CN111971262A - 复合材料部件的制造方法 - Google Patents

复合材料部件的制造方法 Download PDF

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Publication number
CN111971262A
CN111971262A CN201980025225.3A CN201980025225A CN111971262A CN 111971262 A CN111971262 A CN 111971262A CN 201980025225 A CN201980025225 A CN 201980025225A CN 111971262 A CN111971262 A CN 111971262A
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particles
silicon carbide
powder composition
carbide particles
group
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奥雷利亚·克莱伦堡
埃米莉·门德斯
埃里克·菲利普
丹尼斯·维奇阶
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Safran Ceramics SA
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Safran Ceramics SA
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Abstract

本发明涉及一种用于制造陶瓷基复合材料部件的方法，所述方法至少包括：用至少包含硅的熔体渗透组合物渗透包含粉末组合物的纤维结构，以在所述纤维结构的孔隙中形成陶瓷基质，所述粉末组合物至少包含碳化硅颗粒，其中所述碳化硅颗粒具有双峰尺寸分布，其中第一组(E1)碳化硅颗粒具有第一平均尺寸(TM1)，第二组(E2)碳化硅颗粒具有小于所述第一平均尺寸的第二平均尺寸(TM2)，所述第一组中的颗粒数量大于所述第二组中的颗粒数量。

