CN101553445A - 钛酸铝质陶瓷蜂窝状结构体的制造方法 - Google Patents
钛酸铝质陶瓷蜂窝状结构体的制造方法 Download PDFInfo
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- CN101553445A CN101553445A CNA2007800456794A CN200780045679A CN101553445A CN 101553445 A CN101553445 A CN 101553445A CN A2007800456794 A CNA2007800456794 A CN A2007800456794A CN 200780045679 A CN200780045679 A CN 200780045679A CN 101553445 A CN101553445 A CN 101553445A
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- titanate
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- particle diameter
- honeycomb structure
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Abstract
钛酸铝质陶瓷蜂窝状结构体的制造方法,其为将配制好的TiO2和Al2O3的摩尔比为45∶55~55∶45范围的TiO2源粉末及Al2O3源粉末、助烧剂及/或助形剂进行混合及混炼,将形成的可塑性坯土挤压成形后,进行干燥及烧结的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述TiO2源粉末具有如下粒度分布,即:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大(相对于[log(粒径)]的质量基准的频率分布)。
Description
技术领域
本发明涉及钛酸铝质陶瓷蜂窝状结构体的制造方法。其中还涉及适合在大型陶瓷蜂窝状过滤器中使用的钛酸铝质陶瓷蜂窝状结构体的制造方法,所述大型陶瓷蜂窝状过滤器被用来净化含有从柴油机等中排放的PM的废气。
背景技术
柴油机的废气中,包含以含有炭质的煤烟和含有高沸点烃成分的SOF部分(Soluble Organic Fraction:可溶性有机成分)为主要成分的PM(Particulate Matter:粒状物质),这些物质释放到大气中后,可能会对人体、环境产生恶劣影响。因此,以往都在柴油机的排气管之中安装用于捕集PM的陶瓷蜂窝状过滤器(以下将陶瓷蜂窝状过滤器略称为“蜂窝状过滤器”)。捕集、净化废气中的PM的一例蜂窝状过滤器如图5(a)及图5(b)所示。蜂窝状过滤器10由陶瓷蜂窝状结构体、以及将流出侧封止流路3及流入侧封止流路4的废气流入侧端面8及废气流出侧端面9相互封止为交替排列的方格的上流侧封止部6a和下流侧封止部6c组成,该陶瓷蜂窝状结构体由形成多个流出侧封止流路3及流入侧封止流路4的多孔质隔壁2和外周壁1组成(以下有时简称为蜂窝状结构体)。
作为构成该蜂窝状结构体的隔壁的陶瓷,以往一直使用堇青石、碳化硅等耐热性陶瓷。其中,堇青石具有良好的耐热冲击性、捕集效率以及小的压力损失性能,从这点来看是最优选的陶瓷类,但是在使捕集的PM燃烧时,一旦处于非控制燃烧状态,则发生堇青石局部熔融的问题。局部熔融的发生与PM的捕集效率降低相关,故不优选。另一方面,碳化硅与堇青石相比熔点高,不易发生熔损,但是比堇青石的热膨胀系数大,耐热冲击性差,所以需要使多数截面积小的蜂窝状结构体贴在一起来制造,存在制造成本巨大的问题。
