CN111542431A - 通过将粉末注入纤维增强件并由复合过滤层排出,制备由复合材料制成的部件的方法 - Google Patents
通过将粉末注入纤维增强件并由复合过滤层排出,制备由复合材料制成的部件的方法 Download PDFInfo
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- CN111542431A CN111542431A CN201880084323.XA CN201880084323A CN111542431A CN 111542431 A CN111542431 A CN 111542431A CN 201880084323 A CN201880084323 A CN 201880084323A CN 111542431 A CN111542431 A CN 111542431A
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- filter layer
- fibrous
- refractory ceramic
- fibrous structure
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Abstract
一种复合材料部件的制备方法,其包括以下步骤:由耐火陶瓷纤维形成纤维织构体(10);在模具(110)中放置纤维织构体(10),在纤维织构体和排出端口(112)之间插入过滤层(130),该过滤层(130)包括部分致密化的纤维结构;将含有耐火陶瓷颗粒(1500)的浆料(150)加压注入纤维织构体(10);通过过滤层(130)排出已经通过纤维织构体(10)的浆料的溶剂,并且通过过滤层(130)将耐火陶瓷颗粒的粉末保留在该织构体内,从而获得至少包括填充有耐火陶瓷颗粒(1500)的纤维织构体(10)和过滤层(130)的纤维预制件;对存在于预制件的纤维织构体(10)中的耐火陶瓷颗粒(1500)进行热处理以形成复合材料部件,该复合材料部件至少包括由耐火陶瓷基质致密化的纤维织构体和过滤层。
Description
技术领域
本发明涉及用于制造部件的方法,所述部件由热结构复合材料制得,特别是由氧化物/氧化物类型或陶瓷基质复合物(CMC)制成,即包括由耐火陶瓷材料纤维形成的纤维增强件,该耐火陶瓷材料被也是由耐火陶瓷材料制成的基质致密化。
背景技术
由氧化物/氧化物复合材料制成的部件通常通过以下方式来制造:在模具中铺设多个纤维层,该层由耐火氧化物纤维制成,每个层预先用填充有耐火氧化物颗粒的浆料进行浸渍。然后,这样布置的层的组件通过反凸模具或真空油布和高压釜中的通道被压实。然后,对这样获得的填充预制件进行烧结或陶瓷化热处理,从而在预制件中形成耐火氧化物基质并获得由氧化物/氧化物复合材料制成的部件。该技术也可以用于制造碳基陶瓷基质复合物(CMC)部件。在这种情况下,纤维层由碳化硅(SiC)或碳纤维制成,并且用填充有碳化物(例如SiC)、硼化物(例如TiB2)、硅化物(例如MoSi2)或氮化物(例如Si3N4)颗粒的浆料进行浸渍。
另一种通过液体途径制造由氧化物/氧化物复合物或CMC材料制成的部件的解决方案包括以下步骤:用浆料浸渍纤维织构体,例如在氧化物/氧化物复合材料的情况中用填充有氧化铝颗粒的浆料进行浸渍,或者在CMC材料的情况中用填充有碳化硅(SiC)颗粒的浆料进行浸渍。浸渍步骤是通过在压力下在纤维织构体中注入填充浆料(浆料传递模塑(Slurry Transfer Moulding),或STM)来进行的。在这种情况下,必须排出或过滤浆料的液相,以获得固体填料对纤维织构体中存在的残余孔隙的最佳填充。在文献WO 2016/102839中描述了这种工艺。因此,有必要使用插入纤维织构体和模具中供浆料的溶剂从中抽出的部分之间的过滤器元件。过滤器元件可以由多孔材料刚性件形成,当注入填充浆料并过滤溶剂后将纤维织构体从模具中移出时,其必须与纤维织构体分离。
这种过滤器元件的使用会引起困难。实际上,将其从纤维织构体中去除可能是困难的,并可能导致注入的纤维织构体降解。此外,在纤维织构体具有复杂几何形状的情况下,同时适应模具几何形状和纤维织构体的过滤器元件可能难以设计。
发明内容
