CN1313416C - 用于高温应用的锶长石钛酸铝 - Google Patents

用于高温应用的锶长石钛酸铝 Download PDF

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CN1313416C
CN1313416C CNB038060671A CN03806067A CN1313416C CN 1313416 C CN1313416 C CN 1313416C CN B038060671 A CNB038060671 A CN B038060671A CN 03806067 A CN03806067 A CN 03806067A CN 1313416 C CN1313416 C CN 1313416C
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weight
aluminium titanates
iron
magnesium
described structure
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CN1642872A (zh
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S·B·奥古米
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Corning Inc
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Corning Inc
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

公开了一种高温下使用的结构，它包含多孔陶瓷材料，所述材料基本上由约50—90重量%铁或镁稳定的钛酸铝(AlTiO5)和约10—50重量%锶长石(SrO(Al2O3)(2SiO2))组成，所述结构在室温到1000℃温度范围内的热膨胀系数约为-10×10-7/℃到+15×10-7/℃，在500℃下热容大于3.2J/cm3K，孔隙率约为15—50体积%，较好是40-50体积%，孔径中值约为5-50微米，较好是8—15微米。所述结构尤其用作柴油机排气颗粒过滤器。

Description

用于高温应用的锶长石钛酸铝
发明背景
本发明涉及锶长石钛酸铝陶瓷。本发明尤其涉及用于柴油机排气过滤应用的热膨胀低、耐热冲击性高、具有合适孔隙率且孔径分布窄的锶长石钛酸铝陶瓷。
在工业中，堇青石(2MgO·2Al2O3·5SiO2)由于其综合了良好的耐热冲击性、过滤效率以及多数操作条件下的耐久性，是选择用于高温过滤应用的成本有效的材料。但是，在某些情况下，堇青石过滤器容易损坏，甚至会引起灾难性事故。在未受控的再生过程中存在偶然的热量失控，导致堇青石局部熔融。当操作过程中将来自机油、催化添加剂或排气口衬垫的溶蚀金属的金属杂质带入过滤器时会出现另一个导致故障的因素。通常，当温度超过1300℃时，这些金属形成氧化物，并和堇青石结构反应。材料故障的证据通常是过滤器上的小孔，在此起初沉积金属并反应，导致溶蚀以及材料熔融。
最近，在制造柴油机颗粒过滤器时已经使用碳化硅(SiC)来代替堇青石。但是，SiC成本高，且必须进行分段，这是因为其固有的热膨胀系数(CTE)高，耐热冲击性差。
因此，要求有一种适于高温应用的陶瓷，它没有堇青石的不足，但具有其所有的优点。本发明提供了这种陶瓷。
发明概述
本发明是基于发现锶长石钛酸铝为膨胀低、耐热冲击性高的陶瓷(下文称为SAT)来进行的。本发明陶瓷包含锶长石(SrO·Al2O3·2SiO2)(SAS)相和另一个钛酸铝(Al2TiO5)(AT)相，它可以挤出成蜂窝状结构。发现AT相中的铁(Fe)或镁(Mg)取代可以提高陶瓷材料抗分解的稳定性，尤其是在800℃以上的高温下。本发明中，AT中的铝的Fe和Mg同型取代度范围约为0-60摩尔％，较好是1-10摩尔％。
本发明结构体的配方基本上由约50-90重量％Fe或Mg稳定的AT以及约10-50重量％SAS组成。优点包括热膨胀系数低、耐热冲击性高、体积热容高、互连孔隙率高且孔径中值大。
