CN110382444A - 用于生产固结的纤维预制件的方法 - Google Patents

用于生产固结的纤维预制件的方法 Download PDF

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Publication number
CN110382444A
CN110382444A CN201880016796.6A CN201880016796A CN110382444A CN 110382444 A CN110382444 A CN 110382444A CN 201880016796 A CN201880016796 A CN 201880016796A CN 110382444 A CN110382444 A CN 110382444A
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fiber preform
prefabricated component
fiber
transient state
slurry
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CN110382444B (zh
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蒂埃里·盖·泽维尔·泰松
马克西姆·弗朗索瓦·罗杰·卡林
西蒙·蒂博
雷米·杜邦
拉姆齐·博利
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Safran SA
Safran Ceramics SA
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Safran SA
Safran Ceramics SA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

一种用于制造固结的纤维预制件的方法，所述纤维预制件用于制造一种由复合材料制成的部件，所述方法包括以下步骤：‑在加热的金属模具(20)中成形纤维织构(10)，所述织构被预先浸渍有瞬态或瞬时材料(30)，或在金属模具中成形纤维织构并将瞬态或瞬时材料注入到在所述金属模具中被保持形状的纤维织构内，‑冷却所述模具，‑从所述模具移除被固定的纤维预制件，‑用含有陶瓷或碳颗粒粉末的浆料涂覆所述纤维预制件，‑热处理被涂覆的纤维预制件，从而通过固结所述浆料而在所述纤维预制件周围形成一多孔的壳体，从而移除所述纤维预制件中存在的瞬态或瞬时材料，‑通过气相化学渗透固结所述纤维预制件。

Description

用于生产固结的纤维预制件的方法
技术领域
本发明涉及纤维预制件的固结以及由陶瓷或至少部分由陶瓷基复合材料，以下简称CMC材料制成的部件的制造。
本发明的一种应用领域是在使用过程中旨在接触高温的部件的生产，尤其是在航空航天领域，特别是热航空涡轮机部件的工件，已经注意到本发明可应用在其他领域，例如工业燃气轮机的领域。
背景技术
CMC复合材料具有良好的热结构性能，即使其能够形成结构部件并使其能够在高温下保持这些性能的高机械性能。
因此，已经建议对于在使用过程中接触高温的部件使用CMC材料代替金属材料，只要CMC材料的密度明显地低于它们所替换的金属材料。
一种由CMC材料制造部件的已知方法包括以下步骤：
-从碳或碳化硅(SiC)的纤维层编织一种纤维织构，
-通过在由化学蒸汽渗透(CVI)制成的织物的纤维表面上沉积中间相来固化纤维预制件，该纤维织物在CVI过程中保持在构象装置中，
-在纤维预制件中喷射浆料(“浆料浇铸”或“浆料传递模塑”)，
-用具有熔融的硅基组合物渗透所述预制件以形成陶瓷基质，致密化工艺被称为MI(“熔融渗透”)工艺，
-加工操作，
-形成涂层。
