CN106396713A - 改进cmc材料中的纤维间隔的均匀性 - Google Patents
改进cmc材料中的纤维间隔的均匀性 Download PDFInfo
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- CN106396713A CN106396713A CN201610613863.5A CN201610613863A CN106396713A CN 106396713 A CN106396713 A CN 106396713A CN 201610613863 A CN201610613863 A CN 201610613863A CN 106396713 A CN106396713 A CN 106396713A
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Abstract
提供一种预浸渍复合带(20),包括:基质材料(22);多个纤维(16),其形成封闭在基质材料(22)内的成单向阵列的丝束;以及散布在带(20)中的相邻纤维(16)之间的多个填料颗粒(24)。纤维(16)具有大约5微米至大约40微米的平均纤维直径,并且以大约15%至大约40%的体积分量包括在带(20)内。多个填料颗粒(24)具有对数正态体积中值颗粒大小,使得带(20)具有的对数正态体积中值颗粒大小与平均纤维直径的比为大约0.05:1至大约1:1。还提供一种用于形成陶瓷基质复合物的方法。
Description
技术领域
大体上,本发明涉及新颖处理技术和浆料改良,其结合了小直径纤维,关于它们的间隔,均匀性得到改进。
背景技术
为了提高燃气涡轮的效率,不断探索其更高的运行温度。虽然已经通过制定铁、镍和钴基超合金来显著地提高了高温能力,但已经调查研究了备选材料。CMC材料是著名的示例,因为它们的高温能力可显著地降低冷却空气要求。CMC材料大体包括嵌在陶瓷基质材料中的陶瓷纤维加强材料。加强材料可为分散在基质材料中的不连续的短纤维或者定向在基质材料内的连续纤维或纤维束,并且在基质有裂纹的情况下用作CMC的承载负载的成分。进而,陶瓷基质保护加强材料,保持其纤维的定向,并且用来使负载扩散到加强材料。作为基质和/或加强材料的硅基复合物(诸如碳化硅(SiC))特别受到高温应用的关注,例如,燃气涡轮的高温构件,包括飞机燃气涡轮发动机和在功率生产行业中使用的陆基燃气涡轮发动机。
CMC材料以及特别是SiC/Si-SiC(纤维/基质)连续纤维加强式陶瓷复合物(CFCC)材料和过程的示例在下者中公开:US专利No.5,015,540、No.5,330,854、No.5,336,350、No.5,628,938、No.6,024,898、No.6,258,737、No.6,403,158和No.6,503,441,以及美国专利申请公布No. 2004/0067316。这样的过程一般需要使用多个预浸层来制造CMC,各个预浸层都呈“带”的形式,其包括期望陶瓷纤维加强材料、由CMC基质材料制成的一个或多个前体和粘合剂。根据传统实践,可通过用包含陶瓷前体和粘合剂的浆料浸渍加强材料来形成预浸带。前体的优选材料将取决于对于CMC构件的陶瓷基质而言理想的特定成分,例如,SiC粉末和/或一个或多个含碳材料,如果期望基质材料为通过熔体浸渗路线处理的SiC的话。著名的含碳材料包括碳精、酚醛树脂和呋喃树脂,包括糠醇(C4H3OCH2OH)。其它典型的浆料成份包括可提高预浸带的柔韧性的粘合剂(例如,聚乙烯醇缩丁醛(PVB)),以及用于粘合剂的溶剂(例如,异丙醇、甲苯和/或甲基异丁基酮(MIBK)),该溶剂提高浆料的流动性,以使得能够浸渍纤维加强材料。浆料可进一步包含意于存在于CMC构件的陶瓷基质中的一种或多种微粒填料,例如,在Si-SiC基质的情况下的SiC粉末。
在允许浆料部分地变干之后,并且如果合适的话,部分地使粘合剂凝固(B型分级),用其它带铺设在所产生的预浸带上,并且然后压实它,而且如果合适的话,在使其经受升高的压力和温度时凝固,以产生预制坯。然后预制坯在真空或惰性气氛中加热(燃烧),以使粘合剂分解,移除任何剩余溶剂,并且将前体转换成期望的陶瓷基质材料。由于粘合剂分解且进一步失去有机物,所以得到多孔CMC本体,其可经受填密过程,诸如熔体浸渗(MI)、化学气相浸渗(CVI),或者聚合物浸渍和热解(PIP),以填充孔隙率和产生CMC构件。关于以上过程的具体处理技术和参数将取决于材料的特定组成。
