CN1955144A - 生产一种陶瓷基体复合材料制品的方法和由此形成的制品 - Google Patents

生产一种陶瓷基体复合材料制品的方法和由此形成的制品 Download PDF

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CN1955144A
CN1955144A CNA2006101060999A CN200610106099A CN1955144A CN 1955144 A CN1955144 A CN 1955144A CN A2006101060999 A CNA2006101060999 A CN A2006101060999A CN 200610106099 A CN200610106099 A CN 200610106099A CN 1955144 A CN1955144 A CN 1955144A
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ceramic matrix
ceramic
protective layer
cmc
matrix composite
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CN1955144B (zh
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G·S·科尔曼
H·C·麦圭根
M·K·布龙
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General Electric Co
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General Electric Co
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Abstract

一种CMC制品(18)和生产该制品(18)使其表面具有保护制品(18)内加强材料(15)免受损害的层(22)的方法。本方法要求提供一种在含陶瓷基体材料(16)前体的基体材料中含有陶瓷加强材料(15)的主体。加强材料(15)的一部分存在于并可能暴露于主体表面。然后主体表面被提供一种由浆料形成的表面层，该表面层含有颗粒材料但没有主体的加强材料(15)。通过将主体内的前体转化成含有加强材料(15)的陶瓷基体材料(16)，并且通过将表面层转化为覆盖暴露于主体表面的加强材料(15)的任何部分的保护层(22)，将主体和表面层加热形成制品(18)。

Description

生产一种陶瓷基体复合材料制 品的方法和由此形成的制品
本发明是根据能源部颁发的第DE-FC02-92CE41000号协议在政府的支持下实现的。政府享有本发明中的某些权利。
技术领域
本发明通常涉及陶瓷基体复合材料(CMC)和由此生产的制品。本发明尤其涉及形成一种CMC制品的方法，该制品带有保护性的外阻挡层，其可防止损害制品内部的近表面加强材料。
背景技术
CMC材料通常包含一种包埋于陶瓷基体材料中的陶瓷纤维加强材料。该加强材料在基体破裂的情况下起到CMC中承载组分的作用，同时陶瓷基体保护加强材料，维持其纤维的排列方向，并起到消除加强材料负载的作用。对于高温应用尤其有益的是硅基复合材料，如碳化硅(SiC)作为基体和/或加强材料。SiC纤维已经被用作多种陶瓷基体材料的加强材料，包括SiC、TiC、Si3N4和Al2O3。连续纤维加固的陶瓷复合材料(CFCC)是CMC的一种类型，可为多种高温承载应用提供轻重量、高强度和高刚度。CFCC材料特征通常在于，连续纤维(长丝)可被排列成单向纤维系，或捆扎成束后被排列成单向纤维束系，或捆扎为纤维束后被编成二维织物，或编成或织成三维织物。对于三维织物，单向纤维束组可以，例如被相互横穿交织。单个纤维束可被覆以隔离剂，如氮化硼(BN)或碳，形成一种稀薄的界面涂层，其允许纤维束与陶瓷基体材料之间受限制和受控制的滑动。随着CMC裂痕的发展，一个或更多跨过裂痕的纤维起到了向邻近纤维和基体材料区域再分配负载的作用，因此阻止或至少减缓了裂痕的进一步蔓延。
