CN100512920C - 基于钛酸铝的陶瓷体 - Google Patents

基于钛酸铝的陶瓷体 Download PDF

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CN100512920C
CN100512920C CNB2004800326176A CN200480032617A CN100512920C CN 100512920 C CN100512920 C CN 100512920C CN B2004800326176 A CNB2004800326176 A CN B2004800326176A CN 200480032617 A CN200480032617 A CN 200480032617A CN 100512920 C CN100512920 C CN 100512920C
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2sio
source
tio
component
ceramic body
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CN1874834A (zh
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S·B·奥古米
P·O·特珀谢
R·R·武诗丽卡
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Corning Inc
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Abstract

一种具有以下化学式组成的钛酸铝基陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，而且满足以下条件：0.5＜a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0＜e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d＞0.01。提供了一种用来形成该陶瓷体的方法。该陶瓷体可用于柴油机废气过滤之类的汽车排放控制系统。

Description

基于钛酸铝的陶瓷体
本申请要求Steven B.Ogunwumi等人在2003年4月11日提交的名为＂CeramicBased on Titanate＂的美国临时申请第60/517,348号的优先权。
技术领域
本发明涉及具有可用于高温用途的低热膨胀、高孔隙率和高强度的基于钛酸铝的陶瓷体。
背景技术
堇青石陶瓷体，特别是形成蜂窝状多孔结构的堇青石陶瓷体可用于许多种高温用途，例如催化转化器，NOx吸附器，电加热催化剂，熔融金属过滤器，回热器芯，化学处理基材，用于加氢脱硫、加氢裂化或加氢处理的催化剂，以及柴油机颗粒过滤器之类的过滤器。
在柴油机废气过滤中，能够提供低CTE的低成本材料堇青石成为一种可选择的材料。自从20世纪80年代早期，已开始使用壁流式多孔堇青石陶瓷过滤器从一些柴油发动机的废气中除去颗粒。柴油机颗粒过滤器(DPF)将以下性质理想地结合：低CTE(为了抗热冲击性)，低压降(为了发动机效率)，高过滤效率(为了从废气流中除去大部分颗粒)，高强度(为了耐受处理、封装和使用中的振荡)和低成本。堇青石的问题包括低体积热容和低热导率，这可能会造成在某些条件下对过滤器进行再生操作时，会产生无法接受的高温，以及低的热耐久性。另外，柴油机废气中所含的无机颗粒(被称为灰分)会与堇青石发生反应，使得过滤器失效。
一种可代替堇青石用于DPF生产的材料是SiC。尽管这种材料同时具有高体积热容和高热导率，但是由于其较高的热膨胀和高弹性模量，其抗热冲击性很差。由于这种差的抗热冲击性，需要将SiC过滤器分段，以免使用时发生热冲击失效。另外，处理要求(即高温、惰性气氛和分段)导致高生产成本。
需要提供可用于汽车排放控制系统之类的高温用途的较低CTE材料。需要提供具有低CTE和优秀的抗热冲击性的材料。本发明提供了这样的陶瓷材料，及其制备和使用方法。
发明内容
