CN117545606A - 使用在纤维预制件中就地生成的过滤器注入陶瓷粉末的方法 - Google Patents

使用在纤维预制件中就地生成的过滤器注入陶瓷粉末的方法 Download PDF

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Publication number
CN117545606A
CN117545606A CN202280042575.2A CN202280042575A CN117545606A CN 117545606 A CN117545606 A CN 117545606A CN 202280042575 A CN202280042575 A CN 202280042575A CN 117545606 A CN117545606 A CN 117545606A
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fibrous texture
suspension
fibrous
filter layer
particles
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CN202280042575.2A
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迪迪埃·伊夫·乔治·莫卡尔
埃米莉·莱西扎
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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将陶瓷颗粒注入到纤维织构体(10)中的方法，包括：将纤维织构体(10)放置在模具(110)中，从一侧注入包含大过滤颗粒粉末的第一悬浮液以形成过滤层(130)，从相对侧向纤维织构体中注入第二悬浮液，该第二悬浮液包含小耐火陶瓷颗粒的粉末，然后通过所述过滤层(130)排出已经穿过所述纤维织构体的第二悬浮液的液相，以及通过过滤层将耐火陶瓷颗粒粉末保留在所述纤维织构体(10)内部，从而获得纤维预制件，该纤维预制件至少包括填充有耐火陶瓷颗粒的纤维织构体和过滤层(130)。

Description

使用在纤维预制件中就地生成的过滤器注入陶瓷粉末的方法
技术领域
本发明涉及一种用于将陶瓷颗粒注入到纤维织构体中的方法，该纤维织构体用于制造由氧化物/氧化物或陶瓷基复合材料(CMC)材料(即，包括：由耐火陶瓷材料的纤维通过也属于耐火陶瓷材料的基体致密化形成的纤维增强材料)制成的部件。
背景技术
通过注入制造由具有氧化物/氧化物或SiC/SiC类型的陶瓷基体的复合材料制成的部件通常包括：用填充悬浮液(例如在氧化物/氧化物CMC的情况下为氧化铝颗粒，或者在SiC/SiC CMC的情况下为碳化硅(SiC)颗粒)浸渍纤维织构体的步骤。浸渍步骤是通过在压力下将填充悬浮液注入纤维织构体内来进行的(浆料传递模塑(STM)工艺)。在这种情况下，有必要排出或过滤液相的悬浮液以便获得用固体填料对纤维织构体中存在的残余孔隙的最佳填充。这种方法尤其是在文献WO 2016/102839中进行了描述。因此，需要使用介于纤维织构体与模具的悬浮液中的溶剂被排空的部分之间的过滤元件。过滤元件可以由一块刚性多孔材料组成，在注入填充悬浮液和过滤溶剂之后，在其脱模期间，该块多孔材料必须与纤维织构体分离。
使用这样的过滤元件会带来困难。事实上，将其从纤维织构体中去除可能很困难，并导致注入的纤维织构体降解。此外，由于这种过滤元件是刚性的，因此难以适应复杂的部件几何结构。为了解决这些问题，可能需要用包括部分致密化的纤维结构的过滤层替代刚性多孔材料部件，该过滤层将是最终复合材料部件的组成部分。这种过滤层尤其是在文献WO 2019/129983中进行了描述。
然而，使用过滤层仍然存在缺点。实际上，过滤层包括纤维结构，该纤维结构必须被部分致密化以便在该层中形成具有精确的确定尺寸的孔隙网络，从而允许悬浮液溶剂通过，同时保留耐火陶瓷颗粒。因此，必须在过滤层被沉积到模具中之前制造和处理该过滤层，从而为注入工艺增加额外的步骤。
