CN111747768A - 接合材料及碳化硅系蜂窝结构体 - Google Patents

接合材料及碳化硅系蜂窝结构体 Download PDF

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Publication number
CN111747768A
CN111747768A CN202010101060.8A CN202010101060A CN111747768A CN 111747768 A CN111747768 A CN 111747768A CN 202010101060 A CN202010101060 A CN 202010101060A CN 111747768 A CN111747768 A CN 111747768A
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silicon carbide
carbide honeycomb
honeycomb structure
bonding
bonding material
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木村佳祐
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NGK Insulators Ltd
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NGK Insulators Ltd
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    • C04B38/0006—Honeycomb structures
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Abstract

本发明提供接合材料及碳化硅系蜂窝结构体，所述接合材料能够有效利用制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时产生的加工粉。该接合材料用于将多个碳化硅系蜂窝单元的侧面接合来制造碳化硅系蜂窝结构体。该接合材料含有0.1～50质量％的制造碳化硅系蜂窝单元和/或碳化硅系蜂窝结构体时产生的加工粉，加工粉的平均粒径D50为0.5～60μm。

Description

接合材料及碳化硅系蜂窝结构体
技术领域
本发明涉及接合材料及碳化硅系蜂窝结构体。
背景技术
作为废气的集尘用过滤器、例如用于对废气中包含的粒子状物质(颗粒)进行捕捉并除去的柴油颗粒过滤器(DPF)、汽油颗粒过滤器(GPF)，广泛使用蜂窝结构体。
作为上述用途中使用的蜂窝结构体，例如已知如下碳化硅系蜂窝结构体，其具备：多个碳化硅系蜂窝单元、以及将各碳化硅系蜂窝单元的侧面间接合的接合层。此处，碳化硅系蜂窝结构体是指以碳化硅为主成分的材质的蜂窝结构体，包括像重结晶SiC那样仅包含碳化硅的材质、以及碳化硅和金属硅、玻璃等其他成分复合化得到的材质的蜂窝结构体在内。接合层是采用包含碳化硅粉末、氧化铝粉末等无机粉末、多铝红柱石纤维等无机纤维、中空粒子等造孔剂、粘合剂、分散剂等的接合材料而形成的(例如专利文献1)。
另一方面，在如上所述的碳化硅系蜂窝结构体的制造中，在制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时会产生加工粉。作为加工粉，可例示：对碳化硅系蜂窝单元或碳化硅系蜂窝结构体进行磨削而使其为规定形状时产生的磨削粉、将碳化硅系蜂窝单元或碳化硅系蜂窝结构体的不合格品等粉碎得到的粉末等。上述加工粉有时在碳化硅系蜂窝单元的制造中进行再利用，不过，在除此以外的用途中的再利用尚无进展。
