CN1288874A - 纤维束增强的陶瓷基质复合材料 - Google Patents
纤维束增强的陶瓷基质复合材料 Download PDFInfo
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- CN1288874A CN1288874A CN00127054A CN00127054A CN1288874A CN 1288874 A CN1288874 A CN 1288874A CN 00127054 A CN00127054 A CN 00127054A CN 00127054 A CN00127054 A CN 00127054A CN 1288874 A CN1288874 A CN 1288874A
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- fibrous bundle
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Abstract
本发明涉及一种新型的纤维束增强的陶瓷基质复合材料以及涉及它们的生产方法和应用。
Description
末发明涉及一种新型的纤维束增强的陶瓷基质复合材料,以及涉及它的生产方法和应用。
用耐高温的纤维和/或纤维束增强的陶瓷基质复合材料已经知道约10年了,并用于许多应用场合,在这些应用场合中,对材料设定了许多极高的要求,例如高的耐热性以及同时具有高强度和高韧性。
纤维和/或纤维束增强的陶瓷基质复合材料下文中简称为CMC复合材料,它们可用于在高温下需要耐热性的各种应用领域,其应用范围不只是取决于复合材料的基质结构。只要复合材料的基质由各种相组成,在CMC复合材料表面上的基质结构可能由于基质相在较低温度下熔融以及受到化学过程例如氧化过程的侵袭造成基质相洗提而遭到破坏,其结果是,目前CMC复合材料的使用期限受到限制。如果CMC复合材料还受到机械磨损,那么这些问题变得更严重。在这个时候,新的基质结晶总会释放出来,它们可能在较低温度下早已受到侵袭,并迅速解体。而且,在基质结构中由洗提掉的结晶产生的空隙提供了产生更高机械侵袭的机会。此外,有裂纹的基质结构也对机械负荷在CMC复合材料表面产生应力起作用,因为在有裂纹的基质情况下,在机械上基质组分更容易从复合材料中抽出。
在机械负荷起重要作用的CMC复合材料的应用领域例如是CMC复合材料用作滑动轴承组件和摩擦衬片,例如制动片和闸衬片。首先,在摩擦衬片领域中,特别是碳纤维增强的碳基质复合材料,即所谓的CFC复合材料已被应用。但是,它们的缺点是材料的耐热性差,这种材料耐氧化侵袭能力不够高。所以,其间努力用更耐氧化的基质来代替这种复合材料的碳基质。在这一方面,特别是使用在更高得多的温度(1500℃)下能耐氧化的SiC基质,它可有另外的表面保护层或没有另外的表面保护层,以致今天特别是使用碳纤维增强的SiC基质复合材料(下文中称为C/SiC复合材料)来生产摩擦衬片,例如制动片和闸衬片。
在此期间,有许多种制造C/SiC复合材料的方法,特别是以使用它们作制动系统组件为目的。因此,在DE 19710105和DE 19711829中公开了制造C/SiC复合材料的方法,其中有至少一碳层或固化的粘合剂层的纤维束与碳质粘合剂混合,后者有另外的填充剂或没有另外的填充剂,然后在混合物被碳化可能被石墨化以前将它们压制和固化,最后用液体硅渗透。
在DE19749462中公开了一种制造C/SiC复合材料的改进方法。在这种情况下,碳纤维的织物制成的预制件首先用树脂渗透,然后固化。如已在其他方法中描述的,然后将这一方法生产的未加工材料碳化,然后用液体硅渗透。
迄今根据上述方法制造的所有C/SiC复合材料都有不均匀的基质结构,在DE19710105和DE19711829的方法的情况下,首先显而易见的是,该基质具有大的裂纹,它使复合材料的单个纤维和/或纤维束之间有通道。这是由碳纤维和生成的SiC基质的明显不同的热膨胀系数引起的,由于这一结果,在硅化的样品冷却过程中,在基质中产生应力,它通过裂纹而减弱(材料周刊(Werkstoffwoche)′98,第Ⅶ卷,第551页)。而且,该基质还有纯碳和/或硅相,所以它没有均匀的基质组成。碳区域在较高的温度负荷下氧化,也就是从复合材料中燃烧掉,而硅区域在大约1400℃下已熔融。所以,迄今还不能用这些方法得到适合在高温下特别是还在机械负荷下经受住永久热负荷的C/SiC复合材料的基质结构。
同样,根据DE19749462的方法制造的C/SiC复合材料也没有均匀的基质。在这一制造方法中,在碳化过程中,在基质中已形成大的裂纹。然后这些裂纹在最后的硅化过程中被液体硅填满,后者与碳基质反应生成SiC。但是,在基质中的碳区域不完全转化成SiC,因此在基质中的裂纹结构仍然存在。
因此,用这些用于制造C/SiC复合材料的传统方法,迄今还不能制造出硅相和碳相部分尽可能小以及尽可能没有裂纹结构或裂纹结构在机械负荷产生应力过程中没有不好影响的C/SiC复合材料。虽然用另外的方法可得到有尽可能小的硅相和碳相部分的C/SiC复合材料。在DE19736560的方法中,将平均粒度至多为2微米的细粒部分和平均粒度为1.5-30微米的粗粒部分的碳化硅粉末与增强纤维混合,然后模化和烧结。因为在这一方法中,生产出有开孔的C/SiC复合材料,它随后用可碳化的材料渗透,然后碳化,通常最后用液体硅渗透并硅化。这一制造方法的确达到改进基质的目的,但与其他方法相比,它的缺点是,甚至在第一次生成SiC基质以后,仍需要用给予碳的材料进一步的渗透步骤和随后的硅化,其结果是已不能用这一方法经济地生产C/SiC复合材料。而且,用这一方法也没有解决裂纹结构问题。