制造CMC部件的该方法需要在中间相的沉积过程中使用构象装置。这类装置对应于多孔模具，其内部形状可以与纤维织构一致，并且其多个穿孔可以在其几何结构中设置织构，同时允许在中间相的沉积过程中使用气相以穿透该织构并使其固结。该构象装置例如由石墨制成，因为这是一种与在中间相的沉积过程中所使用的反应性大气兼容的材料，同时相对于碳或碳化硅纤维无害。
然而，这类构象装置具有以下的缺点：
-成本高(纯石墨块的加工)，
-脆弱性(在石墨块的夹持过程中断裂的风险，对力的机械阻力差)，
-有限寿命(多种穿孔和夹持系统的污染)，
-频繁需要更换装置的夹持构件，
-由于用于装配和夹持工具的夹持构件而体积很大。
发明内容
本发明特别地旨在提供一种用于固化纤维预制件的技术方案，所述纤维预制件旨在制造一种由不具有上述缺点的复合材料制成的部件。
通过一种用于生产固结纤维预制件的方法实现了该目的，所述固结纤维预制件用于制造一种由复合材料制成的部件，所述方法包括以下步骤：
-在加热的金属模具中成形纤维织构，所述织构被预先浸渍有瞬态或挥发物质，或在金属模具中成形纤维织构并喷射瞬态或挥发物质到在所述金属模具中被保持适当形状的纤维织构内，
-冷却所述模具，
-从所述模具移除被设置的纤维预制件，
-用含有陶瓷或碳颗粒粉末的浆料涂层所述纤维预制件，
-热处理被涂层的纤维预制件，从而通过固结所述浆料而在所述纤维预制件周围形成一种多孔的壳体，并且从而移除所述纤维预制件中存在的瞬态或挥发物质，
-通过气相化学渗透固结所述纤维预制件。
根据本发明的方法允许明显地降低生产成本，尤其是由于与石墨构象装置相比具有更大的牢固性和寿命的金属模具的使用，这可以节省石墨构象器的循环更换成本。通过在金属模具中相对于石墨模具成形，进一步优化了预制件的尺寸控制。实际上，部件(不包括涂层)的原始最终形状由以下限定：
-所述金属模具，以及
-由部件的后续制造步骤所产生的超厚或任何变形，例如气相渗透、浆料喷射(“浆料浇铸”或“浆料传递模塑”)，或用预制件的熔融硅基组合物(熔融渗透，或MI)的渗透。此外，一旦在多孔壳体中设置形状，预制件可以经受用于制造由复合材料制成的部件的后续步骤，而无需使用构象装置。
根据本发明方法的第一方面，在通过气相化学渗透固化纤维预制件的步骤之前，在壳体中进行穿孔。这使得可以增加壳体的孔隙度，并增加预制件中材料的渗透和/或喷射的有效性。
根据本发明方法的第二方面，所述模具包括一种形状与待生产的纤维预制件的形状对应的成型腔，以及从所述成型腔延伸的一个或多个通道，所述通道在喷射纤维织构到模具内的过程中填充有瞬时或挥发物质，所述瞬时或挥发物质在移除所述预制件后在所述预制件的表面上形成突出元件，所述突出元件在热处理过程中被消除从而在壳体中形成通道开口。当人们希望增加其多孔性时，人们因此避免了在壳体形成后必须穿透它。所述突出元件也可以附接或形成在所述预制件上，在其被移除之后并且在其涂层有旨在形成壳体的浆料之前，这些元件例如能够手动地或通过加成制造附接在支撑件上，支撑件在这里为固结的预制件。
根据本发明方法的第三方面，所述瞬态或挥发物质对应于待喷射的蜡或挥发树脂。
根据本发明方法的第四方面，所述纤维预制件由通过三维或多层编织以单件制成的纤维织构或由多个三维纤维层制成。纤维织构尤其可以由碳化硅(SiC)、氮化硅(Si3N4)或碳(C)纤维制成。
根据本发明方法的第五方面，通过化学蒸气渗透固结所述纤维预制件的所述步骤包括在所述预制件中沉积中间相，所述中间相由以下材料之一组成：热解碳(PyC)、氮化硼(BN)、掺硼碳(BC)和碳化硅(SiC)。
本发明还涉及一种用于制造由复合材料制成的部件的方法，包括根据本发明的方法制造固结纤维预制件，以及在通过气相渗透的固结步骤之后振荡分离壳体的步骤，喷射浆料到所述纤维预制件内的步骤，以及用熔融的硅基组合物渗透所述预制件从而在所述预制件中形成陶瓷基质的步骤。
本发明进一步涉及一种制造由复合材料制成的部件的方法，包括根据本发明的方法生产固结纤维预制件，在通过气相渗透的固结步骤之后，喷射浆料到所述纤维预制件内的步骤，以及用熔融的硅基组合物渗透所述预制件从而在所述预制件中形成陶瓷基质的步骤。
附图说明
参照附图，在阅读作为非限制性示例提供的本发明具体实施例的以下描述时，本发明的其他特征和优点将显而易见，其中：