本发明是基于具有适用于汽车排放控制之类的高温用途的性质的低膨胀钛酸铝基陶瓷体的发现，所述汽车排放控制包括但不限于汽车催化转化器和柴油机废气后处理系统，例如柴油机颗粒过滤器。
本文提供了一种具有以下组成的陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，而且满足以下条件：0.5<a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0<e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d>0.01。
一种制备本发明的陶瓷体的方法，该方法包括：(a)将包含二氧化硅源，氧化铝源，锶源，氧化钛源，钡源，钙源和/或氧化铁源的无机原料与包括增塑剂、润滑剂、粘合剂的有机处理助剂以及作为溶剂的水配合成批料，混合形成均匀的增塑的混合物；(b)使增塑的混合物成形，形成生坯体；(c)在一定温度下对生坯体加热一定时间，制得上述钛酸铝基陶瓷体。加热优选在1350°-1600℃炉顶温度(toptemperature)下进行，保持4-8小时。
在一实施方式中提供了一种陶瓷过滤器，例如包括由本发明的陶瓷体形成的堵塞的(plugged)壁流式蜂窝过滤体的柴油机颗粒过滤器。柴油机废气过滤器的成功使用需要有热循环过程中的低压降和高耐久性。柴油机颗粒过滤器由堵塞的壁流式蜂窝体形成，该蜂窝体具有进口端和出口端，以及从进口端延伸到出口端的大量的孔，这些孔具有多孔的壁，其中部分的孔在进口端沿其一部分长度被堵塞，余下部分的孔在进口端敞开，而在出口端沿其一部分长度被堵塞，使得从进口端到出口端流经蜂窝体孔的发动机废气流入敞开的孔，通过孔壁，然后在出口端通过开放的孔离开该结构。
在另一实施方式中，柴油机颗粒过滤器包括由具有如下组成的本发明陶瓷体构成的端部堵塞的壁流式蜂窝状过滤体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，其中a＝0.7，b＝0.04，c＝0.185，e＝0.075，d，f，g，h，i＝0。
在另一实施方式中，根据本发明的柴油机颗粒过滤器具有以下性质：CTE(RT至1000℃)小于10×10-7/℃；孔隙率为40-55体积％；中值孔径为5-20微米，优选10-15微米；从孔密度为200孔/平方英寸(cpsi)、壁厚0.016英寸的蜂窝体上沿平行于孔道的方向切下多孔棒，在这些多孔棒上用四点法测得的断裂模量为150-400psi，优选150-300psi；在对孔密度为273cpsi，孔壁厚0.013英寸的5.51＂×5.90＂的样品以210scfm的流速加载高达5克/升的人造炭黑时，压降等于或小于5千帕。
附图说明
参照附图，结合以下详细描述可完全理解本发明，在图中：
图1是组成为a＝0.6965，e＝0.075，h＝0.0035，c＝0.225-b，其中b＝0-0.225，d，f，g，i都等于0的本发明组合物的孔隙率和最大均热(soak)温度(8小时)的关系的示意图；
图2是组成为a＝0.6965，e＝0.075，h＝0.0035，c＝0.225-b，其中b＝0-0.225，d，f，g，i都等于0的本发明组合物的热膨胀和最大均热(soak)温度(8小时)的关系的示意图；
图3是具有实施例19中表7提供的组合物的柴油机颗粒过滤器，在210scfm的气体流速下，进口端和出口端之间的压降差(千帕)与炭黑加载(克/升)的关系的示意图。
具体实施方式
本文提供了一种具有以下组成的钛酸铝基陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，而且满足以下条件：0.5<a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0<e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d>0.01。
本发明的结构具有对于微裂纹的低热膨胀系数(CTE)，良好的抗热冲击性和良好的热耐久性。因此，本发明的陶瓷体可用于柴油机废气过滤。具体来说，本发明的结构适合用作壁流式柴油机颗粒过滤器。