在图1中示意性地描绘了CFCC材料的示例包括多个层片12,它们各自源自单独的预浸带,其包括浸渍有陶瓷基质前体的单向对齐的加强材料14。因此,各个层片12包含封闭在陶瓷基质18中的加强材料14,通过使陶瓷基质前体在燃烧和熔体浸渗期间转化来全部或部分地形成陶瓷基质18。
虽然上面描述的类型的过程和材料已经成功地用来生产用于燃气涡轮和其它应用的CMC构件,但仍然需要一种层间强度得到改进的构件,这可通过提高基质中的纤维分布来实现。
发明内容
将在以下描述中部分地阐述本发明的各方面和优点,或者根据该描述,本发明的各方面和优点可为明显的,或者可通过实践本发明来学习本发明的各方面和优点。
大体提供一种预浸渍复合带。在一个实施例中,预浸渍复合带包括:基质材料;多个纤维,其形成封闭在基质材料内的成单向阵列的丝束;以及散布在带中的相邻纤维之间的多个填料颗粒。纤维具有大约5微米至大约40微米的平均纤维直径,并且以大约15%至大约40%的体积分量包括在带内。多个填料颗粒具有中值颗粒大小,使得带具有的中值颗粒大小与平均纤维直径的比为大约0.05:1至大约1:1。
还大体提供一种用于形成陶瓷基质复合物的方法。在一个实施例中,方法包括:提供大量纤维,各个纤维具有介于5微米和40微米之间的平均纤维直径;用浆料合成物浸渍大量纤维,浆料合成物包括粘合剂、溶剂和填料粉末;以及使经浸渍的大量纤维形成为单向带。填料粉末渗入大量纤维,使得填料颗粒散布在带中的相邻纤维之间,并且填料颗粒具有中值颗粒大小,中值颗粒大小与平均纤维直径的比为大约0.05:1至大约1:1。然后带形成为成形预制坯,接着通过将预制坯加热到大约400℃或更高的温度来使预制坯热解,以分解有机组分,以及将粘合剂的任何预陶瓷聚合物或形成碳的聚合物组分分别转换成陶瓷或碳。最后,使用化学气相浸渗、聚合物浸渍和热解或熔体浸渗对复合预制坯进行填密。
技术方案1. 一种预浸渍复合带,包括:
基质材料;
多个纤维,其形成封闭在所述基质材料内的成单向阵列的丝束,其中,所述纤维具有大约5微米至大约40微米的平均纤维直径,以及其中,所述多个纤维以大约15%至大约40%的体积分量包括在所述带内;以及
散布在所述带中的相邻纤维之间的多个填料颗粒,其中,所述多个填料颗粒具有中值颗粒大小,以及其中,所述带具有的所述中值颗粒大小与所述平均纤维直径的比为大约0.05:1至大约1:1。
技术方案2. 根据技术方案1所述的带,其特征在于,所述填料粉末的所述中值颗粒大小与所述平均纤维直径的比为大约0.07:1至大约0.7:1。
技术方案3. 根据技术方案1所述的带,其特征在于,所述填料粉末的所述中值颗粒大小与所述纤维直径的比大约0.1:1至大约0.5:1。
技术方案4. 根据技术方案1所述的带,其特征在于,所述填料粉末包括SiC颗粒、碳颗粒、硼颗粒、B4C颗粒、Si3N4颗粒、Mo5Si3颗粒、MoSi2颗粒、硅化物颗粒、氧化物颗粒、聚合物颗粒或者它们的混合物。
技术方案5. 根据技术方案1所述的带,其特征在于,所述填料粉末包括SiC颗粒。
技术方案6. 根据技术方案1所述的带,其特征在于,所述基质材料包括形成陶瓷的粉末。
技术方案7. 根据技术方案1所述的带,其特征在于,所述形成陶瓷的粉末包括多个碳颗粒。
技术方案8. 根据技术方案1所述的带,其特征在于,所述填料颗粒以大约5%至大约40%的体积分量包括在所述带内。
技术方案9. 根据技术方案1所述的带,其特征在于,所述纤维是连续的且捆成丝束,以及其中,所述纤维是包含碳化硅的纤维。
技术方案10. 根据技术方案1所述的带,其特征在于,所述纤维是连续的且布置成单向定向。
技术方案11. 根据技术方案1所述的带,其特征在于,所述纤维是连续的且经过编织。
技术方案12. 一种用于形成陶瓷基质复合物的方法,所述方法包括:
提供大量纤维,各个纤维具有介于5微米和40微米之间的平均纤维直径;
用浆料合成物浸渍所述纤维,所述浆料合成物包括粘合剂、溶剂和填料粉末;
使经浸渍的大量纤维形成为单向带,其中,所述填料粉末渗入所述大量纤维,使得所述填料颗粒散布在所述带中的相邻纤维之间,以及其中,所述填料颗粒具有中值颗粒大小,所述平均颗粒大小与所述平均纤维直径的比为大约0.05:1至大约1:1;
使所述带形成为成形预制坯;
通过将所述预制坯加热到大约400℃或更高来使其热解,以分解有机组分,并且分别将所述粘合剂的任何预陶瓷聚合物或形成碳的聚合物组分转换成陶瓷或碳;以及
使用化学气相浸渗、聚合物浸渍和热解或熔体浸渗来对复合预制坯进行填密。
