CN111566072B - 用于制造含有陶瓷基质的复合部件的方法 - Google Patents

用于制造含有陶瓷基质的复合部件的方法 Download PDF

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CN111566072B
CN111566072B CN201880082359.4A CN201880082359A CN111566072B CN 111566072 B CN111566072 B CN 111566072B CN 201880082359 A CN201880082359 A CN 201880082359A CN 111566072 B CN111566072 B CN 111566072B
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ceramic
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CN111566072A (zh
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阿诺·德勒胡兹
埃里克·布伊隆
雅恩·勒佩蒂科尔
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Centre National de la Recherche Scientifique CNRS
Universite de Bordeaux
Safran Ceramics SA
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Universite de Bordeaux
Safran Ceramics SA
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Abstract

本发明涉及一种用于制造复合材料部件的方法，所述复合材料部件包括由陶瓷基质致密的颗粒增强体，所述方法包括以下步骤：通过将包含粘合剂、用于形成所述部件的颗粒增强物的第一陶瓷或碳颗粒以及不同于所述第一颗粒的第二陶瓷或碳颗粒的混合物成形来形成要制造的部件的毛坯；去除或热解所述毛坯中存在的粘合剂以获得所述部件的多孔预制件；以及通过包含金属的熔融组合物渗透所述预制件的孔隙，以获得所述部件。

Description

用于制造含有陶瓷基质的复合部件的方法
发明背景
本发明涉及制造由陶瓷基复合材料制成的部件的方法的一般领域。
陶瓷基复合材料(CMC)以其良好的机械性能而著称，使其适合用作结构元件并在高温下保持这些性能，是替代传统金属部件的可行选择。与金属同类产品相比，它们的质量降低，使其成为航空领域应对提高效率和减少发动机污染排放问题的理想选择。
CMC部件可以包括机织织物形式的通常连续的纤维增强体，该纤维增强体由陶瓷基质致密化。因此，纤维增强体包括通常连续长纤维，其取向可以在使用过程中适应部件的主要应力方向。形成纤维增强体的预制件必须使用合适的织机从连续纤维编织到部件的尺寸(例如，通过二维或三维编织)。编织步骤是一个漫长而昂贵的过程，这不是制造小部件的最佳方法。
因此，需要一种易于实施且成本较低的制造小部件的陶瓷基复合材料部件的制造方法。
发明内容
因此，本发明的主要目的是通过提出一种制造复合材料部件的方法来弥补这些缺点，所述复合材料部件包括由陶瓷基质致密的颗粒增强体，所述方法包括以下步骤：
通过将包含粘合剂、用于形成所述部件的颗粒增强体的第一陶瓷或碳颗粒以及不同于第一颗粒的第二陶瓷或碳颗粒的混合物成形来形成要制造的部件的毛坯，