在一实施方式中，柴油机颗粒过滤器包括具有如下组成的端部堵塞的壁流式蜂窝状陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，其中a＝0.7，b＝0.04，c＝0.185，e＝0.075，d，f，g，h，i＝0。
蜂窝状过滤体具有进口端和出口端，以及从进口端延伸到出口端的大量孔道，这些孔具有多孔性的壁。其中部分的孔在进口端沿其一部分长度被堵塞，余下部分的孔在进口端敞开，而在出口端沿其一部分长度被堵塞。这种堵塞结构使得从进口端到出口端流经蜂窝体孔的发动机废气流流入敞开的孔，通过孔壁，然后在出口端通过开放的孔离开该结构。柴油机颗粒过滤器的孔密度宜为70孔/平方英寸(10.9孔/平方厘米)至800孔/平方英寸(124孔/平方厘米)。
在另一实施方式中，根据本发明的柴油机颗粒过滤器具有以下性质：CTE(RT至1000℃)小于10×10-7/℃；孔隙率为40-55体积％；中值孔径为5-20微米，优选10-15微米；从孔密度为200孔/平方英寸(cpsi)、壁厚0.016英寸的蜂窝体上沿平行于孔道的方向切下多孔棒，在这些多孔棒上用四点法测得的断裂模量为150-400psi，优选150-300psi；在对孔密度为273cpsi，孔壁厚0.013英寸的5.51＂×5.90＂的样品以210scfm的流速加载高达5克/升的人造炭黑时，压降等于或小于5千帕。
本发明还涉及一种制备本发明的钛酸铝基陶瓷体的方法，该方法包括：用包含二氧化硅源，氧化铝源，锶源，氧化钛源，钡源，钙源和/或氧化铁源的无机粉末状原料形成混合物。将这些原料与包括增塑剂、润滑剂、粘合剂的有机处理助剂以及作为溶剂的水混合。使该混合物成形，形成生坯体，任选经过干燥，然后烧制形成产物结构。可任选地使用石墨或聚乙烯珠粒之类的成孔剂来改进孔隙率和中值孔径。成孔剂是一种短效的颗粒材料，这种材料会在对生坯体进行干燥或加热时通过燃烧而蒸发或气化，从而制得所需的，经常是更高的孔隙率和/或更粗的中值孔径。原料具有大粒径是不优选的。
氧化铝源是一种在不含其他原料的条件下加热至足够高温度时，能够生成相当纯的氧化铝的粉末，其包括α-氧化铝，γ-氧化铝或ρ-氧化铝之类的过渡型氧化铝，水合氧化铝，三水铝石，勃姆石，氢氧化铝及其混合物。氧化铝源的粒径可高达25微米。二氧化硅源包括方英石，熔凝二氧化硅或溶胶-凝胶二氧化硅之类的非晶态二氧化硅，有机硅树脂，沸石，和硅藻土二氧化硅，高岭土和石英。二氧化硅源的中值粒径高达30微米。
氧化钛源优选但不限于金红石。氧化钛源的中值粒径是很重要的，以免因为在结构中快速生成晶核而包覆未反应的氧化物。因此，中值粒径高达20微米。锶源是碳酸锶，其中值粒径高达20微米。钡源是碳酸钡或硫酸钡，其中值粒径高达20微米。钙源是碳酸钙，其中值粒径高达20微米。氧化铁源的中值粒径高达0.5微米。
原料中可能必须包含成孔剂，为柴油机颗粒过滤器用途提供合适的孔隙率和中值孔径。石墨或聚乙烯珠粒适用于该目的。成孔剂是一种短效的材料，这种材料会在对生坯体进行干燥或加热时通过燃烧而蒸发或气化，从而制得经常是更高的孔隙率和/或更粗的中值孔径。以无机原料为100重量％计，成孔剂的加入量通常为20-40重量％。
将无机粉末状原料与甲基纤维素粘合剂、油酸/三乙醇胺表面活性剂之类的有机处理组分混合，形成增塑的均匀的混合物。该增塑的混合物通过任何常规的方法成形，优选通过蜂窝状模头挤出成形。任选地干燥所得的生坯体，然后在1350°-1600℃的各种温度间隔下加热，在炉顶温度温度下保持6-8小时，制得最终产品结构。
为制得壁流式过滤器，如本领域已知的，所述蜂窝结构中一部分孔在进口端或进口面被堵塞。仅堵塞孔的端部，堵塞深度通常约为1-20毫米，但是该深度也可改变。在出口端将一部分孔堵塞，但是这部分孔不是在入口端堵塞的孔。因此，每个孔仅有一端被堵塞。优选的结构是，在特定的面上，以棋盘图案形式，每隔一个孔进行堵塞。
为了更全面地说明本发明，列出了以下非限制性实施例。除非另外说明，否则所有的份数、分数和百分数均以重量为基准计。
实施例
称取干组分，将它们与有机组分和水混合，在不锈钢研磨机中捏和这些混合物使其形成塑性体，从而制得试验样品。表1-4提供了批料的份数和比例，以及本发明化学式中组分的重量分数。
