2(b)所示，流路4的两端用封堵件5a、5b交替封住。
用蜂巢式过滤器10如图2(b)所示那样进行废气净化。废气20a流入到过滤器10的流路4，经过多孔质隔壁3的细孔从相邻接的流路4如20b所示那样排出。包含在废气中的微粒子在经过隔壁3的细孔时被收集。另外，在流出端一侧的各封堵件5的内面上，积蓄着微粒子30。由于当被收集在流路4上的微粒子超过允许水准时过滤器10就会发生堵塞，所以用燃烧炉或电加热器使其燃烧，对过滤器10进行再生。
对于这样的微粒子收集用过滤器，压力损失、微粒子收集效率、耐损坏性以及耐溶损性等的过滤器特性是很重要的。虽然压力损失能够通过加大隔壁的气孔率或气孔尺寸、减小废气阻力而降低，但是如果加大隔壁的气孔率，则会降低隔壁的强度，从而降低过滤器的耐损坏性。而且，在蜂巢式过滤器的两端设置封堵件，这样不仅会使压力损失上升，而且还会降低耐热冲击性。因此很难同时满足压力损失和耐损坏性的两个必要条件。
在特开平7-332064号中已公开了一种方法，即，为了防止因封堵件而使陶瓷蜂巢式过滤器的压力损失上升、将废气流出侧的封堵件的细孔以三维地链式连接，把其气孔率设定为是隔壁气孔率的110～140％。但是，在特开平7-332064号公开的陶瓷蜂巢式结构件，如其实施例所记述的，由于气孔率为45％、很小，而且封堵件的气孔率也在40～65％、很小，所以存在陶瓷蜂巢式过滤器的压力损失大的问题。另外，由于在流出侧的封堵件上有气孔，而在流入侧的封堵件上没有气孔，所以废气不能通过流入侧的封堵件，降低压力损失的效果也就不充分。
在特开平8-281034号中公开了在再生时的热冲击集中于蜂巢式过滤器的隔壁的未封堵区域和封堵区域的交界处，以及为了防止因热冲击而造成的蜂巢式过滤器的损坏，必须不将其交界(根据封堵的深度)连续成一直线状的内容。但是，蜂巢式过滤器的封堵深度如果不均匀，则在封堵深度大的地方过滤器的有效面积就变小、而压力损失就会变大。另外，封堵深度如果不均匀，则对于每个产品的过滤面积就有误差，存在蜂巢式过滤器质量不稳定的问题。而且，由于在封堵深度小的地方封堵件与隔壁的结合强度小，所以因由废气所产生的压力或热冲击会将封堵件剥落。
一般的陶瓷蜂巢式结构件，如图10(a)及(b)所示，具有正方形的单元(流路)，在陶瓷蜂巢式结构件内隔壁的厚度实质上是均匀的。具有这样结构的陶瓷蜂巢式结构件，在平行于隔壁的方向上具有高强度，但在相对于隔壁的倾斜方向上强度较低。因此，在使用催化剂转换器或微粒子收集用过滤器时，有如图6所示的因热冲击和热应力而在隔壁交叉部发生裂纹13、在单元的对角线方向发生破坏的情况。
为了解决这样的缺陷，在特开昭55-147154号中公开了通过把外周壁附近的隔壁形成得比内部的隔壁厚来提高陶瓷蜂巢式结构件整体的强度的技术。但是，在陶瓷蜂巢式结构件的中心部，由于隔壁不厚，所以隔壁交叉部的强度均匀，在隔壁交叉部产生的裂纹链式地向中心部内传播。
在特公昭51-20435号中公开了为了防止在应力集中的隔壁交叉部产生裂纹、或在废气流动差的流路的角部(面对隔壁交叉部的面)催化反应效率低，而把隔壁交叉部扩大为圆弧形或直线形的内容。但是，由于隔壁交叉部的强度陶瓷蜂巢式结构件内是均匀的，所以因热冲击和热应力而发生裂纹在隔壁交叉部链式地传播。
在特开昭61-129015号中公开了一种隔壁的细孔由孔径为5～40μm的小孔和孔径为40～100μm的大孔组成并且小孔数是大孔数的5～40倍的废气净化用过滤器。虽然没有记载气孔率，但累计细孔容积为0.3～0.7cm3/g，所以，如果把堇青石的真实比重设为2.5，则气孔率为43～64％。
在特公昭61-54750号中公开了通过对开口孔隙率和平均孔径的控制能够设计出从高收集率式到低收集率式的过滤器。被记载的最合适的气孔率范围为33～90％。
专利第2578176号公开了气孔率范围为40～55％、直径为2μm以下、细孔容积为0.005cm3/g以下的、微粒子收集时间长的多孔质陶瓷蜂巢式过滤器。
特开平9-77573号公开了一种蜂巢式结构件，即，具有55～80％的气孔率和25～40μm的平均孔径，隔壁的细孔由具有5～40μm的孔径的小孔和具有40～100μm的孔径的大孔组成、并且小孔数是大孔数的5～40倍，具有高收集率、低压力损失和低热膨胀率。
