CN100522883C - 耐热冲击的陶瓷复合材料 - Google Patents

耐热冲击的陶瓷复合材料 Download PDF

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CN100522883C
CN100522883C CNB02827122XA CN02827122A CN100522883C CN 100522883 C CN100522883 C CN 100522883C CN B02827122X A CNB02827122X A CN B02827122XA CN 02827122 A CN02827122 A CN 02827122A CN 100522883 C CN100522883 C CN 100522883C
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ceramic composite
net
matrix
alumina
sol
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CN1615283A (zh
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K·-H·肖法尔维
G·C·多兹
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Stanton Advanced Ceramics Inc
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Abstract

一种能重复耐受超过1204.4℃(2200℉)的温度而不会由于热冲击而产生裂纹的陶瓷复合材料。该复合材料含有增强纤维网，和在烧制步骤后基本构成网的基体。用含有氧化铝，和在某些情况下稀土氧化物的溶胶浸渍该网，并且在浸渍后烧制该复合材料，这样在该网周围形成这种基体。该网可以是一种增强纤维的三维正交编织物，其中这些纤维是过渡相氧化铝。该复合材料是基本无第I族和第II族金属和过渡金属氧化物的。该复合材料可用作耐火砖或衬里，也因其非化学活性而可以用作隔热材料。

Description

耐热冲击的陶瓷复合材料
技术领域
本发明涉及一种有陶瓷纤维增强材料的陶瓷基体复合材料。更具体地，本发明涉及有氧化铝增强材料的陶瓷基体复合材料。更具体地，本发明涉及有氧化铝增强材料的陶瓷基体复合材料，其中该增强材料在预浸料中为活性氧化铝形式。
背景技术
材料在如钢铁工业的应用中要经受高温，因此通常需要使用陶瓷复合材料。由于材料经受高热冲击与复合结构的限制，温度高于约1204.4℃(2200℉)就要限制大多数陶瓷只使用一次。陶瓷复合材料在钢铁工业中的典型应用包括滑动门、漏斗式喷枪和如锥形漏斗、轧辊之类的各种可铸形状。其他应用包括燃料电池和电炉陶瓷砖。在另一高温应用中，目前制造火箭喷嘴的材料包括聚合物基体复合材料和碳-碳复合材料。聚合物基体复合材料的烧蚀性和腐蚀性制约了喷嘴的性能，而碳-碳复合材料需要高昂的生产成本，还可能对环境造成危险。为了满足对高性能的多方面要求，例如耐腐蚀性、抗烧蚀性和耐热冲击性，以及低的生产成本，必须采取独特的喷嘴制造方法。
有许多方法可生产要求不高，应用温度又较低的陶瓷复合材料。一种方法可生产大量微裂化的多相陶瓷，这种陶瓷能经受酷热条件。简言之，通过陶瓷纤维浸没在预制陶瓷溶胶中可以浸渍陶瓷纤维的机织预成型坯或毡毯，然后烧制。在烧制过程中，预成型坯纤维与溶胶中的胶体陶瓷微粒进行反应，生成具有组成梯度的陶瓷材料，该组成梯度基本上与最初纤维方向垂直。可通过温度与选择材料控制纤维与基体之间的反应程度，限制这个反应程度，以使残留纤维结构不变。通过原料的适当组合和尺寸，可以保证在烧制陶瓷过程中形成高的微裂纹度。通过一个或多个真空预浸渍和烧制循环，可将产品的孔隙度降到所要求的水平。大量微裂纹使陶瓷具有一定程度的耐热冲击性。残留纤维结构使陶瓷具有裂纹偏转网络，微裂纹的分布会提供某些附加的应力消除机制，防止由于大的突然温度变化而导致宏观失效。