在制备样品时，首先将三乙醇胺(TEA)与水混合，然后与油酸和/或浮油(分散剂)混合。所得的溶液在使用前在室温下贮存24小时，然后冷冻过夜。将包括二氧化硅，氧化钛，碳酸锶，碳酸钡，碳酸钙，氧化铁，氧化铝，氢氧化铝，有机硅树脂，石墨，聚乙烯珠粒和/或甲基纤维素粘合剂的干组分在研磨机中干混。在连续混合过程中缓慢加入浮油/TEA/水溶液，以均化和增塑。
然后使增塑的混合物挤压通过模头，形成孔密度约200cpsi、壁厚约0.016英寸的蜂窝体。将制得的蜂窝体切割成所需的长度，在烘箱内85℃加热至干燥。样品在电炉内在1350-1500℃的各种温度间隔下烧制，在炉顶温度保持6-8小时，制得最终产品结构，关闭电炉的电源进行冷却。实施例17在1375℃和1425℃烧制。实施例18在1375-1455℃的温度范围内烧制。实施例19在第一温度1475℃烧制1小时，然后在1450℃烧制15小时。
测量这些样品的性质结构列于表5-10。这些性质包括断裂模量，其单位为磅/平方英寸(psi)(除非另外说明，否则都是在从孔密度为200孔/平方英寸(cpsi)、壁厚0.016英寸的蜂窝体上沿平行于孔道的方向切下的多孔棒上测量)；孔隙率，其单位为体积％；中值孔径，其单位为微米；热膨胀，其单位为10-7/℃；和最大尺寸差(最大dL)，其单位为变化％。
在实施例1-5中，c＝0(不含SrO·Al2O3·2SiO2)，或者b＝0(纯BaO·Al2O3·2SiO2)或d＝0(纯CaO·Al2O3·2SiO2)。表5显示了这些具体烧制条件下的实施例的性质。实施例2和5得到了极低的热膨胀和热膨胀滞后，以及高孔隙率和高平均孔径。如果需要较低的烧制温度，实施例3-5(d＝0)更佳。对于需要更耐火的材料的用途，实施例1-2(b＝0)更佳。可以通过改变批料组成和/或原料来调节孔隙率。
在实施例5-10中，a＝0.6965(Al2O3·TiO2)，d＝0(不含BaO·Al2O3·2SiO2)，e＝0.075，h＝0.0035，余量为可变含量的b(CaO·Al2O3·2SiO2)和c(SrO·Al2O3·2SiO2)。在选择的烧制条件下得到的实施例5-10的性质列于表6。在本发明的样品中，可通过控制批料中的b/c比例，在不明显改变热膨胀或孔隙率的前提下控制烧制温度。
图1和图2显示实施例5-10的孔隙率和热膨胀随着烧制温度(1395-1530℃)的变化关系。用少量的b代替c(实施例6和7，其中b＝0.005和0.015，与之对比的是，实施例10中b＝0)，似乎会在较高烧制温度下导致增大的孔隙率。用中等量的b代替c(实施例8和9，其中b＝0.045和0.135)会使得孔隙率和热膨胀随烧制温度有更大的渐进变化。
在实施例11-14中，b＝0，在两个h(时间)水平各自具有两种c/d比例。表7显示在1485℃烧制8小时的实施例11-14的性质。这四个实施例的热膨胀值都低于10×10-7/℃，孔隙率都等于或大于45％。这些实施例说明在相同烧制条件下，d(BaO·Al2O3·2SiO2)相对于c(SrO·Al2O3·2SiO2)比例的增大会使得热膨胀和孔隙率都略微减小。
在实施例15-17中，c＝0，具有三种b/d比例。如表8所示，这些样品具有负的热膨胀值，但是也具有较低的孔隙率。实施例17显示b组分和d组分的混合物使得能够在较低温度下烧制形成低CTE。在实施例18中，b＝c＝d＝0.075。表9显示了该样品随温度的变化关系。实施例18说明可以按照与温度的关系对本发明陶瓷体的性质进行调节。
实施例19提供了优选的组合物。实施例19的性质列于表10。该组合物特别适合用来制造包括堵塞的壁流式蜂窝体的柴油机颗粒过滤器。因此，使用钛酸铝粉末制成的冷固化糊剂在挤出的蜂窝体的进口端和出口端进行端部堵塞。该样品的尺寸为：直径5.51英寸，长5.90英寸，孔密度为292cpsi，孔壁厚0.013英寸。在210scfm的流速下对该样品加载人造炭黑(与复印机色粉类似)，加载量高达5克/升，测量进口端和出口端之间的压降，其单位为千帕。所得的数据在图3中作图，图中显示1.8-4千帕的极好的压降。
应当理解尽管已经结合某些示例性的具体实施方式详细描述了本发明，但是本发明并不限于此，可以在不背离所附权利要求书的范围和本发明精神的前提下通过其它方式实施。
表1.实施例1-6的组成和批料组分。
