CN100480215C - 蜂窝结构体及其制造方法 - Google Patents

蜂窝结构体及其制造方法 Download PDF

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CN100480215C
CN100480215C CNB2005800064568A CN200580006456A CN100480215C CN 100480215 C CN100480215 C CN 100480215C CN B2005800064568 A CNB2005800064568 A CN B2005800064568A CN 200580006456 A CN200580006456 A CN 200580006456A CN 100480215 C CN100480215 C CN 100480215C
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fibre
honeycomb structured
structured body
inorganic
weight
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CN1926076A (zh
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恒川肇
国枝雅文
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Ibiden Co Ltd
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Abstract

本发明涉及一种包含陶瓷粒子和无机纤维而成的蜂窝结构体及其制造方法,其中,所述无机纤维满足长径比≥纤维强度(GPa)/0.3。以无机纤维的长径比(=纤维长度/纤维直径)与纤维强度(GPa)除以0.3所得到的值一致的情况为界,当等于或大于该值时,所述蜂窝结构体显示出很高的强度。即,当使用满足上述表达式的无机纤维时,可以得到具有高强度的蜂窝结构体。

Description

蜂窝结构体及其制造方法
技术领域
本发明涉及一种蜂窝结构体及其制造方法,更具体地说,涉及一种包含陶瓷粒子和无机纤维的蜂窝结构体及其制造方法。
技术背景
以前,包含陶瓷粒子、无机纤维和无机粘合剂的蜂窝结构体是为人们所知的。例如,在特开平5-203681号公报中公开了一种制造蜂窝结构体的制造方法,该制造方法中,调制将诸如氧化铝、氧化硅等陶瓷粉末以及诸如陶瓷纤维、金属纤维等无机纤维和诸如硅胶、氧化铝溶胶、粘土矿物等无机粘合剂进行混合而成的含有陶瓷的组合物;将所述组合物挤出成型;将成型物加热干燥后进行烧制。这样制造的蜂窝结构体具有优异的耐热性、强度,并且不易脆性破裂。
发明内容
但是,在上述专利公报中,关于无机纤维,有纤维长度约为0.02毫米~2毫米和纤维直径约为0.1微米~20微米。然而,即使使用具有在该范围内的纤维长度和纤维直径的无机纤维,对于某些种类的无机纤维来说,也有不能得到高强度的蜂窝结构体的情况。
本发明是鉴于这样的问题提出的,本发明的目的之一是提供一种包含陶瓷粒子和无机纤维并且具有高强度的蜂窝结构体。此外,本发明的另一目的是提供适合于制造这样的蜂窝结构体的制造方法。