所以,本发明在这一问题的基础上使纤维束增强的陶瓷基质复合材料可得到,与现有技术相比,这种复合材料有改进的基质,尽可能均匀的相组成,以及至多还有细小的裂纹结构,并且这种复合材料可根据迄今已使用的方法来制造。
上述问题用权利要求1和28的表征部分来解决。
本发明的纤维束增强的陶瓷基质复合材料的特征在于,它含有由两种有不同的平均纤维束长度的不同部分组成的纤维束,这两种纤维束部分在相对于纤维束长度的复合材料的纤维束重量的总纤维束分布中用纤维束分布的最小值来区分开。
一方面,CMC复合材料含有这样一纤维束部分,它比另一纤维束部分至少有大得多的平均纤维束长度。
本发明的复合材料有纤维束、也就是单根纤维形成的束作为基质的主要增强组分。另一方面,各单根纤维在复合材料中至多以这样的程度存在,以致它们单根并不对显著增强复合材料作出贡献。
在本发明的复合材料中,有更长纤维长度的纤维束部分的纤维束作用相当于在CMC复合材料中纤维束的增强作用和增韧作用,正如CMC复合材料现有技术已知的。所以,这一纤维束部分在下文中称为增强纤维束部分。
但是,至少由于短得多的平均纤维束长度而与增强纤维束部分不同的第二种纤维束部分的作用是令人吃惊的。与增强纤维束部分不同,这一部分不仅有现有技术传统意义中的增强作用。这种有较短平均纤维束长度的纤维束部分在下文称为基质纤维束部分,它还影响CMC复合材料的结构,因为它产生均匀的基质结构,其特点是基质中有较少和较小的裂纹以及基质的不同物质组分的均匀分布,以致与预期的相不同的其他相仅有很少在基质组成中存在。
与增强纤维束部分的长度和其他尺寸相比,由于基质纤维束部分的长度短得多,还可能有更小的纤维束厚度和高度,基质纤维束有可能以很好的方式在增强纤维束的组织中自由排列,特别是可填充在增强纤维束之间的空间。这就使本发明的CMC复合材料的密度增加以及使基质结构变得更加均匀,因为在硅化以前比迄今由现有技术已知的更细小得多的孔系遍及本发明的复合材料的纤维束骨架。此外,几何学上更小的基质纤维束还影响基质中裂纹的形成,因为基质与基质纤维束的连接不会在基质中产生与增强纤维束连接相同的应力。在这两种情况下,基质和纤维束之间的确有不同的热膨胀系数,但是在基质纤维束的情况下,由于纤维束/基质体系的温度变化,在基质纤维束中也产生应力,而在大的刚性增强纤维束的情况下,不产生这种应力。因此,通过加入基质纤维束减少了基质中的应力的数量,其结果是,本发明的CMC复合材料的基质有更少和更小裂纹的裂纹体系。这一效果由这一事实而增强,当基质与纤维束反应时,特别是有较小尺寸的基质纤维束受侵袭时,其结果它们失去一些物质,以致剩余的较少的物质可容纳由纤维束和基质的不同热膨胀产生的更高程度的应力。
此外,本发明还涉及制造纤维束增强的陶瓷基质复合材料的方法,其中两种有不同平均纤维束长度的不同纤维束部分-增强纤维束部分和基质纤维束部分-在制造方法中用作基础材料,以及这两种纤维束部分通过在该制造方法中使用的复合材料的纤维束重量相对于纤维束长度的总纤维束分布中基质纤维束部分和增强纤维束部分的平均纤维束长度之间纤维束分布的最小值来区分开。
本发明的特征在于,迄今已知的制造CMC复合材料的方法都可用制造本发明的复合材料,如上所述如果在复合材料的制造过程中用增强纤维束部分和基质纤维束部分代替单一的纤维和纤维束部分的话。用这一方法,仅由于改变了原料就能制造本发明的CMC复合材料,除非迄今现有的制造方法的其他已知优点不存在了。
本发明的CMC复合材料含有的纤维束或用于本发明制造CMC复合材料的方法的纤维束最好有保护层,以便防止它们在与基质体系反应过程中受到太强烈的侵袭,以致它们不会丧失它们的增强性能。结合在本发明的CMC复合材料中的纤维束的另一改进的保护作用可用几种可能不同的相互重叠的保护层来达到。优选使用的保护层由碳、石墨、热解碳、TiC、TiN、SiC、二硼化钛、二硼化锆、二硼化铪、基于Si、B、C、N的化合物及其组合物组成。另外的纤维束保护作用可通过在制造过程中用至少一层可热解的粘合剂涂覆所用的纤维束然后将它固化来达到。特别是,用这一方法涂覆的纤维束也可用于本发明的制造方法。在本发明的CMC复合材料的制造过程中将保护层热解。
所有耐高温的纤维,特别是碳纤维、石墨纤维、SiC纤维、氧化铝纤维、Al2O3·SiO2纤维、Al2O3·SiO2-B2O3纤维、碳化型纤维素纤维、木纤维和其他有机纤维以及基于含Si、C、B、N、Al的化合物的极耐高温的纤维都可用来增强本发明的CMC复合材料以及用于本发明的制造方法。同样,毫微纤维、金属须和毫微管也可代替纤维束中所含的纤维用于增强CMC复合材料和用于它们的制造中。
本发明的CMC复合材料的陶瓷基质优选有碳、硅、硼、铝、锆中至少一种物质和/或碳化硅、氮化硅、氧化硅、氮化硼、碳化硼、SiBCN、Al2O3、ZrO2、TiC、硅化铁和其他硅化物中的合金以及玻璃陶瓷的至少一相。特别优选的是,本发明的复合材料有由几乎仅一种上述物质和合金和仅很少数量相邻主相的化合物区域组成的基质。这就意味着,对于作为基质的合金来说,仅有小部分的单个合金组分相在基质中存在。此外,本发明CMC复合材料的陶瓷基质还可含有铁、铬、钛、钼、镍或铝。