一项制造CMC的技术涉及多层“预浸料”，通常为带状结构的形式，包含用CMC基体材料前体浸渍过的理想的CMC的加强材料。预浸料必须经过处理(包括烧结)来将前体转化为理想的陶瓷。用于CFCC材料的预浸料往往包含一种含有单向排列的纤维束单层的二维纤维系，其用基体材料前体浸渍以产生通常的二维层压材料。获得的预浸料多层板被堆积并压实以形成层压板预制体，这一方法被称为“堆叠(lay-up)”。预浸料一般被排列以使预浸料坯的纤维束互相定向横穿(如，垂直地)，这为预制体的层状平面(与最终CMC组件的主要(承载的)方向相对应)提供更高的强度。
堆叠后，当经受施加的压力(debulking)和升高的温度，如在高压釜中时，层压板预制体一般将经历压实和固化。在被熔体浸渗(MI)的CMC制品的例子中，被压实和固化的预制体经受额外的处理。首先，为了分解有机粘合剂，预制体在真空中或在惰性气体中被加热，至少一种粘合剂在这种热处理中热解形成焦碳，并为熔体浸渗生产一种多孔预制体。进一步加热，或者作为与粘合剂烧出步骤同一热循环的一部分或者在独立的后续加热步骤中，预制体例如用外部提供的熔融硅进行熔体浸渗。熔融硅渗透进入气孔，与基体的碳组分反应形成碳化硅，并填满气孔以产出理想的CMC组件。
SiC/Si-SiC(纤维/基体)CFCC材料的实施例和方法在共同转让的美国专利No.5,015,540、5,330,854、5,336,350、5,628,938、6,024,898、6,258,737、6,403,158和6,503,441以及共同转让的美国专利申请公开No.2004/0067316中公开。图1中描述了CFCC材料的一个实例，该图表示CFCC组件10的一个表面区域，其包含多层板12，每层来源于包括用陶瓷基体前体浸渍过的单向排列的纤维束14的单个预浸料坯。结果，每层板12含有单向排列纤维15，其包在由陶瓷基体前体在烧结和熔体浸渗中转化形成的陶瓷基体16中。
为了最大化CMC，特别是预浸料MI型CMC的机械性能，让加强材料很好地分散于复合材料基体中很重要。如图1显示，这样的分散必然的将部分加强材料置于复合材料表面附近，在此由于处理、加工、为后续处理步骤如环境阻挡层(EBC)的沉积进行的表面准备、或高温下氧化攻击，加强材料很容易受损。图3中显示了含有分散的加强材料纤维的预浸料MI型CMC的横断面。可以看到，大量的加固纤维比较接近表面(在约0.005英寸(约125mm)内)，因而容易受损。
根据以上观点，保护CMC中近表面的加强材料将是大有裨益的。但是，这么做绝不能损失复合材料的机械、热学、或结构性能，同时必须在化学和热学(相同的热膨胀)方面与CMC材料的主体相匹配。
发明内容
本发明提供一种CMC制品和一种生产该CMC制品的方法，使制品表面具有一外部阻挡层，其保护制品内部加强材料免受后续处理、加工和表面处理过程中的物理损害，和高温下的化学/氧化损害。
本发明的方法一般要求提供一种在含陶瓷基体材料前体的基体材料中含有陶瓷加强材料的主体。加强材料的部分存在于并可能暴露于主体表面。然后在主体表面沉积一表面层来限定主体的最外表面。该表面层包含一种含有颗粒材料的浆料，但没有主体的加强材料。接着主体和其上的表面层被加热形成在陶瓷基体复合材料基底上含有陶瓷保护层的CMC制品。较为特别的是，表面层转化成陶瓷保护层，同时主体中的前体转化成含有陶瓷加强材料的陶瓷基体材料，以至于产生陶瓷基体复合材料基底。陶瓷保护层定义为CMC制品的最外表面，并覆盖了最初暴露于主体表面的部分加强材料。本发明优选的实施方案中，最初沉积于主体的表面涂层可含有切碎的(chopped)或磨碎的(milled)碳纤维或半连续的碳纤维片以防止主体在后续处理，包括在其转化形成CMC的保护层过程中收缩开裂。
根据本发明的一个优选方面，限定为CMC制品最外表面的保护层保护CMC制品内近表面的加强材料免受处理损害，而且也在CMC表面提供能被加工而不损害下层的加强材料的标称量材料。后一方面尤其对于即将施加EBC涂层的CMC的应用有利，这种情况下，一般通过如磨料喷砂(abrasive gritblasting)来实施表面粗化处理，以促进涂层的粘附力。因为保护层没有加强材料，因此稀薄的界面涂层通常施加于加强材料，考虑到在浸渗后的制品的清理过程中或为EBC应用进行的表面准备过程中更具侵蚀性的喷砂处理，保护层可以比下层的CMC硬很多。在CMC会经受空气或燃烧气体中暴露于高温的应用中，保护层提供一个屏障，其会在含纤维的CMC材料遭受攻击前氧化和/或挥发，因此延长了CMC制品会发生的任意机械降解前的时间。