因此，从室温(RT)到1000℃的热膨胀系数(CTE)约为-10×10-7/℃到+15×10-7/℃，较好是从室温到800℃的热膨胀系数约为-0.5×10-7/℃到+6×10-7/℃。所述体积热容在500℃下测量时大于3.2J/cm3K。所述总的孔隙率约为15-50体积％，较好是40-50体积％，孔径中值约为5-50微米，较好是8-15微米。
本发明陶瓷较好基本上由约70-80重量％Fe稳定的AT以及约20-30重量％SAS组成，且在室温到800℃的温度范围内，热膨胀系数约为-0.3×10-7/℃到+2×10-7/℃，总的孔隙率约为40-45体积％，孔径中值约为15-20微米。
本发明陶瓷适于在高温下应用，如柴油机排气过滤用壁流式过滤器和汽车用催化转化器。包含本发明结构体的壁流式过滤器具有高体积热容，在所述过滤器长度两端的压力降低。本发明陶瓷较好挤出成蜂窝状结构，它具有进口端和出口端，以及从进口端延伸到出口端的许多孔，所述孔具有多孔壁，其中，沿其部分长度在进口端处堵塞部分孔，沿其部分长度在出口端处堵塞在进口处敞开的其余部分孔，使发动机排气流从进口端向出口端流经蜂窝状结构的孔，通过孔壁进入敞开的孔，并通过敞开的孔在出口端流出所述结构体。
本发明提供一种柴油机排气颗粒过滤器，它包括由多孔陶瓷材料构成的堵塞的壁流式蜂窝状过滤器主体，并包括许多平行的末端堵塞的孔通道，所述通道从其前进口端到出口端横贯所述主体，其中，所述陶瓷材料基本上由50-90重量％钛酸铝和10-50重量％分子式为锶长石SrO·Al2O3·2SiO2的锶长石组成，所述钛酸铝用铁或镁稳定，钛酸铝相中铁或镁的取代度为0-60摩尔％；所述结构体陶瓷材料在室温到1000℃温度范围内的热膨胀系数为-10×10-7/℃到+15×10-7/℃，在500℃下体积热容大于3.2J/cm3K，总的孔隙率为15-50体积％，孔径中值为5-50微米且孔径分布均匀。
附图简要说明
图1A-B是本发明实施例5的扫描电子显微图。
图2A-B是本发明实施例6的扫描电子显微图。
图3证明通过壁流式过滤器可以使过滤器长度两端的压力降低，所述过滤器包含本发明的SAT陶瓷，图示了气体流速为26.25scfm时的实施例5和6。
发明详述
本发明是主要为两相的陶瓷，它具有镁(Mg)或铁(Fe)稳定的钛酸铝(Al2TiO5)的主要的第一相(AT)以及第二锶长石(SrO·Al2O3·2SiO2)相(SAS)。也可以存在次要相，这些包括氧化铝和二氧化钛(TiO2)。这种独特的相组合提供了本发明的结构体，它极难熔，且CTE接近于0，使之适于高温应用，如过滤柴油机排气颗粒物质。
AT具有1860℃的高熔点，其各向异性热膨胀高(即沿晶轴的膨胀差异大)，沿a轴约为-26×10-7/℃，沿b轴约为118×10-7/℃，沿c轴约为194×10-7/℃。所述极大的各向异性导致在大AT颗粒中产生内应力。当所述材料冷却时产生严重的微裂缝，这归因于其热膨胀系数低。根据粒度或微裂缝程度，AT的整体CTE约为-3×10-7/℃到+9.7×10-7/℃。但是，更大的颗粒生长和后续微裂缝会导致形成强度低的材料。加入作为第二相的SAS起到提高强度(MOR)并平衡CTE的作用。所得复合AT-SAS陶瓷结构会出现微裂缝，且CTE接近0，使耐热冲击性高。微裂体会使CTE偏向于CTE最负的部分，这是因为冷却时微裂缝的打开提供所述普通正的部分。因此，在本发明SAT结构中，如在室温(RT)到1000℃的温度范围内通过膨胀测量法进行测量，所述CTE约为-10×10-7/℃至+15×10-7/℃，较好是从RT-800℃的CTE约为-0.5×10-7/℃到+5×10-7/℃。
所述AT结构证实在800-1300℃之间结构不稳定。要求用Fe或Mg进行同型取代，提高AT在800℃以上抗分解的稳定性。在本发明中，用Fe和Mg取代AT相中的铝的同型取代的限制范围约为0-60摩尔％，较好是1-10摩尔％。本发明SAT陶瓷的组合物基本上由约50-90重量％Fe或Mg稳定的AT和约10-50重量％SAS组合物。所述组成较好由约70-80重量％Fe或Mg稳定的AT和约20-30重量％SAS组成。
