CN1313187C - 富铝红柱石－钛酸铝柴油机排气过滤器 - Google Patents

富铝红柱石－钛酸铝柴油机排气过滤器 Download PDF

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CN1313187C
CN1313187C CNB038229412A CN03822941A CN1313187C CN 1313187 C CN1313187 C CN 1313187C CN B038229412 A CNB038229412 A CN B038229412A CN 03822941 A CN03822941 A CN 03822941A CN 1313187 C CN1313187 C CN 1313187C
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micron
mullite
oxide
tio
diesel particulate
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CN1684754A (zh
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S·B·奥古米
P·D·特珀谢
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Corning Inc
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Corning Inc
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Abstract

本发明涉及一种富铝红柱石-钛酸铝多孔柴油机微粒过滤器，它由多孔陶瓷体构成，以总体的重量%计，所述陶瓷体包含60-90%，较好是70-80%，最好是70%的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及10-40%，较好是20-30%，最好是30%的富铝红柱石(3Al2O3·2SiO2)；以氧化物的重量%计，它基本上由3-15%SiO2、55-65%Al2O3、22-40%TiO2和0-10%Fe2O3组成，它可用于过滤柴油机的排气。本发明的柴油机微粒过滤器显示互连孔隙率高、中值孔径大、当烧至1650-1700℃时渗透性高，以及耐热冲击性高和过滤性能良好。

Description

富铝红柱石-钛酸铝柴油机排气过滤器
发明背景
本发明涉及柴油机排气过滤器。尤其是本发明涉及富铝红柱石-钛酸铝柴油机排气过滤器及其制造方法。
在工业领域中，堇青石(2MgO.2Al2O3.5SiO2)是选择用于柴油机排气后处理应用如，壁流过滤器的低成本高利润的材料，这是因为其在大多数操作条件下具有良好的耐热冲击性、过滤效率以及耐久性的综合性能。但是，在某些情况下，堇青石过滤器容易损坏，甚至严重损坏。在未受控的再生条件下出现偶尔热失控，会导致局部堇青石熔化。在运行过程中，当机油中的金属杂质、催化添加剂或排气管道夹层的腐蚀金属进入过滤器时，会出现导致损坏的另一个因素。通常，当温度超过1300℃时，这些金属形成和堇青石结构反应的氧化物。所述损坏材料的证据通常是过滤器上的小孔，在此，金属开始沉积和反应，导致腐蚀和熔化所述材料。
最近，已经制得市售碳化硅(SiC)壁流过滤器，用于柴油机排气过滤。但是，SiC过滤器制造成本太高，且由于其固有的热膨胀系数(CTE)高，耐热冲击性差，必须进行分段处理。
已经提出使用钛酸铝(尤其是富铝红柱石-钛酸铝)作为过滤器，尤其是柴油机微粒过滤器(例如在美国专利No.4483944、4767731、4855265、5290739和EP0036462及EP 0873775)。但是，预计这种过滤体的渗透性低，从而因为孔隙率低或者孔径小而导致对引擎的压力降或背压高；或者在其它情况下，预计孔隙率和孔径太大，使得在除去气流中微粒时的过滤效率差。
因此，要求存在一种富铝红柱石-钛酸铝柴油机微粒过滤器，其渗透性比目前所达到的要高，同时其具有有效的过滤效率，热膨胀低、热容高、耐热冲击性高、机械强度高以及在热循环中耐久性提高。