为了解决这种问题,近年来对于将耐热性良好的低热膨胀的钛酸铝质陶瓷类在蜂窝状过滤器中使用的尝试,进行了如下探讨。
日本特表2005-519834号公开了以下蜂窝状过滤器,即:由用Fe或Mg稳定的约50~90质量%的钛酸铝及约10~50质量%的锶·长石形成,具有低热膨胀系数、高耐热冲击性、高体积热容量、高相互连续气孔率及大的中位数细孔径,在800℃以上的热稳定性得到改善的蜂窝状过滤器。其中记载了该蜂窝状过滤器可通过以下方法制造,即:将二氧化硅、氧化铝、碳酸锶、二氧化钛、氧化铁、碳酸镁等陶瓷原料和增塑剂、润滑材料、粘合材料、溶剂等有机成分混合,将形成的混合物进行成形,根据需要干燥后进行烧结而制造。其中还记载了在该以往技术中,作为用于合成钛酸铝的原料的二氧化钛的供给源,优选具有约7~15μm粒径的金红石,对于Al2O3源粉末,优选约10~25μm粒径的氧化铝。
WO2005/018776号公开了由钛酸铝烧结体形成的蜂窝状过滤器,该钛酸铝烧结体为:将使TiO2(二氧化钛)和Al2O3(氧化铝)中含有1~10质量份的碱性长石、含Mg尖晶石型结构的氧化物、或MgO或通过烧结转化为MgO的含Mg化合物的原料混合物进行烧结而成的钛酸铝烧结体。其中记载了该蜂窝状过滤器在具有原来的高耐热性和低热膨胀系数的同时,改良了以往钛酸铝具有的在800~1280℃时热分解的问题、低机械强度。其中还记载了在该以往技术中,适合将上述原料充分混合,尽量粉碎细致,优选使平均粒径为30μm以下,特别优选为8~15μm。
在日本特表2005-519834号及WO2005/018776号中,均公开了通过调整在TiO2源粉末及Al2O3源粉末中的添加剂的种类、组成及添加量,获得在维持原来具有的高耐热性和低热膨胀系数的优点的同时,在800~1280℃的热分解、低机械强度的问题得到改良的钛酸铝的技术。
但是,例如对于具有外径为100mm以上及总长为150mm以上的形状的尺寸大的蜂窝状结构体,应用日本特表2005-519834号及WO2005/018776号公开的技术时,具有发生烧结破损的问题。即:在TiO2源粉末及Al2O3源粉末中添加二氧化硅、碳酸锶、氧化铁、碳酸镁、碱性长石、含Mg尖晶石型结构的氧化物、MgO或通过烧结转化为MgO的含Mg化合物等时,这些添加剂在烧结过程中形成液相进一步致密化,所以烧结收缩率变大。其结果,蜂窝状结构体的中心部和外周部因温度差而产生收缩差,使蜂窝状结构体发生烧结破损。这种现象,蜂窝状结构体的尺寸越大越容易发生,具有外径为100mm以上及总长为150mm以上的形状的蜂窝状结构体,特别容易发生烧结破损。并且烧结收缩率大时,平均细孔径变小,产生作为蜂窝状过滤器的必要的气孔性失去的问题。
发明内容
因此,本发明的目的为:提供在维持钛酸铝具有的低热膨胀性的良好性能的同时,发生烧结破损少,平均细孔径大的钛酸铝质陶瓷蜂窝状结构体的制造方法。
基于上述目的进行精心研究的结果,本发明者发现:在将混合TiO2源粉末及Al2O3源粉末形成的坯土进行烧结,得到由钛酸铝形成的陶瓷蜂窝状结构体的方法中,通过使用具有0.2~4μm范围的粒径较小的粒子和10~100μm范围的粒径较大的粒子的TiO2源粉末,可以得到在维持低热膨胀系数的良好性能的同时,破损少、且具有大的平均细孔径的钛酸铝质陶瓷蜂窝状结构体,于是想出了本发明。
即制造钛酸铝质陶瓷蜂窝状结构体的本发明的方法为:将配制好的TiO2和Al2O3的摩尔比为45∶55~55∶45范围的TiO2源粉末及Al2O3源粉末、助烧剂及/或助形剂进行混合及混炼,将形成的可塑性坯土挤压成形后,进行干燥及烧结的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述TiO2源粉末具有如下粒度分布,即:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大(相对于[log(粒径)]的质量基准的频率分布)。