现有技术文献
专利文献
专利文献1：日本特开2017－178722号公报
发明内容
对于碳化硅系蜂窝结构体的接合层要求接合强度高且杨氏模量低，但是，如果提高接合层的接合强度，则存在接合层的杨氏模量也上升这样的权衡关系。如果接合层的杨氏模量升高，则难以表现出缓和热应力的功能，因此，无法充分确保碳化硅系蜂窝结构体的耐久性。
因此，为了使用于形成碳化硅系蜂窝结构体的接合层的接合材料的接合强度升高且杨氏模量降低，详细地规定所使用的成分的种类及含量，认为很难将制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时产生的加工粉在接合材料中进行有效利用。
本发明是为了解决如上所述的问题而实施的，其目的在于，提供能够将制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时产生的加工粉有效利用的接合材料及碳化硅系蜂窝结构体。
本发明的发明人为了解决上述问题而进行了潜心研究，结果发现，通过着眼于制造碳化硅系蜂窝单元和/或碳化硅系蜂窝结构体时产生的加工粉的含量及平均粒径D50与接合层的接合强度及杨氏模量密切相关的情况并控制其含量及平均粒径D50，能够将该加工粉有效利用于接合材料，以至完成本发明。
即，本发明是用于将多个碳化硅系蜂窝单元的侧面接合来制造碳化硅系蜂窝结构体的接合材料，其中，含有0.1～50质量％的制造所述碳化硅系蜂窝单元和/或所述碳化硅系蜂窝结构体时产生的加工粉，所述加工粉的平均粒径D50为0.5～60μm。
另外，本发明是具备多个碳化硅系蜂窝单元、以及将多个所述碳化硅系蜂窝单元的侧面间接合的接合层的碳化硅系蜂窝结构体，其中，所述接合层为所述接合材料的固化层。
发明效果
根据本发明，能够提供可以将制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时产生的加工粉有效利用的接合材料及碳化硅系蜂窝结构体。
附图说明
图1是本发明的一个实施方式所涉及的碳化硅系蜂窝结构体的立体图及其局部放大图。
符号说明
1…碳化硅系蜂窝单元、2…接合层、3…隔室、4…隔壁、5…外周涂层、10…碳化硅系蜂窝结构体。
具体实施方式
以下，参照附图，对本发明的实施方式具体地进行说明。本发明并不限定于以下的实施方式，应当理解，在不脱离本发明的主旨的范围内基于本领域技术人员的通常知识对以下的实施方式适当加以变更、改良等得到的实施方式也落在本发明的范围内。
本发明的一个实施方式所涉及的接合材料用于将多个碳化硅系蜂窝单元的侧面接合来制造碳化硅系蜂窝结构体。
此处，将碳化硅系蜂窝结构体的立体图及其局部放大图示于图1。如图1所示，碳化硅系蜂窝结构体10具备：多个碳化硅系蜂窝单元1、以及将多个碳化硅系蜂窝单元1的侧面间接合的接合层2。接合层2为接合材料的固化层。
作为碳化硅系蜂窝单元1，没有特别限定，可以使用该技术领域中公知的碳化硅系蜂窝单元。
在1个实施方案中，碳化硅系蜂窝单元1具备区划形成多个隔室3的隔壁4，该多个隔室3从一个端面延伸至另一个端面。作为碳化硅系蜂窝单元1的与隔室3延伸的方向垂直的截面的形状，没有特别限定，可以为三角形、四边形、六边形、八边形等各种形状，不过，优选为四边形(正方形或长方形)。通过采用上述形状的碳化硅系蜂窝单元1，使得碳化硅系蜂窝结构体10的制造变得容易。
另外，作为碳化硅系蜂窝单元1的隔室3的形状(与隔室3延伸的方向垂直的截面中的隔室3的形状)，没有特别限定，可以为三角形、四边形、六边形、八边形、圆形等各种形状，不过，优选为四边形(正方形或长方形)。