技术方案13. 根据技术方案12所述的方法,其特征在于,所述填料粉末包括SiC颗粒、碳颗粒、硼颗粒、B4C颗粒、Si3N4颗粒、Mo5Si3颗粒、MoSi2颗粒、硅化物颗粒、氧化物颗粒、聚合物颗粒或者它们的混合物。
技术方案14. 根据技术方案12所述的方法,其特征在于,所述填料粉末包括SiC颗粒。
技术方案15. 根据技术方案12所述的方法,其特征在于,所述填料粉末的所述中值颗粒大小介于所述平均纤维直径的0.07倍和0.7倍之间。
技术方案16. 根据技术方案12所述的方法,其特征在于,所述填料粉末的所述中值颗粒大小介于所述平均纤维直径的0.1倍和0.5倍之间。
技术方案17. 根据技术方案12所述的方法,其特征在于,在期望颗粒大小范围内的填料颗粒在所述带内的体积分量介于5%和40%之间。
技术方案18. 根据技术方案12所述的方法,其特征在于,所述浆料合成物进一步包括形成陶瓷的粉末,其中,所述形成陶瓷的粉末包括多个碳颗粒。
技术方案19. 根据技术方案12所述的方法,其特征在于,所述填料颗粒以大约5%至大约40%的体积分量包括在所述带内。
参照以下描述和所附权利要求,本发明的这些和其它特征、方面和优点将变得更好理解。附图结合在本说明书中且构成说明书的一部分,附图示出本发明的实施例,并且和描述共同用来说明本发明的原理。
附图说明
在说明书中特别指出和明确要求保护了被视为发明的主题。但是,可通过参照结合附图得到的以下描述来最佳地理解本发明,其中:
图1示意性地表示示例性CMC物件的部分横截面图;
图2示意性地表示能够用来形成图1的CMC物件的类型的预浸带的部分横截面图;
图3描绘用来用浆料合成物浸渍纤维丝束的鼓缠绕设备的示意图;
图4是形成有SiC颗粒的CMC面板的横截面的放大50倍的光学图象,SiC颗粒具有0.6 µm的中值大小,如示例中论述的那样;
图5是形成有SiC颗粒的CMC面板的横截面的放大50倍的光学图象,SiC颗粒具有7 µm的中值大小,如示例中论述的那样;
图6A显示示例性CMC物件中的被四个颗粒间隔开的四个纤维的横截面的示意图;
图6B显示示例性CMC物件中的被间隙颗粒间隔开的四个纤维的横截面的示意图;
图7A显示根据示例的中值SiC颗粒大小与纤维邻居间隔的标图;以及
图7B显示中值SiC颗粒大小与标准化平均层间抗拉强度(ILT)的标图。
在本说明书和附图中重复使用参照符号意于表示本发明的相同或相似特征或元件。
具体实施方式
现在将详细参照本发明的实施例,在图中示出实施例的一个或多个示例。以阐明本发明而非限制本发明的方式提供各个示例。实际上,对本领域技术人员显而易见的将是,可在本发明中作出各种修改和变化,而不偏离本发明的范围或精神。例如,被示为或描述成一个实施例的一部分的特征可用于另一个实施例,以产生又一个实施例。因而,意于的是本发明覆盖落在所附权利要求及其等效物的范围内的这样的修改和变化。
将按照用于生产CMC物件(包括CFCC物件)的过程来描述本发明。本发明特别关注的材料是作为加强和/或基质材料的包含硅的那些,诸如包含碳化硅的CMC,其特定示例是碳化硅基质中的连续碳化硅纤维。但是,其它复合物材料也在本发明的范围内,包括陶瓷,诸如氮化硅;硅化物(金属间化物),诸如硅化铌和硅化钼;以及氧化物,诸如氧化铝和二氧化硅。虽然可预见各种应用,但关于可用本发明生产的类型的CMC物品的特定应用包括燃气涡轮发动机的构件,诸如燃烧器衬套、叶片、导叶、护罩和位于燃气涡轮的热气路径内的其它构件。
以下论述将参照图1和2。之前提到图1代表CFCC构件10,但其它类型的CMC材料也在本发明的范围内。作为CFCC材料,构件10优选地能够对高温承载应用提供低重量、高强度和高硬度。CFCC构件10表示为包括多个层片12,它们各自源自单独的预浸带。各个层片12包含陶瓷纤维加强材料14,其封闭在陶瓷基质18中,通过转化陶瓷基质前体来全部或部分地形成陶瓷基质18。如图1和2中描绘的那样,加强材料14为成单向阵列的丝束的形式,它们各自包含连续纤维(细丝)16。作为成单向阵列的丝束的备选方案,加强材料14可只是包括布置成形成单向纤维阵列的纤维16,或者加强材料14可包括编织成形成二维纤维或者编织成或编成形成三维纤维的丝束。适当的纤维直径和丝束直径将取决于特定应用、特定层片12和用其形成的带20的厚度、期望纤维体积分量和其它因素,因此在图1或2中未按比例表示。在一个实施例中,纤维16具有大约5 µm至大约40 µm的平均纤维直径,并且/或者多个纤维16以大约15%至大约40%的体积分量包括在带20内。