但是，由于这些多孔质陶瓷蜂巢式过滤器具有高气孔率，所以必然地强度就低。而且，作为造孔剂，由于使用的是碳或石黑等比较扁平的粉末，所以细孔的长短径比就比较大并具有锐角部。因此在细孔上容易产生应力集中，这就成为陶瓷蜂巢式结构件强度低的原因。所以，在作为柴油发动机的废气的微粒子收集用过滤器被使用时，会因热应力或热冲击、组装时的机械紧固力或振动而发生损坏。
发明内容
因此，本发明的目的是要提供一种压力损失小、并能够防止因当再生过滤器时的热应力或热冲击而产生的裂纹的陶瓷蜂巢式过滤器以及用于这种过滤器的陶瓷蜂巢式结构件。
本发明的另一目的是要提供一种对应力集中的隔壁交叉部在单元对角线方向上使裂纹难以形成链式进展的陶瓷蜂巢式结构件。
本发明的又一目的是要提供一种即使气孔率在50％以上、也能够作为微粒子收集用过滤器而长期稳定使用的高强度陶瓷蜂巢式结构件。
鉴于上述目的，本发明的发明人等对陶瓷蜂巢式过滤器的隔壁以及封堵件进行了各种研究结果发现，通过对与隔壁组合的封堵件的气孔率、细孔形状以及封堵深度进行调节，能够不仅不降低耐破坏性而且可降低压力损失，进而完成了本发明。
即，本发明的陶瓷蜂巢式结构件，具有分割成多个流路的多孔质隔壁，其特征在于，形成所述流路的所述隔壁的厚度是不均匀的，构成隔壁交叉部的各流路的隔壁厚度不同。所述隔壁的厚度的平均值Tav、最大值Tmax以及最小值Tmin最好满足Tav/(Tmax-Tmin)≤40的条件。
根据本发明的理想实施例的陶瓷蜂巢式过滤器以及结构件，分别所述隔壁具有50～80％的气孔率，所述隔壁的任意截面上的具有1000μm2以上截面积的细孔的至少一部分具有圆形截面。
在本发明的陶瓷蜂巢式过滤器以及结构件中，在所述隔壁的任意截面上的具有1000μm2以上截面积的所述细孔中，最好具有1～10不圆度的细孔数的比例为50％以上。气孔率最好为60～70％。细孔的平均孔径最好为10～40μm。所述隔壁的厚度最好为0.1～0.5mm，所述隔壁的间隔最好为1～3.5mm。本发明的理想的蜂巢式过滤器以及结构件具有3MPa以上的A轴压缩强度。
本发明的陶瓷蜂巢式过滤器以及结构件，由具有以42～56质量％的SiO2、30～45质量％的Al2O3和12～16质量％的MgO组成为主成分化学组成的堇青石构成。
附图说明
图1(a)是表示本发明陶瓷蜂巢式结构件一例的主视图，图1(b)是图1(a)所示的陶瓷蜂巢式结构件的部分剖面的侧视图。
图2(a)是表示陶瓷蜂巢式过滤器一例的主视图，图2(b)是图2(a)所示的陶瓷蜂巢式过滤器的部分剖面的侧视图，图2(c)是表示图2(b)的陶瓷蜂巢式过滤器中废气流动的概略剖视图。
图3是表示本发明的陶瓷蜂巢式过滤器其他例的剖视参考图。
图4是表示制造参考图3所示的陶瓷蜂巢式过滤器的方法的剖视参考图。
图5(a)是表示本发明的陶瓷蜂巢式结构件的隔壁的一例的部分主视图，图5(b)是表示本发明的陶瓷蜂巢式结构件的隔壁的另一例的部分主视图，图5(c)是表示本发明的陶瓷蜂巢式结构件的隔壁的又一例的部分主视图
图6是表示图13(a)所示的陶瓷蜂巢式结构件的破坏例的概略主视图。
图7(a)是表示对陶瓷蜂巢式结构件的隔壁的厚度测定处的图，图7(b)是图7(a)的部分放大图。
图8(a)是表示用于挤出成形陶瓷蜂巢式结构件的模具的剖视图，图8(b)是使用图8(a)中的模具挤出成形陶瓷蜂巢式结构件的剖视图。
图9是表示用于图8(a)中的模具的口模的主视图。
图10(a)是表示以往的陶瓷蜂巢式结构件的隔壁的一例的主视图，图10(b)是表示以往的陶瓷蜂巢式结构件的隔壁的另一例的主视图。
图11是表示求出细孔的长短径比以及不圆度的隔壁剖面的一例的概略剖视图。
具体实施方式
(实施例)
在本发明的实施例中，陶瓷蜂巢式结构件的隔壁的厚度不是均匀的。例如如图5(a)～(c)所示，陶瓷蜂巢式结构件1的的横方向截面上的隔壁3a、3b的厚度不同。由于隔壁3的厚度不均匀，所以隔壁交叉部3c的强度对每个单元就不一样，在陶瓷蜂巢式结构件内不是一定的。因此，由于不存在连续的具有同等程度强度的隔壁交叉部3c，所以因热冲击或热应力会使裂纹链式地在隔壁交叉部3c上行进，能够防止在单元对角线方向上破坏陶瓷蜂巢式结构件的现象。其结果是使这种陶瓷蜂巢式结构件具有良好的耐冲击特性。而且，由于如图5(c)所示的隔壁交叉部3c具有曲面部，所以有应力集中小的优点。