为了解决上述问题,本发明的发明人深入研究了无机纤维的长径比、纤维强度和蜂窝结构体的弯曲强度之间的关系,结果发现当长径比和纤维强度具有一定关系时,弯曲强度稳定在高数值,从而完成了本发明。
即,本发明提供一种包含陶瓷粒子和无机纤维而成的蜂窝结构体,其中所述无机纤维满足长径比≧纤维强度(GPa)/0.3。以无机纤维的长径比(=纤维长度/纤维直径)与纤维强度(GPa)除以0.3所得到的值一致的情况为界,当等于或大于该值时,所述蜂窝结构体显示出很高的强度。即,当使用满足上述表达式的无机纤维时,可以得到具有高强度的蜂窝结构体。此外,所谓纤维强度是指纤维材料的拉伸强度。
在此,作为所述陶瓷粒子,没有特别的限制,例如,可以举出选自以下的一种或两种以上的粒子:氧化铝、氧化硅、氧化锆、氧化钛、氧化铈、莫来石(mullite)及沸石。其中优选氧化铝。所述陶瓷粒子优选占总体的30重量%~90重量%。当所述陶瓷粒子的含量低于30重量%时,有助于提高比表面积的陶瓷粒子的含量相对减少,并且所述蜂窝结构体每单位体积的比表面积减小,可能产生一些不合适的情况,例如催化剂成分不能高度分散等。当所述陶瓷粒子的含量超过90重量%时,有助于提高强度的无机纤维、无机粘合剂的含量相对减少,所述蜂窝结构体的强度可能不能充分提高。此外,所述陶瓷粒子的2次粒子的平均粒径优选为1微米~5微米,比表面积优选为100平方米/克以上。
此外,作为所述无机纤维,没有特别的限制,例如,可以举出陶瓷纤维、玻璃纤维、金属纤维、碳纤维、岩石纤维、矿渣纤维等。其中优选陶瓷纤维、玻璃纤维。在此,所谓陶瓷纤维是指非金属无机材料的纤维,例如,可以举出碳化硅纤维、碳化硼纤维等碳化物类陶瓷纤维;氮化硅纤维、氮化硼纤维等氮化物类陶瓷纤维;氧化锆纤维、氧化铝纤维、氧化硅纤维、氧化硅-氧化铝纤维、氧化铝-氧化硼(boroar)-氧化硅纤维、钛酸钾纤维、硼酸铝纤维等氧化物类陶瓷纤维等。此外,作为所述玻璃纤维,例如,可以举出硼硅酸类玻璃纤维、碱石灰类玻璃纤维(soda lime glass fiber)、石英玻璃纤维等。此外,作为所述金属纤维,例如,可以举出不锈钢纤维、钢纤维等。无机纤维的含量优选为总体的5重量%~30重量%。当所述无机纤维的含量低于总体的5重量%时,可能不能充分地获得基于无机纤维的增强效果。当其含量超过总体的30重量%时,无机粒子的含量相对减少,作为蜂窝结构体可能不能得到足够的比表面积。此外,所述无机纤维的长径比优选为5以上。无论无机纤维的种类是哪种,如果长径比不到5以上,则有可能不能充分地获得基于无机纤维的增强效果。
作为本发明的蜂窝结构体中包含的无机粘合剂,没有特别的限制,例如可以举出无机溶胶、粘土类粘合剂等。其中,作为所述无机溶胶,例如,可以举出选自以下的一种或两种以上的无机溶胶:氧化铝溶胶、氧化硅溶胶、氧化钛溶胶和水玻璃等。作为所述粘土类粘合剂,例如,可以举出选自以下的一种或两种以上的粘土类粘合剂:陶土、高岭土、蒙脱土和多链结构型粘土(海泡石(sepiolite)、绿坡缕石(attapulgite))等。作为在所述蜂窝结构体中包含的固体成分,在所述蜂窝结构体中包含的无机粘合剂的含量优选为50重量%以下,更优选为5重量%~50重量%,进一步优选为10重量%~40重量%,最优选为15重量%~35重量%。当所述无机粘合剂的含量超过50重量%时,成型性变差。