大体上,本文描述的材料具有改进的纤维分布均匀性。不希望受任何特定理伦的约束,目前相信这种改进的纤维分布均匀性可改进层间属性,并且更特别的是提高层间强度。
在一个实施例中,预浸渍复合带包括基质材料;多个纤维,它们形成封闭在基质材料内的成单向阵列的丝束;以及分散在带中的相邻纤维之间的多个填料颗粒。例如,图6A和6B显示纤维16,显示了纤维16与相邻纤维16被颗粒24间隔开。
用普通的粉末加工过程(诸如通过磨擦或其它碾磨)生产的陶瓷粉末将典型地具有对数正态型颗粒大小分布,意思就是颗粒在一系列体积内的频率将以类似于正态概率函数的方式随颗粒直径的对数改变。本文所有对“中值颗粒大小”的引用都表示颗粒大小的球直径,使得50体积%的颗粒具有大于中值体积的体积,并且50体积%的颗粒具有小于中值体积的体积。但是,这不要求实际颗粒大小分布紧密地遵循理论对数正态分布,而是实际上可具有任何随机分布。
在一个特定实施例中,带具有的填料颗粒中值颗粒大小与平均纤维直径的比为大约0.05:1至大约1:1(即,填料粉末的中值颗粒大小为平均纤维直径的大约0.05倍至大约等于平均纤维直径)。在特定实施例中,带具有的填料颗粒中值颗粒大小与平均纤维直径的比为大约0.07:1至大约0.7:1(即,填料粉末的中值颗粒大小为平均纤维直径的大约0.07倍至大约0.7倍),诸如大约0.1:1至大约0.5:1(即,填料粉末的中值颗粒大小是平均纤维直径的大约0.1倍至大约0.5倍)。纤维直径和颗粒大小的这个特定组合可改进纤维在带内的分布。
填料颗粒可以大约5%至大约40%的体积分量包括在带内。
参照图6A,显示了纤维16与相邻纤维16被定位在各个纤维16之间的颗粒24间隔开。因而,各个纤维16之间的表面间间隔25由定位在它们之间的颗粒24设定。虽然这个表面间间隔可基本等于颗粒24的中值颗粒大小,但是颗粒具有非圆形形状和某个纵横比。由于在制造过程期间的剪切力,颗粒可与纤维对齐,颗粒的较小尺寸设定表面间间隔。这个较小尺寸不必与颗粒定径过程中测得的尺寸相同。在颗粒大小和间隔之间存在关系,但也许不是1:1,而是可有一些变化,这取决于颗粒的纵横比。在大多数实施例中,各个纤维16之间的表面间间隔与颗粒24的中值颗粒大小的比为大约0.3:1至大约1:1(例如,大约0.3:1至大约0.7:1,诸如大约0.3:1至大约0.5:1)。
备选地,参照图6B,单个颗粒24定位在限定在相邻纤维16之间的空隙空间17内。在这个实施例中,可使用颗粒24来控制相邻纤维16之间的间隔,颗粒24具有设定纤维16之间的填隙间隔27的中值颗粒大小。例如,在一个实施例中,空隙空间17的大小可为颗粒24的中值颗粒大小的大约0.9至大约1.1(即,可基本等于颗粒24的中值颗粒大小)。
适当的纤维材料还将取决于特定应用。例如,包含碳化硅的纤维可包括(但不限于)碳化硅、Si-C-N、 Si-C-O、 Si-C-O-N、 Si-C-O-Ti、 Si-C-O-Zr或者它们的混合物。包含氧化物的纤维可包括(但不限于)Al2O3、SiO2、ZrO2、Y2O3或者它们的混合物。通用电气公司已经开发出了CFCC材料(其名称为HiperComp®)的值得注意但非限制性的示例,并且示例包含在碳化硅和元素硅的基质或硅合金中的连续碳化硅纤维。
在某些实施例中,纤维16在其上可具有至少一个涂层。在特定实施例中,至少一个涂层可具有选自下者组成的组的层:氮化物层(例如,氮化硅层)、碳化物层(例如,碳化硅层)、硼层(例如,氮化硼层,包括掺硅氮化硼层)、碳层和它们的组合。例如,至少一个涂层可淀积成选自下者组成的组的涂层系统:氮化物涂层和碳化硅涂层;氮化硼、碳化物和氮化硅涂层系统;氮化硼、碳化硅、碳化物和氮化硅涂层系统;氮化硼、碳、氮化硅和碳涂层系统;和碳、氮化硼、碳、氮化硅和碳涂层系统;以及它们的混合物。如果存在,涂层厚度可为大约0.1µm至大约4.0 µm。
图2示意性地表示可用来形成图1的各个层片12的类型的预浸带20。因而,带20表示为包含成丝束的陶瓷纤维16的形式的加强材料14,它将用作构件10的加强相。
加强材料14在图2中表示为封闭在固体基质材料22内,除了别的之外,固体基质材料22由将形成构件10的陶瓷基质18的一种或多种粘合剂和一个或多个微粒材料(例如,多个碳颗粒和/或填料颗粒)形成。
可使用任何填密过程来生产CMC构件,诸如熔体浸渗(MI)、化学气相浸渗(CVI)或聚合物浸渍和热解(PIP),这取决于材料的特定组成。虽然以下论述针对的是熔体浸渗过程,但要理解的是,不排除其它填密过程(例如CVI、PIP等,以及它们的组合)。