陶瓷复合材料的某些制造方法可使用如硅酸镁玻璃之类的增强材料，其中在烧制陶瓷复合材料时，增强材料与溶胶基体以这样一种方式反应，以致使得它不能与基体相互区分，从而制约了材料的耐热冲击性。可以保留纤维基体，但基体和纤维的温度限制依然将陶瓷的使用限于低于约1204.4℃(2200℉)的应用。而且，所得到陶瓷复合材料的耐热冲击性和抗冲击强度对于要求更高、温度更高的应用是不足的。
提供更高温度的陶瓷复合材料是人们所希望的，因此是本发明的一个目的，该陶瓷复合材料将耐热冲击、冲击、化学侵蚀并经得住高于1204.4℃(2200℉)的温度。
发明内容
本发明的这个目的和其他目的是提供一种陶瓷复合材料，它能重复耐受高于1204.4℃(2200℉)的温度，不会由于热冲击而破裂，特别地提供一种陶瓷复合材料，它含有增强纤维网和由氧化铝溶胶形成的基体，该溶胶在烧制步骤前浸渍该网，所述的基体基本上在烧制步骤后埋置该网。
在本发明的某些具体实施方案中，通过在浸渍溶胶中掺杂至少一种稀土金属氧化物，该基体还含有至少一种稀土金属氧化物。以该溶胶中的氧化铝计，稀土金属氧化物的量可以是约0-60重量％。
在一个优选的具体实施方案中，该网是增强纤维的三维正交编织物，纤维在烧制步骤前含有过渡相氧化铝尤其如此，过渡相氧化铝是γ-氧化铝更尤其如此。
在本发明的一些具体实施方案中，在烧制步骤之后，该网占复合材料的10-40重量％。
在本发明的大多数具体实施方案中，复合材料基本不含有第I族和第II族金属和过渡金属氧化物。
在本发明的大多数具体实施方案中，在浸渍步骤中，增强纤维被用于生产基体的溶胶部分吸收，这种部分吸收与烧制步骤结合产生网纤维的微裂纹。
本发明的复合材料由于其耐热冲击性和化学不反应性，可用作耐火砖和隔热材料。
优选具体实施方案的详细说明
为了得到具有高温耐热冲击性，即在高于约1204.4℃(2200℉)温度下的耐热冲击性与有可接受生产成本的陶瓷，可以设想一种氧化铝增强的氧化铝基体复合材料。但是，典型的氧化铝纤维增强材料由α-氧化铝生产。使用α-氧化铝生产氧化铝基体复合材料可得到一种材料，它的耐热冲击性差，基体与增强材料的粘附也差。由于α-氧化铝本质上是一种“末段”材料，所以在胶凝和烧制过程中，它与基体没有任何明显程度地反应。
相反，现已发现使用氧化铝溶胶和活性氧化铝增强材料，可以制造具有高耐热冲击性的陶瓷复合材料。在温度高达3100℉的应用中可以使用这些材料。一种这样的增强材料是称之γ-氧化铝的过渡相氧化铝，它是一种α-氧化铝的欠氧化前体。γ-氧化铝有活性表面，可与氧化铝溶胶反应生成均匀的复合材料，该材料在基体与增强材料之间有较好的界面粘附作用。得到的复合材料具有所希望的热冲击性和高使用温度。典型地，用这种复合材料制成的物品在熔融铁钢的应用中可以使用几次，而不是使用现有技术的材料通常只是使用一次。
使用本发明方法和材料可获得几个好处，其中包括：
1)生产成本低。使用从市场购买的原料就可完成材料合成和组分生产。可在空气中进行复合材料的热处理。不必使用真空炉、高压釜或特殊加工气体。
2)耐腐蚀性改进。提出的材料是非烧蚀性的材料，并可以进行表面硬化，因此不再需要硬化嵌件。
3)出色的耐热冲击性。该材料在温度远高于1204.4℃(2200℉)的应用中可耐热冲击，而通常认为1204.4℃(2200℉)是已知陶瓷材料的温度上限。
陶瓷复合材料生产中使用的代表性材料列在表1中。对于如在现有技术中所描述的较低温度的应用，该陶瓷含有用硅酸镁玻璃增强的氧化铝基体。这样得到的陶瓷局限于在温度约1204.4℃(2200℉)下的应用内。