今天已用于有大量需求的技术目的的CMC复合材料优选含有碳纤维和石墨纤维,因为它们可按商业规模获得。它们绝大部分由潘恩(PAN)纤维、沥青纤维、中间相沥青、粘胶纤维、酚醛纤维、聚苯纤维和中空纤维热解来制造。所以,本发明的CMC复合材料也优选用碳纤维束或石墨纤维束增强,而碳纤维束和石墨纤维束优选用于本发明的制造方法。
本发明的CMC复合材料显示出作为C/SiC复合材料的特别明显的性质,也就是说,这些复合材料其陶瓷基质基本上含硅、碳和碳化硅相。
制造用于本发明的CMC复合材料的纤维束部分有各种可能方法。一种可能方法是将有保护层或没有保护层的新鲜纤维束在切割单元中切割到预定的长度。在这种情况下,差不多将复合材料中可构成不连续纤维长度的纤维束的长度分布放在一起。在这种情况下以及在其他情况下,有可能构成不同纤维束部分的基质纤维束部分和/或增强纤维束部分。但是,本发明的特征是,两部分的平均纤维束长度彼此明显不同。
制造单个纤维束部分的纤维束的另一方法是,用粉碎和/或研磨过程将已含有制造本发明CMC复合材料所需的纤维束的复合材料转变成一种研磨料,然后研磨料具有由经破坏的不同长度的复合材料得到纤维束作为组分。然后可用分级的方法,例如筛分将研磨料单个纤维束分成有不同的尺寸的,特别是有不同的纤维束长度单个纤维束部分。然后,可将用这一方法制造的有不同长度分布的纤维束部分用作制造本发明的复合材料的基质纤维束部分和/或增强纤维束部分。研磨料分级以后,特别是筛分以后,单个纤维束部分除了含有规定纤维束长度的纤维束以外还含有过长的纤维束部分,也就是说该纤维束的纤维束长度比所希望部分的要长得多,因为这些有合适截面的纤维束在一定程度甚至例如可纵向穿过筛孔。因为这些过长的纤维束对制造本发明的CMC复合材料没有任何明显的影响,所以在本发明的制造方法中可将它们加入。因此,本发明的CMC复合材料的纤维束分布除基质纤维束部分和增强纤维束部分外还有较少部分过长的纤维束。
本发明的CMC复合材料本身的特点是与现有技术的CMC复合材料不同的复合材料中所含的纤维束的几何尺寸分布的特殊选择。同样,本发明的制造方法按那样的方式改进了CMC复合材料的制造,以致用于该方法的纤维束的几何尺寸分布经过选择。
这些经选择的分布在下文中和在权利要求书中用所谓的纤维束分布来描述。在下文中,通过它了解相对于纤维束长度的纤维束重量分布,也就是说,可从这一分布中得出,某纤维束长度的纤维束重量分别有某纤维束长度的纤维束相对纤维束总重的重量分数。
本发明的CMC复合材料的纤维束分布以及有关的制造方法,简言之本发明的纤维束分布特别是有以下特点:
增强纤维束部分的平均纤维束长度通常为4-20毫米、优选5-16毫米、特别优选6-12毫米。增强纤维束部分的纤维束长度分布的最大半宽通常为0.01-15毫米、优选0.1-12毫米、特别优选1-8毫米。
基质纤维束部分的平均纤维束长度通常为0.2-5毫米、优选0.5-4毫米、特别优选1-3.5毫米。基质纤维束部分的纤维束长度分布的最大半宽通常为0.01-5毫米、优选0.1-4毫米、特别优选1-3.5毫米。
增强纤维束部分的平均纤维束宽度通常为0.02-5毫米、优选0.1-3毫米、特别优选0.5-2毫米。增强纤维束部分的纤维束宽度分布的最大半宽通常为0.05-10毫米、优选0.1-7毫米、特别优选0.5-3毫米。
基质纤维束部分的平均纤维束宽度通常为0.02-2毫米、优选0.1-1毫米、特别优选0.3-0.7毫米。基质纤维束部分的纤维束宽度分布的最大半宽通常为0.05-3毫米、优选0.1-2毫米、特别优选0.5-1.5毫米。
增强纤维束部分的平均纤维束长度与基质纤维束部分的平均纤维束长度的比通常为1.5-10、优选1.8-7、特别优选2.1-5。
增强纤维束部分的平均纤维束长度与平均纤维束宽度的比通常为2-500、优选3-100、特别优选4-20。
基质纤维束部分的平均纤维束长度与平均纤维束宽度的比通常为2-500、优选3-100、特别优选4-20。
常用它来描述纤维束的几何尺寸的另一数量是纤维束的长度/宽度/高度比(L/W/H比),其中考虑了纤维束的三个几何尺寸:纤维束的长度、纤维束的宽度和纤维束的高度。在这里纤维束长度首先用纤维束宽度除,然后用纤维束高度除。
对于本发明的纤维束分布来说,以下的描述可构成这一纤维束分布。增强纤维束部分的平均长度/宽度/高度比通常为2-50000、优选5-2000、特别优选10-100,而基质纤维束部分的平均长度/宽度/高度比通常为2-50000、优选10-5000、特别优选30-500。
而且,本发明的纤维束分布的特征在于,基质纤维束部分的重量与纤维束总重的比通常为0.1-0.8、优选0.2-0.5、特别优选0.27-0.33。
本发明制造CMC复合材料的制造方法其中包括所有现有技术已知用于制造CMC复合材料的方法,就用于制造的纤维束说来,它具有本发明的纤维束分布。
优选的制造方法的变通方案包括以下的,例如在DE19749462中公开的方法,第一步将两种不同的纤维束部分混合,然后压制,随后用聚合物,特别是可热解的聚合物浸透用这一方法制造的模制材料体。在这个时候,另外的填充剂也可与聚合物一起浸透。
但是,在本发明大部分制造方法中,在混合过程中将两种不同的纤维束部分加到制造复合材料的其他组分中。在混合过程中优选将两种不同的纤维束部分与至少一种可碳化的粘合剂混合。可加入另外的材料作为填充剂,特别是碳颗粒、炭黑、焦炭、石墨、硅、碳化物、氮化物、硅化铁和其他硅化物以及硼化物。此外,在混合过程中,还可加入其他粘合剂,例如聚乙烯醇、甲基纤维素、乙基纤维素和丁基纤维素粘合剂。