本发明的蜂窝结构体可以用作车辆尾气净化装置的一个构成要素。例如,其可以用作车辆尾气净化用的催化剂载体,还可以用作过滤和净化包含在柴油发动机的尾气中的微粒的柴油机微粒过滤器(DPF)。当所述蜂窝结构体用作催化剂载体时,作为所负载的催化剂成分,没有特别的限制,可以是贵金属、碱金属化合物、碱土类金属化合物、氧化物等。作为所述贵金属,例如,可以举出选自以下的一种或两种以上贵金属:铂、钯、铑等。作为所述碱金属化合物,例如,可以举出选自钾、钠等的一种或两种以上的化合物。作为所述碱土类金属化合物,例如,可以举出钡等的化合物。作为所述氧化物,例如,可以举出钙钛矿(La0.75K0.25MnO3等)及二氧化铈(CeO2)等。虽然所得到的蜂窝催化剂没有特别的限制,但是可以用作例如汽车尾气净化的所谓三元催化剂和NOX吸收储藏催化剂。此外,催化剂成分的负载没有特别的限制,既可以在蜂窝结构体制造之后进行所述催化剂的负载,也可以在原料的陶瓷粒子的阶段进行所述催化剂的负载。所述催化剂成分的负载方法没有特别的限制,可以通过例如浸渍法等进行负载。此外,当所述蜂窝结构体用作DPF时,形成为蜂窝形状的多个通道中,一端开口、另一端闭口的通道和一端闭口、另一端开口的通道同时存在。
下面,对上述的本发明的蜂窝结构体的制造方法的一个实例进行说明。首先,使用以所述陶瓷粒子、无机纤维和无机粘合剂作为主要成分的原料糊并且进行挤出成型,以制作蜂窝成型体。除上述物质之外,还可以结合成型性向所述原料糊中适量加入有机粘合剂、分散介质及成型助剂。作为所述有机粘合剂,例如,可以举出选自以下的一种或两种以上的有机粘合剂:甲基纤维素、羧甲基纤维素、羟乙基纤维素、聚乙二醇、酚树脂(phenol resin)和环氧树脂等。相对于陶瓷粒子、无机纤维和无机粘合剂的总体,所述有机粘合剂的混合量优选为1重量%~10重量%。作为所述分散介质,例如,可以举出水、有机溶剂(苯等)和醇(甲醇等)等。作为所述成型助剂,例如,可以举出乙二醇、糊精、脂肪酸、脂肪酸皂及多元醇。然后,将所得到的成型体在干燥机中进行干燥。作为所述干燥机,例如,可以举出微波干燥机、热风干燥机、介电干燥机、减压干燥机(evacuation drying machine)、真空干燥机或者冷冻干燥机等。此外,优选将干燥后的成型体进行脱脂。所述脱脂的条件根据所述成型体中所含有机物的种类和含量可以进行适当选择,例如可以在400摄氏度下进行约2小时的脱脂。然后,将所述成型体进行烧制。作为烧制条件,例如,优选为600~1000摄氏度。当所述烧制温度低于600摄氏度时,所述陶瓷粒子等的烧结可能难以进行,并且所述蜂窝结构体的强度可能不能充分提高。相反地,当所述烧制温度超过1000摄氏度时,所述陶瓷粒子等的烧制可能进行的过度,并且每单位体积的比表面积可能减小。通过上述过程,可以得到蜂窝结构体。
在所述蜂窝结构体的制造方法中,例如,也可以在成型为与所述最终形状相同形状的蜂窝成型体之后,经过将成型体干燥、脱脂和烧制的各过程得到目标蜂窝结构体。或者,也可以成型为比最终形状小的小型蜂窝成型体;经过干燥、脱脂、烧制的各过程得到蜂窝单元之后,利用密封层将多个所述蜂窝单元相互粘结、堆积,以构成比最终形状大的形状;然后进行切割、研磨,得到目标蜂窝结构体。在这种情况下,作为所述密封层,例如可以使用与所述原料糊相同的材料。另外,利用所述密封层将所述蜂窝单元相互粘结之后,可以只进行干燥而不进行脱脂和烧制;或者,也可以进行到干燥-脱脂而不进行烧制;或者,也可以进行到干燥-脱脂-烧制。此外,本发明的蜂窝结构体的剖面形状没有特别的限制,可以是圆形、椭圆形或者多边形(例如,三边~八边形)。