本发明的目的在于改进上述缺点并提出一种解决方案,该解决方案通过在纤维织构体中注入填充浆料,有利于制备由陶瓷基质复合物(CMC)、氧化物、碳化物或碳基复合材料制成的部件。
为此,本发明提供一种制造复合材料部件的方法,所述方法包括以下步骤:
·由耐火陶瓷纤维形成纤维织构体,
·在具有至少一个注入端口和至少一个排出端口的模具中放置纤维织构体,在纤维织构体和所述至少一个排出端口间插入过滤层,该过滤层包括部分致密化的纤维结构,
·将含有耐火陶瓷颗粒的浆料加压注入纤维织构体,
·通过过滤层排出已经通过纤维织构体的浆料的溶剂,并且通过过滤层将耐火陶瓷颗粒保留在所述织构体内,从而获得至少包括填充有耐火陶瓷颗粒的纤维织构体和过滤层的纤维预制件,溶剂通过所述至少一个排出端口排出,
·对存在于预制件的纤维织构体中的耐火陶瓷颗粒进行热处理以形成复合材料部件,该复合材料部件至少包括由耐火陶瓷基质致密化的所述纤维织构体和过滤层。
因此,通过使用作为最终复合材料部件的组成部分的过滤层,消除了去除现有技术中所使用的过滤器元件的问题。此外,该过滤层不是刚性的并可以成形为不同的几何形状,其有利于制备具有复杂形状的复合部件。
根据本发明方法的具体特征,过滤层含有与纤维织构体的耐火陶瓷纤维性质相同的耐火陶瓷纤维,用经预烧结的与沉积在纤维织构体中的耐火陶瓷颗粒性质相同的耐火陶瓷颗粒将过滤层部分致密化。
根据本发明方法的另一个具体特征,过滤层的平均孔径在0.1μm至20μm之间,平均体积孔隙率小于50%。
根据本发明方法的另一个具体特征,纤维织构体包括通过二维编织或三维(或多层)编织或自动放置单向纤维而获得的纤维结构。
根据本发明方法的另一个具体特征,纤维织构体对应于与多孔或充气结构的一个面相对放置的纤维皮,该纤维皮和多孔结构被放置在模具中,并且在所述纤维皮和所述多孔结构间插入过滤层,获得的复合材料部件包括由耐火陶瓷基质致密化的纤维皮、过滤层和多孔结构。
根据本发明方法的另一个具体特征,纤维织构体对应于与多个泡状结构的面相对放置的纤维皮,该纤维皮和泡状结构被放置在模具中,并且在所述纤维皮和所述泡状结构间插入过滤层,获得的复合材料部件包括由耐火陶瓷基质致密化的纤维皮、过滤层和泡状结构。
根据本发明方法的另一个具体特征,模具具有环形或截头圆锥形的旋转几何形状,当放置在模具中时,纤维织构体和过滤层根据环形或截头圆锥形的旋转几何形状成形。在这种情况下,获得的复合材料部件可以特别构成飞机发动机的主体后部、燃烧室或曲柄箱。
预制件的纱线可以是由纤维形成的纱线,所述纤维由以下材料中的一种或多种构成:氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅和碳。
耐火陶瓷颗粒可以由选自以下的材料制成:氧化铝、莫来石、二氧化硅、铝硅酸盐、铝磷酸盐、氧化锆、碳化物、硼化物、硅化物和氮化物或这些材料中的几种的混合物。
附图说明
本发明的其它特点和优势通过下文关于本发明具体实施方式的描述并参照附图而显而易见,所述具体实施方式以非限制性示例的形式给出,附图中:
·图1是根据本发明的一实施方式的工具的示意性分解透视图,
·图2是显示由位于其中的纤维织构体和过滤层密闭的,图1的工具的示意性剖视图,
·图3是显示根据本发明的一实施方式,用填充到图2的工具中的浆料浸渍纤维织构体的步骤的示意性剖视图,
·图4是显示填充有耐火陶瓷颗粒的,图3的纤维织构体的示意性剖视图,
·图5是根据本发明的另一个实施方式的工具的示意性分解透视图,
·图6是显示由位于其中的纤维皮、过滤层和蜂窝结构密闭的,图5的工具的示意性剖视图,
·图7A至7C显示了旨在形成蜂窝结构的可展开纤维结构的制造;
·图8A至8C显示了形成蜂窝结构的另一个可展开纤维结构的制造;
·图9是显示根据本发明的一实施方式,用填充到图6的工具中的浆料浸渍纤维皮的步骤的示意性剖视图,
·图10是显示填充有耐火陶瓷颗粒的,图9的纤维皮的示意性剖视图,
·图11是显示所得预制件的示意性透视图。
具体实施方式
根据本发明的用于制造由复合材料,特别是由CMC类型的复合材料制成的部件的方法开始于制造旨在形成部件的增强件的纤维织构体。