本发明SAT陶瓷的互连孔隙率高，孔径中值大，使之适于高温过滤应用，如壁流式过滤器。因此，由水银孔隙率测定法测定，总的孔隙率约为15-50％，较好是约40-50％。所述孔径分布均匀，其孔径中值为5-50微米，较好是8-15微米。另一优点是热容高。要求热容高是由于在再生过程中它降低了过滤器应用中温度升高的数值。在500℃下测定的体积热容大于3.2Jcm-3K-1，较好是3.7-3.7Jcm-3K-1。
制造本发明陶瓷的合适方法是通过将颗粒原料、任选成孔剂以及有机粘合剂、润滑剂、增塑剂和/或溶剂的混合物制成坯体，任选干燥，然后烧制成所述产品结构。
所述形成SAT的原料是(1)反应形成SAS和Mg或Fe稳定的AT相的氧化物源，和/或(2)部分或完全预反应的SAS和Mg或Fe稳定如AT粉末。好的原料包括二氧化硅、氧化铝、碳酸锶、二氧化钛、氧化铁和/或碳酸镁。可以任选地包含成孔剂，使最终产品结构中的孔隙率较大，和/或孔径中值较大。原料和可以包含增塑剂、润滑剂、粘合剂和溶剂的有机组分掺合在一起。也可以任选地加入水作为溶剂。所述混合物成形为坯体、任选干燥，然后在一定温度下烧制足够时间，形成所述最终产品结构。
选择所有起始原料，限制组合物中碱性物质的存在。氧化铝源是粉末，在没有其它原料存在下加热至足够高的温度，产生基本上纯的氧化铝，它包括α-氧化铝、过渡氧化铝如γ-氧化铝或ρ-氧化铝、勃姆石、氢氧化铝及其混合物。氧化铝的形态必须是管状，且为在最终结构中产生微裂缝，粒度应足够大，但是也应足够小，便于良好挤出。因此，较好粒度约为10-25微米。
所述氧化硅源包括粘土和石英，但是较好是石英，其烧结温度比粘土源高。使用石英代替粘土有利于在高温下在最终结构中形成孔隙。推荐使用赤铁矿作为氧化铁源。优选使用粒度约为7-15微米的金红石，较好是购自Cranbury，NJ的Kronos，Inc.的Kronos 3020金红石作为二氧化钛源。当Al3+离子扩散到所述二氧化钛(TiO2)中时，存在形成钛酸铝的反应。所述机理已经实验证实。TiO2源的粒度对于避免因快速生成产物核而夹杂未反应的氧化物来说很重要。未反应的氧化物会导致最终烧结体中的热膨胀明显更高。
并不一定需要成孔剂来获得所需的性质和最佳颗粒分布，但是若需要的话可以加入以提高孔隙率。推荐的成孔剂是玉米淀粉。当为玉米淀粉时，成孔剂的量至多为原料混合物的20重量％。若使用石墨，要求至多为原料混合物的30重量％。使用甲基纤维素作为有机粘合剂，它在以后烧制过程中被烧掉。较好使用油酸作为分散剂。由于会受钠的污染，因此并不推荐使用硬脂酸钠。可以使用硬脂酸二甘醇酯，但是在挤出过程中通常会导致粘合性差，造成烧制过程中产生裂缝。若使用硬脂酸二甘醇酯，要求加入约1-2％聚乙二醇作为润滑剂来改进挤出。
本发明陶瓷尤其适于高温过滤应用。具体的是，本发明陶瓷尤其适于柴油机颗粒过滤器应用。对于这种应用，所述原料混合物较好通过挤出成形为蜂窝状多孔结构，如本领域技术所知的。通常干燥所得成形的蜂窝状坯体，然后在约30-50小时内加热至1485-1500℃的最高温度，并在所述最高温度下保持约8-14小时。
虽然过滤器结构可以是任何适于具体应用的形状或几何构型，但是优选它为多孔结构，如蜂窝状结构。所述蜂窝状结构具有进口和出口端或进口和出口端面，以及从进口端向出口端延伸的许多孔，所述孔具有多孔壁。本发明过滤器的孔密度约为100个孔/平方英寸(15.5个孔/平方厘米)到400个孔/平方英寸(62个孔/平方厘米)。
为了制得壁流式过滤器，如本领域所知，堵塞进口端或端面处蜂窝体的一部分孔。堵塞操作仅在孔的末端进行，通常深度约为5-20mm，虽然这可以是不同的。堵塞出口端的一部分孔，而所述部分的孔并不对应于进口端上堵塞的孔。因此，各孔仅堵塞一端。所述优选排列是使在指定端面上的每隔一个孔方格图案形状。(？)
本发明制得壁流式柴油机排气颗粒过滤器，它相比市售SiC的对应物而言，过滤器长度两端的压力降低，发动机的背压低。过滤器两端的压力降是积聚在柴油机颗粒过滤器壁上含碳烟灰的函数。当积聚的烟灰量增大时，其阻止排气流经过滤器壁和含碳烟灰层的阻力就逐渐增大。这种流动阻力表现为压力降，它可以在过滤器长度的两端进行测量，并导致发动机的背压增大。