发明概述
本发明的主要方面是富铝红柱石-钛酸铝陶瓷制件，其互连孔隙率高，中值孔径大，且渗透性高，能用作柴油机排气用的过滤器，其对引擎的压力降低和背压低。同时，本发明制件的热膨胀低，热容高，耐热冲击性高且机械强度高，以及具有有效的过滤效率，在热循环过程中耐久性提高。
具体地是，本发明涉及一种柴油机微粒过滤器，它包括***的壁流式蜂窝状过滤器主体，所述主体包含多孔陶瓷材料，且具有从前入口端向其出口端贯穿所述主体的许多平行的末端堵塞的孔通道。以总体的重量％计，所述多孔陶瓷包含60-90％，较好是70-80％，最好是70％的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及10-40％，较好是20-30％，最好是30％的富铝红柱石(3Al2O3.2SiO2)；以氧化物的重量％计，它基本上由3-15％(较好是6-12％)的SiO2、55-65％，(较好是57-61％)的Al2O3、22-40％(较好是26-35％)的TiO2和0-10％(较好是0.5-5％)的Fe2O3组成。
本发明结构的性能通常包括如下：35-55体积％(较好是40-50体积％)的孔隙率；8-20微米(较好是10-15微米)的中值孔径；当烧制至1650-1700℃时至少0.30×10-12m2(较好是0.33×10-12-1.00×10-12m2)的渗透率；当所述过滤器受到7分钟的200-1100℃的升温和7分钟的1100-200℃的冷却的热循环100次作用之后其线性尺寸的增量小于1％；从室温到1000℃测得的CTE为5×10-7/℃到15×10-7/℃，较好为5×10-7/℃到10×10-7/℃；在500℃下的热容至少为3.2Jcm-3K-1，至少为3.9Jcm-3K-1；在圆形截面的实心棒上测得的断裂的四点模量至少为500磅/平方英寸，较好是800磅/平方英寸。
本发明另一方面是制造柴油机微粒过滤器的方法，所述方法包括形成选择用于制得陶瓷制件的粉末状原料混合物，以氧化物的重量％计，所述陶瓷制件基本上由3-15％的SiO2、55-65％的Al2O3、22-40％的TiO2和0-10％的Fe2O3组成；将所述混合物成形为陶瓷制件坯，较好是通过挤出成具有入口和出口端以及从入口端延伸到出口端的许多孔的蜂窝体，所述孔具有多孔壁；并将所述陶瓷制件坯烧制至1650-1700℃，烧制时间足以形成富铝红柱石-钛酸铝。
附图简要说明
图1是本发明柴油机微粒过滤器的示意图。
图2是本发明结构在放大500倍时的微结构SEM照片。
图3是经过热循环试验之后，本发明结构在放大500倍时的微结构SEM照片。
发明详述
本发明的柴油机排气净化用壁流式过滤器如图1所示。过滤器结构10包括具有入口端12、出口端13以及许多在入口端12和出口端13之间平行延伸的孔11的蜂窝体15。孔11具有多孔壁14，且仅在一端(入口端12或出口端13)具有塞子61。塞子61以方格图案设置，使通过入口端12处的开孔11进入过滤器结构10的排气通过多孔壁14，离开出口端13。
过滤器结构10的蜂窝体15包含多孔陶瓷材料，它基本上由两种晶体相(即钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及富铝红柱石，其化学计量式为3Al2O3.2SiO2)组成。微结构在放大500倍时的典型SEM照片如图2所示，照片中，钛酸铝相由数字20表示，富铝红柱石相由数字22表示。
如本领域已知的(见美国专利No.4855265)，钛酸铝在800-1300℃的高温下会显示结构不稳定性。发现用铁(Fe)同晶型取代钛酸铝相中的铝(Al)可以提高材料抗分解的稳定性。因此，在本发明中可以加入氧化铁(Fe2O3)。
因此，以氧化物的重量％计，本发明制件的组合物基本上由3-15％(较好是6-12％)的SiO2、55-65％(57-61％)的Al2O3、22-40％(较好是26-35％)的TiO2和0-10％(较好是0.5-5％)的Fe2O3组成。若所述结构在低于1650℃下烧制，可以存在痕量的玻璃相以及痕量的未反应的氧化铝(Al2O3)以及二氧化钛(TiO2)。