-图1至8是示出根据本发明一个实施例的纤维预制件的固结的示意图，
-图9是用于纤维预制件的致密化的气相渗透设备的剖面示意图，
-图10是根据本发明一个实施例的固结纤维预制件的剖面示意图，
-图11和12是示出根据本发明一个实施例变型的在固结纤维预制件表面上的分段的实施例的示意性剖面图，以及
-图13是根据本发明一个实施例的一种用于固化纤维预制件的方法的步骤的流程图。
具体实施方式
本发明首先提出了一种用于生产固结的纤维预制件的制造方法，所述纤维预制件用于制造一种由陶瓷基复合(CMC)材料制成的部件，即由由至少部分通过陶瓷基质致密化的碳或陶瓷纤维制成的增强件所形成的材料制成的部件。
本发明的方法的显著之处在于，其不使用石墨构象装置，从而通过化学气相渗透来固结所述纤维预制件。如下文中所详细解释的那样，根据本发明，石墨构象装置由一种围绕成形的纤维织构形成的牺牲壳体替代，所述壳体使得可通过化学蒸气渗透维持纤维织构在其固结过程中的成形。
将参照图1至13描述根据本发明方法的CMC材料的一实施例。
第一步骤S1(图13)包括生产纤维织构10，一种形状接近待制造部件的纤维预制件由所述纤维织构制成(图1)。这种纤维织构可以通过多层或三维编织由导线或电缆获得。也可以由例如织物或导线或电缆束的二维纤维织构形成接下来将编织为一种形状并可选择性地彼此结合合，例如通过导线的缝合或植入来结合的层。在这此所描述的例子中，纤维织构10用于形成一种由CMC材料制成的形状为Pi或倒π的涡轮环扇区，其具有环形底座，两个弯曲接片由所述环形底座延伸。为此，纤维织构10通过碳化硅或碳的三维编织制成，具有断开区域11和12，所述断开区域11和12布置为使得可分离与环扇区的弯曲凸缘对应的织构部件13和14(图2)。
如图所示，编织可以是互锁式的。可以使用其他的三维或多层编织，例如多布编织或多缎纹编织。具体可参照文献WO 2006/136755。
组成纤维织构的纤维优选为陶瓷纤维，例如基本由碳化硅SiC(以下称为SiC纤维)或氮化硅Si3N4形成的纤维。尤其可以使用日本Ube工业有限公司以商标“Tyranno ZMI”、“Tyranno Lox-M”和“Tyranno SA3”销售的SiC纤维，或日本Nippon Carbon公司以商标“Nicalon”、“Hi-Nicalon”和“Hi-Nicalon(S)”销售的SiC纤维。在一变例中，可以使用碳纤维。
在已知的方式中，对于陶瓷纤维，尤其是SiC纤维，在形成中间相沉积之前优选对SiC纤维进行表面处理，以消除纤维上存在的过度喷涂和表面氧化层，例如二氧化硅SiO2。
以下步骤包括在金属模具20中保持纤维织构的成形并设置金属模具20以获得一种形状接近待制造部件的预制件(图3)。为此，纤维织构10被放置在金属模具20中，其成型腔21对应于待制造部件的形状(步骤S2)，瞬态或瞬时材料30被注入由此保持形状的所述织构内(步骤S3)(图3)。根据一个实施变例，纤维织构10在其在金属模具中成型之前(步骤S5)，可以瞬态或瞬时材料浸渍(步骤S4)。瞬态或或瞬时材料优选具有大大高于环境温度(20℃±5℃)的熔化和蒸发温度，例如比环境温度(20℃±5℃)至少高50℃。瞬态或瞬时材料尤其可以由可喷射蜡或瞬态树脂制成，例如丙烯酸PMMA树脂或聚乙烯醇(PVA)树脂。
在金属模具冷却之后，移除纤维预制件40，由于其中瞬态或瞬时材料以固态存在，因此该预制件被固定并自支撑(步骤S6，图4)。
由此制成的纤维预制件40被涂覆以一种含有陶瓷或碳颗粒粉末的浆料50(步骤S7)。该粉末可由以下元素的一种或几种制成：氧化物型颗粒(二氧化硅、硅酸铝等)，带或不带胶态氧化硅的碳化硅颗粒，碳颗粒。可以通过在浆料50浴中浸泡纤维预制件(图5)或由本领域技术人员已知的任何其他技术(浸泡、喷洒、涂层、喷涂等)进行纤维预制件的涂覆。为了提高生产节奏并且降低部件的单位生产成本，可以考虑以串组装几个预制件。