纤维织构体是通过已知的方式用提花型织机(Jacquard type loom)进行编织来制造的,在该提花型织机上,将一束经纱或股线以多层形式布置,经纱通过纬纱连接,反之亦可。纤维织构体可以通过堆叠由二维(2D)编织得到层的或层片来实现。纤维织构体也可以通过三维(3D)编织直接以单件形式制得。“二维编织”是传统的编织方法,通过该方法,每根纬纱从单个经纱层的纱线的一侧穿至另一侧,反之亦可。本发明的方法特别适用于,允许在2D纤维织构体中引入填充浆料,即通过堆叠2D层或层片而获得的具有显著厚度的织构体,即厚度至少为0.5mm、优选至少1mm的2D纤维结构。
“三维编织”或“3D编织”或“多层编织”是指一种编织方法,通过该编织方法,至少一些纬纱将几层经纱上的经纱以编织的方式结合在一起,反之亦可,该编织的方式对应于可以特别从以下编织中选择的编织:互锁(interlock)编织、多纬(multi-weft)编织、多缎纹(multi-satin)编织和多斜纹(multi-twill)编织。
本文所用术语“互锁编织”是指3D编织,其中每层经纱将几层纬纱连接,而同一经列的所有纱线在编织平面内的运动相同。
本文所用术语“多平纹编织”是指使用多层纬纱的3D编织,每个层的基本织法(basic weave)等同于常规的平纹编织,但是编织中的某些点将纬纱层结合在一起。
本文所用术语“多缎纹编织”是指使用多层纬纱的3D编织,每个层的基本织法等同于常规的缎纹编织,但是编织中的某些点将纬纱层结合在一起。
本文所用术语“多斜纹编织”是指使用多层纬纱的3D编织,每个层的基本织法等同于常规的斜纹编织,但是编织中的某些点将纬纱层结合在一起。
3D织构体具有复杂的几何结构,其中很难引入和均匀分布悬浮的固体颗粒。本发明的方法也非常适合将填充浆料引入3D编织纤维织构体中。
纤维织构体也可以由单向(UD)层或网制得,所述单向层或网如文献US9102571或US2015/328799所述成形。
用于编织旨在形成复合部件的纤维增强件的纤维织构体的纱线可具体由耐火陶瓷纤维制成,所述耐火陶瓷纤维由以下材料中的一种制成:氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅、碳或这些材料中的几种的混合物。
在制得纤维织构体后,将其放置在根据本发明的包含过滤层的模具中,如下所述,其允许用耐火陶瓷颗粒将纤维织构体致密化。
根据图1和图2所示的第一实例,将纤维织构体10放置在工具100中。在这里描述的实例中,纤维织构体10根据如上所述技术(UD或2D层堆叠或3D编织)之一由Nextel 610TM氧化铝纱线制成。纤维织构体10在此旨在形成由氧化物/氧化物复合材料制成的部件的纤维增强件。
工具100由模具110和反凸模具120组成。模具110包括具有孔道112的底部111。模具110还包括侧壁113,其与底部111形成模腔114。在所示实例中,工具100(其中存在有纤维织构体10)在其下部被模具110封闭,并且在其上部被反凸模具120封闭,该反凸模具120形成封闭工具100的盖。模具110和反凸模具120用于确定预制件的尺寸,从而确定所获得的部件的尺寸,并用于调节所获得的部件中的纤维含量。
反凸模具120具有多个注入端口121,旨在通过该注入端口121注入填充有耐火陶瓷颗粒的液体以通过纤维织构体10的第一面10a渗透纤维织构体10的孔隙。图1和图2所示的实例中,旨在通过在模腔的不同区域中开放的多个注入端口121注入填充液体。然而,当液体通过单个注入端口注入时,并不超出本发明的范围。
模具110进而具有单个液体孔道112。当然,当实施多个出口孔道时,并不超出本发明的范围。
根据本发明,将过滤层130插入到纤维织构体10和包括孔道112的模具110的底部111之间。根据本发明的过滤层对应于通过沉积单向(UD)、二维(2D)或三维(3D)编织的耐火陶瓷纤维纱线获得的纤维结构,该耐火陶瓷纤维纱线由以下材料中的至少一种制成:氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅、碳或这些材料中的几种的混合物。过滤层优选由与纤维织构体的耐火陶瓷纤维性质相同的耐火陶瓷纤维制成。过滤层的厚度优选为0.1mm至1mm。
在这里描述的实例中,过滤层130对应于由Nextel 610TM氧化铝纱线制成的2D织物层。