隔壁4的厚度没有特别限定，优选为4～70mil(0.010～0.177cm)，更优选为4.5～30mil(0.011～0.076cm)，进一步优选为5～20mil(0.013～0.050cm)。通过使隔壁4的厚度为4mil(0.010cm)以上，能够确保充分的强度。另外，通过使隔壁4的厚度为70mil(0.177cm)以下，能够抑制压力损失增大。因此，例如将碳化硅系蜂窝结构体10用于DPF等的情况下，能够抑制发动机的输出降低。
碳化硅系蜂窝单元1的隔室密度没有特别限定，优选为50～500隔室/平方英寸(7.7～77.5隔室/cm2)，更优选为70～450隔室/平方英寸(10.8～69.8隔室/cm2)，进一步优选为80～400隔室/平方英寸(12.4～62.0隔室/cm2)。通过使碳化硅系蜂窝单元1的隔室密度为50隔室/平方英寸(7.7隔室/cm2)以上，能够确保充分的强度。另外，通过使碳化硅系蜂窝单元1的隔室密度为500隔室/平方英寸(77.5隔室/cm2)以下，能够抑制压力损失增大。
碳化硅系蜂窝单元1可以按照该技术领域中公知的方法来制造。具体而言，如下制造。首先，在陶瓷原料中添加粘合剂、分散剂(表面活性剂)、造孔材料、水等，进行混合及混炼，制成坯土。接下来，将该坯土挤压成型为规定的蜂窝形状并切断为所期望的长度，接下来，利用微波、热风等进行干燥后，进行烧成。另外，在烧成后，根据需要进行磨削等，以使其成为规定形状。
陶瓷原料为由陶瓷材料形成的无机粉末及无机纤维。作为陶瓷原料，包含碳化硅系陶瓷作为主成分即可，没有特别限定。此处，本说明书中主成分是指：在整体中所占的比例超过50质量％。作为碳化硅系陶瓷，可以举出碳化硅或硅－碳化硅系复合材料。作为其他陶瓷原料的例子，可以举出：堇青石化原料、堇青石、多铝红柱石、氧化铝、二氧化钛、尖晶石、碳化硅－堇青石系复合材料、硅酸锂铝、钛酸铝、铁－铬－铝系合金等。这些陶瓷原料可以单独使用，或者，将2种以上组合使用。应予说明，本说明书中“堇青石化原料”是将二氧化硅、氧化铝以及氧化镁按二氧化硅在42～56质量％的范围内、氧化铝在30～45质量％的范围内、氧化镁在12～16质量％的范围内的化学组成进行配合得到的陶瓷原料，经烧成而成为堇青石。在采用硅－碳化硅系复合材料的情况下，将碳化硅粉末及金属硅粉末混合得到的物质作为陶瓷原料。陶瓷原料的含量相对于成型原料整体而言，优选为40～90质量％。
作为粘合剂，没有特别限定，可以举出：胶体二氧化硅(二氧化硅溶胶)、氧化铝溶胶、膨润土以及蒙脱石这样的粘土等无机粘合剂、甲基纤维素、羧甲基纤维素、羟丙氧基纤维素、羟乙基纤维素、聚乙烯醇(PVA)、聚乙烯醇缩丁醛(PVB)、其他各种吸水性树脂等有机粘合剂。这些粘合剂可以单独使用，或者，将2种以上组合使用。
作为分散剂(表面活性剂)，没有特别限定，可以举出：油酸PEG、乙二醇、糊精、脂肪酸皂、多元醇等。这些分散剂可以单独使用，或者，将2种以上组合使用。
作为造孔材料，在烧成后成为气孔的材料即可，没有特别限定，可以举出：淀粉、发泡树脂、吸水性树脂、硅胶、碳等。这些造孔材料可以单独使用，或者，将2种以上组合使用。
另外，对于碳化硅系蜂窝单元1，可以在碳化硅系蜂窝单元1的2个端面中的任意一个端面形成有将隔室3的一个端部封孔的封孔部。通常，按一个端面和另一个端面呈互补的棋盘格状的方式将相邻的隔室3交替地封孔。封孔部的构成材料优选使用与碳化硅系蜂窝单元1相同的材料，以便减小与碳化硅系蜂窝单元1之间的热膨胀差。
在对隔室3形成封孔部的情况下，可以在对隔室3形成封孔部之前进行烧成，也可以在对隔室3形成封孔部之后与封孔部的烧成一同进行烧成。作为对隔室3形成封孔部的方法，可以使用该技术领域中公知的方法。具体而言，在碳化硅系蜂窝单元1的端面粘贴片材后，在该片材的与待封孔的隔室3相对应的位置开孔，以粘贴有该片材的状态，将碳化硅系蜂窝单元1的端面浸渍于将封孔部的构成材料浆料化得到的封孔用浆料中，通过在片材所开的孔，向待封孔的隔室3的开口端部内填充封孔用浆料，将其干燥和/或烧成，使其固化。