在可碳化的粘合剂中,优选使用树脂类和沥青类粘合剂。在树脂类中,特别使用热塑性树脂、酚醛树脂、呋喃树脂、聚丙烯酸酯树脂、聚亚酰胺树脂、氰酸酯树脂和环氧树脂。特别使用固体和液体沥青、中间相沥青、煤焦油沥青和石油沥青作为沥青树脂。但是,也可使用聚硅烷、聚碳硅烷、聚硅氮烷、单糖化物和多糖化物、聚烯丙基碳化亚二胺、油和焦油作为可碳化粘合剂。
加入混合过程的纤维束的重量百分数通常为混合物总重的50-99%、优选60-90%、特别优选65-80%。
加入混合过程的增强纤维束的重量百分数通常为混合物总重的20-80%、优选35-65%、特别优选42-55%。
加入混合过程的基质纤维束的重量百分数通常为混合物总重的10-40%、优选15-35%、特别优选20-30%。
由混合步骤得到的混合物大多数随后被压制。这一压制优选在模冲压机、各向均压机、连续铸压机、活塞压机或挤塑机例如双螺杆挤塑机中进行。此时,有压实过程知识的专业人员这样调节作用在混合物上的压力,以致在制造方法结束时,他可得到本发明的CMC复合材料。这一混合物的压制优选在升温下进行,如果树脂作为粘合剂在混合物中存在,特别优选在树脂粘合剂的固化温度以上的温度下进行。但是,也可使压制模制的材料体随后仅进行回火过程处理。因此,用树脂作为粘合剂时,也可将压制后的模制材料体在树脂粘合剂的固化温度以上进行回火过程,以便通过它使模制材料体固化。
就本发明制造CMC复合材料的制造方法来说,其基质含有碳和/或碳化物,例如C/SiC复合材料,粘合剂大多数在进一步的工艺步骤中碳化。
此外,本发明的制造方法还可包括以下工艺步骤,其中可碳化的物质通过一次或几次CVI过程或浸渍到要制造的复合材料产生孔系中,随后将制造的复合材料进行碳化步骤。如果要制造基质含有碳和/或碳化物的CMC复合材料或者在制造过程中要压制的话,优选使用这些工艺步骤。
上述复合材料的碳化步骤后可接着使经碳化的固化产物在2000℃以上的温度下石墨化作为下一工艺步骤。
本发明制造其基质还含有硅和/或硅化物的CMC复合材料,例如C/SiC复合材料的制造方法优选包括这样一最后的工艺步骤,在这一工艺步骤中进行硅化。这最后的硅化可通过以下方法进行:液体硅或选自铁、铬、钛、钼、镍和铝的硅化物的硅合金浸渍,或硅、碳化硅或其他硅化合物的CVI沉积。
本发明制造SiC基质复合材料例如C/SiC复合材料的制造方法的另一实施方案为DE19736560中公开的方法,但是使用的纤维束部分有本发明的纤维束分布。
在这些制造方法中,纤维束首先与碳粉末和/或碳化硅粉末和/或二硅化钼粉末和/或碳化硼粉末和/或氮化硼粉末和/或氮化铝粉末和/或碳化钛粉末混合。而且,也可将溶剂加到混合物中。混合以后,然后按上述工艺步骤将混合物压制。压制后将形成的模制的材料体烧结,然后用可碳化的物质浸渍,并碳化。最后,在这里也可进行上述的硅化步骤。
本发明的CMC复合材料特别适用于有大的温度应力的场合,也就是说,例如用作燃气涡轮机的部件,例如涡轮机叶轮、涡轮部件、喷嘴及其部件、热燃气管、测量探针、探针套管;航天器和飞机发动机的热保护组件;热屏蔽板;镜、天线和反射板的承载组件;火箭组件;炉条和换热器组件。但是,本发明的CMC复合材料的优选应用范围是机械负荷还加在大的温度应力的那些应用场合。这样的应用的例子是摩擦材料,例如轨道车辆和汽车的制动片和闸衬片以及滑动轴承组件和滑动元件。
附图
图1作为例子表示本发明CMC复合材料的总纤维束分布1。在这里,给出基质纤维束部分的纤维束分布2和增强纤维束部分的纤维束分布3之间的差别,由纤维束分布2和3的总和得到总纤维束分布。可以清楚地看出,基质纤维束部分的平均纤维束长度4与增强纤维束部分的平均纤维束长度5明显不同,其结果总的纤维束分布1在平均纤维束长度4和5之间有最小值6。此外,单个纤维束部分的纤维束分布尤其是可用基质纤维束部分7和增强纤维束部分8的单个纤维束分布的最大半宽来表征。
图2表示本发明的另一CMC复合材料的总纤维束分布1。这一纤维束分布本身的特点在于,基质纤维束部分的纤维束分布2与增强纤维束部分的纤维束分布3同样分别有很小的最大半宽7和8。由此结果得到,在总的纤维束分布1中出现一间隙9。例如,如果在CMC复合材料制造方法中使用的纤维束为切割成预定长度的两种纤维束部分,那么这里所示的纤维束分布就存在。
图3表示一种筛分部分的总纤维束分布10,例如如果含有碳纤维束的复合材料被研磨,并在筛板中将研磨料分离成单个筛分部分,结果就是这样。在筛分过程中,通过筛子不仅得到打算用作这一纤维部分有纤维束分布11的纤维束,而且还有可能某一部分很长的纤维束纵向通过筛孔,只要该纤维束的截面能通过。由此,在每一筛分部分中都有一部分过长的纤维束,它的分布12在图3中在实际筛分部分的分布11上表示。分布11和12加起来得到筛分部长的总纤维束分布10。但是,筛分部分的最大半宽13不受过长纤维束部分的影响。
图4表示本发明另一CMC复合材料的总纤维束分布1。在这一实施例中,复合材料的纤维束由若干单个筛分部分组成。基质纤维束部分由一个筛分部分组成,其纤维束分布2也有额外的过长纤维束部分16。在这一实施例中,增强的纤维束部分由两个筛分部分组成,它们的纤维束分布14和14′分别在图4中表示。由此,在单个筛分部分的平均值15和15′之间,总的纤维束分布1在增强纤维束部分的范围内有小的最小值19。但是,这要比基质纤维束部分和增强纤维束部分之间的总纤维束分布的最小值6差得多。由于两种筛分部分的增强纤维束部分的组合,增强纤维束的纤维束分布比基质纤维束分布的最大半宽7有大得多的最大半宽8。此外,在这一分布中,另一特征是,单个筛分部分的过长纤维束部分,也就是说基质纤维束的过长纤维束部分16与增强纤维束的单个筛分部分的过长纤维束部分17和17′加起来得到复合材料中过长纤维束的总纤维束分布18。