隔壁3厚度的平均值Tav、最大值Tmax以及最小值Tmin最好满足Tav/(Tmax-Tmin)≤40的关系。Tav/(Tmax-Tmin)的值表示了对于隔壁3厚度平均值的误差程度。如果Tav/(Tmax-Tmin)在40以下，则由于隔壁厚度很不均匀，所以能够防止因热冲击或热应力使裂纹链式地在隔壁交叉部3c上行进。另一方面，如果Tav/(Tmax-Tmin)超过40，则隔壁厚度不是很不均匀，所以因热冲击或热应力会使裂纹容易链式地在隔壁交叉部3c上行进。
Tav/(Tmax-Tmin)的值最好是1～40，优选2～30。当Tav/(Tmax-Tmin)的下限不足1时，最小壁厚Tmin与最大壁厚Tmax的差过大，从挤出成形用机头的缝部排出的配料速度就不均等，成形体就会发生2弯曲或龟裂。
主要构成作为除去从柴油发动机废气中的微粒子的过滤器而使用的本发明的陶瓷蜂巢式过滤器的多孔质陶瓷蜂巢式结构件以及封堵件，最好由耐热性好的陶瓷材料形成。其中最好从由堇青石、氧化铝、莫来石、氮化硅、碳化硅以及硅氧锂铝(LAS)构成的组中至少选择一种作为主要成分的陶瓷材料使用，尤其是堇青石，价廉且耐热性及耐腐蚀性好，另外，由于具有低热膨胀性是最理想的。在使用堇青石时，最好是具有由42～56质量％的SiO2、30～45质量％的Al2O3和12～16质量％的MgO组成的主成分化学组成的材料。
当用本发明的陶瓷蜂巢式过滤器收集的微粒子达到规定量时，以由燃烧器或电热器燃烧微粒子的交替再生的方式、或通过由载持在陶瓷蜂巢式结构件上的催化剂的作用连续地使微粒子燃烧的连续再生的方式等进行陶瓷蜂巢式过滤器的再生。
以上对本发明的陶瓷蜂巢式过滤器及其结构件用各实施例进行了说明，但各个陶瓷蜂巢式过滤器及其结构件的特征(例如隔壁的厚度以及气孔率等)，如果不特别判断则会理解为所有的实施例是通用的。
以下，通过实施例对本发明进行详细说明，但本发明并不局限于此。
(参考例1～7，比较例1～6)
为了制成具有由49～51质量％的的SiO2、35～37质量％的Al2O3和13～15质量％的MgO组成的主成分组成的堇青石，在由陶土粉末、焙烧陶土粉末、氧化铝粉末、氢氧化铝粉末、硅石粉末以及滑石粉末组成的堇青石原料粉末中添加由规定量的粘合剂、润滑剂以及球状树脂粉末组成的造孔剂，加入规定量的水并且进行充分的混合、调制成按蜂巢式构造能够挤出的分批配料。
调整挤出成形用模具以及造孔剂的添加剂，制作成流路截面为四角形的具有各种厚度以及气孔率的隔壁的蜂巢式成形体。在各成形体干燥后进行煅烧，制作出直径150mm×长度150mm的陶瓷蜂巢式结构件。得到的陶瓷蜂巢式结构件的隔壁的间距为1.5mm，并且隔壁具有各种厚度和气孔率。而且，隔壁的气孔率，可使用Micromeritics公司产的AutoporeIII9410，用水银压入法测定。
如参考图4所示，在各陶瓷蜂巢式结构件的两端11、11上用粘接剂粘上覆盖膜12后，以只封堵各流路4的一端花纹样式地对覆盖膜12穿孔，形成封堵部12a和开放部12b。
与上述同样地向堇青石原料粉末中添加造孔剂、水以及粘合剂，制成稀混凝土14，并放入容器16内。为了得到具有各种气孔率的封堵件，可以改变添加在各稀混凝土14中的造孔剂的量。
如参考图4所示，把陶瓷蜂巢式结构件1的端面11以规定的深度浸在稀混凝土14中，通过覆盖膜12的流路4内的开放部12a导入稀混凝土14。将陶瓷蜂巢式结构件1抬起并使进入端部的稀混凝土14充分干燥后，将陶瓷蜂巢式结构件1倒置，并同样地进行向稀混凝土14浸入和干燥处理。在附着在陶瓷蜂巢式结构件1上的所有的稀混凝土14干燥后，将覆盖膜12剥离。这样就得到了在两端部以规定的方式设置封堵件5的陶瓷蜂巢式结构件1。最后将设置有封堵件5的陶瓷蜂巢式结构件1放在间歇式煅烧炉(未图示)内煅烧，从而获得具有各种气孔率的封堵件的陶瓷蜂巢式过滤器10。
对所获得的陶瓷蜂巢式过滤器10测定了隔壁3的厚度以及气孔率、封堵件5的气孔率以及深度。沿蜂巢式结构件1的X轴以及Y轴方向，分别在5处、共计25处从单元的开口端***直径为0.8mm的金属棒，通过测定该金属棒的***深度求出封堵厚度。封堵厚度是25处测定的平均值。另外，对各陶瓷蜂巢式过滤器10的压力损失以及耐热冲击性进行了以下的评价。