去除或热解所述毛坯中存在的粘合剂以获得所述部件的多孔预制件，以及
通过包含金属的熔融组合物渗透所述预制件的孔隙，以获得所述部件。
因此，根据本发明的方法使得可以通过熔体渗透法生产CMC部件而无需编织纤维增强体。由于使填充有第一颗粒和第二颗粒的混合物成形并且然后通过去除或热解粘合剂而获得多孔预制件的步骤，根据本发明的方法使得可以省去编织纤维增强体的步骤。这对于制造不受高热机械应力影响的小部件特别有利，这意味着可以节省制造时间和成本。也可以从本发明的方法中获得具有复杂形状和所需尺寸的部件，而无需额外的机械加工。
粘合剂和颗粒之间的混合物可以均匀且紧密。
在一示例性实施方式中，熔融组合物可包括金属间化合物。在一个示例性实施方式中，熔融组合物可包括硅。
熔融组合物可以由纯熔融硅组成，或者可替代地为硅与一种或多种其他成分的熔融合金的形式。熔融组合物可以主要包括硅，即，具有按质量计50％以上的硅含量。熔融组合物可以例如具有按质量计大于或等于75％的硅含量。硅合金中存在的成分可以选自B、Al、Mo、Ti及其混合物。特别地，熔融组合物可以包括二硅化钼(MoSi 2)。在渗透过程中，熔融组合物与多孔预制件中存在的碳(例如，热解残留物)之间可能发生化学反应，从而形成碳化硅(反应熔体渗透过程)。
在一个示例性实施方式中，可以加热混合物以使粘合剂流化并促进成形步骤以形成毛坯。混合物也可以在成形之前经受真空以去除混合物中存在的任何气泡。毛坯的尺寸可以大于或等于最终部件的尺寸，以便在去除或热解粘合剂后在毛坯内部留下多孔网络。粘合剂的去除或热解步骤(也称为“脱粘”)优选可以在惰性气体，例如氩气下进行，以避免毛坯的氧化，氧化会降低毛坯在最终部件的不同加工步骤之间的机械强度。在下文中，当提到“粘合剂去除”步骤时，总是被理解为是指“粘合剂去除或热解”步骤，其中热解包括去除粘合剂并留下残留物。
在示例性实施方式中，第一颗粒可以是短纤维。换句话说，第一颗粒可以具有大体上圆柱形的形状。
在一个示例性实施方式中，短纤维的长度可以优选地在50μm至5000μm之间，或更优选地，短纤维的长度可以在100μm至300μm之间。
在一个示例性实施方式中，短纤维可以通过机械切割或研磨从长纤维获得。
在示例性实施方式中，第一颗粒可以是细粒。换句话说，第一颗粒可以是球形或椭圆形的。在这种情况下，第一颗粒的平均尺寸(D50)可以在10μm至300μm之间，更优选在40μm至100μm之间。
在一个示例性实施方式中，第一颗粒的中值基本体积可以大于或等于第二颗粒的中值基本体积。颗粒的基本体积是该颗粒所占的体积。
在示例性实施方式中，混合物的成形可以包括将混合物注入模具中。
在一个示例性实施方式中，粘合剂可包含至少一种热塑性聚合物。例如，粘合剂可包含选自以下的至少一种化合物：聚乙烯醇(PVA)、聚乙二醇(PEG)、聚丙烯(PP)、聚甲醛(POM)、聚对苯二甲酸乙二醇酯(PET)。
在一个示例性实施方式中，粘合剂可包含至少一种热固性聚合物。例如，粘合剂可以包含至少一种选自以下的化合物：环氧树脂、酚醛树脂、陶瓷前驱体树脂。
在一个示例性实施方式中，混合物可包含两种可热去除的粘合剂，每种具有不同的去除温度。因此，粘合剂去除步骤可以包括在两个不同温度下热去除每种粘合剂的两个子步骤。
在一个示例性实施方式中，混合物可包含可通过溶解去除的第一粘合剂和加热去除的第二粘合剂。因此，粘合剂去除步骤可以包括两个去除子步骤：通过溶解去除第一粘合剂，然后通过热去除第二粘合剂。该设置是有利的，因为其允许在溶解去除第一粘合剂之后通过打开毛坯中的孔隙来更有效地去除第二粘合剂。