此外,在本说明书中使用的各物理性质值通过以下方式得到。即,平均粒径使用MALVERN粒度分析仪,通过激光衍射散射法得到。此外,纤维直径、纤维长度从使用SEM得到的放大图像求得,但是也可以使用光学显微镜和激光显微镜获得。此外,长径比根据纤维直径和纤维长度通过计算求得。此外,纤维强度使用制造商公布的值。
附图说明
图1是蜂窝催化剂载体的透视图;
图2是蜂窝单元的透视图;
图3是蜂窝单元集合体的透视图;
图4是说明使用玻璃纤维时长径比和弯曲强度的关系的图表;
图5是说明使用氧化硅-氧化铝纤维时长径比和弯曲强度的关系的图表;
图6是说明使用钛酸钾纤维时长径比和弯曲强度的关系的图表;
图7是说明使用碳化硅纤维时长径比和弯曲强度的关系的图表;
图8是说明使用硼酸铝纤维时长径比和弯曲强度的关系的图形。
具体实施方式
下面,根据附图对本发明的实施方式进行说明。图1是本发明的一个实施方式的蜂窝催化剂载体10的透视图。图2是基本蜂窝单元20的透视图。图3是单元集合体30的透视图。
蜂窝催化剂载体10是本发明的蜂窝结构体的一个实例,如图1所示,其为圆柱形,并且具有贯穿底表面10a和上表面10b的多个通道12。所述蜂窝催化剂载体10具有配置在中央区域的多个长方体形状的基本蜂窝单元20、将这些基本蜂窝单元20的周围围起而沿圆周配置的变形蜂窝单元22、将所述基本蜂窝单元20和所述变形蜂窝单元22的外表面进行相互粘结的密封层24和覆盖所述变形蜂窝单元22的外周面形成的圆筒状的包覆层26。
如图2所示,所述基本蜂窝单元20为具有正方形剖面的长方体,并且具有沿轴向并置的多个通孔20a。所述通孔20a形成所述蜂窝催化剂载体10的通道12。所述基本蜂窝单元20,例如可以如下所述进行制作。即,首先,将γ氧化铝粒子(平均粒径2微米)、无机纤维和作为无机粘合剂的氧化硅溶胶(固体浓度30重量%)分别以40重量%、10重量%、50重量%的比例进行混合,相对于所得到的混合物为100重量份,再加入6重量份作为有机粘合剂的甲基纤维素和少量增塑剂和滑润剂,并且进一步进行混合、混练以得到原料糊。此时,使用长径比即(纤维长度/纤维直径)等于或大于纤维强度(GPa)除以0.3所得到的值的无机纤维。然后,将所述原料糊通过挤出成型机进行挤出成型,得到未加工的成型体。将所述未加工的成型体的形状制成与在图2中所示的基本蜂窝单元20相同的形状。接下来,使用微波干燥机及热风干燥机将未加工的成型体进行充分干燥,并且在400摄氏度下保持2小时以进行脱脂。然后,在800摄氏度下保持2小时以进行烧制,从而得到基本蜂窝单元20,其形状为长方体(34.3毫米×34.3毫米×150毫米)、孔(cell)密度为62个/平方厘米(400cpsi)、壁厚为0.25毫米。
所述变形蜂窝单元22为在剖面的一部分上具有圆弧形状的柱状体,并且具有沿轴向并置的多个通孔22a。所述通孔22a形成所述蜂窝催化剂载体10的通道12。所述变形蜂窝单元22通过以下步骤得到:首先,利用密封层24将多个基本蜂窝单元20以相邻的基本蜂窝单元20之间在外表面互相粘结的方式进行堆积,以此制成尺寸上包含最终形状的圆柱形的单元集合体30(参见图3);然后,切割该单元集合体30以使其变为圆柱形的最终形状;此时,将沿所述圆柱形集合体30的外周圆并置的基本蜂窝单元20被切割成在剖面的一部分上具有圆弧形的圆柱体,这就是所述变形蜂窝单元22。