所述组合物也可以总体的重量％表示，为60-90％，较好是70-80％，最好是70％的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及10-40％，较好是20-30％，最好是30％的富铝红柱石(3Al2O3.2SiO2)。
钛酸铝的熔点高，为1860℃，各向异性热膨胀高(即沿晶轴的膨胀有很大不同)，沿a-轴约为-29×10-7/℃，沿b-轴约为103×10-7/℃，沿c-轴约为201×10-7/℃。所述极端的各向异性导致在大的钛酸铝晶粒中产生内应力。当材料冷却时，由于其热膨胀系数低，会导致出现严重的微裂缝。但是，晶粒生长较大并随之产生微裂缝使得材料的强度低。
加入作为第二相的富铝红柱石，可以提高所述强度(断裂模量)，并平衡所述CTE。具体地是，富铝红柱石通过抑制晶粒生长和微裂缝扩大来提高最终主体的总强度。所得富铝红柱石-钛酸铝制件显示微裂缝，且CTE很低，使耐热冲击性高。有微裂缝的主体使CTE偏向于大多数负值的CTE组分，这是因为冷却时微裂缝打开容纳一般正值的组分。
本发明过滤器具有适于对引擎的低压力降和背压以及最佳效率的所需性能。这些性能包括互连孔隙率高、中值孔径大、孔径分布窄，以及渗透率高，同时仍旧保持低的热膨胀系数、高热容、高耐热冲击性和高机械强度，并结合在重复热循环中的高耐久性。如以下说明显而易见的，所述合适的性能可以通过仔细选择具有具体粒度限制的原料，并将由此形成的结构置于具体的加热条件下来达到。
如水银孔隙率检测法所测得的，所述敞开孔隙率约为35-55体积％，较好约为40-50体积％。如水银孔隙率检测法所测得的，所述中值孔径约为8-20微米，较好约为10-15微米。
使用Perm Automated Porometert第6.0版(Porous Materials，Inc.Ithaca.NY)在孔壁的烧制的条或片上测量空气在施压条件下通过本发明结构的渗透性。如下所述获得渗透性值。将一片烧制的孔壁用环氧化物安装到具有圆形开口的盘状样品架上。所述环氧化物绕开口的周边施加，使所述样品覆盖所述开口，使空气不能在不经过样品的条件下流过所述开口，并使空气流经的样品面积和样品架的圆形开口面积基本相同。然后，将所述样品置于自动气孔计的腔室中，并在样品两端施加空气差压。测量样品出口端上的空气体积流量与作为施加到样品入口面上压力的关系。然后由以下关系式计算所述比渗透率k：
k = ηQL AP
式中，η是空气在室温下的粘度，其单位是兆帕斯卡.秒；L是样品的厚度，单位是米；Q是空气流经样品的单轴体积流速，单位是立方米/秒；A是空气流经所述样品的面积，约等于样品架的开口面积，单位是平方米，P是样品厚度两侧的差压，单位是兆帕斯卡。以单位平方米表示，所述渗透率是10-12m2。因此，对引擎的压力降低且背压低时，所述渗透率至少约为0.30×10-12到1.00×10-12m2，较好为0.33×10-12到1.00×10-12m2。
虽然本发明结构的互连孔隙率高，中值孔径大，但是仍旧保持低热膨胀系数、高热容、高耐热冲击性和高机械强度。如膨胀测定法所测得的，从室温(22℃)到1000℃的热膨胀系数(CTE)为5×10-7/℃到15×10-7/℃，较好为5×10-7/℃到10×10-7/℃。在圆形截面的实心棒上测得的所述结构断裂的四点模量至少为500磅/平方英寸(psi)，较好是800psi。在1000℃下热循环50次之后的试验中，强度损失小于15％。
在600-1100℃的高温下进一步进行实验，每单位体积本发明结构所吸收的热量估计比目前市售堇青石柴油机微粒过滤器高约25％。这表明其热容高，在相同部件设计(孔隙率、孔密度和壁厚)的条件下，未受控再生过程中本发明制得结构的过滤器温度比堇青石的要低。在500℃下测得的热容大于3.2Jcm-3K-1，较好是至少3.9Jcm-3K-1。在最高烟炱负载量(20g/l)下所观察的最高温升不大于约1010℃。考虑到目前堇青石柴油机微粒过滤器所观察到的温升高达1400℃，这一点是很明显的。
本发明结构的另一优点是提高在热循环过程中的耐久性。在进行实验时，热循环试验中的热曲线由温度在7分钟内从200℃升至1100℃以及在7分钟内从1100℃冷却至200℃组成。当受这种热循环中100次作用之后，所观察的增大小于1％。在试验前后，用超级测微计测量所试验的样品的尺寸。图3是图2所示相同样品经过200℃到1100℃之间的热循环100次之后在放大500倍时的SEM照片。所述富铝红柱石相22保持完整。