根据其计划温度潜在能力和纤维与溶胶组分的利用率，预制表1所列材料体系。根据加工和成本因素的考虑以及温度限制，实际考虑使用各种材料。使用氧化锆纤维获得最高温度的能力。但是，氧化锆纤维比较昂贵，但可能是成本低的，只使用随意取向的毡原料。
加工考虑因素包括可以加工溶胶体系的相对难易程度。溶胶稳定性、控制溶胶胶凝的能力、预成型坯中溶胶与纤维的反应性和产品产率构成最主要的加工考虑因素。原料，特别是纤维预成型坯，构成了表1所列陶瓷体系生产中的主要成本因素。
表1  材料体系
 
体系号r      初始增强材料     基础溶胶&填料或第二溶胶(浸渍剂)      得到的材料体系           计划稳定态温度潜在能力(℉/℃)     
1 硅酸镁玻璃       氧化铝溶胶+氧化铝粉末          堇青石，富铝红柱石和刚玉多相陶瓷     2200/1254
2 氧化铝<sup>＊</sup> 氧化铝溶胶+氧化钇粉末          有浓度梯度的氧化铝-氧化钇固体溶液   3100/1704
3 氧化铝<sup>＊</sup> 氧化锆溶胶+YAG和氮化铪粉末         多相陶瓷 3300/1816
4 氧化锆<sup>＊</sup> 氧化锆溶胶+YAG和氮化铪粉末         多相陶瓷 3700/2038
＊机织预成型坯或毡毯
硅酸镁玻璃纤维是最不贵的增强材料，而氧化锆纤维是最为昂贵的。如成本是唯一标准，则可以选择在现有技术中已知的材料体系1(表1)。
为了成本的原因，除了使用机织预成型坯，还使用毡毯。编织预成型坯比机织预成型坯的生产成本低得多。机织预成型坯可提供良好的硬度和控制相取向以及定向性能；但连续纤维多方向织成硬预成型坯比较昂贵。这个基材提供了对结构随意取向的非机织纤维增强材料与直接关联取向的机织纤维增强材料可进行直接成本和性能比较。
温度潜在能力限制了材料对于一定应用的可用性。如果温度潜在能力是唯一的选择标准，则可选择表1中的材料体系号4。这个材料也是最贵的，但生产量和/或使用随意取向的毡抑制了成本。曾讨论对于应用来说很重要的其他性能，耐腐蚀性和耐热冲击性。用等离子喷射的碳化铪层或其它相容耐火陶瓷碳化物层使其表面硬化，可增强耐腐蚀性。
曾用其他陶瓷材料确定了该生产方法的一些方面。用氧化铝前体润湿二氧化硅-氧化镁玻璃的预成型坯。该前体由聚合氧化铝溶胶组成。在加热到至少1380℉时，玻璃中的二氧化硅和镁与氧化铝反应生成结结晶相堇青石和富铝红柱石。基本上没留下任何玻璃纤维。这与本发明方法不同之处在于，本发明方法为以后机械强度和增加热冲击留下大量纤维结构。最后的结构具有组成梯度，在离玻璃纤维初始位置最近的区域硅浓度较高，随着离玻璃纤维位置的距离增加而硅浓度降低。二氧化硅浓度较高的地方，氧化铝浓度就较低，二氧化硅浓度较低的地方，氧化铝浓度就较高。浓度梯度与具有不同热膨胀系数的结结晶相均匀混合物导致产生大量微裂纹结构。也曾用氧化铝纤维和二氧化硅前体开始生产含有相同结晶相的耐热冲击陶瓷，氧化硅前体例如是二氧化硅溶胶或硅酸溶液，或二者的混合物。
在本方法中，过渡相氧化铝，特别地γ-氧化铝增强材料是用氧化铝前体润湿的。可选择地，氧化铝前体可包括稀土粉末，如氧化钇、氧化钕、氧化镨、氧化铒和氧化镧，其中包括这些稀土粉末的混合物，即使是在“有意”(“as mined”)情况下。氧化铝前体中可以包括一种或多种稀土。该溶胶应该基本上不含硅酸盐、氧化钙和在已知陶瓷材料中其它用于实现粘附作用的化合物。
为了制备氧化铝前体溶胶，氧化铝粉末与水混合，达到适合于用作浸渍溶胶的浓度。稀土粉末可包括氧化铝。氧化铝和稀土(如果有的话)在水中的浓度可以是约10-40重量％。可选择地，氧化铝和稀土(如果有的话)在水中的浓度可以是约20重量％。氧化铝和稀土(如果有的话)在水混合物中与无机酸混合，达到混合物的低pH。在一个具体实施方案中，可用HNO3或HCl滴氧化铝/水混合物定，使其pH达到约3-4。该混合物搅拌约24小时，使溶胶稳定。由该混合物得到的上清波可作为复合材料浸渍剂无限期储存直到使用。现在给出详细实验步骤。