(a)压力损失
在压力损失实验装置(未图示)中，将含有碳黑的规定流量的空气以碳黑的流量为3g/小时、流过蜂巢式过滤器10经2小时后，测定了蜂巢式过滤器10的入口和出口的压差。以下是压力损失的评价标准。对400mmAq以下的◎以及○同时作为合格。
◎：不足380mmAq。
○：380～400mmAq。
×：超过400mmAq。
(b)耐热冲击性
将过滤器10以设定的各种温度保持在电炉中30分钟，然后急剧冷却到室温，经目视观测有无裂纹。把在发现裂纹时的加热温度与室温(25℃)的温度差作为耐热冲击温度。以下是记入的是耐热冲击温度的评价标准。并且600℃以上作为合格。
◎◎：700℃以上。
◎：650℃以上并不到700℃。
○：600以上并不到650℃。
×：不到600℃。
压力损失和耐热冲击性的综合判断按以下标准进行。
◎◎：压力损失为◎、耐热冲击性为◎◎。
◎：压力损失和耐热冲击性两方都为◎。
○：压力损失和耐热冲击性无论哪一方都合格。
×：压力损失和耐热冲击性至少其中有一个不合格(NG)。
各蜂巢式过滤器10的隔壁的厚度和气孔率、封堵件的气孔率和封堵深。度、压力损失和耐热冲击性的评价结果以及综合判断出示在表1中。
表1
例No.   陶瓷蜂巢式结构件     封堵件
  隔壁的厚度(mm)     气孔率(％)   隔壁的间隔(mm)     气孔率(％)     深度(mm)
参考例1   0.15     50   1.46     55     3
参考例2   0.20     55   1.46     65     5
参考例3   0.22     60   1.52     69     10
参考例4   0.22     65   1.52     75     10
参考例5 0.25 75 1.52 80 12
参考例6   0.31     65   1.52     80     11
参考例7   0.30     78   1.52     85     15
比较例1   0.08     51   1.46     55     5
比较例2   0.12     45   1.46     22     2
比较例3   0.28     70   1.52     45     12
比较例4   0.25     85   1.52     90     15
比较例5   0.60     51   1.52     55     5
比较例6   0.15     50   1.52     55     18
表1(续)
例No.     评价结果     综合判定
    压力损失     耐热冲击性
参考例1     ○     ○     ○
参考例2     ○     ○     ○
参考例3     ○     ○     ○
参考例4     ◎     ○     ○
参考例5     ◎     ○     ○
参考例6     ◎     ○     ○
参考例7     ◎     ○     ○
比较例1     ○     ×     ×
比较例2     ×     ×     ×
比较例3     ×     ×     ×
比较例4     ◎     ×     ×
比较例5 × ○ ×
比较例6     ×     ○     ×
在参考例1～7的蜂巢式过滤器中，隔壁具有0.1～0.5mm以内的厚度和50～80％以内的气孔率，并且封堵件的气孔率比隔壁的气孔率大。另外封堵深度为3～15mm。因此压力损失和耐热冲击性的评价为良好，综合判断为○。尤其是参考例4～7，由于封堵件的气孔率在70～90％的最适当范围内，所以压力损失的评价为◎。
比较例1的蜂巢式过滤器，由于隔壁的厚度未达到0.1mm，所以耐热冲击性差。比较例2的蜂巢式过滤器，由于隔壁的气孔率未达到50％，封堵件的气孔率比隔壁的气孔率小，所以压力损失大，并且由于封堵深度未达到3mm，所以耐热冲击性差。比较例3的蜂巢式过滤器，由于封堵件的气孔率比隔壁的气孔率小，所以压力损失大并且耐热冲击性也差。比较例4的蜂巢式过滤器，由于隔壁的气孔率超过了80％，所以耐热冲击性差。比较例5的蜂巢式过滤器，由于隔壁的厚度超过了0.5mm，所以压力损失大。比较例6的蜂巢式过滤器，由于封堵深度超过了15mm，所以压力损失大。