图5图示现有技术的CMC复合材料的结构,例如它可在显微照片中观测到。首先,表示在复合材料中的纤维束20、20′、20″和20_,在这一实施例中为了简化,它们按一个方向排列,但是一般来说它们也可彼此有其他位置。此外,这一区域的其余部分表示复合材料的陶瓷基质24。这一基质有通过它的宽的裂纹,例如22、22′、22″、22_和22″″,它有从一纤维束到另一纤维束的通道,这些裂纹大多数是在复合材料制造以后的冷却过程中产生的,但它们也可由材料上大的热应力产生。正如上面已解释的,产生裂纹的原因是纤维束和基质不同的热膨胀性质,在热负荷的情况下,它在基质中产生应力,然后通过产生裂纹将这一应力释放。
图6图示表示本发明的CMC复合材料对应于图5的结构,例如它可在显微照片中观测到。与图5中的实施例相比,可以看出,一部分增强纤维束20、20′已被更短的、大多数还更薄的基质纤维束21、21′、22″、22_、22″″代替。尽管增强纤维束按一个方向排列,但更短的基质纤维束可在增强纤维束之间按任何方向排列。发现另一主要差别是,本发明的CMC复合材料的基质24有完全不同的裂纹结构。在基质中仅找到较少的小得多的裂纹21、21′、21″、21_、21″″,如与图5表示的现有技术的相应CMC复合材料的结构有的裂纹相比。而且,例如裂纹23、23″″未显示出象在图5的结构中显示的在增强纤维束之间那样均匀排列。此外,还可观测到一部分裂纹例如裂纹23″″没有从一纤维束到另一纤维束的通道,而由纤维束产生的裂纹例如21″″在基质中终止。正如上面已讨论的,因为这种裂纹结构形成,在本发明的CMC复合材料上有热负荷的情况下,由纤维束和基质的不同热膨胀性质产生的应力不仅在基质本身中出现,而且也在基质纤维束中出现。此外,在基质体系中贮存的较低应力能导致只能一部分贮存的能量通过裂纹来减少。为此,通常还减小了裂纹的尺寸和裂纹在基质本身中终止。
实施例
在下文中,本发明的CMC复合材料和与它们有关的改进可以C/SiC复合材料作例证来表示。在这方面,C/SiC复合材料仅仅是本发明的CMC复合材料的一个例子。根据上述说明,用其他CMC复合材料也可观测到类似的结果。
在这些实施例中,按照公布的专利申请书DE19710105中公开的方法,在增强纤维束部分和基质纤维束部分基础上制造的本发明C/SiC复合材料将与相应的但仅有一种纤维束部分的C/SiC复合材料比较。
实施例的样品含有以下纤维束组分:
表1:实施例的纤维束部分的组成
基质纤维束部分 | 增强纤维束部分 | |||
样品号 | 纤维束重量[%] | 平均纤维束长度[毫米] | 纤维束重量[%] | 平均纤维束长度[毫米] |
1 | 0 | - | 100 | 18±2.7 |
2 | 0 | - | 100 | 15±2.55 |
3 | 0 | - | 100 | 11±2.5 |
4 | 20 | 3±1.5 | 80 | 16±2.6 |
5 | 20 | 3±1.5 | 80 | 15±2.55 |
6 | 20 | 3±1.5 | 80 | 11±2.5 |
7 | 30 | 3±1.5 | 121840 | 15±2.5511±2.58±2.5 |
在这些样品中使用的纤维束部分在这里有以下纤维束厚度:
表2:实施例的单个纤维束部分的尺寸
平均纤维束长度[毫米] | 平均纤维束厚度[毫米] |
3±1.5 | 0.5±0.4 |
8±2.5 | 1.46±0.7 |
11±2.5 | 1.46±0.75 |
15±2.55 | 1.46±0.8 |
16±2.6 | 10±1.5 |
18±2.7 | 15±2.5 |
实施例的所有7个样品制造如下:
首先由3K碳纤维束(3000单长丝)制造预浸渍体,所以所用的碳纤维在PAN纤维的基础上制造。为此,将纤维束交织成斜纹织物,随后将该织物在酚醛树脂(可溶酚醛树脂型)中饱和,然后在两侧贴上隔离纸。此后,将树脂浸渍的织物加热到130℃,以便形成一定厚度的预浸渍体。
随后,将预浸渍体板放在其他预浸渍体板上面,并压制成压制品。然后将它在900℃下烘烤,在400-600℃范围的加热曲线的斜率为5℃/分。然后将用这一方法制得的CFC材料体首先用软化点为60℃的煤焦油沥青连续浸渍3次,然后再在900℃下烘烤,以便使它进一步致密。
然后将用这一方法制得的CFC材料体首先在颚式破碎机(制造商:Alpine Hosokawa)中破碎,然后在切削碎机(制造商:Alpine Hosokawa)中切成纤维束。最后将纤维束在手摇筛选设备(制造商:Allgaier)中分级成单个纤维束部分,此时,按照ISO 9044,筛底(筛面积1.15米2)有0.5毫米、1毫米、2毫米、3毫米、4毫米和6毫米的畅通筛孔。由于这一筛分程序的结果,制得上述纤维束部分,此时在每一情况下±符号后面的数值表示单一部分的最大半宽,它是由单个纤维束部分的纤维束重量相对于纤维束长度和纤维束宽度的纤维束分布推测出来的。