所述密封层24在此可以使用与制作所述基本蜂窝单元20时使用的原料糊相同的材料,并且起到将所述相邻的基本蜂窝单元20、变形蜂窝单元22的外表面相互粘结的作用。将所述基本蜂窝单元20、变形蜂窝单元22互相粘结之后,将所述密封层24是经过了干燥、脱脂的,但没有经过烧制。此外,所述密封层24的厚度优选设定为0.5毫米~2毫米。当厚度小于0.5毫米时,可能不能得到足够的粘结力,而当厚度大于2毫米时,没有作为催化剂载体功能的所述密封层24所占比例提高,可能不能将催化剂充分地分散和负载。
所述包覆层26在此可以使用与制作所述基本蜂窝单元20时所用的原料糊相同的材料,并且起到以下作用:填补在切割所述单元集合体30成为圆柱形的最终形状时所述变形蜂窝单元22的通孔22a中通道壁被破坏的部分,同时将所述蜂窝催化剂载体10的外周面修饰成为平滑圆筒面。与所述密封层24同样,所述包覆层26也是经过了干燥、脱脂的,但没有经过烧制。此外,所述包覆层26的厚度优选设定为0.1毫米~2毫米。当厚度小于0.1毫米时,所述包覆层26可能不能充分地保护外圆周面,而当厚度大于2毫米时,没有作为催化剂载体功能的所述包覆层26所占比例提高,可能不能将催化剂充分地分散和负载。
下面,对本实施方式的蜂窝催化剂载体10的使用例进行说明。首先,将所述蜂窝催化剂载体10在硝酸铂溶液中浸泡,并且进行调节以使所述蜂窝催化剂载体10的每单位体积的铂重量变为2克/升,然后在600摄氏度下保持1小时,借此得到蜂窝催化剂。将所述蜂窝催化剂收容在配置于汽车发动机的排气集管的下游侧的套管中,实现净化从发动机排出的尾气的作用。
以上详述的本实施方式的蜂窝催化剂载体10主要由基本蜂窝单元20、变形蜂窝单元22构成,所述基本蜂窝单元20、变形蜂窝单元22是包含γ氧化铝粒子和无机纤维的烧制体。由于在此所用的无机纤维的长径比等于或大于纤维强度(GPa)除以0.3所得到的值,因此可以得到作为蜂窝结构体其强度高的蜂窝催化剂载体。这一点已经通过下述实验例进行了验证。
此外,由于可以如此得到具有高强度的蜂窝催化剂载体10,因此可以防止以下问题的发生:在蜂窝催化剂载体10的制造过程中的破裂、破损等问题、将蜂窝催化剂载体10收容在套管内的时候的破裂、破损等问题、将蜂窝催化剂载体10收容在套管内和使用的时候的震动和热等造成的破裂、破损等。
实施例
[实验例1~22]
首先,混合40重量%γ氧化铝粒子(平均粒径2微米)、10重量%无机纤维(纤维种类、纤维强度、纤维长度、纤维直径、长径比如表1所示)和50重量%氧化硅溶胶(固体浓度30重量%),相对于所得到的混合物为100重量分,再加入6重量份作为有机粘合剂的甲基纤维素和少量的增塑剂、润滑剂,并且进一步进行混合、混练以得到混合组合物。然后,通过挤出成型机将该混合组合物进行挤出成型,得到未加工的成型体。然后,利用微波干燥机及热风干燥机将未加工的成型体进行充分干燥,并在400摄氏度下保持2小时以进行脱脂。然后,在800摄氏度下保持2小时以进行烧制,从而得到基本蜂窝单元,该基本蜂窝单元形状为长方体(34.3毫米×34.3毫米×150毫米)、孔密度为62个/平方厘米(400cpsi)、壁厚为0.25毫米。
[3点弯曲强度]
进行实验例1~22的3点弯曲强度测量。该测量使用Instron公司生产的5582作为测量仪器,以JIS-R1601为标准进行测量。具体地,十字头移动速率设为1毫米/分钟、跨距L设为135毫米,垂直于基本蜂窝单元的轴向施加载荷并测量破坏载荷W。通过扣除贯通孔的部分的力矩以计算剖面2次力矩Z。然后,通过下式算出3点弯曲强度σ。其结果示于表1和图4~图8。
σ=WL/4Z
表1
 