接合材料含有0.1～50质量％的制造碳化硅系蜂窝单元1和/或碳化硅系蜂窝结构体10时产生的加工粉。通过使加工粉为0.1质量％以上，能够将加工粉有效利用于接合材料。另外，通过使加工粉为50质量％以下，能够形成接合强度良好的接合层2。从有效利用加工粉的观点考虑，加工粉的含量优选为0.5质量％以上，更优选为1质量％以上，进一步优选为3质量％以上。另外，从接合层2的接合强度的观点考虑，加工粉的含量优选为48质量％以下，更优选为45质量％，进一步优选为43质量％以下。
此处，本说明书中，制造碳化硅系蜂窝单元1时产生的加工粉是指：对碳化硅系蜂窝单元1进行磨削使其成为规定形状时产生的磨削粉、以及将碳化硅系蜂窝单元1的不合格品等粉碎得到的粉末。另外，本说明书中，制造碳化硅系蜂窝结构体10时产生的加工粉是指：对碳化硅系蜂窝结构体10进行磨削使其成为规定形状时或对端面进行磨削使其平滑化时产生的磨削粉、以及将碳化硅系蜂窝结构体10的不合格品等粉碎得到的粉末。
加工粉的平均粒径D50为0.5～60μm。通过使加工粉的平均粒径D50为该范围，能够确保接合层2所需求的接合强度及杨氏模量。从接合层2的接合强度及杨氏模量的观点考虑，加工粉的平均粒径D50优选为0.8μm以上，更优选为1.0μm以上，进一步优选为1.5μm以上。同样地，从接合层2的接合强度及杨氏模量的观点考虑，加工粉的平均粒径D50优选为58μm以下，更优选为56μm以下，进一步优选为55μm以下。
此处，本说明书中，平均粒径D50是指：利用激光衍射散射法求出的累计粒度分布(体积基准)中的累计值50％处的粒径。
加工粉的平均粒径D10没有特别限定，优选为0.1～10μm，更优选为0.3～9.8μm，进一步优选为0.5～9.5μm。通过将加工粉的平均粒径D10控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
另外，加工粉的平均粒径D90没有特别限定，优选为4～150μm，更优选为5～130μm，进一步优选为6～120μm。通过将加工粉的平均粒径D10控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
此处，本说明书中，平均粒径D10及D90分别是指：与平均粒径D50同样地利用激光衍射散射法求出的累计粒度分布(体积基准)中的累计值10％及90％处的粒径。
接合材料除了含有上述的加工粉以外，可以进一步含有选自无机粉末、无机纤维、造孔材料、粘合剂以及分散剂中的1种以上。
作为这些成分，没有特别限定，可以使用该技术领域中公知的物质。另外，这些成分可以与碳化硅系蜂窝单元1中使用的成分相同，也可以不同，不过，通过使其与碳化硅系蜂窝单元1中使用的成分相同，容易形成接合强度及杨氏模量良好的接合层2。
接合材料中的无机粉末的含量没有特别限定，优选为50质量％以下，更优选为1～48质量％，进一步优选为5～46质量％。通过将无机粉末的含量控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
接合材料中的无机纤维的含量没有特别限定，优选为25质量％以下，更优选为1～20质量％，进一步优选为3～15质量％。通过将无机纤维的含量控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
接合材料中的造孔材料的含量没有特别限定，优选为10质量％以下，更优选为0.1～8质量％，进一步优选为1～6质量％。通过将造孔材料的含量控制在上述范围内，容易形成具有与碳化硅系蜂窝单元1同种程度的气孔率且接合强度与杨氏模量之间的平衡良好的接合层2。
接合材料中的粘合剂的含量没有特别限定，优选为15质量％以下，更优选为1～12质量％，进一步优选为3～10质量％。通过将粘合剂的含量控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