此后,每一样品在Z型桨叶捏合机(制造商:Werner & Pfleiderer)中生产由70%上述组成的纤维束总重、21%酚醛树脂(可溶酚醛树脂型)总重作为粘合剂和9%煤焦油沥青总重(软化点:230℃)组成的混合物。随后,将混合物在冲模压机中、在比压12千帕/厘米2和温度130℃下压制。接着样品在900℃下在惰性气体中碳化和在2000℃下石墨化24小时。最后,在1700℃和在真空中用液体硅渗透,提供样品重量1.5倍的硅,其结果产生样品基质的SiC结构。
当在光学显微镜中观测上述样品的抛光部分时,可清楚地看出样品基质的差别,这取决于它们是否含有基质纤维束部分。观测到的结构对应于图5和6中的图示。虽然仅含有增强纤维束部分的样品在基质中有相当大数量的大裂纹,这些裂纹具有从纤维束到纤维束的通道,但本发明的C/SiC样品的结构仅有较少数量的细裂纹,此时部分从基质纤织束开始的裂纹在基质中终止。
借助在表3中给出的样品密度还可看出本发明的C/SiC样品有不同的和更大的密度。
而且,在表3中给出样品所含的单个硅相、碳相和SiC相的相重量百分数。可以看出,在本发明的C/SiC样品中硅相和碳相的百分数明显下降,它是使用这些材料得到明显改进的可能性。由此认为,大部分碳部分由碳纤维束产生。这样的材料特别适用于有机械负荷的应用场合,例如摩擦衬片。用这样的材料已得到很好的结果,尤其是用作制动片。
表3:样品的密度和重量百分组成
样品号 | 密度[克/厘米3] | SiC重量百分数[%] | Si重量百分数[%] | C重量百分数[%] |
1 | 2.10 | 31.2 | 24.8 | 44.0 |
2 | 2.01 | 30.0 | 25.0 | 45.0 |
3 | 2.08 | 30.0 | 25.2 | 44.8 |
4 | 2.43 | 51.8 | 16.7 | 31.5 |
5 | 2.41 | 51.2 | 16.5 | 32.3 |
6 | 2.43 | 51.6 | 16.5 | 31.9 |
7 | 58.0 | 11.0 | 31.0 |
Claims (46)
1.一种用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,复合材料含有两种有不同平均纤维束长度(4,5)的不同纤维束部分(20,21)-增强纤维束部分(20)和基质纤维束部分(21),它们在相对于纤维束长度的总纤维束分布(1)中用最小值(6)区分开。
2.根据权利要求1的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,在复合材料中所含的至少一部分纤维束(20,21)至少部分有至少一层保护层。
3.根据权利要求1或2的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,纤维束(20,21)中的纤维为选自碳纤维、石墨纤维、SiC纤维、氧化铝纤维、Al2O3SiO2纤维、Al2O3SiO2B2O3纤维、碳化型纤维素纤维、木纤维和其他有机纤维以及基于含Si、C、B、N、Al的化合物的高度耐温纤维的纤维。
4.根据权利要求1-3中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,在复合材料中所含的毫微纤维、金属须和/或毫微管完全地或部分地代替纤维束(20,21)中所含的纤维。
5.根据权利要求1-4中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,陶瓷基质(24)含有至少一种碳、硅、硼、铝、锆物质和/或选自碳化硅、氮化硅、氧化硅、氮化硼、碳化硼、SiBCN、Al2O3、ZrO2、TiC、硅化铁和其他硅化物的合金以及玻璃陶瓷的相。
6.根据权利要求5的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,陶瓷基质还含有铁、铬、钛、钼、镍或铝。
7.根据权利要求3、5或6中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,复合材料仅含有碳和石墨纤维束。
8.根据权利要求5-7中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,陶瓷基质(24)含有硅、碳和/或碳化硅相。
9.根据权利要求1-8中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,复合材料除含有增强纤维束部分(20)和基质纤维束部分(21)外还含有一部分过长的纤维束。
10.根据权利要求1-9中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)和/或基质纤维束部分(21)由几种有不同平均纤维长度(15,15’)的纤维束部分(14,14’)组成。
11.根据权利要求1-10中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的平均纤维束长度(5)为4-20毫米、优选5-16毫米、特别优选6-12毫米。
12.根据权利要求1-11中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的平均纤维束长度(4)为0.2-5毫米、优选0.5-4毫米、特别优选1-3.5毫米。
13.根据权利要求1-12中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的平均纤维束宽度为0.02-5毫米、优选0.1-3毫米、特别优选0.5-2毫米。