通过对加强材料14施用浆料合成物,然后部分地使浆料合成物变干以容许操纵带20,而形成基质材料22。 可使用各种技术来对加强材料14施用浆料合成物,例如,通过在将丝束缠绕到鼓上时,直接对连续的丝束绳施用浆料合成物。参照图3,例如,在鼓缠绕设备中在纤维导引件5之间的一些对齐滑轮4上从供应卷轴3中连续地拉出纤维2,将纤维2拉过定量器7(由定量器定位器6保持就位),并且将纤维2拉到回转接收鼓8上。可首先用Teflon®卷绕鼓8,以允许在后面的过程中轻易地移除纤维/基质带。接收鼓8沿着其轴线以受控制的速率平移,使得连续纤维丝束卷之间的间隔得到控制。定量器7是器皿(例如,玻璃管),它容纳基质浆料且具有纤维出口处的大小受控制的孔。而在定量器7中,纤维丝束2是湿的且被基质浆料浸渍。在通过定量器孔离开时,从纤维丝束上刮掉多余的基质浆料,从而控制丝束获得的浆料量。不需要使用定量器来浸渍纤维丝束,而是可通过将丝束拉过浆料浴池来完成。调节接收鼓上的纤维间隔,以提供单层纤维丝束,使得连续的丝束卷彼此触碰。纤维在浆料仍然是湿的时候缠绕到接收鼓上,使得浆料可填满纤维丝束之间的不规则部,并且使得浆料的表面张力将趋向于在缠绕丝束的外表面上变平滑。
在缠绕操作之后,可允许浆料合成物部分地变干,在此之后可从鼓上移除产生的预浸带20,将其与其它带放在一起,然后在升高的压力和温度下压实,而形成预制坯。然后可在真空或隋性气氛中加热预制坯,以使粘合剂分解,并且将陶瓷基质前体转换成CMC构件10的基质18的陶瓷材料。构件10可进一步经历填密过程(例如,MI、CVI或PIP),以填充由于粘合剂在燃烧期间分解而在基质18内产生的气孔。
例如,MI过程包括,在预制坯燃烧且固化之后,用熔融硅浸渗预制坯中的掺合物,掺合物包含大量纤维和碳(和其它化合物,如果存在的话)。在执行本过程中,预制坯接触硅浸渗剂。浸渗手段允许熔融硅浸渗剂浸渗到预制坯中。特别地,熔融硅浸渗剂是运动的且对元素碳的反应性高,以形成碳化硅。还在基质中形成硅相穴。硅相限定为基本包含元素硅,其中诸如硼的其它元素可在硅相中溶解。可按经验确定浸渗所需的周期,并且这主要取决于预制坯的大小和所需浸渗程度。产生的浸渗本体在大气中且以对其无重大有害作用的速率变冷。
CVI过程使用气相前体来使SiC基质在预制坯的气孔空间内淀积。CVI还可用来使其它基质化学物淀积,包括(但不限于)C、Si3N4、SiO2、Al2O3和B4C。
PIP过程使用聚合物前体来浸渗到多孔预制坯中,以产生SiC基质。由于聚合物-陶瓷转化过程的原因,这个方法大体产生低化学计量和低结晶度。另外,在这个转化过程期间还发生收缩,从而产生10-20%的残余孔隙率。可执行多次浸渗来补偿收缩。PIP还可用来产生其它基质化学物,包括(但不限于)C、Si-N-C、Si-O、Si-O-C和Al-O。
现在将参照浆料合成物,它们特别适合形成纤维分布均匀性得到提高的CMC。在一个实施例中,浆料合成物包含粘合剂、溶剂、形成陶瓷的粉末(例如,多个碳颗粒)和多个填料颗粒(例如,多个碳化硅颗粒)。在另一个实施例中,浆料包含粘合剂、溶剂、形成气孔的粉末(例如,多个聚丙烯颗粒)和多个填料颗粒(例如,多个碳化硅颗粒)。
大体上,形成陶瓷的粉末由足够量的碳组成,以与浸渗的Si反应而在产生的CMC中形成SiC。在一个特定实施例中,陶瓷前体单独包括多个碳颗粒,或者除了其它陶瓷粉末(例如,较多的其它包含碳的微粒材料)之外还包括多个碳颗粒。多个碳颗粒在一个特定实施例中具有大约0.01 µm至大约2 µm(例如,大约0.02 µm至大约1 µm)的中值颗粒大小。如本领域中已知的那样,这些碳颗粒(和任何其它包含碳的微粒材料)与浸渗液体Si反应而形成SiC。当具有亚微米的中值颗粒大小时(例如,大约0.1 µm至大约1 µm),碳颗粒能够分布在纤维之间,并且在填密之后形成与纤维混和的SiC基质。
取决于填料颗粒的材料,多个填料颗粒在燃烧过程期间大体不转换或者以别的方式反应。例如,当填料颗粒包括SiC颗粒、B4C颗粒、Si3N4颗粒、MoSi2颗粒、硅化物颗粒、氧化物颗粒或者它们的混合物时,颗粒在燃烧过程期间大体不转换或者以别的方式反应。但是,其它材料可在燃烧过程期间转换,诸如当填料颗粒包括碳颗粒、Mo5Si3颗粒或聚合物颗粒时。在使用聚合物颗粒的实施例中,选择在溶剂系统中不可溶解且在燃尽过程之前仍然存在的聚合物颗粒。