另一个优点就是减少车辆发动机中排气携带的金属氧化物“烟灰”粒子。金属氧化物“烟灰”粒子是不可燃的，因此，不能在再生过程中除去。在工业中存在的问题是当在再生工艺中的温度达到足够高的值时，所述烟灰会烧结到过滤器材料上，或者甚至和过滤材料反应，导致部分熔融。实验表明，AT相的存在提高了包含本发明陶瓷的过滤体的耐烟灰性。而且，本发明陶瓷的热容高，可以降低再生过程中过滤器中温度升高的数值。再生过程中过滤器中的温度较低，烧结的金属氧化物烟灰也较少，烟灰和过滤器的反应也较少，由此提高过滤器的使用寿命。
虽然优选的应用是柴油机颗粒过滤器，但是应注意本发明陶瓷也同样适于作为汽车流过基材。
实施例
为了更全面地说明本发明，在表I和II中列出了以下挤出蜂窝体的非限制性实施例。表I记录了本发明实施例的组成以及所得的相组合。表II记录了本发明样品所测得的物理性质。除非另有说明，所有份数、比例和百分数均以原料的总重量计。
在加入其余干燥原料和有机组分之前将作为分散剂的油酸和二氧化硅混合约10-15分钟。所得混合物连续混合，进行均化。然后在研磨机中逐渐加入足量的去离子水，使所述混合物具有塑性。在捏合之后，通过模头将所述混合成分挤出，形成每平方英寸具有100-200个孔且壁厚约为0.010-0.025英寸的蜂窝体。将由此形成的蜂窝体切割成所需的长度，并在85℃的烘箱中加热，直到干燥。
在电炉中，以20-40℃/小时的速度加热至1485-1500℃的最高温度，在各温度区间内烧结所述样品30-50小时，并保持在所述最高温度下约8-14小时，形成所述最终产品的结构，并通过切断供给电炉的电源进行冷却。
表II记录了样品所测定的物理性质。相组合通过粉末X-射线衍射法鉴别。通过水银孔隙率测定法测得所选样品的孔隙率和孔径。总孔隙率以体积％计，孔径以微米计。使用膨胀计测量从室温到800℃以及到1000℃的平均热膨胀系数，并以10-7/℃记录。
从室温到1000℃的热膨胀系数(CTE)约为-10×10-7/℃到+6×10-7/℃，较好是，从室温到800℃的热膨胀系数约为-0.5×10-7/℃到+3×10-7/℃。现在参考图1A-B和2A-B，分别图示了实施例5和6的微结构，其通过扫描电子显微镜观察。所述孔隙率分布基本上均匀，通常约为15-50％，较好约为40-50％，具有良好的互连孔隙结构。所述平均孔径通常约为5-50微米，较好约为8-15微米。在实验室测试中，本发明结构体的这些性质使得背压低，如图3所示。该图图示以Kpa表示的压力降，作为烟灰负载的函数(g/L)，对实施例5和6而言，流速为26.25scfm(标准立方英寸/分钟)。
目前，最优选的AT和SAS组合看来是80重量％Fe稳定的AT和20重量％SAS，在室温到800℃的温度范围内热膨胀系数约为-0.3×10-7/℃到+2×10-7/℃，总的孔隙率约为40-45体积％，孔径中值约为15-20微米，如实施例5和6中所述。
应理解虽然本发明已经详细公开了某些说明性的具体实施方式，但是不应认为本发明受到这些实施方式的限制，在不背离本发明精神和附带权利要求书的范围的条件下本发明可以以其它方式使用。
                                    表I：样品化学组成
  实施例   1   2   3   4   5   6
  原料或成孔剂
  氧化硅   11.38   6.5   5.4   5.4   6.5   6.5
  氧化铝1   9.69   5.54   4.6   4.6   --   5.54
  氧化铝2   --   --   --   36.22   49.01   43.47
  氧化铝3   35.32   43.47   36.22   --   --   --
  碳酸锶   13.39   7.96   6.6   6.6   7.96   7.96
  氧化铁   1.63   2.0   1.7   1.7   2.0   2.0
  二氧化钛   28.05   34.35   28.76   28.76   34.53   34.35
  玉米淀粉   --   --   16.67   --   --   --
  石墨   --   --   --   16.67   --   --
  粘合剂、润滑剂和溶剂