14.根据权利要求1-13中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的平均纤维束宽度为0.02-2毫米、优选0.1-1毫米、特别优选0.3-0.7毫米
15.根据权利要求1-14中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的平均纤维束长度(5)与基质纤维束部分(21)的平均纤维束长度(4)的比为1.5-10、优选1.8-7、特别优选2.1-5。
16.根据权利要求1-15中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的平均纤维束长度(5)与增强纤维束部分(20)的平均纤维束宽度的比为2-500、优选3-100、特别优选4-20。
17.根据权利要求1-16中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的平均纤维束长度(4)与基质纤维束部分(21)的平均纤维束宽度的比为2-500、优选3-100、特别优选4-20。
18.根据权利要求1-17中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的平均长度/宽度/高度比为2-50000、优选5-2000、特别优选10-100。
19.根据权利要求1-18中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的平均长度/宽度/高度比为2-50000、优选10-5000、特别优选30-500。
20.根据权利要求1-19中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的重量与所有纤维束总重的比为0.1-0.8、优选0.2-0.5、特别优选0.27-0.33。
21.根据权利要求1-20中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,增强纤维束部分(20)的纤维束长度分布(3)的最大半宽(8)为0.01-15毫米、优选0.1-12毫米、特别优选1-8毫米。
22.根据权利要求1-21中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料,其特征在于,基质纤维束部分(21)的纤维束长度分布(2)的最大半宽(7)为0.01-5毫米、优选0.1-4毫米、特别优选1-3.5毫米。
23.一种制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,两种有不同平均纤维束长度(4,5)的不同纤维束部分(20,21)-增强纤维束部分(20)和基质纤维束部分(21)在制造方法中用作基础材料,以致相对于用于复合材料的纤维束(20,21)的纤维束长度的总纤维束分布(1)有一最小值(6),它在增强纤维束部分(20)和基质纤维束部分(21)的平均纤维束长度(4,5)之间。
24.根据权利要求23的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在第一步中,将两种不同的纤维束部分(20,21)混合和随后压制,此后将用这一方法制造的模制材料体用聚合物、特别是可热解的聚合物渗透。
25.根据权利要求24的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,除了聚合物外,还用其他填充剂渗透。
26.根据权利要求23的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在混合过程中,将两种不同的纤维束部分(20,21)加到用于制造复合材料的其他组分中。
27.根据权利要求23-26中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,至少一部分纤维束(20,21)至少一部分有至少一层保护层。
28.根据权利要求23-27中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,仅碳和石墨纤维束用于制造中。
29.根据权利要求26-28中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在混合过程中,将两种不同的纤维束部分(20,21)与至少一种可碳化的粘合剂混合。
30.根据权利要求29的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,选自树脂和沥青的粘合剂用作可碳化的粘合剂。
31.根据权利要求26-30中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,将混合物在混合以后压制。
32.根据权利要求31的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在升温下进行压制。
33.根据权利要求31或32的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在压制以后,将模制的材料体在混合物中树脂粘合剂的固化温度以上的温度下进行回火过程。