本发明的其他目的和优点将从后面的详述中得到更好地体现。
附图说明
图1图示了现有技术中CMC制品的部分横断面视图。
图2图示了本发明中具有保护层的CMC制品的部分横断面视图。
图3为显微拍照的扫描影像，显示现有技术中没有保护层的CMC制品的横断面视图，也显示加固纤维集中在制品表面附近，在此其容易受到机械或化学(氧化)损害。
图4为显微拍照的扫描影像，显示本发明第一个实施方案中具有无填充物保护层的CMC制品的横断面视图。
图5和6为显微拍照的扫描影像，显示本发明其它实施方案中具有含填充物的保护层的CMC制品的横断面视图，其填充物分别由切碎的碳纤维和半连续碳纤维垫构成。
图7为用于生产图6中CMC制品的碳垫(carbon mat)类型的扫描影像。
具体实施方式
本发明涉及利用外保护层保护CMC制品外表面。如图2所示，一种CMC组件18被显示为具有基本上与图1中组件10相同的CMC基底20，但在其上面，形成一个保护层22来限定组件18的最外表面24。保护层22没有任何加强材料，如CMC组件18下层的基底20的纤维束14。相反，保护层22主要且潜在地完全由陶瓷材料形成，该陶瓷材料能够按配方制备以与CMC组件18的陶瓷基体材料16基本一致。将保护层22施加到CMC组件18的方法可根据用于生产组件18的特殊处理技术而变化。在图2显示的预浸料MI-CMC类型的特例中，包括浸渍或喷涂保护层22的前体的各种技术均是可能的。将保护层22施加到预浸料MI-CMC复合材料如CMC组件18的特别优选的方法是，在复合材料堆叠的过程中将富含基体、不含加强材料的带层压到复合材料预制体表面。通过形成保护层22，使其基本上具有与CMC基底20的下层基体材料16相同的化学组成，保护层22就更易于与基底20充分匹配。
本发明的优选实施方案中，CMC组件18的基体16通过硅MI方法形成，以使基体16含有SiC和一些游离硅。组件18的优选材料和处理技术在共同转让的美国专利No.5,015,540、5,330,854、5,336,350、5,628,938、6,024,898、6,258,737、6,403,158和6,503,441以及共同转让的美国专利申请公开No.2004/0067316中公开，其涉及CMC的组成和方法的公开内容在此引入作为参考。这些共同转让专利中，纤维束14的优选材料为SiC纤维，以使组件18可以被称为SiC/Si-SiC(纤维/基体)CMC。适合纤维束14的材料中一个著名的市场化的例子是，来自Nippon Carbon有限公司的HI-NICALON。合适的纤维束14的直径范围是约2到约20微米，不过更大和更小直径的纤维也在本发明的范围内。也与前述专利一致，纤维15优选地被覆以材料，来带给CMC基底20某些理想性能，如碳或氮化硼界面层(未显示)，其上面可沉积SiC或Si3N4涂层(未显示)以在熔体浸渗过程中保护纤维15。根据公知的实践，可通过CVI沉积这种界面层和SiC或Si3N4涂层，不过其他沉积技术也可以实现。本领域技术人员会明白，本发明教导的内容也适用于其他CMC材料组合，并且这种组合是在本发明范围内的。
图4为贯穿CMC基底20的局部横断面显微拍照的扫描影像，一个带在烧结前被层压在CMC基底20外表面上，该带通过烧结产生本发明的第一个实施方案的外保护层22。利用HI-NICALON纤维形成的纤维束加强材料生产CMC基底20。该纤维被覆以连续多层的氮化硼、碳、氮化硅和碳。通过将浸渍过的预浸带堆叠来生产CMC基底20的预制体，每个含有加强材料和浆料的预制体由基体浆料铸造，基体浆料含有，按质量，约25％的SiC粉末、约11％的碳粉、约16％的有机粘合剂、以及约48％的粘合剂的溶剂。用于保护层22的带是被铸造为与用在下层CMC基底20的生产中相同的基体浆料薄片的带。结果，保护层22在成分上与基底20的陶瓷基体一致，但没有任何加强材料。带的厚度为约0.4mm，它使得保护层22也具有最终的约0.4mm的厚度。用于CMC基底20的带被堆叠以生产预制体后，将用于保护层22的带层压到预制体的表面，接着整个层压结构经过高压釜处理、粘合剂烧出、和使用标准操作的熔融硅浸渗，生产出图4所示的样本。
如图4所示，尽管前面的方法对复合材料基底20表面生产保护层22有效，但保护层22在烧出和浸渗步骤中容易破裂。一个这样的裂痕在图4中可见，并且被归结为基体仅有的层22在处理过程中的小而有限的收缩(如，一般小于0.5％)造成的。复合材料基底20中，基体的收缩被加强材料的存在所限制。结论是，发生在基体仅有的保护层22内的少量收缩足以产生相对较大的基体裂痕。