优选上述烧结时的保持温度为1450~1650℃、保持时间为8~30小时。
优选上述TiO2源粉末的平均粒径为2~20μm。优选上述TiO2源粉末含有粒径低于10μm的粉末50~80质量%。
优选上述Al2O3源粉末具有如下粒度分布(相对于[log(粒径)]的质量基准的频率分布),即:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大。
优选上述Al2O3源粉末的平均粒径为2~20μm。优选上述Al2O3源粉末含有粒径低于10μm的粉末50~80质量%。
根据本发明的制造方法,可以得到在维持钛酸铝的低热膨胀系数的良好性能的同时,烧结破损少,且具有大的平均细孔径的钛酸铝质陶瓷蜂窝状结构体。
附图说明
[图1]表示实施例及比较例中使用的TiO2源粉末的粒度分布。
[图2]表示粒度分布的一例的模式图。
[图3]表示粒度分布的另外一例的模式图。
[图4]表示粒度分布的又一另外例的模式图。
[图5(a)]与流路垂直表示的一例蜂窝状过滤器的模式截面图。
[图5(b)]与流路平行表示的一例蜂窝状过滤器的模式截面图。
具体实施方式
[1]制造方法
本发明的钛酸铝质陶瓷蜂窝状结构体的制造方法,并不使用将钛酸铝粉末混炼成的坯土,而是将烧结后变为钛酸铝的原料粉末混炼制成坯土,再将成形为蜂窝形状的坯土进行烧结来制造钛酸铝质的陶瓷蜂窝状结构体。因此,不需要预先通过烧结及粉碎来生成钛酸铝粉末的工序,总体上使工序简化。
本发明的方法,因为在烧结的同时进行钛酸铝的合成,因此需要提高合成效率。原料粉末的粒径越小,烧结时钛酸铝的合成就越快速,合成率提高,所以蜂窝状结构体的热膨胀系数变小。但是,原料粉末的粒径越小,烧结收缩率就越大,蜂窝状结构体容易产生烧结破损。此外,原料粉末的粒径越小,蜂窝状结构体的气孔率和平均细孔径就越小。为了在使热膨胀系数变小的同时,使烧结收缩率变小,并且使蜂窝状过滤器具有优选气孔率及平均细孔径,需要将粒径小的原料粉末和粒径大的原料粉末混合的混合物。即需要在粒度分布图中存在2个峰值的双态分布(Bimodal)粉末。
但是,仅用上述双态分布(Bimodal)粉末并不能充分解决上述问题。还需要使具有粒度分布图中的2个峰值之间的粒径的原料粉末极其少。具有这种粒度分布时,在烧结前的蜂窝状结构体中,原料粉末通过石墙效应、即在粒径大的原料粉末间的缝隙间填充粒径小的原料粉末而密集存在,所以可使钛酸铝的合成率提高,使热膨胀系数变小。同时因为原料粉末密集存在,所以烧结收缩率变小。并且因为存在粒径大的原料粉末,所以不会使气孔率及平均细孔径降低。
(1)TiO2源粉末
本发明的制造方法中使用的TiO2源粉末,其特征在于具有如下粒度分布,即:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大。在此,上述粒度分布表示相对于粒径的常用对数[log(粒径)]的质量基准的频率分布,[log(粒径)]的刻度设定在(直方图级别)0.03~0.06的范围。该刻度变大时,上述最大值有时也会变大,只要设定在0.03~0.06范围,可得到实质上同样的粒度分布图。
粒径低于0.2μm的TiO2源粉末增加时,烧结收缩增大,容易发生烧结破损,同时气孔率及平均细孔径变小。粒径大于4μm低于10μm的TiO2源粉末增加时,烧结收缩增大,容易发生烧结破损,同时热膨胀系数变大。粒径大于100μm的TiO2源粉末增加时,热膨胀系数变大。