复合材料的制备
首先如下配制氧化物溶胶。选择零电荷点(ZPC)9.1的氧化铝，还选择8.95ZPC的Y2O3。这样的氧化铝源是CATAPAL牌可分散氧化铝。称取200克氧化铝，将100克加到1800克去离子水中，用磁力搅拌盘剧烈搅拌，同时加入该氧化物。混合时，往氧化物/水混合物缓慢添加HNO3(65-70％被分析物)。测量该混合物的pH，用硝酸滴定，直到pH在3-4范围内。然后加入余下的100克氧化铝，再次加入硝酸，滴定混合物达到pH3-4范围。紧紧盖住该系统，使其蒸发最少，并混合24小时。在24小时结束后，关掉搅拌器，取下混合棒，溶胶静置陈化24小时。在此期间，会沉降出最粗的聚结颗粒。
虹吸上清液，注意不要扰动沉淀颗粒。干燥并称量沉淀颗粒。这种溶胶现在应该能够无限期储存，而不会再沉淀出颗粒。可以计算溶胶的浓度。
以类似的方法制备稀土混合氧化物溶胶，但在这种情况下使用1200克去离子水。称取两批等量的Pr6O11粉末，各重37.83克。还称取两批等量的Y2O3粉末，各重2克。在磁力搅拌器搅拌下，往水中加入一批各两种粉末。加入约10毫升HNO3，混合8小时，之后该混合物滴定达到pH3-4范围。如果必要，加入另一批粉末，并再用硝酸滴定。
为氧化铝浸渍机织预成型坯而制备的典型溶胶应该包括100％氧化铝溶胶、60％氧化铝和40％氧化钇的掺混溶胶，和40％氧化铝、40％氧化钇和20％氧化镨的共混物。所有上述百分比都是以重量计的。
以这种方式生产的溶胶可用于浸渍预成型坯，特别地含有过渡相氧化铝的预成型坯，更特别地，含有三维正交编织物转换相氧化铝纤维的预成型坯。在400℃空气中加热约4小时可以烧掉预成型坯的任何纤维涂胶。溶胶和预成型坯分别称重和测量，该预成型坯再浸没在烧杯的溶胶中，进行初始渗透。该烧杯用钟形容器或其他合适真空设备抽真空达到压力约28英寸汞柱，直到停止鼓泡，这将花约5-10分钟。由于这种真空渗透开始就可能伴随着激烈的鼓泡和起泡，所以应该密切注意这一操作，控制真空，防止溶胶由于鼓泡而溢出。停止鼓泡时，打开钟形容器，从溶胶中取出预成型坯，让其在溶胶上滴干几分钟，收集过量的溶胶。然后该预成型坯在50℃干燥2小时。
应该测量该溶胶的pH，如果必要，用硝酸调整到3-4。在测量干预成型坯的重量之后，重复前段的浸渍步骤，如必要可重复多次，直到所要求量的溶胶浸渍到预成型坯中。
一旦预成型坯已适当浸渍了，就将预成型坯在400℃烧制，使渗透剂溶胶机械地锁定在预成型坯宏观结构中。从浸渍到这种烧制步骤的这些步骤如必要可重复进行，以便在预成型坯周围达到所要求的溶胶基体水平。典型地，将使用7-9个循环。
在浸渍剂机械锁定完成之后，可将该复合材料煅烧至1800℃达2小时，使溶胶基体化学锁定在适当的位置。
氧化铝溶胶可以包括稀土金属氧化物材料。例如，使用约60重量％氧化铝和40重量％氧化钇的混合物，或40重量％氧化铝、40重量％氧化钇和20重量％氧化镨的混合物时，该溶胶可以含有约20重量％氧化铝和稀土金属氧化物。可使用氧化铝和稀土金属的其他组合，如一种普通技术人员无需过度试验所确定的。
氧化铝和稀土金属溶胶用于浸渍γ-氧化铝纤维增强材料。可用任何适当的纤维制成这种γ-氧化铝纤维增强材料。一种γ-氧化铝纤维源是3M公司(St.Paul，Minnesota)的试验纤维XN-508。这种纤维是1500旦尼尔170涂胶12.3微米预结晶NEXTEL(TM)610粗纱。该复合材料的渗透和烧制条件列在表2中。优选的增强材料是三维正交编织物。
已用几类溶胶制成氧化锆前体，这些溶胶包括水合氯化锆和乙酸锆。可通过载有要求浓度YAG(钇铝石榴石)和氮化铪粉末的氢氧化锆溶胶制备氧化锆前体。YAG可提供烧结成核位点和颗粒间的CTE裂纹平面。氮化铪粉末应具有与碳化铪等离子喷涂材料的化学相容性，该碳化铪等离子喷涂材料用于涂层与本体的化学键合粘结。