  甲基纤维素   4.5   4.5   4.5   4.5   4.5   4.5
  油酸   0.5   0.5   0.5   0.5   0.5   0.5
  聚乙二醇   1.0   1.0   1.0   1.0   --   --
  水   21.4   21.4   28.5   27.5   20.0   19.0
  烧制条件
  炉子类型   电炉   电炉   电炉   电炉   电炉   电炉
  最高温度(℃)   1500   1485   1485   1485   1485   1485
  持续时间(小时)   8   8   8   8   8   8
                                            表II样品性质
  实施例   1   2   3   4   5   6
  相组合
  Fe稳定的AT(重量％)   65   80   80   80   80   80
  Fe摩尔％   3   3   2.2   2.2   3   3
  SAS(重量％)   35   20   20   20   20   20
  性质
  平均CTE(RT-800℃)(10-7/℃)   -4.8   -0.9   3.5   -4.0   2.0   -0.3
  平均CTE(RT-1000℃)(10-7/℃)   4.0   8.0   12.0   2.0   13.0   6.0
  孔径中值(微米)   29   26   25   12   15   17
  总孔隙率(体积％)   34   34   40   25   41   44

Claims (10)

1.一种包含多孔陶瓷材料的结构体，所述陶瓷材料基本上由50-90重量％钛酸铝和10-50重量％分子式为SrO·Al2O3·2SiO2的锶长石组成，
其特征在于，所述钛酸铝用铁或镁稳定，钛酸铝相中铁或镁的取代度为0-60摩尔％；
所述结构体在室温到1000℃温度范围内的热膨胀系数为-10×10-7/℃到+15×10-7/℃，在500℃下体积热容大于3.2J/cm3K，总的孔隙率为15-50体积％，孔径中值为5-50微米且孔径分布均匀。
2.权利要求1所述的结构体，其特征在于，钛酸铝中铁或镁取代度范围为1-10摩尔％。
3.权利要求2所述的结构体，其特征在于，在室温到800℃温度范围内的热膨胀系数为-0.5×10-7/℃到+6×10-7/℃。
4.权利要求3所述的结构体，其特征在于，所述总的孔隙率为40-50体积％。
5.权利要求4所述的结构体，其特征在于，所述孔径中值为8-15微米。
6.权利要求1所述的结构体，其特征在于，所述陶瓷基本上由70-80重量％铁稳定的钛酸铝和20-30重量％锶长石组成。
7.权利要求6所述的结构体，其特征在于，在室温到800℃温度范围内的热膨胀系数为-0.3×10-7/℃到+2×10-7/℃。
8.权利要求1所述的结构体，其特征在于，所述结构体具有蜂窝形状，它具有进口端、出口端以及从进口端延伸到出口端的许多孔。
9.一种柴油机排气颗粒过滤器，它包括由多孔陶瓷材料构成的堵塞的壁流式蜂窝状过滤器主体，并包括许多平行的末端堵塞的孔通道，所述通道从其前进口端到出口端横贯所述主体，
其特征在于，所述陶瓷材料基本上由50-90重量％钛酸铝和10-50重量％分子式为SrO·Al2O3·2SiO2的锶长石组成，所述钛酸铝用铁或镁稳定，钛酸铝相中铁或镁的取代度为0-60摩尔％；
所述陶瓷材料在室温到1000℃温度范围内的热膨胀系数为-10×10-7/℃到+15×10-7/℃，在500℃下体积热容大于3.2J/cm3K，总的孔隙率为15-50体积％，孔径中值为5-50微米且孔径分布均匀。
10.权利要求9所述的过滤器，其特征在于，钛酸铝中铁或镁取代度范围为1-10摩尔％。
CNB038060671A 2002-03-14 2003-03-12 用于高温应用的锶长石钛酸铝 Expired - Lifetime CN1313416C (zh)

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