接合材料中的分散剂的含量没有特别限定，优选为3质量％以下，更优选为2质量％以下，进一步优选为0.1～1质量％。通过将分散剂的含量控制在上述范围内，容易形成接合强度与杨氏模量之间的平衡良好的接合层2。
接合材料可以如下制造，即，在上述成分中添加水，使用混合器等混炼机进行混合及混炼，使其成为糊料状，由此制造接合材料。
如上所述得到的接合材料可以有效利用制造碳化硅系蜂窝单元1或碳化硅系蜂窝结构体10时产生的加工粉。另外，该接合材料可以提供接合强度高且杨氏模量低的接合层2。此外，该接合材料使用制造碳化硅系蜂窝单元1或碳化硅系蜂窝结构体10时产生的加工粉，因此，碳化硅系蜂窝单元1的色调和接合层2的色调相近。因此，能够容易地采用自动外观检查机来检查碳化硅系蜂窝结构体10的外观不良等，上述检查以往因色调差较大而比较难以实施。
碳化硅系蜂窝结构体10使用上述的碳化硅系蜂窝单元1及接合材料来制造。其制造方法没有特别限定，可以利用该技术领域中公知的方法来进行。
具体而言，在碳化硅系蜂窝单元1的侧面涂布接合材料，将碳化硅系蜂窝单元1的侧面间接合后，使其干燥，由此能够使接合材料固化而形成接合层2。作为干燥条件，根据接合材料的组成进行适当调节即可，优选于60～170℃进行0.5～6.0小时干燥。另外，可以一边通过从外部施加压力而使碳化硅系蜂窝单元1彼此压接，一边进行干燥。
另外，对于将所有碳化硅系蜂窝单元1借助接合层2而接合得到的接合体，可以根据需要对外周部进行磨削加工等，将其加工成圆柱状等所期望的形状。在这种情况下，通过加工将外周壁除去，使其处于内部的隔壁4和隔室3暴露出来的状态，因此，优选进行以涂覆材料被覆露出面等操作而重新形成外周涂层5。
碳化硅系蜂窝结构体10的形状没有特别限定，除了圆柱状以外，可以制成端面为椭圆形的柱状、端面为正方形、长方形、三角形、五边形、六边形等多边形的柱状等。
对于碳化硅系蜂窝结构体10，接合层2的接合强度(剪切强度)优选为200～2000kPa，更优选为300～1500kPa，进一步优选为400～1200kPa。如果接合层2的接合强度在上述范围内，则能够确保DPF及GPF等各种用途中所需求的碳化硅系蜂窝结构体10的粘接强度。
对于碳化硅系蜂窝结构体10，接合层2的杨氏模量优选为4～100MPa，更优选为5～80MPa，进一步优选为6～60MPa。如果接合层2的杨氏模量在上述范围内，则能够充分确保DPF及GPF等各种用途中所需求的缓和热应力的功能。
对于碳化硅系蜂窝结构体10，接合层2的气孔率优选为40～85％，更优选为45～83％，进一步优选为50～80％。如果接合层2的气孔率在上述范围内，则能够确保粘接强度与杨氏模量之间的平衡。
对于碳化硅系蜂窝结构体10，接合层2的热膨胀系数优选为2.0×10-6～8.0×10-6/K，更优选为2.5×10-6～7.5×10-6/K，进一步优选为3.0×10-6～7.0×10-6/K。如果接合层2的热膨胀系数在上述范围内，则能够充分确保缓和热应力的功能。
具有如上所述特征的碳化硅系蜂窝结构体10有效利用制造碳化硅系蜂窝单元1或碳化硅系蜂窝结构体10时产生的加工粉，因此，能够降低制造成本。另外，该碳化硅系蜂窝结构体10由于接合层2的接合强度高且杨氏模量低，可确保缓和热应力的功能，所以耐久性高。另外，该碳化硅系蜂窝结构体10由于碳化硅系蜂窝单元1的色调和接合层2的色调相近，所以还能够容易地进行使用自动外观检查机来检查碳化硅系蜂窝结构体10的外观不良等。
碳化硅系蜂窝结构体10可以用作DPF、GPF等集尘用过滤器。在用作集尘用过滤器的情况下，优选如上所述在碳化硅系蜂窝单元1的2个端面中的任意一个端面形成将隔室3的一个端部封孔的封孔部。通常，按一个端面和另一个端面呈互补的棋盘格状的方式将相邻的隔室3交替地封孔。