在一个特定实施例中,多个填料颗粒大体包括在燃烧过程期间不转换或以别的方式反应的多个碳化硅颗粒。在特定实施例中,多个碳化硅颗粒具有的中值颗粒大小为大约2µm至大约10 µm (例如,大约3 µm至大约7 µm,诸如大约4 µm至大约5.5 µm),已经发现这将在产生的CMC层中引起较均匀的纤维分布。在一个特定实施例中,填料粉末基本由碳化硅颗粒组成,碳化硅颗粒具有的中值颗粒大小为大约2 µm至大约10 µm (例如,大约3 µm至大约7 µm,诸如大约4 µm至大约5.5 µm),使得在浆料合成物中存在不超过50%的碳化硅颗粒具有超出这种范围的颗粒大小。
不希望受任何特定理论的约束,相信通过渗入丝束和防止纤维在带缠绕期间成团,较粗糙的碳化硅颗粒可改进纤维分布。还发现使用较粗糙的碳化硅颗粒可降低浆料粘度,这可使得在缠绕期间更好地浸渍丝束。
与前面使用亚微米碳化硅颗粒(例如,中值颗粒大小小于1 µm)的过程相比,已经发现纤维分布的均匀性大有改进。另外,发现较大的颗粒(例如,中值颗粒大小大于10 µm)趋向于使纤维间隔伸展得大到使得丝束厚度从本来在使用较小颗粒实现的厚度增大。
形成陶瓷的粉末和填料粉末构成浆料合成物的固体组分,并且优选地占浆料合成物的至少30重量%至大约60重量%,并且优选地占浆料合成物的大约35重量%至大约50重量%。
在一个实施例中,粘合剂是有机粘合剂。用于在浆料合成物中使用的一个示例性粘合剂是聚乙烯醇缩丁醛(PVB),可从Solutia公司获得其商业示例,其名称为BUTVAR®B-79。取决于它们的分子量,适当的PVB粘合剂在高于准备和压实预浸带20所必需的温度且低于用来燃烧预制坯和使陶瓷前体转换成基质18的期望陶瓷材料的温度的温度下分解。有机粘合剂的其它候选物包括其它聚合物材料,诸如聚碳酸酯、多乙酸乙烯酯和聚乙烯醇。对于适当或优选的粘合剂的选择将部分地取决于与浆料成分的其余部分的相容性。在另一个实施例中,粘合剂是预制陶瓷聚合物。
额外的材料还可包括在浆料合成物中,诸如形成碳或陶瓷的树脂(例如,炭生产量高的树脂)、塑化剂,以及粘合剂在其中溶解的溶剂。
作为特定示例,在生产SiC/Si-SiC CMC材料时,可提供和选择炭生产量高的树脂,以由于燃烧过程而形成碳炭,然后碳炭可在熔体浸渗期间与熔融硅或熔融硅合金反应,以形成额外的SiC基质材料。关于以上过程的具体处理技术和参数将取决于材料的特定组成,而且它们在本领域技术人员的能力之内,并且因此这里不再详细论述。在一个实施例中,存在至少一种炭生产量高的树脂,以提高燃尽强度和产生硬且结实的预制坯。用语“炭生产量高的树脂”的意思是指在燃尽之后,树脂分解且留下固体材料,诸如碳、碳化硅和氮化硅。炭生产量高的树脂在燃尽和随后的硅熔体浸渗步骤对预制坯结构提供完整性。炭生产量高的树脂还提高凝固预制坯结构的可操作性和可加工性。适合在浆料合成物中使用的、炭生产量高的示例树脂是形成碳的树脂和形成陶瓷的树脂。形成树脂的碳可包括酚醛塑料、糠醇,源自其中的部分地聚合的树脂、石油沥青和煤焦油沥青。形成树脂的陶瓷包括热解而形成固体相(晶状或无定形)的那些树脂,包含下者中的一个或多个:碳化硅、碳、二氧化硅、氮化硅、碳氧化硅、碳氮化硅、碳化硼、氮化硼,以及金属碳化物,或者其中金属典型地是锆或钛的氮化物。另外的示例是聚碳硅烷、聚硅烷、聚硅氨烷和聚硅氧烷。
在某些实施例中,预浸带可具有重量%或更多的溶剂含量10。备选地,带20可具有限于溶剂含量小于10重量%的溶剂含量,更优选地小于7重量%。为了补偿此实施例中的带20中的有限溶剂量(这通常对于产生柔韧预浸带是必需的),可将浆料合成物配制成使得从中产生的带20将包含能够对带20提供所需柔韧性的足够大量的塑化剂。
可在浆料合成物中使用的合适溶剂包括(但不限于):水基溶剂、水、有机物基溶剂、甲苯、二甲苯、甲乙硐、甲基异丁基甲酮(4-甲基-2-戊酮) 丙酮、乙醇、甲醇、异丙醇、1,1,1-三氯乙烷、四氢呋喃、四氢化糠醇、溶纤剂和本基溶纤剂。
如上面提到的那样,塑化剂可包括在浆料合成物中,以补偿溶剂含量较低的预浸带20,以便提高带20的柔韧。适当的塑化剂是三乙二醇双(2-己酸乙酯),其商业示例可从首诺的名称S-2075获得。塑化剂的其它潜在候选物包括酞酸酯,例如苯二酸二丁或邻苯二甲酸丁苄酯。