在本发明中规定的TiO2源粉末的粒度分布,仅仅混合平均粒径大的TiO2源粉末和平均粒径小的TiO2源粉末,并不容易获得。如图2的模式所示,将具有平均粒径D1及粒度分布A的粒子和具有平均粒径D2及粒度分布B的粒子进行混合时,混合后的粒度分布变为如C所示的形状。使用具有这种粒度分布的TiO2源粉末时,不能明确地发挥本发明的效果。如为具有图3所示的粒度分布的粒子时,因为P1<P2,所以不能明确发挥本发明的效果,如为具有图4所示的粒度分布的粒子时,因为P3<P4,所以也不能明确发挥本发明的效果。将粒径大的原料粉末和粒径小的原料粉末混合,为了获得具有本发明中规定的粒度分布的原料粉末,需要选定粒径分布窄的原料粉末,并根据情况进行筛分。而且各原料粉末的混合比例也很重要,该比例不合适时会成为图3或图4例的粒度分布,需要注意。
在粒度分布图中,将粒径在0.2~4μm粒径范围显示频率的最大值的粒径设为Dmin,将粒径在10~100μm粒径范围显示频率的最大值的粒径设为Dmax时,优选Dmax/Dmin为20以上,更优选为30以上。Dmax/Dmin只要为20以上,则可同时合成钛酸铝和降低收缩率。
烧结时的保持温度优选为1450~1650℃,保持时间优选为8~30小时。使用合成后的钛酸铝的粉末时,例如即使烧结时的保持温度为1400℃的低温,保持时间为约4小时的短时间,也可获得蜂窝状结构体。此外,在烧结蜂窝状结构体的同时合成钛酸铝时,即使原料粉末的粒径小时,也可在比较低的温度和短的保持时间合成钛酸铝,获得热膨胀系数小的蜂窝状结构体。使用具有10μm以上的大粒径的TiO2源粉末的本发明方法中,为了提高钛酸铝的合成率,获得低热膨胀系数的蜂窝状结构体,优选在1450℃以上的温度保持8小时以上。另一方面,因为使保持温度过高或使保持时间过长时烧结收缩变大,所以优选保持温度为1650℃以下且保持时间为30小时以下。根据这样的烧结条件,烧结收缩更加降低,可防止烧结破损。更优选烧结温度为1450~1600℃,更优选保持时间为9~25小时。
上述TiO2源粉末的平均粒径优选2~20μm。平均粒径为2~20μ时,更容易生成钛酸铝,可降低烧结收缩率。
上述TiO2源粉末,优选含有粒径低于10μm的粉末50~80质量%。也就是说优选含有粒径10μm以上的粉末20~50质量%。通过增加粒径低于10μm的小粉末的比例,更容易生成钛酸铝。更优选含有粒径低于10μm的粉末60~80质量%。
作为上述TiO2源粉末,可以为金红石型二氧化钛、锐钛型二氧化钛中的任一种,优选金红石型二氧化钛。
(2)Al2O3源粉末
为了获得低热膨胀系数及烧结收缩小的且具有充分的气孔率及平均细孔径的蜂窝状过滤器,Al2O3源粉末也优选具有与TiO2源粉末同样的粒度分布。因此在本发明的方法中,上述Al2O3源粉末优选具有如下粒度分布(相对于[log(粒径)]的质量基准的频率分布),即:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大。此外,上述大小2个粒度范围中,大的粒度范围优选粒径20~70μm,小的粒度范围优选粒径0.5~4μm。
上述Al2O3源粉末的平均粒径优选为2~20μm。平均粒径为2~20μm时,更容易生成钛酸铝,烧结收缩率变小。
上述Al2O3源粉末优选含有粒径低于10μm的粉末50~80质量%。也就是说优选含有粒径10μm以上的粉末20~50质量%。通过增加粒径低于10μm的小粉末的比例,更容易生成钛酸铝。更优选含有粒径低于10μm的粉末60~80质量%。
作为上述Al2O3源粉末,只要是加热至高温时生成氧化铝的粉末即可,优选α-氧化铝、γ-氧化铝、氢氧化铝等。
(3)其他添加剂
作为助烧剂,优选二氧化硅、碳酸锶、氧化铁、碳酸镁、碱性长石、含Mg尖晶石型结构的氧化物、MgO或通过烧结转化为MgO的含Mg化合物等,适合含有3~30质量%。
作为助形剂,优选分散剂、表面活性剂、粘合剂、润滑剂等,特别是作为粘合剂,优选将2%水溶液的粘度(20℃)为5Pa·s以下的甲基纤维素(M)和2%水溶液的粘度(20℃)为20Pa·s以上的羟丙基甲基纤维素(H)在使上述甲基纤维素(M)和上述羟丙基甲基纤维素(H)的质量比(M/H)为50/50~90/10范围的条件下,进行配合,同时相对于陶瓷类粉末100质量份,以总量7~12质量份配合上述甲基纤维素(M)和上述羟丙基甲基纤维素(H)。