根据本发明,将过滤层部分致密化以在该层中形成给定尺寸的孔隙网,该孔隙网允许浆料的滤液(即其液相)通过,同时保留存在于注入的浆料中的耐火陶瓷颗粒。
作为一个实例,过滤层被部分致密化后,其平均孔径可以在0.1μm至20μm之间,平均体积孔隙率可以小于50%。
旨在形成过滤层的纤维结构可以通过几种方法部分致密化。特别地,可以用填充有耐火颗粒的浆料预浸渍或注入纤维结构。在这种情况下,通过控制粒径、填充率和浆料中的粘合剂来调节颗粒预烧结后过滤层中的致密化率,从而调节孔隙率。也可以通过将填充有耐火颗粒的浆料注入纤维结构中来获得过滤层,最初引入的颗粒量控制堆叠厚度,从而控制最终基质体积比(Tvm)。涂覆或淬火工艺也可以用于将旨在形成过滤层的纤维织构体部分致密化。
在这里描述的实例中,过滤层130由氧化铝纱线2D织物制成,其注入了填充有25体积%的氧化铝颗粒的浆料,该颗粒已经被预烧结以将过滤层部分致密化。
由于在出口孔道112和注入端口121之间施加压力梯度,过滤层130允许浆料中的溶剂从纤维织构体10中排出并通过出口孔道112排出。
在将浆料注入纤维织构体10之前,可以通过夹紧模具或通过压机施加压实压力以压实模具110和反凸模具120间的纤维织构体10,并且可以在注射过程中保持该压实压力。如Polyflex法,压实压力也可以由压实液体经由膜施加。
任选地,可以在开始注入填充液体后施加并保持压实压力。压实压力的施加可用于压实织构体,以帮助排出液体并实现纤维预制件的目标厚度而不会损坏预制件。
在这里描述的实例中,填充液体是含有耐火陶瓷颗粒的浆料。图3显示了注入浆料150和从浆料中排出液体介质的过程中所获得的构造。在压力下将浆液150通过注入端口121注入以通过纤维织构体10的第一面10a渗透纤维织构体10。存在于浆料150中的耐火陶瓷颗粒1500旨在允许在纤维织构体10的孔隙中形成耐火陶瓷基质。在一个实例中,该耐火陶瓷基质可以是耐火氧化物基质。
浆料例如可以是氧化铝粉末在水中的悬浮液。氧化铝粉末的平均粒径(D50)可以在0.1μm和2μm之间。所用的氧化铝粉末可以是α-氧化铝粉末。
更一般地,浆液可以是含有平均粒径在0.1μm至10μm之间的耐火陶瓷颗粒的悬浮液。在注入之前,浆料中颗粒的体积含量可以在5%至50%之间。耐火陶瓷颗粒可以包括选自以下的材料:氧化铝、莫来石、二氧化硅、铝硅酸盐、铝磷酸盐、氧化锆、碳化物、硼化物、硅化物和氮化物或这些材料中的一种或多种的前体。取决于它们的基础组成,耐火陶瓷颗粒可以另外与氧化铝颗粒、氧化锆颗粒、铝硅酸盐颗粒、稀土氧化物颗粒、稀土硅酸盐颗粒(例如可以用于环境屏障或热屏障)或用于使所获得的复合材料部件功能化的任何其他填料(例如碳黑、石墨或碳化硅)混合。
用于浆料的溶剂例如可以包括具有酸性pH(即pH低于7)的水相和/或含有例如乙醇的醇相。浆料可以包括酸化剂,例如硝酸,并且液体介质的pH可以例如在1至5之间。浆料也可以包括有机粘合剂,例如聚乙烯醇(PVA),其可溶于水。
如图3所示,将浆料150注入纤维织构体10的孔隙中之后,存在耐火陶瓷颗粒1500。箭头151代表注入纤维织构体10的浆料150的运动。如图4所示,箭头152代表由过滤层130排出的浆料的介质或液相的运动。
反凸模具120在注入步骤过程中和之后在纤维织构体10上施加压力。
此外,在排出过程中可以在出口孔道112处进行泵吸P,例如使用初级真空泵进行。该泵吸改善排出并更快地干燥纤维织构体。
在该构造中,过滤层130使得最初存在于浆料中的颗粒1500能够保留在纤维织构体10中,并且该颗粒的全部或部分通过过滤沉积在纤维织构体10中。
在进行了注入和过滤步骤后,获得了纤维预制件15,其包括填充有耐火陶瓷颗粒的纤维织构体10和结合在织构体10上的过滤层130。在注入过程中,过滤层和纤维织构体之间实现了粘合。材料沉积在过滤层和纤维织构体之间,并且由于压实,组件是一体的。然后,烧结热处理在颗粒间形成桥,其使粘合完成。
然后将获得的预制件干燥,然后使其脱模,该预制件能够在脱模后保持模腔中采用的形状,例如由于浆料中存在的粘合剂(例如PVA),在模具和反凸模具之间压实之后采用的形状。
然后,对预制件进行热处理,例如这里是在空气中在1000℃至1200℃之间的温度下进行烧结,以预烧结耐火陶瓷颗粒,从而在纤维织构体和与其一体的过滤层的孔隙中形成耐火陶瓷基质。然后获得复合材料部件,例如氧化物/氧化物复合材料部件,其具有由纤维预制件形成的纤维增强件,该纤维增强件将纤维织构体和过滤层结合并具有高的基质体积比,并且耐火陶瓷基质在整个纤维增强件中均匀分布。