在将浆料合成物准备成具有上面提到的组分和量之后,可通过任何适当的过程将合成物施用到加强材料14上。然后允许浆料合成物通过溶剂的部分蒸发而部分地变干,从而产生柔韧预浸带20,柔韧预浸带20包括嵌在基质材料22中的加强材料14,加强材料14基本由下者形成:陶瓷前体、粘合剂、塑化剂和任何微粒填料材料,以及在形成带20的期间未蒸发的溶剂的其余部分。在一个实施例中,带20内的基质材料22包含大约60重量%至大约70重量%的固体粉末组分(包括陶瓷前体和任何额外的微粒材料)、大约10重量%至大约18重量%的粘合剂、大约10重量%至大约14重量%的塑化剂,以及小于10%(更优选地,小于7%)的溶剂。在另一个实施例中,带20内的基质材料22包含大约20重量%至大约40重量%的固体粉末组分(包括陶瓷前体和任何额外的微粒材料)、大约50%至大约75%的粘合剂,以及小于10%(更优选地,小于7%)的溶剂。然后将带20与其它带铺设在一起,并且在升高的压力和温度下压实预浸带叠堆,以形成预制坯。压实温度低于粘合剂和塑化剂的分解温度。在压实(额外的溶剂在此期间蒸发)之后,各个带20优选地包含小于1重量%的溶剂,并且更优选地小于0.1重量%的溶剂。由于溶剂有额外损耗,所以一个实施例中的带20将典型地包含由陶瓷前体和任何额外的微粒材料形成的大约25重量%至大约40重量%的固体粉末组分、大约4重量%至大约8重量%的粘合剂,以及大约4重量%至大约8重量%的塑化剂,其余为加强材料14。
然后可在真空或隋性气氛中将预制坯加热到足以使粘合剂和塑化剂分解的温度,然后加热到足以使基质材料22内的陶瓷前体转换成CMC构件10的基质18的陶瓷材料的燃烧温度。如前面提到的那样,构件10可进一步经历熔体浸渗或另一个填密过程,以填充由于粘合剂在燃烧期间分解而在基质18内产生的任何气孔。
虽然上面按照预浸处理来进行论述,但本发明还可扩展到使用其它过程制成的纤维加强式复合物,包括浆料铸造技术。例如,可根据已知的浆料铸造技术用本发明的浆料合成物浸渍由铺设纤维布形成的预制坯,接着使溶剂部分地蒸发,燃烧,而且如有必要,熔体浸渗。因此,虽然已经按照具体实施例来描述了本发明,但显而易见的是,本领域技术人员可采用其它形式。因此,本发明的范围仅由所附权利要求限制。
然后本复合物由经涂覆的小直径纤维状材料和基质相构成。在一个实施例中,基质相分布在整个经涂覆纤维状材料中,并且大体上它基本填充空间且通过是互连的。大体上,经涂覆纤维状材料完全被基质相包围。基质相包含在碳化硅和硅的原位上形成的相或多个相。纤维状材料构成复合物的至少大约5体积%,或者至少大约10体积%。基质包含复合物的大约5体积%至95体积%的量的碳化硅相,或者大约10体积%至80体积%,或者大约30体积%至60体积%。基质可包含复合物的0体积%至50体积%的量的元素硅相。
示例
使用溶剂、粘合剂、树脂、塑化剂、碳粉末和SiC粉末、来形成浆料。对所测试的不同迭代,唯一变化是原来的大量 SiC粉末由不同中值大小的另一个SiC粉末1:1地代替。对浆料或处理条件不作改变。在图4中显示CMC层形成有中值大小为0.6 µm的SiC颗粒,而图5中则显示CMC层形成有中值大小为7 µm的SiC颗粒。
使用涂覆丝束过程来准备所显示的样本。通过将丝束穿过浆料浴池且通过计量孔(其控制丝束上的浆料量)来将预浸带缠绕在鼓上。在变干固定时间之后从鼓上移除预浸带。将带切割成层片,并且层片堆叠在一起形成具有0:90构造的面板。在高压锅中使用热和压力使面板固结。然后移除其余有机物,或者通过在隋性气氛中加热其余有机物使其热解,从而产生多孔预制坯。多孔预制坯通过在真空炉中的熔体浸渗进行填密。
在通过熔体浸渗进行填密之后,使用菱形多刃刀片将面板切开,并且准备好机械测试和微结构样本。将微结构样本安装在环氧树脂中且对其抛光。获得光学显微图且使用专有图像分析软件来识别纤维和计算各个纤维的最邻近邻居的距离(边缘到边沿)。图7A显示中值SiC颗粒大小与纤维邻居间隔(相邻纤维之间的表面间间隔)。图7B显示中值SiC颗粒大小与平均层间抗拉强度(ILT),其显示了:大约3.6 µm的颗粒大小显示相对于1 µm以下的颗粒大小,平均ILT有26%的改进,而大约7 µm的颗粒大小则显示39%的改进。
本书面描述使用示例来公开本发明,包括最佳模式,并且还使本领域任何技术人员能够实践本发明,包括制造和使用任何装置或系统,以及实行任何结合的方法。本发明的可取得专利的范围由权利要求限定,并且可包括本领域技术人员想到的其它示例。如果这样的其它示例包括不异于权利要求的字面语言的结构要素,或者如果它们包括与权利要求的字面语言无实质性差异的等效结构要素,则它们意于处在权利要求的范围之内。
Claims (9)
1.一种预浸渍复合带(20),包括:
基质材料(22);
多个纤维(16),其形成封闭在所述基质材料(14)内的成单向阵列的丝束(2),其中,所述纤维(16)具有大约5微米至大约40微米的平均纤维直径,以及其中,所述多个纤维(16)以大约15%至大约40%的体积分量包括在所述带(20)内;以及