在示例性实施方式中，可以将包含混合物的液体介质注入模具中，模具可以配备有用于液体介质的过滤装置，并且形成毛坯的步骤可以另外包括通过过滤装置来过滤液体介质。液体介质可以是水性介质，或者可以包括例如醇。
在一个示例性实施方式中，混合物的成形可以包括向混合物施加压力。在这种情况下，粘合剂包括增塑剂以改善混合物的致密性。这种增塑剂可以是硬脂酸。在这种情况下，混合物的成形可涉及将混合物冷等静压入模具中。
在一个示例性实施方式中，该方法可以包括在渗透步骤之前，对去除或热解粘合剂之后获得的多孔预制件进行等静压。该等静压步骤可以热或冷进行。该等静压步骤使得可以部分关闭由粘合剂去除或热解步骤产生的孔隙，以便控制该孔隙率并促进随后的渗透步骤。
还可以在渗透步骤之前，再次对脱粘毛坯进行自由(即无应力)烧结热处理，以控制脱粘毛坯的孔隙率。该自由烧结热处理可以在冷等静压步骤之后和热等静压步骤之前进行。
在示例性实施方式中，第一颗粒可以由碳化硅制成。在短纤维的情况下，它们的氧含量可以小于或等于1原子百分比。例如，这种短纤维可以是日本NGS公司销售的Hi-Nicalon S型纤维。替代地，短纤维可以由选自以下的材料制成：碳、氧化物，例如氧化铝(Al2O3)。
在一个示例性实施方式中，第一颗粒可以涂覆有中间相。这种中间相可以例如由热解碳(PyC)、氮化硼(BN)或碳化硅(SiC)制成。中间相可以包括几层，每层包括不同的材料。中间相具有降低复合材料的脆性的功能，促进在基质中传播之后到达中间相的可能的裂纹的偏转，从而防止或延迟由了此类裂纹引起的增强体的断裂。该中间相还在其形成过程中保护基质材料的纤维的第一颗粒。
该中间相可以在第一颗粒引入混合物中之前沉积在第一颗粒上。如果是短纤维，则可以在将长纤维切割或磨碎之前将中间相沉积在长纤维上。可通过化学气相沉积(CVD)工艺或通过电解沉积工艺或通过熔融盐将中间相直接沉积在短纤维上。也可以将与待形成的基质材料相容的陶瓷涂层代替中间相沉积或在中间相上沉积与待形成的基质材料相容的陶瓷涂层。
在一个示例性实施方式中，第二陶瓷颗粒可以由选自以下的材料制成：SiC、MoSi2、TiSi2、CoSi2、ZrSi2、HfSi2、ZrB2、HfB2、TiB2及其混合物。
在一个示例性实施方式中，部件中的第一颗粒的体积含量可以在10％至70％之间，优选地在25％至50％之间。
在一个示例性实施方式中，部件中的第二颗粒的体积含量可以在30％至90％之间，优选地在50％至75％之间。
在一个示例性实施方式中，第二颗粒的平均尺寸(D50)可以在0.5μm至200μm之间，更优选地在0.7μm至75μm之间。
附图说明
根据以下给出的描述，参考附图，本发明的其他特征和优点将变得显而易见，所述附图示出了示例性实施方式，而没有任何限制特征。图1是示出根据本发明的实施方式的方法的各个步骤的流程图。
具体实施方式
现在将结合图1中的流程图描述根据本发明的实施方式的方法的步骤。这里的目的是获得陶瓷基复合材料部件。这样的部件可以是航空部件，例如用于航空涡轮机的部件。这样的部件可以是例如小叶片。
在步骤S1中，可以获得第一陶瓷或碳颗粒，其将用于形成待制造部件的颗粒(例如纤维)增强体。当第一颗粒是短纤维时，它们可以通过以本身已知的方式研磨或机械切割长纤维而获得。短纤维的中位长度可以在50μm至5000μm之间或100μm至300μm之间。第一颗粒的尺寸分布不必是单分散的，而是可以是多分散的。