(参考例8～13)
与参考例1相同，制作了具有外径150mm×长度150mm、把0.3mm厚度的隔壁以1.5mm的间距设置的堇青石材质的陶瓷蜂巢式过滤器10。隔壁的气孔率为65％，封堵件的气孔率为78％，封堵深度为10mm。但是在参考例8～11中，在封堵件用稀混凝土14中添加了由丙烯腈-异丁烯酸甲酯共聚物树脂组成的各种量的球形造孔剂(小球)。
对于各陶瓷蜂巢式过滤器10，对封堵件的任意横方向的截面进行研磨，并从其SEM照片以目视进行了有无具有接近圆形截面的细孔的研究。并且如图11中示例的那样，将SEM照片的数据用市场上销售的图像分析软件(Image-Pro Plus Version3.0 available from Media Cybemetics)进行分析，求出细孔截面的长短径比，算出在具有1000μm2以上的截面积的细孔中、长短径比在2以下的细孔数的比例。
对于各陶瓷蜂巢式过滤器，用与参考例1同样的方法来评价压力损失和耐热冲击性。具有接近圆形截面的细孔的有无、长短径比在2以下的细孔数的比例、压力损失、耐热冲击性以及综合判定出示在表2中。
表2
例No.   封堵件  压力损失  耐热冲击性   综合判定
  有无具有接近圆形截面的细孔    长短径比为2以下的细孔数的比例(％)
参考例8   有    15     ◎     ◎   ◎
参考例9   有    12     ◎     ◎   ◎
参考例10   有    42     ◎     ◎◎   ◎◎
参考例11   有    65     ◎     ◎◎   ◎◎
参考例12   无    0     ◎     ○   ○
参考例13   无    0     ◎     ○   ○
参考例8～11的蜂巢式过滤器，由于在封堵件中存在具有接近圆形截面的细孔，所以压力损失低，并且耐热冲击性好。耐热冲击性的评价无论哪一个都是◎或◎◎，所以综合判定为◎或◎◎。但特别是在参考例10及11中的蜂巢式过滤器，由于在封堵件中具有1000μm2以上的截面积的细孔中，长短径比在2以下的细孔数的比例为20％以上，所以耐热冲击性的评价为(◎◎)，综合判定也为(◎◎)。另一方面，参考例12和13的蜂巢式过滤器，由于在封堵件中不存在具有接近圆形截面的细孔，所以耐热冲击性的评价为○，综合判定也为○。
(参考例14～17，比较例7、8)
与参考例1相同制作了具有外径150mm×长度150mm、把0.3mm厚度的隔壁以1.5mm的间距设置的堇青石材质的陶瓷蜂巢式过滤器10。隔壁的气孔率为65％，封堵件的气孔率为60％，封堵深度为10mm。但是在参考例14～17中，在封堵件用稀混凝土14中添加了由丙烯腈-异丁烯酸甲酯共聚物树脂组成的各种量的球形造孔剂(小球)。
对各陶瓷蜂巢式过滤器，与参考例8～13同样，求出有无具有圆形截面的细孔以及长短径比为2以下的细孔数的比例。另外用与参考例1相同的方法对压力损失以及耐热冲击性进行了评价。有无具有接近圆形截面的细孔、长短径比为2以下的细孔数的比例、压力损失、耐热冲击性以及综合判定出示在表3中。
表3
例No.     封堵件 压力损失 耐热冲击性   综合判定
    有无具有接近圆形截面的细孔    长短径比为2以下的细孔数的比例(％)
参考例14     有    15     ○     ○     ○
参考例15     有    12     ○     ○     ○
参考例16     有    42     ○     ◎     ◎
参考例17     有    65     ○     ◎     ◎
比较例7     无    0     ○     ×     ×
比较例8     无    0     ○     ×     ×