发明内容
本发明的目的在于弥补上述缺点并提出一种解决方案，该解决方案使得可以通过注入加载到纤维织构体中的悬浮液来促进由具有陶瓷基体(CMC)、氧化物、碳化物或碳基的复合材料制成的部件的注塑生产。
为此，本发明提出了一种用于将陶瓷颗粒注入到纤维织构体中的方法，包括以下步骤：
-将纤维织构体放置在模具中，该纤维织构体介于一个或多个第一孔道与一个或多个第二孔道之间，
-通过第一孔道注入包含粒径大于纤维织构体的孔隙网络的间隙尺寸的过滤颗粒粉末的第一悬浮液；
-通过纤维织构体排出第一悬浮液的液相，通过第二孔道排空所述液相并通过纤维织构体保留过滤颗粒，从而在所述纤维织构体与第一孔道之间形成过滤层，
-通过第二孔道将第二悬浮液注入到纤维织构体中，第二悬浮液包含粒径小于纤维织构体的孔隙网络的间隙尺寸的耐火陶瓷颗粒的粉末，
-通过过滤层排出已经穿过纤维织构体的第二悬浮液的液相，并通过过滤层将耐火陶瓷颗粒粉末保留在所述纤维织构体内部，从而获得纤维预制件，所述纤维预制件至少包括填充有耐火陶瓷颗粒的纤维织构体和过滤层，第二悬浮液的液相通过第一孔道被排空。
因此，由于产生形成最终复合材料部件的整体部分的过滤层，克服了移除过滤元件的问题并且极大地改善了部件的过滤器侧的表面状况。另外，与现有技术中使用的过滤层相比，简化了过滤器的制造，因为过滤器界面形成在模具本身内部。这避免了制造部分致密化的纤维织构体所需的预备步骤以及产生精确尺寸的孔隙网络所固有的困难。还省去了设置过滤层的操作。
根据本发明方法的一个具体特征，第一悬浮液的粉末是陶瓷或玻璃前体。
根据本发明方法的另一具体特征，过滤层的平均厚度在100μm与200μm之间。
根据本发明的方法的另一具体特征，第二悬浮液的颗粒的尺寸平均比纤维织构体的孔隙网络的间隙的平均尺寸小5至15倍。
根据本发明方法的另一具体特征，第二悬浮液的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、硅化物和氮化物或其中几种材料的混合物。
根据本发明的方法的另一具体特征，其中纤维织构体包括通过二维编织、或三维或多层编织、或单向纤维的自动放置而获得的纤维结构。
根据本发明方法的另一具体特征，纤维织构体的纱线由纤维形成，所述纤维由以下材料中的一种或多种材料组成：氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅和碳。
根据本发明的方法的另一具体特征，模具具有环形或截锥形的旋转几何结构，纤维织构体在放置于模具中时根据环形或截锥形的旋转几何结构成形。
附图说明
[图1]图1是根据本发明的一个实施例的工具的示意性分解透视图；
[图2]图2是示意性截面图，其示出了用定位在其中的纤维织构体封闭的图1的工具，并且示出了通过注入填充有过滤颗粒的第一悬浮液来形成过滤层，所述过滤颗粒的粒径大于纤维织构体的孔隙网络的间隙尺寸，
[图3]图3是示意性截面图，其示出了用纤维织构体和定位在其中的过滤层封闭的图1的工具，并且示出了用填充有粒径小于纤维织构体的孔隙网络的间隙尺寸的颗粒的第二悬浮液浸渍纤维织构体。
具体实施方式
纤维织构体已经以已知的方式通过二维编织或通过三维编织生产。
这里，“二维编织”是指一种传统的编织方法，其中，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悬浮液，即通过堆叠2D层或褶皱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”在这里是指一种编织方法，通过该编织方法，至少一些纬纱按照与编织图案相对应的编织方式将几层经纱上的经纱连接起来，反之亦可所述编织图案可以特别从以下图案中选择：互锁(interlock)、多平纹(multi-plain)、多缎纹(multi-satin)和多斜纹(multi-twill)。
“互锁图案或编织”在这里是指3D编织图案，其中，每层经纱将几层纬纱连接起来，而同一经列的所有纱线在编织平面内的运动相同。