通过用碳化硅和/或碳的纤维制备纤维织构体和过滤层,并使用填充有碳化物(例如SiC)、硼化物(例如TiB2)、硅化物(例如MoSi2)或氮化物(例如Si3N4)颗粒的浆料,可以以相同的方式获得由氧化物/氧化物材料之外的CMC材料制成的部件。
可选地,注入织构体的填充液体可以含有耐火陶瓷前体的颗粒,例如溶胶-凝胶或聚合物类型。在这种情况下,热处理包括至少一个将耐火陶瓷前体转变为陶瓷材料的步骤(所谓的陶瓷化步骤),然后可能有另一个烧结步骤,以进一步使复合材料部件致密化。
图5至图9例示了根据本发明的一实施方式的用于制备声音衰减模块的方法。如图5和图6所示,将蜂窝结构300和纤维皮400放置于与蜂窝结构的上部面300a相对的工具200中。蜂窝结构300特别可以由金属材料或复合材料或整体陶瓷制成。在复合材料的情况下,蜂窝结构的纤维增强件可以通过多种方式实现,如US5415715中所述,例如,如图7A至7C所示,以交错的方式堆叠并粘合织物层311(例如氧化铝纤维)以形成坯件310。沿着平行的条带312实现层311之间的结合,其中层的一侧上的条带312相对于另一侧上的条带交错(图7A)。例如,可以通过胶粘或缝纫制造用于连接层311的条带312。将层叠体切割成垂直于胶水条带的切片313(图7B)。然后,沿垂直于层的面的方向(图7B中的箭头f1)拉伸每个切片,以通过变形得到具有六边形孔道314的泡状结构3100(图7C)。
根据图8A至8C所示的另一个实施方式,分层并针刺二维层321(例如由SiC纤维制成)以形成坯件320(图8A)。例如,层321是织物层或织物和纤维摇粒绒的复合物,该纤维摇粒绒提供纤维,该纤维可以容易地在针刺穿过层的过程中被针去除。如图8B所示,例如通过水射流或激光在坯件320中交错开设狭缝形切口322,其尺寸和位置限定蜂窝的尺寸和形状。在开设切口之后,将坯件320沿垂直于切口平面的方向拉伸,以通过变形形成蜂窝结构3200,这里蜂窝结构3200具有六边形孔道324(图8C中的箭头f2)。
根据另一个实施方式,可以通过在蜂窝壁的平面内布置织物条带并将这些条带在蜂窝间的结合部分处连接,以实现形成蜂窝结构的加强件的纤维结构。
根据另一个实施方式,如US9631519中所述,通过三维或多层编织来制备可展开纤维结构。
制备后,将蜂窝结构的纤维增强件致密化。在这里描述的实例中,首先用浆料浸渍旨在形成蜂窝结构300的纤维增强件的纤维坯件,该浆料对应于氧化铝粉末在水中的悬浮液。在去除浆料的液相后,展开预制件以使其具有多孔结构的形状。然后,对膨胀的坯件进行热处理以使其固结并形成自支承式蜂窝结构300。
在这里描述的实例中,纤维皮400由Nextel 610TM氧化铝纱线二维编织制成。纤维皮400在此旨在形成由氧化物/氧化物复合材料制成的声音模块皮的纤维增强件。
工具200包括模具210和反凸模具220。模具210包括具有多个孔道212的底部211。模具210还包括侧壁213,其与底部211形成模腔214。在所示实例中,工具200(其中存在有纤维皮400、过滤层230和蜂窝结构300)在其下部被模具210封闭,并且在其上部被反凸模具220封闭,该反凸模具220形成封闭工具200的盖。模具210和反凸模具220用于确定预制件的尺寸。
反凸模具220具有多个注入端口221,旨在通过该注入端口221注入填充有耐火陶瓷颗粒的液体以通过纤维皮400的第一面400a渗透纤维皮400的孔隙。图5和图6所示的实例中,通过在模腔的不同区域中开放的多个注入端口221注入填充液体。
根据本发明,将过滤层230插入到纤维皮400和泡状结构300之间,其位于具有孔道212的模具210的底部211上。根据本发明的过滤层对应于通过单向(UD)沉积、或二维(2D)或三维(3D)编织耐火陶瓷纤维纱线获得的纤维结构,该耐火陶瓷纤维纱线由以下材料中的至少一种制成:氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅、碳或这些材料中的几种的混合物。过滤层优选由与纤维皮的耐火陶瓷纤维性质相同的耐火陶瓷纤维制成。过滤层的厚度优选为0.1mm至1mm。