为了使蜂窝状过滤器具有必要的多孔性,优选添加烧结时会消去的公知的造孔材料。作为造孔材料,可使用发泡后的发泡树脂、微球、天然石墨或人造石墨、碳、小麦粉、淀粉、木炭、纸浆粉、聚乙烯、聚苯乙烯、聚丙烯、尼龙、聚酯、丙烯酸树脂、苯酚、环氧树脂、乙烯-乙酸乙烯共聚物、苯乙烯-丁二烯嵌段共聚物、苯乙烯-异戊二烯嵌段共聚物、聚甲基丙烯酸甲酯、甲基丙烯酸甲酯-丙烯腈共聚物、氨基甲酸乙酯及蜡等的树脂等。
[2]实施例
下面根据实施例对本发明进行具体说明,但本发明并不限于这些实施例。
实施例1~3及比较例1~3
准备具有表1所示的平均粒径、粒度分布(在各粒径范围的频率的最大值)及粒径低于10μm粒子的质量比的二氧化钛粉末A~E,和具有表2所示的平均粒径、粒度分布(在各粒径范围的频率的最大值)及粒径低于10μm粒子的质量比的氧化铝粉末A及B。使用日机装株式会社制的Microtrac粒度分布测定装置,用超声波使粉末在分散溶剂中分散,用激光衍射散射法测定粉末的粒度分布及平均粒径。将二氧化钛粉末A~C的粒度分布图显示于图1。表1及表2所示的粒度分布(在各粒径范围的频率的最大值)值,表示在(a)0.2μm以下、(b)0.2~4μm、(c)4~10μm、(d)10~100μm、及(e)100μm以上的各粒径范围的频率的最大值。在此,频率为横轴[log(粒径)]的刻度宽0.0375的值(%)。
此外,为了获得显示如二氧化钛粉末A及B的粒度分布的粉末,将平均粒径1μm的单分散二氧化钛粉末和平均粒径35μm的单分散二氧化钛粉末混合,从该混合粉体中取出约一半量的粉体进行筛分,除去4~10μm粒径的粉末后,再对剩余的约一半量的混合粉体中进行重复操作。二氧化钛粉末A是重复该操作3次得到的粉末,二氧化钛粉末B是重复该操作1次得到的粉末。氧化铝粉末A及B也是采用与二氧化钛粉末A及B同样的方法而制备的。
采用表3所示的配合比将二氧化钛粉末A~E、氧化铝粉末A及B、熔融二氧化硅粉末、有机发泡材料以及甲基纤维素进行干法混合,加入水制作可塑性坯土。通过使用蜂窝状结构体成形用的已公知的喷嘴(日文:口金),将该坯土挤压成形,可获得陶瓷蜂窝状结构的成形体。通过将成形体进行干燥、在大气环境中按照室温~150℃升温速度为50℃/h、150~300℃升温速度为10℃/h、300~1000℃升温速度为50℃/h、1000℃以上升温速度为30℃/h进行升温,在1550℃保持10小时进行烧结,获得外径为143mm、长度为152mm、隔壁厚度为0.32mm及隔壁间隔为1.6mm的实施例1~3及比较例1~3的钛酸铝质陶瓷蜂窝状结构体。
表1
注(1):用[log(粒径)]刻度宽0.0375表示频率分布时的各粒径范围的频率的最大值(%)。
表1(续)
二氧化钛粉末 | 粒径低于10μm的粒子的质量比(%) | 结晶型 |
A | 62.5 | 金红石型 |
B | 49.7 | 锐钛型 |
C | 100 | 金红石型 |
D | 56.3 | 金红石型 |
E | 66.2 | 锐钛型 |
[表2]
注(1):用[log(粒径)]刻度宽0.0375表示频率分布时的各粒径范围的频率的最大值(%)。
表2(续)
氧化铝粉末 | 粒径低于10μm的粒子的质量比(%) |
A | 99.6 |
B | 61.9 |
[表3]
<烧结收缩率的测定>
测定获得的钛酸铝质陶瓷蜂窝状结构体的烧结前、后的总长,利用下式计算烧结收缩率。
烧结收缩率(%)=[(烧结前的总长)-(烧结后的总长)]/(烧结前的总长)]×100
<烧结破损的评价>
观察沿流路方向切断的蜂窝状结构体的面,确认有无烧结破损。按照以下标准进行评价。
发生烧结破损···不合格(×)
根本未发生烧结破损···合格(○)