散布在所述带(20)中的相邻纤维(16)之间的多个填料颗粒(24),其中,所述多个填料颗粒(24)具有中值颗粒大小,以及其中,所述带(20)具有的中值颗粒大小与平均纤维直径的比为大约0.05:1至大约1:1。
2.根据权利要求1所述的带(20),其特征在于,所述填料粉末的中值颗粒大小与平均纤维直径的比为大约0.07:1至大约0.7:1。
3.根据权利要求1所述的带(20),其特征在于,所述填料粉末的中值颗粒大小与纤维直径的比为大约0.1:1至大约0.5:1。
4.根据权利要求1所述的带(20),其特征在于,所述填料颗粒(24)包括SiC颗粒、碳颗粒、硼颗粒、B4C颗粒、Si3N4颗粒、Mo5Si3颗粒、MoSi2颗粒、硅化物颗粒、氧化物颗粒、聚合物颗粒或者它们的混合物。
5.根据权利要求1所述的带(20),其特征在于,所述基质材料(14)包括形成陶瓷的粉末。
6.根据权利要求5所述的带(20),其特征在于,所述形成陶瓷的粉末包括多个碳颗粒。
7.根据权利要求1所述的带(20),其特征在于,所述填料颗粒(24)以大约5%至大约40%的体积分量包括在所述带(20)内。
8.一种用于形成陶瓷基质复合物(10)的方法,所述方法包括:
提供大量纤维(16),各个纤维(16)具有介于5微米和40微米之间的平均纤维直径;
用浆料合成物浸渍所述纤维(16),所述浆料合成物包括粘合剂、溶剂和填料粉末;
使经浸渍的大量纤维(16)形成为单向带(20),其中,所述填料粉末(20)渗入所述大量纤维(16),使得所述填料颗粒(24)散布在所述带(20)中的相邻纤维(16)之间,以及其中,所述填料颗粒(24)具有中值颗粒大小,所述平均颗粒大小与所述平均纤维直径的比为大约0.05:1至大约1:1;
使所述带(20)形成为成形预制坯;
通过将所述预制坯加热到大约400℃或更高来使其热解,以分解有机组分,以及分别将所述粘合剂的任何预陶瓷聚合物或形成碳的聚合物组分转换成陶瓷或碳;以及
使用化学气相浸渗、聚合物浸渍和热解或熔体浸渗来对复合预制坯进行填密。
9.根据权利要求8所述的方法,其特征在于,所述填料颗粒(24)包括SiC颗粒、碳颗粒、硼颗粒、B4C颗粒、Si3N4颗粒、Mo5Si3颗粒、MoSi2颗粒、硅化物颗粒、氧化物颗粒、聚合物颗粒或者它们的混合物,以及其中,所述填料颗粒(24)的中值颗粒大小介于所述平均纤维直径的0.07倍和0.7倍之间,以及其中,在期望颗粒大小范围内的填料颗粒(24)在所述带内的体积分量介于5%和40%之间,以及其中,所述浆料合成物进一步包括多个碳颗粒,以及其中,所述填料颗粒(24)以大约5%至大约40%的体积分量包括在所述带内。
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CA2974485C (en) * | 2014-12-12 | 2024-01-16 | Kyoto University | Silicon carbide fiber reinforced silicon carbide composite material |
US10723660B2 (en) * | 2017-01-11 | 2020-07-28 | General Electric Company | Carbon yielding resin for melt infiltration |
US10822281B2 (en) | 2018-11-09 | 2020-11-03 | Raytheon Technologies Corporation | Accelerated CVI densification of CMC through infiltration |
DE102019213351A1 (de) * | 2019-09-03 | 2021-03-04 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Herstellung faserverstärkter Verbundwerkstoffe mit stabilisierten Fasern, Faserbeschichtungen und/oder Faserbündelbeschichtungen |
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