在这里描述的实施例中,过滤层230对应于由Nextel 610TM氧化铝纤维纱线制成的2D织物层。
根据本发明,将过滤层部分致密化以在该层中形成给定尺寸的孔隙网,该孔隙网允许浆料的滤液(即其液相)通过,同时保留存在于注入的浆料中的耐火陶瓷颗粒。
举例来说,过滤层被部分致密化后,其平均孔径可以在0.1μm至20μm之间,平均体积孔隙率可以小于50%。
旨在形成过滤层的纤维结构可以通过几种方法部分致密化。特别地,可以用填充有耐火颗粒的浆料预浸渍或注入纤维结构。在这种情况下,通过控制粒径、填充率和浆料中的粘合剂来调节颗粒预烧结后过滤层中的致密化率,从而调节孔隙率。也可以通过将填充有耐火颗粒的浆料注入纤维结构中来获得过滤层,最初引入的颗粒量控制堆叠厚度,从而控制最终基质体积比(Tvm)。涂覆或淬火工艺也可以用于将旨在形成过滤层的纤维织构体部分致密化。
在这里描述的实施例中,过滤层230由氧化铝纱线2D织物制成,其注入了填充有25体积%的氧化铝颗粒的浆料,该颗粒已经被预烧结以将过滤层部分致密化。由于在出口孔道212和注入端口221之间施加压力梯度,过滤层230允许液体从纤维皮400中排出并通过出口孔道212排出,该液体通过蜂窝结构300的孔道到达出口孔道212。
在这里描述的实例中,填充液体是含有耐火陶瓷颗粒的浆料。图9显示了注入浆料250和从浆料中排出液体介质的过程中所获得的构造。在压力下将浆液250通过注入端口221注入以通过纤维皮400的第一面400a渗透纤维皮400。存在于浆料250中的耐火陶瓷颗粒2500旨在允许在纤维皮400的孔隙中形成耐火陶瓷基质。在一个实例中,该耐火陶瓷基质可以是耐火氧化物基质。
浆料例如可以是氧化铝粉末在水中的悬浮液。氧化铝粉末的平均粒径(D50)可以在0.1μm和2μm之间。所用的氧化铝粉末可以是α-氧化铝粉末。
更一般地,浆液可以是含有平均粒径在0.1μm至10μm之间的耐火陶瓷颗粒或耐火陶瓷前体颗粒的悬浮液。在注入之前,浆料中颗粒的体积含量可以在20%至50%之间。耐火陶瓷颗粒可以包括选自以下的材料:氧化铝、莫来石、二氧化硅、铝硅酸盐、铝磷酸盐、氧化锆、碳化物、硼化物和氮化物或这些材料中的一种或多种的前体。取决于它们的基础组成,耐火陶瓷颗粒或耐火陶瓷前体可以另外与氧化铝颗粒、氧化锆颗粒、铝硅酸盐颗粒、稀土氧化物颗粒、稀土硅酸盐颗粒(例如可以用于环境屏障或热屏障)或用于使所获得的复合材料部件功能化的任何其他填料(例如碳黑、石墨或碳化硅)混合。
浆料的液体介质例如可以包括具有酸性pH(即pH低于7)的水相和/或含有例如乙醇的醇相。浆料可以包括酸化剂,例如硝酸,并且液体介质的pH可以例如在1至5之间。浆料也可以包括有机粘合剂,例如聚乙烯醇(PVA),其可溶于水。
如图9所示,将浆料250注入纤维皮400的孔隙中之后,存在耐火陶瓷颗粒2500。箭头251代表注入纤维皮400的浆料250的运动。如图10所示,箭头252代表由过滤层230排出的浆料的介质或液相的运动。
此外,在排出过程中可以在出口孔道212处进行泵吸,例如使用初级真空泵进行。该泵吸改善排出并更快地干燥纤维织构体。
在该构造中,过滤层230使得最初存在于浆料中的颗粒2500能够保留在纤维皮400中,并且该颗粒的全部或部分通过过滤沉积在纤维皮400中。
在进行了注入和过滤步骤后,获得了预制件35,其包括填充有耐火陶瓷颗粒或耐火陶瓷前体颗粒的纤维皮400、过滤层230和蜂窝结构300,过滤层230结合在纤维皮400和蜂窝结构300上。在注入过程中,过滤层和纤维皮之间实现了粘合。材料沉积在过滤层和纤维皮之间,并且由于压实,整体牢固地结合在一起。然后,烧结热处理在颗粒间形成桥,其使粘合完成。然后将获得的预制件干燥,然后使其脱模,该预制件能够在脱模后保持模腔中采用的形状。
然后,对预制件进行热处理,例如这里是在空气中在1000℃至1200℃之间的温度下进行预烧结,以使耐火陶瓷颗粒之间互相桥接,从而在纤维织构体和与其一体的过滤层的孔隙中形成耐火陶瓷基质。
结果是由复合材料制成的声音衰减模块,例如具有由纤维预制件形成的纤维增强件的氧化物/氧化物复合部件,其结合有纤维织构体、过滤层和蜂窝结构。