参考例14～17的蜂巢式过滤器，由于在封堵件中存在具有接近圆形截面的细孔，所以压力损失低，并且耐热冲击性好。耐热冲击性的评价无论哪一个都是○或◎，所以综合判定为○或◎。但特别是在参考例16及17中的蜂巢式过滤器，由于在封堵件中具有1000μm2以上的截面积的细孔中，长短径比在2以下的细孔数的比例为20％以上，所以耐热冲击性的评价为◎，综合判定也为◎。另一方面，比较例7和8的蜂巢式过滤器，由于在封堵件中不存在具有接近圆形截面的细孔，所以耐热冲击性的评价为×，综合判定也为×。
(实施例1～10)
为形成具有与参考例1相同的主成分组成的堇青石，在由陶土粉末、焙烧陶土粉末、氧化铝粉末、氢氧化铝粉末、硅石粉末以及滑石粉末组成的堇青石原料粉末中，以各个规定量混合进粘合剂、润滑剂以及作为造孔剂的球状树脂粉末。在所得到的混合物中加入水并制作成可塑化的成形用分批配料。
使用将口模缝隙的宽度调整为使陶瓷蜂巢式结构件的隔壁的厚度不均匀的挤出成形用模具，将各成形用分批配料进行挤出成形，可获得如具有如图5(a)所示的隔壁的蜂巢式成形体。把所得到的成形体在1400℃进行煅烧、得到外径为267mm和长度为300mm的堇青石质的陶瓷蜂巢式结构件。
如图7(a)及(b)所示，着眼于沿陶瓷蜂巢式结构件1的X轴以及Y轴各5个、共计25个单元，用倍率为100倍的投影仪，在围绕各单元的4个隔壁的中点、测定了其厚度。从所获得的共计100个测定值中求出隔壁3厚度的的平均值Tav、最大值Tmax以及最小值Tmin，并从它们中算出Tav/(Tmax-Tmin)。另外，与参考例1同样，对各陶瓷蜂巢式结构件进行了耐热冲击性评价。其结果出示在表4中。并且陶瓷蜂巢式结构件1的单元数为46.5个/cm2，气孔率为65％，细孔的平均孔径为20μm。
表4
例No.     隔壁的温度     耐热冲击温度(℃)
   平均值Tav(mm)     最大值Tmax(mm)   最小值Tmin(mm)     Tav/(Tmax-Tmin)
实施例1     0.30     0.355     0.251     2.9     767
实施例2     0.30     0.320     0.284     8.3     767
实施例3 0.31 0.320 0.295 12 758
实施例4     0.31     0.316     0.305     28     742
实施例5     0.30     0.304     0.296     38     717
实施例6     0.30     0.320     0.278     7.1     750
实施例7     0.32     0.333     0.308     13     741
实施例8 0.29 0.293 0.286 41 692
实施例9     0.31     0.303     0.296     44     667
实施例10     0.32     0.324     0.317     46     683
隔壁的厚度为不均匀的实施例1～7的陶瓷蜂巢式结构件，具有  700℃以上的耐热冲击温度，比Tav/(Tmax-Tmin)＞40的实施例8～10的耐热冲击温度高。700℃以上的耐热冲击温度，是对于汽油发动机的废气净化催化剂载体或除去柴油发动机废气中的微粒子的过滤器的最好的水准。因此实质上不会因使用中的热冲击而产生裂纹、受到破坏。
(实施例11～14)
为形成具有与参考例1相同的主成分组成的堇青石，在由陶土粉末、焙烧陶土粉末、氧化铝粉末、氢氧化铝粉末、硅石粉末以及滑石粉末组成的堇青石原料粉末中，以各个规定量混合进粘合剂、润滑剂以及作为造孔剂的球状树脂粉末。在所得到的混合物中加入水并制作成可塑化的成形用分批配料。把该分批配料以圆筒形的蜂巢式形状挤出成形并干燥。
将这样得到的直径为143mm和长度为152mm的圆筒形陶瓷蜂巢式成形体在1350～1440℃下煅烧，可获得如图1(a)和(b)所示的具有隔壁3的堇青石质的陶瓷蜂巢式结构件1。并且通过对堇青石的原料组成、成形条件和煅烧条件等进行调整，制造了具有各种细孔特性以及蜂巢式隔壁构造的实施例11～14的陶瓷蜂巢式结构件1。