如果从由如上所述地实施了封孔的碳化硅系蜂窝单元1构成的碳化硅系蜂窝结构体10的一端面通入烟灰等包含颗粒的流体，则流体在该一端面侧从端部未被封孔的隔室3流入到碳化硅系蜂窝结构体10的内部，通过具有过滤能力的多孔质的隔壁4，进入碳化硅系蜂窝结构体10的另一端面侧未被封孔的其他流通孔。然后，在通过该隔壁4时，流体中的颗粒被隔壁4捕捉，除去了颗粒的净化后的流体从碳化硅系蜂窝结构体10的另一端面排出。
对于碳化硅系蜂窝结构体10，可以使催化剂担载于隔壁4的表面或细孔内。作为催化剂，没有特别限定，可以根据碳化硅系蜂窝结构体10的用途进行选择。例如，在将碳化硅系蜂窝结构体10用作DPF的情况下，可以使用用于将废气中的煤烟灰等氧化除去的氧化催化剂、用于将废气中包含的NOx等有害物质分解除去的NOx选择还原催化剂(SCR)以及NOx吸储还原催化剂等。催化剂的担载方法没有特别限定，可以使用该技术领域中公知的方法。
实施例
以下，通过实施例对本发明更具体地进行说明，但是，本发明并不受这些实施例的任何限定。
(碳化硅系蜂窝单元的制作)
作为原料，将碳化硅粉末及金属硅粉末以80：20的质量比例混合，在其中加入造孔材料、粘合剂、表面活性剂以及水，进行混合及混炼，制成坯土。接下来，将得到的坯土挤出成型并切断，利用微波及热风进行干燥，由此，得到隔壁的厚度为300μm、隔室密度为46.5隔室/cm2、与隔室延伸的方向垂直的截面为边长38mm的正四边形、长度为152mm的碳化硅系蜂窝单元。
接下来，针对该碳化硅系蜂窝单元，按端面呈棋盘格状的方式将各隔室的一个端部封孔。应予说明，用于将隔室的端部封孔的封孔用浆料使用与蜂窝单元原料同样的材料。封孔如下进行，即，使填充材料干燥后，将碳化硅系蜂窝单元在大气气氛中于400℃进行脱脂，然后，在Ar惰性气氛中于1450℃进行烧成，由此进行封孔。
(接合材料的制备)
将表1所示的比例的加工粉、无机粉末、无机纤维、粘合剂、造孔剂、分散剂、以及余量(合计为100质量％的比例)的水进行配合、混合，由此制备糊料状的接合材料。作为加工粉，使用上述的碳化硅系蜂窝单元的切削粉及其不合格品的粉碎粉。
(碳化硅系蜂窝结构体的制作)
在碳化硅系蜂窝单元的侧面，按厚度1mm的方式涂布接合材料，并与其他碳化硅系蜂窝单元的侧面接合。反复进行该工序，制作将纵4个×横4个碳化硅系蜂窝单元接合得到的合计16个碳化硅系蜂窝单元的层叠体。然后，一边从外部施加压力而使碳化硅系蜂窝单元彼此压接，一边于120℃进行2小时干燥，得到接合体。接下来，对接合体的外周进行切削加工，以使与得到的接合体的中心轴垂直的方向的截面为圆形。接下来，在其加工面涂布与接合材料相同组成的外周涂覆材料，然后，于600℃加热0.5小时以上，由此使其干燥及固化，形成外周涂层，得到碳化硅系蜂窝结构体。
对上述得到的碳化硅系蜂窝结构体进行下述的评价。
(1)接合层的粘接强度(剪切强度)
从碳化硅系蜂窝结构体中切出2根碳化硅系蜂窝单元接合得到的样品。接下来，沿着该样品的接合层的Y轴方向(长度方向)施加剪切载荷。然后，使用此时的破坏载荷和接合层的面积，利用下式(1)，计算出剪切强度。
σ＝(W/S)×1000…(1)
σ：剪切强度(kPa)
W：破坏载荷(N)
S：接合层的面积(mm2)
(2)接合层的杨氏模量
从碳化硅系蜂窝结构体中切出包含接合层部分的规定尺寸(直径25.4mm、厚度3mm)的圆柱状的样品。然后，对该样品进行Z轴方向上的压缩试验。此处，“Z轴方向”是与接合层和碳化硅系蜂窝单元之间的接合面垂直的方向。应予说明，该试验时，上述样品可以附带有碳化硅系蜂窝单元的一部分。将沿着Z轴方向对试样施加载荷至0～3MPa时的应力－形变曲线中的斜率作为杨氏模量(压缩杨氏模量)，利用下式(2)进行计算。
E＝(W/S)×(t/Δt)…(2)
E：压缩杨氏模量(MPa)
W：载荷(N)
S：样品的面积(mm2)
t：样品的厚度(mm)