因此由浆料50层(图6)涂覆的纤维预制件40在炉70中进行热处理，以烧结或预烧结浆料中存在的颗粒，从而固化预制件40表面上存在的浆料层并在预制件40周围形成壳体60，由此形成的壳体60为多孔的(步骤S8，图7)。以已知的方式，调节颗粒的速率和/或颗粒的尺寸，以获得一种具有与通过气态路径固结该预制件相兼容的孔隙度阵列的壳体。在该步骤中还移除了预制件40的瞬态或瞬时材料，在高于所述瞬态或瞬时材料的熔化和/或蒸发温度的温度下进行热处理。
可以在围绕该预制件的壳体中布置通风孔，所述通风孔可以促进瞬态或的排放。一旦完成了固结热处理，通过遮蔽预制件的某些部分并在壳体中形成通道，可以在用浆料涂覆预制件的过程中设置这些通风孔。通风孔也可以在壳体成形后在壳体中加工。这些通风口可在消除了瞬态或瞬时材料后选择性地再次被堵塞。
因此获得了与预制件60相对应的预制件80，其中通过移除瞬态或瞬时材料，已经重新打开了纤维之间存在的气孔排列，由于壳体60的存在(图8)，进而保持了预制件80的几何结构。壳体60为多孔的，因此，适于预制件80的化学蒸汽渗透。
可选择性地在壳体中穿孔以增加壳体的孔隙度，从而有利于渗透气体通过(步骤S9)。
在壳体的形成过程中也可以制成通道孔。为此，如图11所示，使用一种金属模具120，除与待制造部件的形状相对应的成型腔121外，金属模具120还包括延伸到成型腔121外围并与其连通的多个通道122。因此，在将瞬态或瞬时材料130注入模具12内的过程中，其不仅填充在成型腔121中保持的纤维织构110中存在的孔隙中，还填充在这些通道122中。在冷却和移除后，如图12所示，获得了在其表面具有由瞬态或瞬时材料制成的多个末端或直柱141的预制件140，这将使得可以在用浆料对预制件的随后涂覆的过程中保留通道。在浆料的固结热处理过程中接下来消除段141，从而在成形的壳体内形成孔或通道。因此避免了在壳体形成后必须对壳体穿孔。段可具有不同的形状，特别是非直线形状，使得可限定壳体内气体的不同循环几何结构。
一旦壳体形成，无论具不具有额外的穿孔或通道，固化通过纤维预制件的气相渗透来完成(步骤S10)。为此，如图9所示，保持在壳体60内侧的预制件80放置在化学蒸汽渗透设备或炉200中。以自身已知的方式，化学蒸汽渗透设备200包括一界定一反应室210的圆柱形的罩壳201，所述反应室210的上部由一设置有进气管221的可移除盖部220封闭，所述进气管221通向预热区域222，使得可以在气体在包含待致密化的预制件的反应室210中扩散之前加热气体。通过连接到抽吸装置(未示出)的排放管231，在设备底部230处抽取残余气体。底部230包括支撑件232，由壳体60围绕的预制件40将沉积在所述支撑件232上。
预热区域中以及反应室210内侧的加热由形成一与电感器(未示出)电磁耦合的电枢的石墨感受器211产生。
通过化学蒸汽渗透固结该预制件80。为了确保预制件的固结，含有固结中间相材料的至少一种或几种前驱体的活性气体被引入到反应室210中。沉积到预制件内的中间相具体可以由热解碳(PyC)、或氮化硼(BN)或掺硼碳(BC)(含5at％到20at％的硼，其余为碳)或碳化硅制成。沉积中间相的厚度优选在100nm到1500nm之间。选择中间相和第一基质相的总厚度从而足以固化该纤维预制件，即将预制件的纤维彼此间足以结合，使得可以在保持其形状的同时操纵该预制件，而无需借助于保持装置。该厚度可至少等于500nm。在固结后，预制件保持多孔，最初的孔隙例如仅由中间相和第一基质相填充很少的部分。
PyC、BC、B4C、Si-B-C、Si3N4、BN和SiC通过化学气相沉积法沉积的性能是已知的。具体可参照文献US 5,246,736、US 5,738,951、US 5,965,266、US 6,068,930和US 6,284,358。
一旦完成了固结，就实现了壳体的振荡分离，该壳体将被机械地破坏以便如图10所示释放出与固结的预制件80相对应的预制件100(步骤S11)。预制件100自支撑，并且对于随后的操作不需要任何的形状保持装置。预制件100尤其可以进行用于制造由CMC材料制成的部件的后续步骤，即：
-在该纤维预制件中注入浆料(“浆料浇铸”或“浆料转移浇铸”)，