第一颗粒可任选地涂有中间相涂层(步骤S2)。对于短纤维，可以直接涂覆或在切割或研磨之前通过涂覆长纤维进行涂覆。中间相的厚度可以例如在10nm至1000nm之间，并且例如在10nm至500nm之间。中间相可以是单层或多层。中间相可包含至少一层热解碳(PyC)、氮化硼(BN)、掺硅氮化硼(BN(Si)，硅的质量比例在5％至40％之间，其余为氮化硼)或掺硼碳(BC，硼原子比例在5％至20％之间，其余为碳)。中间相的沉积可通过CVD工艺或电镀工艺或通过熔融盐直接在短纤维上进行。在此，中间相具有复合材料的去纤化功能，其促进了在基质中传播后到达中间相的可能裂纹的偏转，从而防止或延迟由了此类裂纹引起的增强体的断裂。在基质形成的后续步骤中，中间相还可以保护增强体。也可以将与待形成的基质材料相容的陶瓷涂层(例如通过CVI)代替中间相沉积或在中间相的顶部沉积与待形成的基质材料相容的陶瓷涂层，例如通过CVI。
在步骤S3中，然后可以制备包含粘合剂、第一陶瓷或碳颗粒和第二陶瓷颗粒的混合物以形成部件的基质。粘合剂可以例如包含聚合物，例如热塑性或热固性树脂或增塑剂。该混合物可以包括几种粘合剂。加热混合物以使粘合剂流化以促进混合并允许更好的均质化可能是有利的。然后，混合温度取决于所使用的有机粘合剂，以避免热降解和过早聚合。也可以在真空下制备混合物，以减少混合物中气泡的存在。这样制备的混合物可以例如制成颗粒以备后用，或直接在下一步中注入。
在步骤S4中，通过使在步骤S3中制备的混合物成形来形成部件的毛坯。下面将描述执行该步骤的几种方式。
根据第一替代方案，可以通过将混合物注入模具型腔中来执行成形步骤。用于注射的模具型腔可具有比最终部件更大的尺寸，因为有效地执行渗透步骤(步骤S6)需要一个多孔网络。模具可以包括喷嘴，喷嘴的尺寸以已知的方式适应于第一和第二颗粒的尺寸，并且适应于粘合剂以及所选择的注射压力和温度。如有必要，可以对模具进行温度控制，以控制粘合剂在注射后可能的固化。当第一颗粒对应于模具壁附近的短纤维时，该控制也可用于避免第一颗粒的优先取向。可使用预先加热到允许粘合剂流动的温度的混合物进行注射。注射可以在50巴至3000巴之间的压力下进行。一旦将混合物注入模具中并模制了毛坯，就可以将坯件脱模。生成的毛坯呈“胚体”或可塑状态。如上所述，毛坯通常可以大于最终部件。
在第二替代方案中，模具可以配备有过滤装置，并且将包括分散在液体介质中的第一颗粒和第二颗粒的混合物的液体介质注入到模具中，并且形成毛坯的步骤S4还包括通过过滤装置过滤液体介质。液体介质可以是水性介质或包含醇。液体介质可以优选地包括聚乙烯醇(PVA)。它可以是浆液。在注射/过滤过程中，第一颗粒和第二颗粒通过过滤装置保留在模具内部，并逐渐形成毛坯。
在第三替代方案中，粘合剂可包括增塑剂，并且粘合剂成形步骤包括向混合物施加压力，例如混合物的冷等静压。促进压实的增塑剂可以是硬脂酸。然后可以将混合物直接放入模具中，并且可以通过模具向混合物施加压力以使混合物成形。
在步骤S5中，将毛坯中的粘合剂去除或热解以产生脱粘毛坯。粘合剂去除或热解步骤S5的条件通常取决于以本身已知的方式去除的粘合剂的性质。特别地，一些粘合剂可以热去除，即温度使它们分解和/或蒸发，而另一些可以化学去除，例如通过溶解在合适的溶剂中。步骤S5可以涉及热解，在这种情况下，热解残留物可以保留在脱粘毛坯中。可以在中性气氛(例如氩气中)进行步骤S5，以便将碳骨架保留在毛坯中直到去除步骤结束，从而确保更好地保留毛坯，而且还降低了氧化毛坯的风险。
使用几种粘合剂是有利的，例如可以在两个分开的去除步骤中去除的两种粘合剂。在一个示例中，首先通过溶解去除第一粘合剂，然后将第二粘合剂热去除。在另一个示例中，可以在第一去除温度下热去除第一粘合剂，并且可以在高于第一去除温度的第二去除温度下热去除第二粘合剂。通过在去除第一粘合剂之后打开预制件中的孔隙，连续地去除两种粘合剂降低了预制件在步骤S5中破裂的风险，可以通过孔隙从预制件中提出第二粘合剂。在脱粘合剂步骤S5之后，预制件的尺寸通常不会改变。因此，去粘毛坯或多孔预制件包含第一颗粒和第二颗粒，并且具有先前由粘合剂占据的非零孔隙。