Figure C200480032617D00111
表2.实施例7-14的组成和批料组分。
表3.实施例15-18的组成和批料组分。
表4.实施例19的组成和批料组分。
Figure C200480032617D00141
表5 实施例1-5的处理条件和性质
Figure C200480032617D00142
表6 实施例6-10的处理条件和性质
Figure C200480032617D00151
表7 实施例11-14的处理条件和性质
Figure C200480032617D00152
表8 实施例15-17的处理条件和性质
Figure C200480032617D00153
表9 实施例18的处理条件和性质与烧制温度的变化关系
Figure C200480032617D00154
表10 实施例19的处理条件和性质

Claims (7)

1.一种具有以下组成的陶瓷体：
a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，
式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，其中：0.5<a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0<e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d>0.01。
2.一种柴油机颗粒过滤器，它包括由以下组分组成的端部堵塞的壁流式蜂窝状过滤陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，
式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，其中：0.5<a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0<e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d>0.01。
3.如权利要求2所述的柴油机颗粒过滤器，其特征在于，它具有以下性质：在室温至1000℃下的CTE小于10×10-7/℃；孔隙率为40-55体积％；中值孔径为5-20微米；在孔密度为200cpsi、孔壁厚为0.016英寸的多孔棒上测得的断裂模量为150-400psi。
4.如权利要求3所述的柴油机颗粒过滤器，其特征在于，所述中值孔径为10-15微米。
5.如权利要求3所述的柴油机颗粒过滤器，其特征在于，所述断裂模量为150-300psi。
6.一种制备钛酸铝基陶瓷体的方法，该方法包括：
(a)配制包含二氧化硅源，氧化铝源，锶源，钡源，钙源，氧化钛源，和/或氧化铁源的无机原料组分与包括增塑剂、润滑剂、粘合剂的有机处理组分和用作溶剂的水的批料，
(b)对所述无机和有机组分的批料进行混合，形成均匀的增塑的混合物；
(c)对该增塑的混合物进行成形，制成生坯体；
(d)在1350-1600℃的炉顶温度下对该生坯体加热一定时间，制成由以下组分组成的陶瓷体：a(Al2O3·TiO2)+b(CaO·Al2O3·2SiO2)+c(SrO·Al2O3·2SiO2)+d(BaO·Al2O3·2SiO2)+e(3Al2O3·2SiO2)+f(Al2O3)+g(SiO2)+h(Fe2O3·TiO2)+i(MgO·2TiO2)，式中a，b，c，d，e，f，g，h和i是各组分的重量分数，使得(a+b+c+d+e+f+g+h+i)＝1，其中：0.5<a≤0.95；0≤b≤0.5；0≤c≤0.5；0≤d≤0.5；0<e≤0.5；0≤f≤0.5；0≤g≤0.1；0≤h≤0.3；0≤i≤0.3；b+d>0.01。
7.如权利要求6所述的方法，其特征在于，以无机原料组分为100重量份计，该批料还包含20-40重量％的成孔剂。
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EP1680206A1 (en) 2006-07-19
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