各陶瓷蜂巢式结构件1的气孔率以及平均孔径，是使用Micromeritics公司产的AutoporeIII9410，用水银压入法测定。对各陶瓷蜂巢式结构件的任意横方向的截面进行研磨，对是否有截面积为1000μm2以上的细孔中接近截面为圆形的细孔，从SEM照片经目视进行了确认。另外，对截面积为1000μm2以上的细孔的不圆度，如图11所示，通过将SEM照片的数据用市场上销售的图像分析软件(Image-Pro Plus Version3.0 availablefrom Media Cybemetics)进行分析而求出。
对从各陶瓷蜂巢式结构件切除的实验片，按照社团法人汽车技术会的汽车标准(JASO)M505-87，「汽车废气净化催化剂用陶瓷材料载体(Ceramic Monolith Carriers)的实验方法」，测定了A轴压缩强度。
把各陶瓷蜂巢式结构件的端部如图2(a)和(b)所示那样进行封堵，得到了多孔质的陶瓷蜂巢式过滤器。各陶瓷蜂巢式过滤器的过滤特性(耐破坏性、压力损失以及收集效率)按以下记述评价。其结果出示在表5中。
(a)耐破坏性
各过滤器的耐破坏性，通过按照社团法人汽车技术会规定的标准(JASO)M505-87的「汽车废气净化催化剂用陶瓷材料载体(CeramicMonolith Carriers)的实验方法」测定的A轴压缩强度，根据下记的标准进行评价。
◎：A轴压缩强度在7Mpa以上(合格)。
○：A轴压缩强度在3Mpa以上7Mpa以下(合格)。
×：A轴压缩强度抵于3Mpa(不合格)。
(b)压力损失
◎：压力损失在250mmAq以下(合格)。
○：压力损失在250mmAq以上300mmAq以下(合格)。
×：压力损失在超过300mmAq(不合格)。
(c)碳收集效率
为了求出碳的收集效率，在压力损失试验台上，向各蜂巢式过滤器中放入由流量为7.5Nm3/分的空气输送粒径为0.0042μm的碳、以3g/小时的流量经2个小时后，测定了由蜂巢式过滤器的碳的量。碳的收集效率的评价标准为下记内容。
○：碳的收集量超过放入量的90％(合格)。
×：碳的收集量低于放入量的90％(不合格)。
(d)综合判定
根据耐破坏性、压力损失以及碳的收集效率，将综合判定评价以下述的标准进行。
◎：耐破坏性、压力损失以及碳的收集效率无论哪一个都合格、◎判定有一个以上。
○：虽然耐破坏性、压力损失以及碳的收集效率无论哪一个都合格、但没有◎判定。
×：虽然耐破坏性、压力损失以及碳的收集效率有任意一个不合格。
实施例11～14的陶瓷蜂巢式过滤器，由于在隔壁的任意截面上的截面积为1000μm2以上的细孔中包含着具有接近圆形截面的细孔，所以不圆度1～10的细孔数的比例高。因此，陶瓷蜂巢式过滤器的耐破坏性无论哪种情况都合格。另外，压力损失以及收集效率无论哪种情况都合格，综合判定是○或◎。
如果从作为微粒子收集用过滤器的重要的耐破坏性、压力损失以及微粒子的收集效率的测定结果、进行综合判定，则实施例11～14的陶瓷蜂巢式过滤器无论哪种情况都合格。
(比较例9、10)
与参考例1同样地在堇青石原料粉末中混合规定量石墨粉末、碳黑粉末等长短径比大的边平状造孔剂，与实施例11～14同样地制作出各种堇青石质的陶瓷蜂巢式结构件1，测定细孔特性、隔壁构造、A轴压缩强度以及过滤特性并进行综合评价，其结果出示在表5中。
比较例9和10的陶瓷蜂巢式过滤器，由于截面积为1000μm2以上的细孔截面为方形，所以不可能测出不圆度。另外，由于A轴压缩强度也在3MPa以下，所以无路哪中情况耐破坏性都不合格，综合判定为不合格。
表5
例No.     细孔特性     隔壁的构造
    气孔率(％)   平均孔径(μm)     具有接近圆形截面的细孔1) 不圆度为1～10的细孔(％)(2)   隔壁的厚度(mm)  隔壁的间隔(mm)
实施例11 62 13 有 53 0.3 1.8
实施例12     63     12     有     83     0.3     1.8
实施例13     56     12     有     72     0.3     1.8
实施例14     75     18     有     73     0.3     1.8
比较例9     62     13     无     不能测定     0.3     1.8
比较例10 60 16 无 不能测定 0.3 1.8
注(1)有无截面积为1000μm2以上、具有圆形截面的细孔。
(2)在截面积为1000μm2以上的细孔中、不圆度为1~10的细孔数的比例。