本发明结构的另一优点是耐灰分性增大。在柴油机排气中存在金属氧化物“灰分”微粒，它是不能燃烧的；因此，在再生过程中不能容易地除去，如碳烟灰。若在再生过程中过滤器的温度达到足够高的值(即，＞1200℃)，则这些灰分微粒可以烧制成过滤器材料，并进行化学反应。
在本发明中，耐灰分性使用柴油机灰分和微粒Fe2O3来评价。所述实验涉及由约30mm×20mm×5mm的蜂窝状结构制得样品。将每单位面积已知重量的灰分或Fe2O3薄层加入样品的表面上。在所有情况下，所述一般的负载约为0.011g/cm2。选择所述负载，以模拟在行车约100000km之后积聚在直径5.66英寸，长6英寸的标准过滤器上的灰分量，所述过滤器具有200个孔/英寸2，壁厚0.018英寸。
将所述灰分/Fe2O3覆盖样品置于已经预热至所需温度下的炉子中，保持在该炉子中1小时，然后取出并冷却至室温。所述实验在1000℃、1100℃、1300℃和1400℃下进行。然后，所述样品通过肉眼和在立体显微镜下观察反应的程度。所述1小时的保持时间认为是所述过滤器在其使用寿命过程中处于＞1000℃的温度下的累积时间。这基于过滤器使用寿命中600次再生，其中，约10％的是未受控的再生，这会导致每次未受控再生产生1000℃以上的温度约1-2分钟。
发现所述结构很能耐受柴油机灰分和微粒Fe2O3。在最高1400℃下没有观察到任何烧制或反应。而且如上所述，本发明材料有关的高热容降低了在再生过程中过滤器中的温升或温度增加的量。温升越低，导致金属氧化物灰分烧制得越少，灰分和过滤器的反应越少，由此提高过滤器的使用寿命。
为了如所述制得富铝红柱石-钛酸铝柴油机微粒过滤器，已经发现必须遵照严格的制造方法。本发明涉及仔细选择具有特定孔径分布的具体原料。
所述原料包括(1)反应形成钛酸铝和富铝红柱石相的氧化物源，和/或(2)部分或完全预反应的钛酸铝和富铝红柱石粉末。选择所有原料以限制组合物中存在的碱金属元素。对于足够大的中值孔径和高渗透率而言，所述原料的中值粒度必须粗。中值粒度是以体积分布计表示为微米的中值粒径。它通过使用激光衍射技术的粒度分析仪来确定，如本领域那些技术人员所知的。对于部分或完全预反应的铝和富铝红柱石粉末而言，所述批料组分的中值粒度至少约为15微米，较好至少约20微米，更好至少约35微米。但是就原料而言，优选是能反应形成钛酸铝和富铝红柱石相的氧化物源。这些优选原料包括二氧化硅(SiO2)、氧化铝(Al2O3)和二氧化钛(TiO2)。
所述形成氧化铝的来源是当在没有其它原料存在下加热至足够高温度时产生基本上纯的氧化铝的粉末。合适的形成氧化铝的来源包括α-氧化铝、过渡氧化铝如γ-氧化铝或ρ-氧化铝、勃姆石、氢氧化铝和它们的混合物。将所述形成氧化铝的来源选择成粒度足够大，能达到所需孔隙率且同时在最终结构中形成微裂缝的扁平形态。因此，氧化铝源的粒度约为5-25微米，较好是约10-15微米。优选的氧化铝源是Alutab，从Alcan Chemical Limited，Oxon，England购得。
本发明所述优选的形成二氧化硅的来源是石英，如Silverbond200，从Unimin Corporation of Canaan，CT购得。已经发现使用石英在本发明结构中形成所述孔隙率和独特的微结构方面起到重要的作用。其它形成二氧化硅的来源包括方石英、非结晶二氧化硅如热解法二氧化硅或溶胶凝胶二氧化硅、沸石和硅藻土二氧化硅。使用高岭土作为二氧化硅源对本发明不利。这是因为高岭土对孔隙率和微结构存在不利影响，并导致循环稳定性变差。所述二氧化硅源的中值粒度约为5-20微米，较好约为8-15微米。
所述形成二氧化钛的来源较好但不限于金红石，如Titanox Kronos3020，从Cranbury，NJ的Kronos，Inc.购得。所述形成二氧化钛的来源的中值粒度对通过在结构中使核快速生长来避免夹入未反应氧化物很重要。因此，所述中值粒度约为4-20微米，较好是约8-16微米。
所述优选的氧化铁(Fe2O3)来源是粒度约为5-30微米，较好是约14-26微米的二氧化钛铁。最优选的实施例是钛铁矿(llmenite)，从Atlantic EquipmentEngineers of Bergenfield，NJ购得。优选钛铁矿是因为在1100℃下形成液体的倾向促进所述反应，形成用铁稳定的钛酸铝相。在本发明中，用铁同晶型取代钛酸铝相中的铝限于约0-10摩尔％，较好是约8摩尔％。这可以考虑为加入约0-6重量％，较好最高是5重量％的氧化铁。