进行溶胶混合、凝胶化和烧制，以保证氧化铝和氧化锆产物具有可接受的产率。负载氧化锆前体的起始点是商品氢氧化锆溶液，其中加入10重量％氧化锆、5重量％YAG和25重量％氮化铪粉末。在凝胶化之后，该前体制成湿的短纤维束或小块纤维垫。浸渍的样品应烧制到3300℉(1815℃)，分析产物的总产率、组成和形态。如果必要，修改溶胶配方和热处理变量，以得到耐热冲击性特性。
使用以上详细说明的各个材料体系的方法制造各种陶瓷复合材料板。典型地，生产了12种板，各有两种下面选择的材料类型。每种类型为6种板，它们应有机织增强材料，6种应有非机织增强材料。这些24个样品放在两种试验基体中，以研究最佳的离子喷涂厚度和再浸渍循环的理想次数。标称板尺寸是6英寸×6英寸×半英寸(6”×6”×0.5”)。在加工每个板的过程中应进行最少的两次浸渍和烧制。每种材料类型的至少一个板的样品用于等离子喷涂试验。
表2  机械试验和性能计划
Figure C02827122D00101
通过使用上述方法，并且通过使用类似的材料，可提供了一种陶瓷复合材料，该材料循环到超过1204.4℃(2200℉)温度时具有耐热冲击性。人们知道这样一种陶瓷复合材料的大量用途，本发明所提供材料的实用性将毫无疑问地能够研制出现在没有预测到的或不可预测的新用途。该复合材料中因没有如硅酸盐或氧化钙之类的粘合剂而有另外的抗化学性优点，也将会提供以前未预测到的用途。
该复合材料的一种用途是耐火砖或衬里材料，它们在钢铁和水泥熔渣工业(仅仅列出几种)中有已知多种用途。
由于该复合材料不含有硅酸盐和/或氧化钙，因此该复合材料的抗化学性使其成为一种用于高温化学反应系统的有吸引力的隔热材料，其中包括燃料电池(仅仅为了举例说明的目的)。

Claims (11)

1、一种能重复耐受超过1204.4℃的温度而不会由于热冲击而产生裂纹的陶瓷复合材料，该复合材料是通过一个烧制步骤来制备的，所述复合材料含有：增强纤维网；和由氧化铝溶胶形成的基体，该基体在烧制步骤前浸渍该网，在烧制步骤后，所述的基体基本埋置该网。
2、根据权利要求1所述的陶瓷复合材料，其中：
通过在浸渍溶胶中掺杂至少一种稀土氧化物，该基体还含有至少一种稀土氧化物，以所述氧化铝溶胶中的氧化铝计，所述稀土金属氧化物的量为>0到60重量％。
3、根据权利要求1所述的陶瓷复合材料，其中：
该网是一种增强纤维的三维正交编织物。
4、根据权利要求1所述的陶瓷复合材料，其中：
在烧制前，该网含有一种过渡相氧化铝。
5、根据权利要求4所述的陶瓷复合材料，其中：
该过渡相氧化铝是γ-氧化铝。
6、根据权利要求1所述的陶瓷复合材料，其中：
在烧制后，该增强纤维网占该陶瓷复合材料的10-40重量％。
7、根据权利要求1所述的陶瓷复合材料，其中：
该复合材料是无第I族和第II族金属和过渡金属氧化物的。
8、根据权利要求1所述的陶瓷复合材料，其中：
该增强纤维在浸渍所述网的步骤期间被所述溶胶部分吸收。
9、根据权利要求8所述的陶瓷复合材料，其中：
部分吸收和烧制步骤导致网纤维的微裂纹。
10、一种耐火砖，它含有：
一种根据权利要求1-9中任一项的能重复耐受超过1204.4℃的温度而不会由于热冲击而产生裂纹的陶瓷复合材料，
该陶瓷材料含有增强纤维网和基本埋置该网的氧化铝基体。
11、一种燃料电池的隔热材料，它含有：
一种根据权利要求1-9中任一项的能重复耐受超过1204.4℃的温度而不会由于热冲击而产生裂纹的陶瓷复合材料，该陶瓷材料含有增强纤维网和基本埋置该网的氧化铝基体，以及该陶瓷材料是无第I族和第II族金属和过渡金属氧化物的。
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