<钛酸铝合成率>
使用将钛酸铝质蜂窝状结构体的一部分粉碎制作的粒径0.5mm以下的粉末,进行X射线衍射测定,根据钛酸铝的(023)面衍射强度(IAT(230))和TiO2(金红石)的(110)面衍射强度(ITiO2(110)),用下式计算的X射线强度比I表示钛酸铝合成率。
I=IAT(230)/(IAT(230)+ITiO2(110))
<热膨胀系数的测定>
热膨胀系数通过下述方法计算,即:将截面形状为4.8mm×4.8mm×总长50mm尺寸的试验片,以总长方向与流路方向几乎一致的方式切取,使用热机械分析装置(TMA、Rigaku公司制ThermoPlus、压缩荷重方式/示差膨胀方式),在施加固定荷重20g的同时,测定以升温速度10℃/min从室温加热至800℃时的总长方向的长度增加量,作为35~800℃间的平均热膨胀系数计算。
<气孔率的测定>
气孔率的测定采用水银压入法,使用Micromeritics公司制的AutoporeIII来进行。将从陶瓷蜂窝状结构体上切取的12.8mm×12.8mm×10mm的试验片装入测定单元内,使单元内减压后导入水银,进行加压,利用此时的压力和在试样内存在的细孔中押入的水银体积的关系,求出细孔径和累积细孔容积的关系。使导入水银的压力为0.5psi(0.35×10-3kg/mm2),利用压力计算细孔径时的常数,使用接触角=130°及表面张力=484dyne/cm。
评价及测定结果如表4所示。使用具有如下粒度分布的TiO2源粉末制造的实施例1~3的钛酸铝质陶瓷蜂窝状结构体,不发生烧结破损,烧结收缩率小,为4~8%,所述的粒度分布为:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大。并且,钛酸铝的合成率为0.98以上,具有10~13×10-7/℃的低热膨胀系数、58.7~63.4%的高气孔率、以及17.8~20.3μm的平均细孔径。其中,使用具有下述粒度分布的Al2O3源粉末的实施例3的钛酸铝质陶瓷蜂窝状结构体,因为烧结收缩率变得更小,所以推测更难发生烧结破损,所述粒度分布为:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大,此外,实施例1及实施例3中使用的TiO2源粉末和Al2O3源粉末,粒径低于10μm的粉末均占50%以上,钛酸铝合成率比实施例2的大。
另一方面,比较例1的钛酸铝质陶瓷蜂窝状结构体,作为TiO2源粉末,在0.2~4μm粒径范围的频率的最大值虽然为258,但因为在10~100μm粒径范围的频率的最大值为0,比在4~10μm粒径范围的频率的最大值18小,所以认为烧结收缩率变大,发生了烧结破损。
比较例2及比较例3的钛酸铝质陶瓷蜂窝状结构体,同样因为与粒径在0.2~4μm粒径范围的频率的最大值、或粒径在10~100μm粒径范围的频率的最大值相比,在上述2个粒径范围以外的频率的最大值大,所以认为烧结收缩变大,发生了烧结破损。
[表4]
评价内容 | 实施例1 | 实施例2 | 实施例3 | 比较例1 | 比较例2 | 比较例3 |
烧结破损 | ○ | ○ | ○ | × | × | × |
烧结收缩率(%) | 8 | 7 | 4 | 14 | 12 | 13 |
钛酸铝合成率 | 1.0 | 0.98 | 1.0 | 1.0 | 1.0 | 1.0 |
热膨胀系数(10-7/℃) | 12 | 13 | 10 | 11 | 12 | 12 |
气孔率(%) | 58.7 | 60.3 | 63.4 | 52.2 | 54.2 | 53.6 |
平均细孔经(μm) | 17.8 | 18.6 | 20.3 | 5.6 | 18.0 | 9.9 |
实施例4~9