为了充分消除保护层22的破裂趋势，可以把含碳的丝状材料添加到用于形成保护层22的浆料中。例如，切碎的或磨碎的碳纤维可以代替保护层22的基体浆料中的部分或全部碳微粒，或将用于形成保护层22的带处理以结合薄的、多孔的、无方向的(随机)碳纸或垫，作为基体浆料的载体。这种含碳的丝状材料被认为在很大程度上，尽管不是完全，在用熔融硅浸渗的过程中被消耗，结果与硅反应形成碳化硅。任何剩余碳的残留量被认为量足够小，对保护层22或复合材料10总体上的机械或热学稳定性或抗氧化性没有影响。除碳以外或代替碳，可以预见，其他可匹配的材料能够用作切碎的纤维或纤维垫的材料，如碳化硅。将聚合纤维(如，尼龙、纤维素、聚乙烯，等)用作纤维材料也是可能的，只要这种材料在粘合剂烧出过程中热解为碳，并因此不污染保护层22。
在基体浆料中添加切碎或磨碎的碳纤维很容易通过简单地用这些碳纤维代替基体浆料中使用的部分或全部碳颗粒来实现。然后可通过浸渍或喷涂CMC预制体来施加浆料，或将浆带式浇铸(tape casting)，形成可被层压在CMC预制体上的带。可以通过一个浸渍的步骤来很容易地结合碳垫，浸渍步骤中，将基体浆料沉积在垫上，并通过塑料刀片或涂刷器的抹擦压入垫内。后一方法的优点在于，容易将带的厚度控制到基本上是碳垫的厚度。碳纤维或碳垫半连续的性质起到了带内部刚架的作用，并且在带固化、烧出和浸渗过程中抑制收缩。通过减少收缩，保护层22被制造得与下层的CMC基底20更加匹配，而且避免了表面收缩的裂痕。
用与上述相同的方法生产图4中样本的带和复合材料层压预制体，但用于保护层22的一条带是由含切碎的碳纤维的基体浆料生产的，而另一条带是由含碳垫的基体浆料生产的。所用的切碎的碳纤维材料是从Toho Tenax America公司购买的Fortafil 342，并具有约6到7微米的标称直径和从小于100到约450微米的标称长度。将纤维随机分散于基体浆料中，并且随后纤维一般在带式浇铸中从浆料里被随机分散。但是，在带式浇铸过程中有一种趋势，即在带平面内纤维变得定向。切碎的碳纤维代替基体浆料中全部的碳颗粒，并在浇铸和干燥的带内造成约20体积百分比的碳纤维含量。
碳垫是一种厚度约75到约125微米的低密度、无方向的碳纸，并且通过用基体浆料浸渍被结合到带内。碳垫含有随机二维分布在碳垫平面内的约2.5cm长的碳纤维。随机碳纤维构成碳垫所占体积的约4％，其余96％的体积为空隙。合适的碳垫材料是市场上现有的来自加利福尼亚Aerospace Composite Productsof Livermore的，名为“MC-03 0.2 oz碳垫”和“MC-06 0.5 oz碳垫”，其中的一个例子在图7中显示。需要明白的是，其他相似构造的碳垫材料也应该同样适用。含有精细碳颗粒的标准复合材料浆料通常用于浸渍碳垫，其可在带中提供约24体积百分比的总含碳量。
图5为CMC板显微拍照的扫描图，其复合材料层压基底20受到由纤维填充的带生产的层22的保护。如图5所示，保护层22没有图4中所见的收缩裂痕。图6为CMC板显微拍照的扫描图，其中复合材料层压基底20受到由含碳垫的带生产的层22的保护。再次可以看到，保护层22没有收缩裂痕。
上面的观察证实，能够保护CMC基底20的近表面加强材料的保护层22可以通过一种非加固层形成，该非加固层与形成CMC基底20的陶瓷基体所用浆料相同。由于由CMC基体材料形成，保护层22被认为能够保护CMC基体免于多种来源的损害，包括处理和氧化。在缺乏加强材料和通常施加的稀薄界面涂层的情况下，保护层22能够承受加工和其他侵蚀性的表面处理，特别是在CMC组件表面必须通过喷砂粗化以清洁表面或促进接下来要施加于组件的涂层的粘附力的情况下。后者的例子是图2中虚线所代表的EBC 26。合适的EBC材料在共同转让的美国专利No.5,985,470、6,444,335、6,558,814、6,610,385、6,699,607、6,740,364和6,787,195和美国专利申请No.10/709,288、11/160,185和11/160,212，以及美国专利No.6,254,935、6,352,790、6,365,288、6,387,456和6,410,148中公开。这些涉及EBC组成和处理的专利和专利申请的公开内容在此引入作为参考。