在本发明的方法中，较好原料混合物中不存在空隙形成剂，如石墨。空隙形成剂是短效微粒材料，它们在干燥或加热所述坯体时会蒸发或燃烧气化，获得所需通常较大的孔隙率和/或较粗的中值孔径。
没有空隙形成剂提供许多优点，包括减少烧制时间、降低物理性质如背压和CTE的可变性，以及降低这些性质在结构内部和外部之间的梯度。如所述的，若需要的话，空隙形成剂可以任选地加入原料批料中。
原料可以和有机组分掺合在一起，所述有机组分包括增塑剂、润滑剂、粘结剂和溶剂。甲基纤维素可以用作有机粘结剂，它之后在烧制过程中被烧掉。较好使用油酸作为分散剂。并不推荐使用硬脂酸钠，这是因为会夹杂入钠。可以使用硬脂酸二甘醇酯，但是这通常会导致在挤出过程中粘合效果差，在烧制过程中形成裂缝。若使用硬脂酸二甘醇酯，则要求加入约1-2重量％的聚乙二醇，作为润滑剂。也可以任选地加入水作为溶剂。
然后，将所述混合物成形为蜂窝状坯体，如通过挤出，任选进行干燥，并在一定温度下烧制一段足以形成最终的产品结构的时间。所述烧制可以在电加热炉或气体窑中，在25-30小时内以10-200℃/小时的速度经过不同温度间隔升至最高温度1650-1700℃来进行，并通过切断炉子的电源来冷却。在优选的实施方式中，所述烧制工艺过程如下：在约8-10小时内从室温(22-25℃)加热至1500-1600℃；在最高温度下保持约4-8小时，之后在约2-3小时内加热至最高温度1650-1700℃，在此温度下保持约30-60分钟，之后在约1小时内将温度降至约1575-1600℃，在此温度保持约4-5小时。短时间偏移到最高温度对相和微裂缝的形成、低收缩率(＜5％)以及大的互连敞开孔隙率、大的中值孔径和高渗透性是必需的。
通过以下说明性例子可以更好地理解本发明提供的柴油机微粒过滤器的代表性例子及其性能优势，上述例子决不是用于进行限制的目的。
实施例
将约1重量％(以其中所有陶瓷材料计)油酸润滑剂/挤出助剂和约8.36重量％的Silverbond200混合约10-15分钟。陶瓷批料的剩余部分基本上由58.46重量％的Alutab氧化铝、30.14重量％的Rutile Kronos3020二氧化钛和3.13重量％的llmenite二氧化钛铁组成，它们和4％的甲基纤维素增塑剂/粘结剂(以其中所有陶瓷材料的重量％计)干混。所述混合物在混合研磨机中用水塑化，并通过预挤出通心粉状的物质来进一步塑化和除气。之后，所述完塑化和压实的批料挤出形成蜂窝状料坯，在绝缘炉中干燥约15分钟，转移到正规炉中干燥过夜，然后按照上述优选的工艺过程进行烧制。
下表I记录了实施例中以氧化物重量％计的组分以及相集合。表II记录了对其测得的物理性质。高密度(3g/cm3)是主体热容高的表示。高渗透性(0.33×10-12m2)表明压力降低，因此，其对引擎的背压也低。在1700℃以下没有观察到结构的任何变形。
应理解，虽然已经参考某些说明性和具体的实施方式详细说明了本发明，但是在不背离本发明精神以及附带权利要求书范围的条件下，应认为本发明并不限于这些方面，也可以其它方式使用。
表1
  相集合   总体重量％
  钛酸铁铝固溶体   70％
  富铝红柱石   30％
  氧化物组成   氧化物重量％
  Al2O3   58.46％
  TiO2   30.14％
  SiO2   8.36％
  Fe2O3   1.28％
表2
 性质   本发明实施例
 孔隙率(体积％)   41.0
 中值孔径(微米)   11.0
 渗透率(10-12m2)   0.33
 CTE(22-1000℃)10-7/℃   13.0
 CTE(22-800℃)10-7/℃   7.0
 密度(g/ml)   3.37
 熔点(℃)   1700
 收缩率(％)   2.0
 热循环增大(1100℃下100次循环)   ＜1％

Claims (10)

1.一种柴油机排气微粒过滤器，它包括***的壁流式蜂窝状过滤器主体，所述主体包含多孔陶瓷材料，并包括从前入口端向其出口端贯穿所述主体的许多平行的一端堵塞的孔通道，其特征在于，