除保持温度和保持时间如表5所示进行变更之外,其它与实施例3同样,制作实施例4~9的蜂窝状结构体,与实施例1~3同样进行评价。结果如表6所示。保持温度为1450~1650℃、保持温度为8~30小时的实施例5~8,与实施例9相比烧结收缩率小,与实施例4相比热膨胀系数小。特别是保持温度为1450~1600℃、保持时间为9~25小时范围的实施例6及7,烧结收缩率小,热膨胀系数小。
[表5]
烧结条件 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | 实施例8 | 实施例9 |
保持温度 | 1400 | 1450 | 1600 | 1450 | 1650 | 1670 |
保持时间 | 7 | 30 | 9 | 25 | 8 | 35 |
[表6]
评价内容 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | 实施例8 | 实施例9 |
烧结破损 | ○ | ○ | ○ | ○ | ○ | ○ |
烧结收缩率(%) | 4 | 5 | 4 | 4 | 5 | 8 |
钛酸铝合成率 | 0.98 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
热膨胀系数(10-7/℃) | 13 | 10 | 10 | 10 | 10 | 11 |
气孔率(%) | 63.8 | 60.1 | 62.6 | 61.5 | 58.2 | 57.5 |
平均细孔经(μm) | 20.6 | 18.5 | 20.1 | 20.3 | 18.3 | 16.1 |
Claims (7)
1.钛酸铝质陶瓷蜂窝状结构体的制造方法,其为将以TiO2与Al2O3的摩尔比为45∶55~55∶45的范围配制的TiO2源粉末及Al2O3源粉末、助烧剂及/或助形剂混合及混炼而形成可塑性坯土,将该坯土挤压成形后,进行干燥及烧结的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述TiO2源粉末具有如下的粒度分布,所述粒度分布为:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大,所述粒度分布为相对于[log(粒径)]的质量基准的频率分布。
2.根据权利要求1所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述烧结时的保持温度为1450~1650℃,保持时间为8~30小时。
3.根据权利要求2所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述TiO2源粉末的平均粒径为2~20μm。
4.根据权利要求1~3中任一项所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述TiO2源粉末含有50~80质量%的粒径低于10μm的粉末。
5.根据权利要求1~4中任一项所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述Al2O3源粉末具有如下粒度分布,所述粒度分布为:在0.2~4μm粒径范围的频率的最大值及在10~100μm粒径范围的频率的最大值,均比在上述2个粒径范围以外的频率的最大值大,所述粒度分布为相对于[log(粒径)]的质量基准的频率分布。
6.根据权利要求1~5中任一项所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述Al2O3源粉末的平均粒径为2~20μm。
7.根据权利要求1~6中任一项所述的钛酸铝质陶瓷蜂窝状结构体的制造方法,其特征在于,上述Al2O3源粉末含有50~80质量%的粒径低于10μm的粉末。
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