-用具有熔融硅的基底的合成物渗透所述预制件，以形成陶瓷基质，已知为MI(“熔融渗透”)工艺的致密化工艺，
-加工操作，
-形成涂层。
在一个实施例变型中，可在注入浆料并用熔融的硅基合成物渗透的操作过程中保持壳体。
如下给出了一根据本发明的方法的固结的纤维预制件的示例，该纤维预制件用于制造由CMC复合材料制成的部件：
-通过三维编织互锁型的SiC纤维来生产纤维织构，
-用聚乙烯醇(PVA)浸渍所述纤维织构，
-在加热的金属模具中成形所述纤维织构，
-冷却所述模具，
-从所述模具移除设置的纤维预制件，
-用包含85at％的SiC和15at％的SiO2的胶状颗粒的混合物的浆料涂覆所述纤维预制件，
-在150℃下干燥被涂覆的预制件2小时，
-在1000℃下烧结涂覆纤维预制件的颗粒1小时，
-在700℃到900℃之间的温度下，通过气相化学渗透和或其上沉积的氮化物(BN)固结所述纤维预制件。

Claims (10)

1.一种用于生产固结的纤维预制件(100)的方法，所述纤维预制件用于制造一种由复合材料制成的部件，所述方法包括以下步骤：
-在一加热的金属模具(20)中成形一纤维织构(10)，所述织构被预先以瞬态或瞬时材料(30)浸渍，或在一金属模具中成形一纤维织构，并将瞬态或瞬时材料注入到在所述金属模具中被保持形状的该纤维织构内，
-冷却所述模具，
-从所述模具移除被放置的纤维预制件(40)，
-用含有陶瓷或碳颗粒粉末的浆料(50)涂覆所述纤维预制件，
-热处理该被涂覆的纤维预制件(40)，以通过所述浆料的固结而在所述纤维预制件周围形成一多孔的壳体(60)，从而移除存在于所述纤维预制件中的瞬态或瞬时材料(30)，
-通过气相化学渗透固结所述纤维预制件。
2.根据权利要求1所述的方法，其中，在通过气相化学渗透固结所述纤维预制件的步骤之前，在所述壳体(60)中进行穿孔。
3.根据权利要求1所述的方法，其中，所述模具(120)包括一成型腔(121)和一个或几个从所述成型腔延伸的通道(122)，所述成型腔的形状与待生产的所述纤维预制件的形状相对应，所述通道在将所述纤维织构(110)注入到所述模具中的过程中被填充以瞬态或瞬时材料(130)，所述瞬态或瞬时材料在移除所述预制件后在所述预制件(140)的表面上形成突出元件(141)，所述突出元件在热处理过程中被消除，从而在所述壳体中形成通道开口。
4.根据权利要求1所述的方法，还包括：在从所述模具移除所述预制件(40)的步骤之后以及在用浆料(50)涂覆该预制件的步骤之前，在所述预制件的表面上形成突出元件。
5.根据权利要求1至4中任一项所述的方法，其中，所述瞬态或瞬时材料(30)对应于待注入的蜡或瞬时树脂。
6.根据权利要求1至5中任一项所述的方法，其特征在于，所述纤维预制件(40)由通过三维或多层编织制成单件的纤维织构(10)形成或由多个三维纤维层制成。
7.根据权利要求1至6中任一项所述的方法，其特征在于，所述纤维织构(10)由碳化硅(SiC)、氮化硅(Si3N4)或碳(C)的纤维制成。
8.根据权利要求1至7中任一项所述的方法，其中，通过化学蒸气渗透固结所述纤维预制件(80)的步骤包括在所述预制件中沉积中间相，所述中间相由以下材料中的一种组成：热解碳(PyC)、氮化硼(BN)、掺硼碳(BC)和碳化硅(SiC)。
9.一种制造由复合材料制成的部件的方法，包括根据权利要求1至8中任一项所述的生产固结的纤维预制件(100)，所述制造方法还包括，在通过气相渗透进行固结的步骤之后振荡分离壳体的步骤，将浆料注入到所述纤维预制件内的步骤，以及用熔融的硅基合成物渗透所述预制件，从而在所述预制件中形成陶瓷基质的步骤。
10.一种制造由复合材料制成的部件的方法，包括根据权利要求1至8中任一项所述的生产固结的预制件，所述制造方法还包括，在通过气相渗透进行固结的步骤之后，将浆料注入到所述纤维预制件内的步骤，以及用熔融的硅基合成物渗透所述预制件，从而在所述预制件中形成陶瓷基质的步骤。
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