“多平纹图案或编织”在这里是指使用多层纬纱的3D编织，每层纬纱的基本图案等同于传统的平纹图案，但是图案中的某些点将纬纱层连接在一起。
“多缎纹图案或编织”在这里是指使用多层纬纱的3D编织，每层纬纱的基本图案等同于传统的缎纹图案，但是图案中的某些点将纬纱层连接在一起。
“多斜纹图案或编织”在这里是指使用多层纬纱的3D编织，每层纬纱的基本图案等同于传统的斜纹编织，但是图案中的某些点将纬纱层连接在一起。
3D织构体具有复杂的几何结构，其中很难将固体颗粒引入并均匀分布在悬浮液中。本发明的方法也非常适合于将填充悬浮液引入3D编织纤维织构体中。
纤维织构体也可以由单向(UD)层或片材制成。
用于编织旨在形成复合材料部件的纤维增强件的纤维织构体的纱线尤其可以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组成：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。
根据图1至图3所示的第一示例，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是使用如上所述技术(UD或2D层堆叠或3D编织)之一由Nextel 610TM氧化铝纱线制成的。纤维织构体10在这里旨在形成由氧化物/氧化物型复合材料制成的部件的纤维增强件。
工具100包括模具110和对模120。模具110包括：底部111，其设置有多个孔道112。模具110还包括：侧壁113，其与底部111形成模腔114。在所示示例中，含有纤维织构体10的工具100下部由模具110封闭，而上部由对模120封闭，该对模120形成封闭工具100的盖。模具110和对模120用于确定预制件的尺寸从而确定所获得的部件的尺寸，并且用于调节所获得的部件中的纤维含量。
模具110包括：通向模腔114的不同区域的多个孔道112，填充有粒径大于纤维织构体10的间隙尺寸的过滤颗粒的第一悬浮液尤其旨在通过所述孔道112注入以便在模具111的底部与纤维织构体的第二侧10b之间形成过滤层130。然而，当模具包括单个孔道时，这并不超出本发明的范围。在多个孔道的情况下，可以仅通过模具的一部分孔道注入第一悬浮液，以保留另一部分孔道用于第二悬浮液的排空，如下面的描述中详细描述的。
就其本身而言，对模120包括多个孔道121，第一悬浮液的溶剂在穿过纤维织构体10之后将通过所述孔道121被排空。另外，填充有耐火陶瓷颗粒的第二悬浮液旨在通过对模120的多个孔道121注入，以便通过纤维织构体10的第一侧10a渗透到纤维织构体10的孔隙中。在图1至图3所示的示例中，通过对模120的所有孔道121排空第一悬浮液中的溶剂，并且通过对模120的所有孔道121注入第二悬浮液。当对模包括单个孔道时，这不超出本发明的范围。在多个孔道的情况下，可以仅通过对模的一部分孔道排空第一悬浮液中的溶剂，以保留对模的另一部分孔道用于第二悬浮液的注入。
第二悬浮液中的溶剂旨在通过模具110的多个孔道112被排空。在图1至图3所示的示例中，模具110的所有孔道112先前也用于注入第一悬浮液。在模具包括多个孔道的情况下，可以仅通过模具的一部分孔道排空第二悬浮液的溶剂，模具的另一部分孔道已被保留用于第一悬浮液的注入。
根据本发明，过滤层130介于纤维织构体10与模具的底部111之间。过滤层130是在注入填充有粒径大于纤维织构体10的间隙尺寸的过滤颗粒的第一悬浮液之后形成的，所述悬浮液的液相被纤维织构体10排出，然后通过对模120的孔道121被排空，过滤颗粒因此保持介于纤维织构体10与模具的底部111之间。在这里描述的示例中，过滤颗粒是陶瓷或玻璃前体。例如，悬浮液的液相可以是水。
箭头1000表示注入模具110中的第一悬浮液的移动。箭头2000表示由纤维织构体10排出的悬浮液的介质或液相的移动，如图2所示。
预制件可以在模具中保持压缩状态，并且可以完全贴合模具的壁。此外，预制件构成能够被第一次注入和第二次注入的液相渗透的网络。因此，不存在纤维结构在第一次注入或第二次注入的压力作用下变形的风险。