尽管本发明已经以特殊实施方案的形式得到描述，显然其它形式也能够被本领域技术人员所采纳。因此，本发明的范围仅被下列权利要求所限制。

Claims (10)

1.一种生产陶瓷基体复合材料制品(18)的方法，该方法包括以下步骤：
提供一种主体，其中在含有陶瓷基体材料(16)前体的基体材料中含有陶瓷加强材料(15)，加强材料(15)的一部分在主体表面上；
在主体表面形成一个表面层，其包括含颗粒材料的浆料，该表面层限定主体的最外表面并且不含主体的加强材料(15)；然后
将主体和表面层加热，通过将主体内的前体转化成含有陶瓷加强材料(15)的陶瓷基体材料(16)来生产陶瓷基体复合材料基底(20)，并且通过将表面层转化成陶瓷保护层(22)，从而形成在陶瓷基体复合材料基底(20)上含有陶瓷保护层(22)的陶瓷基体复合材料制品(18)，所述陶瓷保护层(22)限定陶瓷基体复合材料制品(18)的最外表面(24)，并覆盖在主体表面的加强材料(15)部分。
2.根据权利要求1的方法，其特征在于表面层含有其量足以抑制表面层转化为保护层(22)时的收缩和开裂的碳纤维分散体。
3.根据权利要求1的方法，其特征在于表面层含有基本上平行于主体表面取向的多孔碳片，该多孔碳片抑制表面层在转化为保护层(22)时的收缩和开裂。
4.根据权利要求1到3任意一项的方法，其特征在于通过层压含浆料的带到表面上，在主体表面沉积表面层。
5.根据权利要求4的方法，其特征在于主体通过堆叠很多预浸带来形成，每个带在一部分基体材料中含有一部分陶瓷加强材料(15)。
6.根据权利要求1到5任意一项的方法，其特征在于陶瓷保护层(22)主要含有与陶瓷基体复合材料基底(20)的陶瓷基体材料(16)相同化学组成的陶瓷材料。
7.根据权利要求1到6任意一项的方法，该方法进一步包括用熔体浸渗材料对主体进行熔体浸渗，特征在于在加热步骤中，熔体浸渗材料与前体反应生成陶瓷基体复合材料制品(18)的陶瓷基体材料(16)。
8.根据权利要求7的方法，其特征在于熔体浸渗材料包括熔融硅，并且反应步骤至少使一部分熔融硅反应形成碳化硅。
9.根据权利要求1到8任意一项的方法，该方法进一步包括以下步骤：
粗化陶瓷基体复合材料制品(18)的最外表面(24)；然后
在粗化的最外表面(24)上沉积一环境阻挡层(26)。
10.通过前述任一权利要求的方法生产的陶瓷基体复合材料制品(18)。
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CN105924198B (zh) * 2015-02-26 2019-07-30 通用电气公司 陶瓷基质复合物制品和用于形成其的方法
CN105924200B (zh) * 2015-02-26 2019-07-30 通用电气公司 陶瓷基质复合物制品及用于形成其的方法
CN105924200A (zh) * 2015-02-26 2016-09-07 通用电气公司 陶瓷基质复合物制品及用于形成其的方法
CN105924198A (zh) * 2015-02-26 2016-09-07 通用电气公司 陶瓷基质复合物制品和用于形成其的方法
CN106393388A (zh) * 2015-07-28 2017-02-15 通用电气公司 层片、制造层片的方法以及利用层片制造制品的方法
CN106393388B (zh) * 2015-07-28 2021-06-08 通用电气公司 层片、制造层片的方法以及利用层片制造制品的方法
CN106396714A (zh) * 2015-07-30 2017-02-15 通用电气公司 改进cmc材料中的纤维间隔的均匀性
CN112694341A (zh) * 2016-03-23 2021-04-23 通用电气公司 具有单峰孔径分布和低纤维体积分数的陶瓷基质复合物
CN112694341B (zh) * 2016-03-23 2022-10-21 通用电气公司 具有单峰孔径分布和低纤维体积分数的陶瓷基质复合物
CN108640698A (zh) * 2018-05-02 2018-10-12 中国航发北京航空材料研究院 一种陶瓷基复合材料构件共固化成型工艺

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