编号 纤维种类 纤维强度(GPa)    纤维长度(微米)   纤维直径(微米)   Rasp 纤维强度/0.3     σ(MPa)
1 玻璃 1.5 50 10 5 5 4.2
2 玻璃 1.5 100 10 10 5 4.3
3 玻璃 1.5 150 10 15 5 43
4 玻璃 1.5 30 5 6 5 4.3
5 玻璃 1.5 20 10 2 5 1.3
6 玻璃 1.5 30 10 3 5 3.2
7 氧化硅氧化铝 1.7 18 3 6 5.67 4.1
8 氧化硅氧化铝 1.7 50 3 16.7 5.67 4.2
9 氧化硅氧化铝 1.7 40 5 8 5.67 4.2
10 氧化硅氧化铝 1.7 15 3 5 5.67 3.4
11 钛酸钾 7 12 0.5 24 23.3 4.3
12 钛酸钾 7 15 0.5 30 23.3 4.3
13 钛酸钾 7 9 0.5 18 23.3 3.6
14 钛酸钾 7 6 0.5 12 23.3 2.3
15 碳化硅 3.4 6 0.5 12 11.3 4.2
16 碳化硅 3.4 15 0.5 30 11.3 44
17 碳化硅 3.4 10 0.5 20 11.3 4.2
18 碳化硅 3.4 3 0.5 6 11.3 2.5
19 硼酸铝 7.8 13 0.5 26 26 4.1
20 硼酸铝 7.8 15 0.5 30 26 4.1
21 硼酸铝 7.8 10 0.5 20 26 3.4
22 硼酸铝 7.8 5 0.5 10 26 1.6
表中,Rasp表示长径比,σ表示弯曲强度。
如表1及图4~图8所示,在任何一类纤维中,以纤维强度(GPa)除以0.3所得到的值作为界,当长径比在界值以上时,显示出基本蜂窝单元的3点弯曲强度σ稳定在较高的数值的倾向。
此外,本发明不受上述实施方案和实验例的任何限制,只要属于本发明的技术范围,可以以各种各样的形式实施。
本发明是以在2004年10月8日提出申请的日本国专利申请2004-296316号作为要求优先权的基础,并且其全部内容被编入本发明。
产业实用性
本发明可适用于搭载发动机的动力机器和车辆等相关的产业,例如,可适用于在汽车产业、摩托车产业等。

Claims (9)

1.一种蜂窝结构体,该蜂窝结构体是包含陶瓷粒子和无机纤维的蜂窝结构体,其中所述无机纤维满足长径比≧纤维强度(GPa)/0.3。
2.如权利要求1所述的蜂窝结构体,其中所述无机纤维的含量为总体的5重量%~30重量%。
3.如权利要求1或2所述的蜂窝结构体,其中所述无机纤维的长径比为5以上。
4.如权利要求1或2所述的蜂窝结构体,其中所述无机纤维为陶瓷纤维或玻璃纤维。
5.如权利要求1或2所述的蜂窝结构体,其中所述蜂窝结构体被用作车辆尾气净化装置的一个构成要素。
6.一种蜂窝结构体的制造方法,该方法包括以下步骤:至少将陶瓷粒子、无机纤维和无机粘合剂进行混合来得到混合组合物;将该混合组合物成型为蜂窝形状来得到成型体;对该成型体进行烧制来得到蜂窝结构体;其中所述无机纤维满足长径比≧纤维强度(GPa)/0.3。
7.如权利要求6所述的蜂窝结构体的制造方法,其中所述无机纤维的含量为总体的5重量%~30重量%。
8.如权利要求6所述的蜂窝结构体的制造方法,其中所述无机纤维的长径比为5以上。
9.如权利要求6~8中任一项所述的蜂窝结构体的制造方法,其中所述无机纤维为陶瓷纤维或玻璃纤维。
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