此外，在例如借助于主真空泵排出期间，可以在对模120的孔道121处进行泵送P1。执行这种泵送可以改善排出并且更快地干燥过滤层130。
例如，过滤层10的平均厚度在100μm至200μm之间。
过滤层130允许：将包含粒径小于纤维织构体10的间隙尺寸的耐火陶瓷颗粒的粉末的第二悬浮液的液相排出到纤维织构体10之外，以及由于在模具的孔道112与对模的孔道121之间施加压力梯度而通过模具110的孔道112排空所述液相。
在将填充有具有最小粒径的颗粒的第二悬浮液注入到纤维织构体10中之前，可以通过拉紧模具110或借助于压力机来施加压实压力，使得可以压实模具110与对模120之间的纤维织构体10；在注入期间可以维持该压实压力。压实压力也可以由压实液体经由薄膜施加，如PolyFlex工艺中那样。
作为变型，可以在第二悬浮液的注入开始之后施加压实压力，然后可以维持压实压力。施加压实压力允许压实织构体，以帮助通过过滤层排出液体并在不损坏纤维预制件的情况下实现纤维预制件的目标厚度。
在这里描述的示例中，第二填充悬浮液对应于填充有耐火陶瓷颗粒的液相。图3示出了在注入第二填充悬浮液和从中排出液体介质期间获得的配置。悬浮液在压力下通过对模120的孔道121注入，从而通过纤维织构体10的第一侧10a渗透纤维织构体10。该悬浮液中存在的耐火陶瓷颗粒旨在允许在纤维织构体10的孔隙中形成耐火陶瓷基体。在实施例的一个示例中，该耐火陶瓷基体可以是耐火氧化物基体。
例如，第二悬浮液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至2μm之间。所使用的氧化铝粉末可以是α氧化铝粉末。
更一般地，第二悬浮液可以是包含粒径平均比纤维织构体的孔隙网络的间隙的平均尺寸小5至15倍的耐火陶瓷颗粒的悬浮液。
在注入之前，悬浮液中颗粒的体积含量可以介于5％至50％之间。耐火陶瓷颗粒可以包含选自以下的材料：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。根据其基本组成，耐火陶瓷颗粒还可以与氧化铝、氧化锆、铝硅酸盐、稀土氧化物、稀土硅酸盐(其可以例如用于环境或热屏障)或可以对要获得的复合材料部件进行功能化的任何其他填料(诸如炭黑、石墨或碳化硅)混合。
第二悬浮液的液相可以包含例如具有酸性pH(即pH小于7)的水相和/或包含例如乙醇的醇相。例如，悬浮液可以包含酸化剂(诸如硝酸)，并且液体介质的pH可以介于1至5之间。此外，悬浮液可以包含有机粘合剂，例如尤其是易溶于水的聚乙烯醇(PVA)。
如图3所示，在将第二悬浮液注入到纤维织构体10的孔隙中之后，存在耐火陶瓷颗粒。箭头3000表示注入到纤维织构体10中的悬浮液的移动。箭头4000表示由过滤层130排出的悬浮液的介质或液相的移动，如图3所示。
在注入第二悬浮液的步骤期间和之后，对模120对纤维织构体10施加压力。
另外，可以在例如借助于主真空泵排出期间在模具110的孔道112处进行泵送P2。执行这种泵送可以改善排出并更快地干燥纤维织构体10。
在该配置中，过滤层130可以将最初存在于第二悬浮液中的颗粒保留在纤维织构体10中，并且使这些颗粒的全部或一部分通过过滤而沉积在纤维织构体10中。
在这里提出的示例中，模具不包括膜。当然，如果以众所周知的方式在膜下进行第一悬浮液和/或第二悬浮液的注入以改善纤维织构体的浸渍，则也不超出本发明的范围。
一旦已进行注入和排出步骤，就获得了纤维预制件，其包括：填充有耐火陶瓷颗粒的纤维织构体10、和连结到纤维织构体10的过滤层130。过滤层130与纤维织构体10之间的粘合是在注入耐火陶瓷颗粒期间实现的。材料沉积在过滤层130与纤维织构体10之间，并且整体借助于压实保持在一起。然后，烧结热处理在颗粒之间形成桥梁，从而完成粘合。
然后将所获得的预制件干燥并脱模，由于在耐火陶瓷颗粒的悬浮液中存在粘合剂(例如PVA)，预制件能够在脱模之后仍保持在模具110与对模120之间压实之后的形状。