Description

复合材料部件的制造方法
本发明涉及通过熔体渗透技术制造陶瓷基复合材料(CMC)部件。
发明背景
CMC部件可以通过熔体渗透技术形成。根据这种技术，可将熔融硅引入包含碳化硅颗粒的纤维结构的孔隙中，以形成使纤维结构致密化的陶瓷基质。
在这种技术中，理想的是熔融硅能均匀地、完全地渗入纤维结构的孔隙中，从而使所得到的部件具有最小的残余孔隙率，因此具有优化的机械性能。
然而，由于熔融硅进入孔隙的程度可能受到限制，导致熔融硅不均匀地渗透到纤维结构中，因此，一些已知的熔融浸渗技术并不能给出完全令人满意的结果。
这种不均匀性在纤维结构中存在碳颗粒的反应性熔体渗透技术中可能更加明显。在后一种情况下，熔融硅与碳颗粒之间的反应产物确实会导致预制件孔隙的局部堵塞，使熔融硅更难前进。
发明内容
根据第一方面，本发明涉及一种用于制造陶瓷基复合材料部件的方法，所述方法至少包括：
用至少包含硅的熔体渗透组合物渗透包含粉末组合物的纤维结构，以在所述纤维结构的孔隙中形成陶瓷基质，所述粉末组合物至少包含碳化硅颗粒，
其中所述碳化硅颗粒具有双峰尺寸分布，其中第一组碳化硅颗粒具有第一平均尺寸，第二组碳化硅颗粒具有小于所述第一平均尺寸的第二平均尺寸，所述第一组中的颗粒数量大于所述第二组中的颗粒数量。
“平均粒度”定义为统计粒度分布到总体一半的尺寸，称为D50。
对存在于纤维结构的孔隙中的碳化硅颗粒实施如上所述的双峰分布，导致孔隙网络促进纤维结构内渗透组合物的推进。这导致纤维结构的均匀致密化，从而使CMC部件具有改进的机械性能。
在一个示例性实施方式中，第一组颗粒按数量占粉末组合物中全部碳化硅颗粒的至少60％。
在示例性实施例中，第一平均尺寸在1μm和5μm之间。
在一个示例性实施方式中，第二组颗粒按数量占粉末组合物中全部碳化硅颗粒的至多40％。
在示例性实施方式中，第二平均尺寸在0.1μm和1μm之间。
在一个实例性实施方式中，第一组颗粒按数量占粉末组合物中全部碳化硅颗粒的60％到90％之间，并且第二组颗粒按数量占粉末组合物中全部碳化硅颗粒的10％到40％之间。
在一个示例性实施方式中，粉末组合物还包含碳颗粒。
本发明在粉末组合物中存在碳的情况下尤其有利，因为通过促进熔融硅的前进，降低了已知技术中遇到的局部堵塞的风险。
或者，粉末组合物可以不含碳颗粒。
在一个示例性实施方式中，粉末组合物中碳颗粒的体积含量大于或等于5％，例如20％。
在一个示例性实施方式中，纤维结构可以包括氧含量以原子百分比计小于或等于1％的碳化硅纱线。
在示例性实施方式中，纤维结构通过三维编织或由多个二维纤维层形成。
在一个示例性实施方式中，在渗透之前，纤维结构被陶瓷基质的第一相部分致密化。
在示例性实施方式中，制造的部件是涡轮发动机部件。该部件可以是航空发动机或工业涡轮机的燃气轮机的热段部件。特别地，该部件可以是喷嘴、燃烧室壁、涡轮环扇区或涡轮发动机叶片的至少一部分。
附图说明
参考以非限制性的方式提供的附图，在以非限制性的方式给出的以下描述中，本发明的其他特征和优点将变得显而易见。
图1是示出根据本发明的方法的示例的一系列步骤的流程图；
图2是可用于本发明的碳化硅颗粒双峰尺寸分布的示例；
图3A和3B是说明当使用具有单峰分布的碳化硅颗粒时获得的毛细上升的照片；
图4A和4B是说明使用具有图2的双峰尺寸分布的碳化硅颗粒时获得的毛细上升的照片；以及
图5是说明在根据本发明的方法的实例中获得的毛细上升的照片。
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CMC部件的制造过程的示例。
该方法的第一步骤S10可以包括形成纤维结构，例如通过三维编织。纤维结构可以由陶瓷纱线，例如碳化硅纱线形成。纤维结构可形成待生产的复合材料部件的纤维增强体。在步骤S10中获得的纤维结构可形成待生产部件的纤维预制件。
可使用的碳化硅纱线的示例有日本NGS公司销售的“Nicalon”、“Hi-Nicalon”或“Hi-Nicalon-S”纱线。纤维结构的陶瓷纱线的氧含量以原子百分比计可达到1％。例如，“Hi-Nicalon-S”纱线就有这样的特点。
“三维编织”或“3D编织”是一种编织方法，其中至少一些经纱将纬纱束缚在多个纬纱层上。在本文中，经纱和纬纱之间的角色倒置是可能的，并且必须认为也被权利要求所涵盖。纤维结构例如可以具有互锁编织。术语“互锁编织”是指一种3D编织，其中每层经纱将几层纬纱连接在一起，同一经纱列的所有纱线在织物平面内的运动相同。
也可以从纤维织构(例如，二维织物或单向网)开始，并通过将此类纤维织构悬垂在模型(forme)上来获得纤维结构。这些织构也可以粘合在一起，例如通过缝纫或植入纱线来形成纤维结构。
在步骤S20中，通过化学气相渗透(CVI)可在纤维结构的纱线上形成脆化释放界面。
界面的厚度可以例如在10nm到1000nm之间，并且例如在10nm到100nm之间。在形成界面之后，纤维结构保持多孔，只有很少的初始可进入孔隙被界面填充。
界面可以是单层或多层。界面可以包括至少一层热解碳(PyC)、氮化硼(BN)、掺杂硅的氮化硼(BN(Si)，其中硅的质量比在5％至40％之间，其余为硼氮化物)或掺硼碳(BC，硼的原子比例为5％至20％，其余为碳)。