以总体的重量％计，所述陶瓷包含60-90％的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及10-40％的富铝红柱石，其化学计量式为3Al2O3·2SiO2；以氧化物的重量％计，所述陶瓷基本上由3-15％的SiO2、55-65％的Al2O3、22-40％的TiO2和0-10％的Fe2O3组成；
所述过滤器的孔隙率为35-55体积％，中值孔径为8-20微米，当烧制至1650-1700℃时其渗透率至少为0.30×10-12m2，当所述过滤器受到7分钟的从200℃升温至1100℃和7分钟的从1100℃冷却至200℃的热循环100次作用之后其线性尺寸的增量小于1％。
2.如权利要求1所述的柴油机排气微粒过滤器，其特征在于，
以总体的重量％计，所述陶瓷包含70-80％的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及20-30％的富铝红柱石，其化学计量式为3Al2O3·2SiO2；以氧化物的重量％计，所述陶瓷基本上由6-12％的SiO2、57-61％的Al2O3、26-35％的TiO2和0.5-5％的Fe2O3组成；
所述过滤器的孔隙率为40-50体积％，中值孔径为10-15微米，渗透率为0.33×10-12到1.00×10-12m2。
3.如权利要求2所述的柴油机排气微粒过滤器，其特征在于，以总体的重量％计，所述陶瓷包含70％的钛酸铁铝固溶体，其化学计量式为Al2(1-x)Fe2xTiO5，式中，x是0-0.1；以及30％的富铝红柱石，其化学计量式为3Al2O3·2SiO2。
4.如权利要求1所述的柴油机排气微粒过滤器，其特征在于，从室温到1000℃所测得的，所述过滤器的CTE为5×10-7/℃到15×10-7/℃；在500℃下的热容至少为3.2Jcm-3K-1；如在圆形截面的实心棒上所测得的断裂的四点模量至少为500磅/平方英寸。
5.如权利要求4所述的柴油机排气微粒过滤器，其特征在于，从室温到1000℃测得的所述过滤器的CTE为5×10-7/℃到10×10-7/℃；在500℃下的热容至少为3.9Jcm-3K-1；在圆形截面的实心棒上测得的断裂的四点模量至少为800磅/平方英寸。
6.一种制造如权利要求1所述的柴油机排气微粒过滤器的方法，所述方法包括：
a.形成选择用于制得陶瓷制件的粉末状原料混合物，以氧化物的重量％计，所述陶瓷制件基本上由3-15％的SiO2、55-65％的Al2O3、22-40％的TiO2和0-10％的Fe2O3组成；
b.将所述混合物成形为陶瓷制件坯；
c.将所述陶瓷制件坯烧制至1650-1700℃，烧制时间足以形成富铝红柱石-钛酸铝陶瓷过滤器，其孔隙率为35-55体积％，中值孔径为8-20微米，渗透率至少为0.30×10-12m2，当所述过滤器受到7分钟的从200℃升温至1100℃和7分钟的从1100℃冷却至200℃的热循环100次作用之后其线性尺寸的增量小于1％。
7.如权利要求6所述的方法，其特征在于，所述原料包含氧化物源，所述氧化物源包括：
粒度为5-20微米的二氧化硅SiO2；
粒度为5-25微米的氧化铝Al2O3；
粒度为4-20微米的二氧化钛TiO2；和
加入占分批加入的所有原料的0-6重量％的氧化铁Fe2O3。
8.如权利要求7所述的方法，其特征在于，所述原料包含氧化物源，所述氧化物源包括：
粒度为8-15微米的二氧化硅SiO2；
粒度为10-15微米的氧化铝Al2O3；
粒度为8-16微米的二氧化钛TiO2；和
加入占分批加入的所有原料的0-5重量％的氧化铁Fe2O3。
9.如权利要求6所述的方法，其特征在于，通过挤出成具有入口和出口端以及从入口端延伸到出口端的许多孔的蜂窝体，将所述混合物成形，所述孔具有多孔壁；其中一部分孔的入口端和一部分孔的出口端被堵塞。
10.如权利要求9所述的方法，其特征在于，所述烧制步骤包括在8-10小时内从22-25℃的室温加热至1500-1600℃；在1500-1600℃温度下保持4-8小时，之后在2-3小时内加热至1650-1700℃，在此温度下保持30-60分钟，之后在1小时内将温度降至1575-1600℃，在此温度保持4-5小时。
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