然后对预制件进行热处理(这里，例如在1000℃至1200℃之间的温度下在空气中进行烧结)，以便对耐火陶瓷颗粒进行预烧结，从而在纤维织构体10的孔隙中形成耐火陶瓷基体。然后获得由氧化物/氧化物复合材料制成的部件，该部件一方面设置有高基体体积比的纤维增强材料并且耐火陶瓷基体在整个纤维增强件中均匀分布，另一方面设置有覆盖有光滑的陶瓷层或玻璃层的表面，该表面具有良好的表面状况，这是由过滤层130产生的。
由除氧化物/氧化物之外的CMC复合材料制成的部件可以通过用碳化硅和/或碳纤维生产纤维织构体和过滤层并通过使用填充有碳化物(例如SiC)、硼化物(例如TiB2)、硅化物(例如MoSi2)或氮化物(例如Si3N4)颗粒的第二悬浮液来以相同的方式获得。
作为变型，注入纤维织构体中的第二填充悬浮液可以包含耐火陶瓷前体的颗粒，例如溶胶-凝胶类型或聚合物类型的颗粒。在这种情况下，热处理包括将耐火陶瓷前体转变成陶瓷材料的至少一个步骤(称为陶瓷化步骤)，可能随后是附加的烧结步骤，以便进一步使复合材料部件致密化。

Claims (9)

1.一种用于将陶瓷颗粒注入到纤维织构体(10)中的方法，包括以下步骤：
将纤维织构体(10)放置在模具(110)中，所述纤维织构体(10)介于一个或多个第一孔道(112)与一个或多个第二孔道(121)之间，
通过所述第一孔道(112)注入第一悬浮液，所述第一悬浮液包含粒径大于所述纤维织构体(10)的孔隙网络的间隙尺寸的过滤颗粒的粉末；
通过所述纤维织构体(10)排出所述第一悬浮液的液相，通过所述第二孔道(121)排空所述液相并通过所述纤维织构体(10)保留所述过滤颗粒，从而在所述纤维织构体与所述第一孔道(112)之间形成过滤层130，
通过所述第二孔道(121)将第二悬浮液注入到所述纤维织构体中，所述第二悬浮液包含粒径小于所述纤维织构体(10)的孔隙网络的间隙尺寸的耐火陶瓷颗粒的粉末，
通过所述过滤层(130)排出已经穿过所述纤维织构体(10)的第二悬浮液的液相，并通过所述过滤层(130)将耐火陶瓷颗粒粉末保留在所述纤维织构体(10)内，从而获得纤维预制件，所述纤维预制件至少包括填充有耐火陶瓷颗粒的纤维织构体(10)和所述过滤层(130)，所述第二悬浮液的液相通过所述第一孔道(112)被排空。
2.根据权利要求1所述的方法，其中，所述第一悬浮液的粉末是陶瓷或玻璃前体。
3.根据权利要求1或2所述的方法，其中，所述过滤层(130)的平均厚度在100μm与200μm之间。
4.根据权利要求1至3中任一项所述的方法，其中，所述第二悬浮液的颗粒的尺寸平均比所述纤维织构体(10)的孔隙网络的间隙的平均尺寸小5至15倍。
5.根据权利要求1至4中任一项所述的方法，其特征在于，所述第二悬浮液的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、硅化物和氮化物或其中几种材料的混合物。
6.根据权利要求1至5中任一项所述的方法，其中，所述纤维织构体(10)包括：通过二维编织、或三维或多层编织、或单向纤维的自动放置而获得的纤维结构。
7.根据权利要求1至6中任一项所述的方法，其特征在于，所述纤维织构体(10)的纱线由纤维形成，所述纤维由以下材料中的一种或多种组成：氧化铝、莫来石、二氧化硅、铝硅酸盐、硼硅酸盐、碳化硅和碳。
8.根据权利要求1至7中任一项所述的方法，其中，所述模具(110)具有环形或截锥形旋转几何结构，所述纤维织构体(10)在被放置于所述模具(110)中时根据环形或截锥形旋转几何结构成形。
9.一种制造复合材料的方法，包括根据权利要求1至8中任一项所述的注入方法，还包括：对存在于所述预制件的纤维织构体(10)中的耐火陶瓷颗粒进行热处理，以便形成复合材料部件，所述复合材料部件至少包括由耐火陶瓷基体致密化的所述纤维织构体(10)和所述过滤层(130)。
CN202280042575.2A 2021-06-15 2022-06-06 使用在纤维预制件中就地生成的过滤器注入陶瓷粉末的方法 Pending CN117545606A (zh)

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