Δt：样品的厚度的变化量
(3)接合层的气孔率
对于接合层的气孔率，从碳化硅系蜂窝结构体中切出接合层部分，使用压汞仪(Micromeritics公司制Autopore IV9500)进行测定。
(4)接合层的热膨胀系数
利用碳化硅系蜂窝结构体制作用的接合材料另行制作接合层的样品，评价热膨胀系数。将使接合材料于140℃干燥2小时得到的干燥体切成纵3mm×横3mm×长度20mm，得到接合层的样品。另外，对于热膨胀系数，依据JIS R1618：2002，测定样品的长度方向上的40～800℃下的平均线热膨胀系数(热膨胀系数)。
(5)接合层的干燥开裂
通过裸眼观察碳化硅系蜂窝结构体的端面处的接合层来评价干燥开裂。将完全没有发现干燥开裂的情形表示为“A”，将仅发现长度为5mm以下的微小干燥开裂的情形表示为“B”，将发现长度超过5mm的干燥开裂的情形表示为“C”。
(6)接合层的接合宽度
通过测定碳化硅系蜂窝结构体的端面处的接合层的接合宽度来评价接合层的接合宽度。将接合宽度为1.5mm以下的情形表示为“A”，将接合宽度超过1.5mm且小于3.0mm的情形表示为“B”，将接合宽度为3.0mm以上的情形表示为“C”。
将上述的各评价结果示于表1。
表1
Figure BDA0002386883690000121
如表1所示，可知，使用包含加工粉的接合材料而制作的实施例1～15的碳化硅系蜂窝结构体具有与使用不含加工粉的接合材料而制作的比较例1的碳化硅系蜂窝结构体相比毫不逊色的接合强度及杨氏模量，可以在接合材料中有效利用加工粉。
另外，如表1所示，使用将加工粉的含量及平均粒径D50控制在规定的范围内的接合材料而制作的实施例1～15的碳化硅系蜂窝结构体与使用加工粉的含量在规定的范围外的接合材料或加工粉的平均粒径D50在规定的范围外的接合材料而制作的比较例2～4的碳化硅系蜂窝结构体相比，接合层的接合强度提高。应予说明，实施例1～15的碳化硅系蜂窝结构体与比较例2～4的碳化硅系蜂窝结构体相比，虽然接合层的杨氏模量升高，但是能够使用的水平。
由以上结果可知，根据本发明，能够提供可有效利用制造碳化硅系蜂窝单元或碳化硅系蜂窝结构体时产生的加工粉的接合材料及碳化硅系蜂窝结构体。

Claims (9)

1.一种接合材料，其用于将多个碳化硅系蜂窝单元的侧面接合来制造碳化硅系蜂窝结构体，
所述接合材料的特征在于，
所述接合材料含有0.1～50质量％的加工粉，所述加工粉是在制造所述碳化硅系蜂窝单元和/或所述碳化硅系蜂窝结构体时产生的，
所述加工粉的平均粒径D50为0.5～60μm。
2.根据权利要求1所述的接合材料，其特征在于，所述加工粉的D10为0.1～10μm。
3.根据权利要求1或2所述的接合材料，其特征在于，所述加工粉的D90为4～150μm。
4.根据权利要求1～3中任一项所述的接合材料，其特征在于，所述接合材料还含有选自无机粉末、无机纤维、造孔材料、粘合剂以及分散剂中的1种以上。
5.一种碳化硅系蜂窝结构体，其具备：多个碳化硅系蜂窝单元、以及将多个所述碳化硅系蜂窝单元的侧面间接合的接合层，
所述碳化硅系蜂窝结构体的特征在于，
所述接合层为权利要求1～4中任一项所述的接合材料的固化层。
6.根据权利要求5所述的碳化硅系蜂窝结构体，其特征在于，所述接合层的接合强度为200～2000kPa。
7.根据权利要求5或6所述的碳化硅系蜂窝结构体，其特征在于，所述接合层的杨氏模量为4～100MPa。
8.根据权利要求5～7中任一项所述的碳化硅系蜂窝结构体，其特征在于，所述接合层的气孔率为40～85％。
9.根据权利要求5～8中任一项所述的碳化硅系蜂窝结构体，其特征在于，所述接合层的热膨胀系数为2.0×10-6～8.0×10-6/K。
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