在此，界面具有使复合材料脆化释放的功能，其促进了在基质中传播后到达界面的可能裂纹的偏转，从而防止或延迟了由此类裂纹引起的纤维断裂。另外，应当注意，可以在形成纤维结构之前，即在执行步骤S10之前，在纱线上形成界面。
接下来执行步骤S30，该步骤S30是在纤维结构的孔隙中，在先前可能已经在纱线上形成的界面上形成陶瓷基质的第一相。基质的第一相可以通过化学气相渗透形成。第一陶瓷基质相可以例如由SiC和/或Si3N4组成。
在该步骤S30之后并且在引入粉末组合物之前，纤维结构的残余孔隙率可以高于或等于25％，例如在30％至35％之间。通常，在步骤S30之后纤维结构的残余孔隙率足以允许将粉末组合物引入到纤维结构的孔隙中并且通过引入渗透组合物形成第二基质相。
可以通过浆料浇铸将粉末组合物引入纤维结构中(步骤S40)。这样的引入技术本身是已知的。
粉末组合物包含至少两组均具有不同平均尺寸(尺寸D50)的碳化硅颗粒。
具有最高平均尺寸的一组碳化硅颗粒比具有最低平均尺寸的一组碳化硅颗粒多得多。
在一个实例性实施方式中，第一组颗粒按数量占粉末组合物中全部碳化硅颗粒的60％到90％之间，并且第二组颗粒按数量占粉末组合物中全部碳化硅颗粒的10％到40％之间。
在示例性实施方式中，第一平均尺寸在1μm至5μm之间，并且第二平均尺寸在0.1μm至1μm之间。
碳化硅颗粒的粒度分布可以通过本身已知的方式通过激光衍射技术确定。
碳化硅颗粒在粉末组合物中具有双峰尺寸分布。图2示出了可以在本发明中使用的这种双峰分布的示例。在该图中，对于给定的粒径x，纵坐标表示具有该粒径x的颗粒的分数。尺寸分布可以是数字分布。
硅颗粒限定第一组碳化硅颗粒E1和第二组碳化硅颗粒E2。
双峰分布是不对称的。双峰分布具有两个不同的峰值(最大值)P1和P2。第一组E1的分布的峰值P1的高度可以不同于，例如高于第二组E2的分布的值峰P2的高度。特别地，峰值P1的高度可以大于峰值P2的高度的两倍甚至三倍。
第一组E1和第二组E2中的每一个的分布可以对应于正态分布。第一组E1的颗粒具有第一平均尺寸TM1，第二组E2的颗粒具有第二平均尺寸TM2。第一平均尺寸TM1大于第二平均尺寸TM2。第二平均尺寸TM2可以与第一平均尺寸TM1相距第一组E1的分布至少两个或甚至至少三个标准偏差。第一平均尺寸TM1和第二平均尺寸TM2之间的差异(数量TM1-TM2)可以大于或等于1μm，例如2.5μm。
作为具有可用于本发明的具有双峰尺寸分布的碳化硅颗粒的示例，可以提及由H.C Starck公司以“B-hp”名称销售的碳化硅粉末。
一旦将粉末组合物引入纤维结构中，例如通过注入浆料，就可以干燥纤维结构。然后获得填充有粉末组合物的纤维结构。粉末组合物存在于纤维结构的孔隙中。
如上所述，粉末组合物还可以包含碳颗粒，例如，其体积含量为5％至30％。可以使用的碳颗粒的例子是Lehmann&Voss&Co以“
Figure BDA0002719352850000051
MT N-991”名称出售的颗粒。可替代地，粉末组合物可以不含碳颗粒。
一旦引入粉末组合物，就执行步骤S50，在该步骤中，用至少包含硅的熔体渗透组合物渗透纤维结构的孔隙，以在纤维结构的孔隙中形成陶瓷基质。该陶瓷基质的形成可用于完成部件的致密化。
该渗透步骤对应于熔体渗透步骤。渗透组合物可以是纯熔融硅，或者可以是硅和一种或多种其他成分的熔融合金的形式。渗透组合物可主要包含按质量计的硅，即硅质量含量大于或等于50％。渗透组合物可以例如具有大于或等于75％的硅质量含量。硅合金中存在的成分可以选自B、Al、Mo、Ti及其混合物。当粉末组合物包含碳颗粒时，在渗透过程中渗透组合物与这些碳颗粒之间可能发生化学反应，从而导致碳化硅的形成。
在步骤S50之后，获得CMC部件。这样的CMC部件可以是涡轮发动机的静态或旋转部件。上面已经提到了涡轮发动机部件的例子。在使用之前，这样的部件也可以涂覆有环境屏障涂层或隔热涂层。
在图1中描述了其中在执行熔体渗透之前在步骤S30期间将纤维结构预致密化的示例，但是当然，当不是这种情况时，也不超出本发明的范围。整个基质可以在渗透步骤中由熔融硅形成。
图3A、3B、4A和4B示出由碳化硅和碳粉的混合物制成的生坯在渗入熔融硅之后获得的结果。
图3A和3B示出了当使用具有单峰尺寸分布的碳化硅粉末时获得的结果。具有这种尺寸分布的碳化硅颗粒不能用于本发明。
图4A和4B示出了当使用具有图2的双峰分布的碳化硅粉末时获得的结果。这些碳化硅颗粒可用于本发明中。在图3A和4A中，在生坯中存在按体积计70％的碳化硅颗粒和按体积计30％的碳颗粒。在图3B和4B中，在生坯中存在按体积计80％的碳化硅颗粒和按体积计20％的碳颗粒。
发明人发现，当使用具有单峰尺寸分布的碳化硅颗粒时，熔融硅的毛细上升是不完整的(图3A和3B)。另一方面，当使用如上所述具有双峰尺寸分布的碳化硅颗粒时，熔融硅的毛细上升完整(图4A和4B)。
图5中的照片显示了通过熔融硅对纤维结构进行渗透后获得的结果，该纤维结构先前填充有粉末组合物，其包含按体积计80％的碳化硅颗粒(具有图2所示的双峰尺寸分布)和按体积计20％的碳颗粒。可以看出，熔融硅能够浸渍纤维结构的整个长度，并获得均匀致密化。
在图5中，致密纤维结构长度的第一半部分位于顶部，致密纤维结构长度的第二半部分位于底部。渗透过程中的阻塞现象不明显，并且获得了均匀的致密化。
表述“包括在...与...之间”应理解为包括边界。