通过用碳化硅和/或碳的纤维制备纤维皮、过滤层和蜂窝结构,并使用填充有碳化物(例如SiC)、硼化物(例如TiB2)、硅化物(例如MoSi2)或氮化物(例如Si3N4)颗粒的浆料,可以以相同的方式获得由氧化物/氧化物材料之外的CMC材料制成的部件。
可选地,注入纤维皮的填充液体可以含有耐火陶瓷前体的颗粒,例如溶胶-凝胶或聚合物类型。在这种情况下,热处理包括至少一个将耐火陶瓷前体转变为陶瓷材料的步骤(所谓的陶瓷化步骤),然后可能有另一个烧结步骤,以进一步使复合材料部件致密化。
声音衰减模块的制备也可以通过在蜂窝结构的下侧形成第二皮进行补充。为此,将消声模块通过以下方式放置在与先前描述的工具200具有类似构造的模具中:将与先前描述的上部纤维皮400类似的下部纤维皮与蜂窝结构的下侧相对放置,将与过滤层230类似的过滤层插入纤维皮和蜂窝结构之间。在这种情况中,所使用的模具与工具200的不同之处在于,在相反的一侧注入填充浆料,即在工具200中存在孔道212的一侧注入,孔道随后被注入端口代替,并且从工具中存在注入端口221的一侧排出浆料的液相,注入端口随后被孔道代替。另外,为了使已经通过过滤层和蜂窝结构的浆料的液相排出,在上部皮上做了穿孔。这些穿孔可以有利地应用于后续的声音衰减模块的操作中。实际上,在此类模块的皮之一上做穿孔以利于捕获在泡状结构的泡中的声波是普遍的。
在声音衰减模块的另一实施方式中,将上部纤维皮和下部皮以及位于其二者之间的蜂窝结构放置在与上述工具200具有相似几何形状的工具中。在这种情况下,将填充浆料同时注入到上部和下部纤维皮中,并且在泡状结构(其上抵靠有一个或多个过滤层)的边缘上排出浆料中的溶剂。
在声音衰减模块的另一实施方式中,在与上述工具200相似的工具中将纤维皮与多个相邻的泡状结构相对放置,并且在纤维皮和泡状结构之间插入过滤层。与工具200中相同,模腔可以具有笔直或弯曲的形状。模腔也可以是完整的环形或环区段形状,其中放置有蜂窝结构、纤维皮和过滤层。通过这种方式,可以在单个操作中形成声音衰减模块,该声音衰减模块例如可以安装在诸如飞机发动机的装置周围。
在另一实施方式中,可以用通风结构代替蜂窝结构,例如波纹板金属或类似形式的通风结构。
本发明的方法也可以有利地用于制备具有复杂几何形状的复合材料部件,特别是具有半环形,环形和截头圆锥形的部件。因此,本发明的方法可用于制备由复合材料制成的部件,例如航空发动机的曲柄箱、燃烧室或主体后部(塞子)。在这种情况下,填充浆料的模具和注入工具匹配所制备部件的形状,所注入的纤维织构体和相关的过滤层容易符合工具的模具的几何形状,而若使用由多孔材料制成的刚性部件排出浆料的液相时会更加复杂。
Claims (10)
1.一种复合材料部件的制备方法,其包括以下步骤:
·由耐火陶瓷纤维形成纤维织构体(10),
·在具有至少一个注入端口(121)和至少一个排出端口(112)的模具(110)中放置纤维织构体(10),在纤维织构体和所述至少一个排出端口间插入过滤层(130),该过滤层(130)包括部分致密化的纤维结构,
·将含有耐火陶瓷颗粒(1500)的浆料(150)加压注入纤维织构体(10),
·通过过滤层(130)排出已经通过纤维织构体(10)的浆料的溶剂,并且通过过滤层(130)将耐火陶瓷颗粒的粉末保留在所述织构体内,从而获得至少包括填充有耐火陶瓷颗粒(1500)的纤维织构体(10)和过滤层(130)的纤维预制件,溶剂通过所述至少一个排出端口(112)排出,
·对存在于预制件的纤维织构体(10)中的耐火陶瓷颗粒(1500)进行热处理以形成复合材料部件,该复合材料部件至少包括由耐火陶瓷基质致密化的所述纤维织构体和过滤层。
2.如权利要求1所述的方法,其中,过滤层(130)含有与纤维织构体(10)的耐火陶瓷纤维性质相同的耐火陶瓷纤维,用经预烧结的与沉积在纤维织构体中的耐火陶瓷颗粒(1500)性质相同的耐火陶瓷颗粒将过滤层部分致密化。
3.如权利要求1或2所述的方法,其中,过滤层(130)的平均孔径在0.1μm至20μm之间,平均体积孔隙率小于50%。
4.如权利要求1至3中任一项所述的方法,其中,纤维织构体(10)包括通过二维编织或三维或多层编织或自动放置单向纤维而获得的纤维结构。