34.根据权利要求29-33中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,粘合剂在另一工艺步骤中碳化。
35.根据权利要求23-34中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,该方法包括在2000℃以上的温度下石墨化作为另一工艺步骤。
36.根据权利要求23-35中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,在最后一工艺步骤中进行硅化。
37.根据权利要求23-36中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的增强纤维束部分(20)的平均纤维束长度(5)为4-20毫米、优选5-16毫米、特别优选6-12毫米。
38.根据权利要求23-37中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的基质纤维束部分(21)的平均纤维束长度(4)为0.2-5毫米、优选0.5-4毫米、特别优选1-3.5毫米。
39.根据权利要求23-38中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的增强纤维束部分(20)的平均纤维束长度(5)与使用的基质纤维束部分(21)的平均纤维束长度(4)的比为1.5-10、优选1.8-7、特别优选2.1-5。
40.根据权利要求23-39中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的增强纤维束部分(20)的平均长度/宽度/高度比为2-50000、优选5-2000、特别优选10-100。
41.根据权利要求23-40中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的基质纤维束部分(21)的平均长度/宽度/高度比为2-50000、优选10-5000、特别优选30-500。
42.根据权利要求23-41中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,送入混合过程的两种纤维束部分的纤维束(20,21)的重量百分数为混合物总重的50-99%、优选60-90%、特别优选65-80%。
43.根据权利要求23-42中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,送入混合过程的增强纤维束部分(20)的纤维束重量百分数为混合物总重的20-80%、优选35-65%、特别优选42-55%。
44.根据权利要求23-43中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,送入混合过程的基质纤维束部分(21)的纤维束重量百分数为混合物总重的10-40%、优选15-35%、特别优选20-30%。
45.根据权利要求23-44中至少一项的制造用纤维束(20,21)增强的陶瓷基质(24)复合材料的方法,其特征在于,使用的基质纤维束部分(21)的重量与使用的所有纤维束重量的比为0.1-0.8、优选0.2-0.5、特别优选0.27-0.33。
46.根据权利要求1-22中至少一项的用纤维束(20,21)增强的陶瓷基质(24)复合材料作为燃气涡轮机的部件,例如涡轮机叶轮、燃烧器的部件、喷嘴及其部件、热燃气管、测量探针、探针套管;摩擦材料,例如飞机、轨道车辆和汽车的制动片和闸衬片;热屏蔽板;空间运载器和飞机发动机的部件;滑动轴承和滑动元件的部件;镜、天线和反射板的承载组件;火箭部件;炉条和换热器部件。
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Also Published As
Publication number | Publication date |
---|---|
EP1084997B1 (de) | 2011-11-09 |
ATE532759T1 (de) | 2011-11-15 |
HU0003650D0 (en) | 2000-09-14 |
PL342559A1 (en) | 2001-03-26 |
EP1084997A3 (de) | 2001-10-10 |
EP1084997A2 (de) | 2001-03-21 |
HUP0003650A3 (en) | 2002-08-28 |
JP4653294B2 (ja) | 2011-03-16 |
US6838162B1 (en) | 2005-01-04 |
KR20010050469A (ko) | 2001-06-15 |
DE19944345A1 (de) | 2001-03-22 |
JP2001089255A (ja) | 2001-04-03 |
SK13392000A3 (sk) | 2001-04-09 |
HUP0003650A2 (hu) | 2001-12-28 |
CA2319702A1 (en) | 2001-03-16 |
CZ20003344A3 (cs) | 2001-11-14 |
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