然后，在步骤S6中，用包含金属(例如金属间化合物或硅)的熔融组合物渗透预制件的孔隙以获得部件。该渗透步骤对应于熔体渗透步骤(MI或RMI过程)。熔融组合物或渗透组合物可以由纯熔融硅组成，或者可替代地为硅与一种或多种其他成分的熔融合金的形式。在步骤S6之后，获得CMC部件。
在去除或热解毛坯中存在的粘合剂的步骤S5之后，并在渗透步骤S6之前，对多孔预制件进行热等静压的步骤，以便在步骤S6之前如果孔隙率过高，则关闭部分孔隙。该热等静压步骤优选在夹套下进行，以确保多孔预制件均匀压实。施加的压力优选地在1000巴至2000巴之间。夹套可以包括石墨和氮化硼。该步骤可以将脱粘毛坯的孔隙率(通常在30％至40％之间)降低至例如约10％的孔隙率，以便保持足够的连通孔网并具有一定的孔隙率，以确保预制件中的熔融金属更好地毛细管上升。另外，在渗透之前进行的该热等静压步骤使得可以减少在渗透期间可以与增强体反应的液态金属的体积，从而通过降低增强体被液态金属溶解的风险来保护增强体。取决于所涉及的基质材料，热等静压步骤可以在1000℃至1600℃之间的温度下进行。对于二硅化钛基质，例如温度可以在1100℃至1500℃之间。

Claims (15)

1.一种用于制造复合材料部件的方法，所述复合材料部件包括由陶瓷基质致密的颗粒增强体，所述方法包括以下步骤：
通过将包含粘合剂、用于形成所述部件的颗粒增强体的第一陶瓷或碳颗粒以及不同于所述第一颗粒的第二陶瓷或碳颗粒的混合物成形来形成要制造的部件的毛坯，
去除或热解所述毛坯中存在的粘合剂以获得所述部件的多孔预制件，以及
通过包含金属的熔融组合物渗透所述预制件的孔隙，以获得所述部件，
特征在于，在渗透步骤之前，所述方法还包括对去除或热解所述粘合剂之后获得的多孔预制件进行热等静压的步骤。
2.根据权利要求1的方法，其中，所述熔融组合物包含硅。
3.根据权利要求1的方法，其中，所述第一颗粒是短纤维，所述短纤维的长度在50μm至5000μm之间。
4.根据权利要求3所述的方法，其中，所述短纤维的长度在100μm至300μm之间。
5.根据权利要求1的方法，其中，所述第一颗粒是球形或椭圆形。
6.根据权利要求1所述的方法，其中，所述第一颗粒的中值基本体积大于或等于所述第二颗粒的中值基本体积。
7.根据权利要求1所述的方法，其中，使所述混合物成形包括将所述混合物注入模具中。
8.根据权利要求7所述的方法，其中，将包含所述混合物的液体介质注入所述模具中，所述模具配备有用于所述液体介质的过滤装置，并且形成所述毛坯的步骤还包括通过所述过滤装置来过滤所述液体介质。
9.根据权利要求1所述的方法，其中，使所述混合物成形包括对所述混合物施加压力。
10.根据权利要求9所述的方法，其中，使所述混合物成形包括将所述混合物冷等静压入模具中。
11.根据权利要求1所述的方法，其中，所述第一颗粒是碳化硅。
12.根据权利要求1所述的方法，其中，所述第一颗粒涂覆有中间相。
13.根据权利要求1所述的方法，其中，所述第二陶瓷颗粒包括选自以下的材料：SiC、MoSi2、TiSi2、CoSi2、ZrSi2、HfSi2、ZrB2、HfB2、TiB2及其混合物。
14.根据权利要求1所述的方法，其中，所述部件中的第一颗粒的体积含量在10％至70％之间，和/或所述部件中的第二颗粒的体积含量在30％至90％之间。
15.根据权利要求1至14中任一项所述的方法，其中，所述部件是用于航空涡轮机的部件。
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