表5(续)
例No.    强度     过滤特性     综合判定
   A轴压缩强度(MPa)     耐破坏性     压力损失     碳的收集效率
实施例11    6.8     ○     ○     ○     ○
实施例12    10.3     ◎     ○     ○     ◎
实施例13    12.6     ◎     ○     ○     ◎
实施例14    5.3     ○     ◎     ○     ◎
比较例9    2.6     ×     ○     ○     ×
比较例10    1.8     ×     ○     ○     ×
如以上详细所述，本发明的陶瓷蜂巢式构过滤器，压力损失小，机械强度以及耐热冲击性良好，能够防止过滤器再生时的因热冲击而产生的裂纹和破坏。

Claims (10)

1.一种陶瓷蜂巢式结构件，具有分割成多个流路的多孔质隔壁，其特征在于：形成所述流路的所述隔壁的厚度是不均匀的，构成隔壁交叉部的各流路的隔壁厚度不同。
2.根据权利要求1所述的陶瓷蜂巢式结构件，其特征在于：
所述隔壁的厚度的平均值Tav、最大值Tmax以及最小值Tmin满足Tav/(Tmax-Tmin)≤40的条件。
3.根据权利要求1或2所述的陶瓷蜂巢式结构件，其特征在于：
所述隔壁具有50～80％的气孔率，所述隔壁的任意截面上的具有1000μm2以上截面积的细孔的至少一部分具有圆形截面。
4.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：
在所述隔壁的任意截面上的具有1000μm2以上截面积的所述细孔中，具有1～10不圆度的细孔数的比例为50％以上。
5.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：
在所述隔壁的任意截面上的具有1000μm2以上截面积的细孔中，长短径比为2以下的细孔数的比例为60％以上。
6.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：所述气孔率为60～70％。
7.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：细孔的平均孔径为10～40μm。
8.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：所述隔壁的厚度为0.1～0.5mm，所述隔壁的间隔为1～3.5mm。
9.根据权利要求3所述的陶瓷蜂巢式结构件，其特征在于：具有3MPa以上的A轴压缩强度。
10.根据权利要求1或2所述的陶瓷蜂巢式结构件，其特征在于：
由具有以42～56质量％的SiO2、30～45质量％的Al2O3和12～16质量％的MgO组成为主成分化学组成的堇青石构成。
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EP1316686B1 (en) 2007-09-05
US6890616B2 (en) 2005-05-10
CN1424493A (zh) 2003-06-18
EP1491734A1 (en) 2004-12-29
DE60222225D1 (de) 2007-10-18
EP1491734B1 (en) 2007-02-28
DE60222225T2 (de) 2008-06-12
DE60218538D1 (de) 2007-04-12
ATE372449T1 (de) 2007-09-15
CN101240728B (zh) 2012-07-04
DE60233448D1 (de) 2009-10-01
EP1316686A3 (en) 2003-08-13
DE60218538T2 (de) 2007-11-08
EP1719882B1 (en) 2009-08-19
US20030165662A1 (en) 2003-09-04
EP1316686A2 (en) 2003-06-04

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