Claims (10)

1.一种制造陶瓷基复合材料部件的方法，至少包括：
用至少包含硅的熔体渗透组合物渗透包含粉末组合物的纤维结构，以在所述纤维结构的孔隙中形成陶瓷基质，所述粉末组合物至少包含碳化硅颗粒，
其中所述碳化硅颗粒具有双峰尺寸分布，其中第一组(E1)碳化硅颗粒具有第一平均尺寸(TM1)，第二组(E2)碳化硅颗粒具有小于所述第一平均尺寸的第二平均尺寸(TM2)，所述第一组中的颗粒数量大于所述第二组中的颗粒数量。
2.根据权利要求1所述的方法，其中所述第一组(E1)颗粒按数量占所述粉末组合物中全部碳化硅颗粒的至少60％。
3.根据权利要求1或2所述的方法，其中所述第一平均尺寸(TM1)在1μm和5μm之间。
4.根据权利要求1至3中任一项所述的方法，其中所述第二组(E2)颗粒按数量占所述粉末组合物中全部碳化硅颗粒的至多40％。
5.根据权利要求1至4中任一项所述的方法，其中所述第二平均尺寸(TM2)在0.1μm至1μm之间。
6.根据权利要求1至5中任一项所述的方法，其中所述第一组(E1)颗粒按数量占粉末组合物中全部碳化硅颗粒的60％到90％之间，并且其中所述第二组(E2)颗粒按数量占粉末组合物中全部碳化硅颗粒的10％到40％之间。
7.根据权利要求1至6中任一项所述的方法，其中所述粉末组合物还包含碳颗粒。
8.根据权利要求7所述的方法，其中所述粉末组合物中碳颗粒的体积含量大于或等于5％。
9.根据权利要求1至8中任一项所述的方法，其中所述纤维结构通过三维编织或由多个二维纤维层形成。
10.根据权利要求1至9中任一项所述的方法，其中所述部件是涡轮发动机部件，并且其中所述纤维结构是所述涡轮发动机部件的纤维预制件。
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