5.如权利要求1至3中任一项所述的方法,其中,纤维织构体对应于与多孔结构(300)的一个面(300a)相对放置的纤维皮(400),该纤维皮和多孔结构被放置在模具(210)中,并且在所述纤维皮和所述多孔结构间插入过滤层(230),获得的复合材料部件包括由耐火陶瓷基质致密化的纤维皮、过滤层和多孔结构。
6.如权利要求1至3中任一项所述的方法,其中,纤维织构体对应于与多个泡状结构的面相对放置的纤维皮,该纤维皮和泡状结构被放置在模具中,并且在所述纤维皮和所述泡状结构间插入过滤层,获得的复合材料部件包括由耐火陶瓷基质致密化的纤维皮、过滤层和泡状结构。
7.如权利要求1至3中任一项所述的方法,其中,模具具有环形或截头圆锥形的旋转几何形状,当放置在模具中时,纤维织构体和过滤层成形为环形或截头圆锥形的旋转几何形状。
8.如权利要求1至7中任一项所述的方法,其特征在于,纤维织构体的纱线是由纤维形成的纱线,所述纤维由以下材料中的一种或多种构成:氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅和碳。
9.如权利要求1至8中任一项所述的方法,其特征在于,耐火陶瓷颗粒由选自以下的材料制成:氧化铝、莫来石、二氧化硅、铝硅酸盐、铝磷酸盐、氧化锆、碳化物、硼化物、硅化物和氮化物或这些材料中的几种的混合物。
10.根据权利要求1至9中任一项所述的方法所获得的复合材料部件,其特征在于,该复合材料部件构成飞机发动机的主体后部、燃烧室或曲柄箱。
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PCT/FR2018/053527 WO2019129983A1 (fr) | 2017-12-28 | 2018-12-21 | Procede de fabrication d'une piece en materiau composite par injection de poudre dans un renfort fibreux avec drainage par strate de filtration composite |
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DE102020106043A1 (de) | 2020-03-05 | 2021-09-09 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Herstellung von (oxid-) keramischen Faserverbundwerkstoffen |
FR3124965B1 (fr) * | 2021-07-07 | 2024-04-05 | Safran Ceram | Procédé de fabrication d’une pièce en matériau composite par injection d’une barbotine chargée dans une texture fibreuse |
DE102021132136A1 (de) | 2021-12-07 | 2023-06-07 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Verfahren und Vorrichtung zur Herstellung keramischer Faserkomposite mit variabler Geometrie |
CN115194919A (zh) * | 2022-08-02 | 2022-10-18 | 北京理工大学唐山研究院 | SPS制备AlON透明陶瓷用模具及制备方法与所得透明陶瓷 |
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US20200339480A1 (en) | 2020-10-29 |
FR3076242B1 (fr) | 2020-01-10 |
EP3768405A1 (fr) | 2021-01-27 |
CN111542431B (zh) | 2023-04-11 |
EP3768405B1 (fr) | 2022-12-21 |
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