CN109195930A - 通过将负载浆料注入纤维织构制造复合材料零件的方法 - Google Patents

通过将负载浆料注入纤维织构制造复合材料零件的方法 Download PDF

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Publication number
CN109195930A
CN109195930A CN201780028223.0A CN201780028223A CN109195930A CN 109195930 A CN109195930 A CN 109195930A CN 201780028223 A CN201780028223 A CN 201780028223A CN 109195930 A CN109195930 A CN 109195930A
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China
Prior art keywords
fibrous texture
texture
refractory
mold
liquid
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CN201780028223.0A
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Inventor
迈克尔·波德哥尔斯基
布鲁诺·丹伯林
艾杜·鲁伊斯
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Safran SA
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Safran SA
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    • B28B23/00—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects
    • B28B23/0006—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects the reinforcement consisting of aligned, non-metal reinforcing elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/24—Producing shaped prefabricated articles from the material by injection moulding
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
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Abstract

一种制造复合材料零件的方法包括将纤维织构(10)置于模具(110)中，所述模具(110)在其下部包括由多孔材料制成的零件(130)，织构(10)的第一面(10b)支撑在所述零件(130)上，在压力下将含有耐火陶瓷颗粒粉末的液体(150)注入纤维织构(10)中，排出已经通过纤维织构(10)的液体，该液体通过由多孔材料制成的零件(120)，并且通过由多孔材料制成的所述零件(130)将耐火陶瓷颗粒粉末保持在所述织构内。刚性穿孔元件(140)插入模具(110)的底部(111)和由多孔材料制成的零件(130)之间。

Description

通过将负载浆料注入纤维织构制造复合材料零件的方法
背景技术
本发明涉及一种制造热结构复合材料零件的方法，所述复合材料特别是氧化物/氧化物或陶瓷基复合材料(CMC)类型的材料，即包括由耐火陶瓷材料纤维制成的纤维增强件，该纤维同样由耐火陶瓷材料制成的基质致密化。
由氧化物/氧化物复合材料制成的零件通常通过在模具中覆盖由耐火氧化物纤维制成的多个纤维层来制备，每个纤维层预先用填充有耐火氧化物颗粒的浆料浸渍。然后以这种方式布置的层的组通过模具盖或真空袋并经由高压釜压实。然后对所得的填充预制件进行烧结或进行陶瓷化热处理，以在预制件中形成耐火氧化物基质，并获得氧化物/氧化物复合材料零件。该技术还可用于制造陶瓷基质复合(CMC)材料零件。在这种情况下，纤维层由碳化硅(SiC)纤维或碳纤维制成，并且它们浸渍有填充有碳化物(例如SiC)或硼化物(例如TiB2)的颗粒或氮化物(Si3N4)的颗粒的浆料。
然而，这种类型的制备使得仅可获得具有在某些方向上受限的机械特性的氧化物/氧化物复合物或CMC材料零件。特别是，这些材料不能很好地承受分层，并且它们不能很好地承受剪切力。
使通过连续经纱和纬纱之间的三维编织获得的纤维织构用于增加材料的机械强度，特别是其承受分层的能力。在这种情况下，同样对于厚的2D纤维织构，只有使用压力梯度的方法，诸如灌注型方法，通过树脂传递模塑(RTM)技术或通过亚微米颗粒抽吸(SPS)的注入模塑才能使填充浆料渗透到厚度可能高达几十毫米的纤维织构，织构的厚度取决于预期的应用。
然而，注入填充浆料的纤维织构部分与浆料液体将被抽空的纤维织构的另一部分之间的压力梯度难以控制整个纤维织构。如果压力在面向模具底部的纤维织构的整个区域上不平衡，该区域包括一个或多个排放口，浆料的液相将通过该排放口排出，则在靠近排放口的区域和更远的区域之间建立了压力差。在这种情况下，难以除去液相，因为它需要从织构中取出而不会干扰已经由浆料沉积的固体颗粒(耐火氧化物、碳化物、硼化物、氮化物等)的分布。具体地说，当它被排出时，液相可以带有颗粒和/或可以改变纤维织构内颗粒的分布，从而导致由于在某些地方缺乏基质而在最终材料中出现大孔。
发明内容
本发明的一个目的是弥补上述缺点并提出解决方案，该解决方案使得可以用复合材料，特别是氧化物/氧化物或CMC类型材料制造零件，同时还使用厚的纤维织构和/或复杂形状的纤维织构，并且以快速和可靠的方式这样做，同时提供对纤维织构内的固体颗粒的沉积和分布的良好控制，以便获得没有任何大孔隙的材料。
为此，本发明提供了一种制造复合材料零件的方法，该方法包括以下步骤：
-由耐火陶瓷纤维形成纤维织构；
-将纤维织构放置在模具中，所述模具在其底部包括由多孔材料制成的零件，所述织构的第一面支撑在所述零件上；
-用面向纤维织构的第二面布置的模具盖或盖子封闭模具；
-在压力下将液体注入纤维织构中，该液体含有耐火陶瓷颗粒的粉末或耐火陶瓷前体颗粒的粉末；
-经由多孔材料零件排出液体，该液体已经通过纤维织构，而所述多孔材料零件将耐火陶瓷颗粒的粉末或耐火陶瓷前体颗粒的粉末保留在所述织构内，以便获得填充有耐火陶瓷颗粒或耐火陶瓷前体颗粒的纤维预制件，该液体经由存在于模具底部的至少一个排放口排出，穿孔的刚性元件插入模具的底部和多孔材料零件之间；
-干燥纤维预制件；
-脱模纤维预制件；和
-对纤维预制件中存在的耐火陶瓷颗粒或耐火陶瓷前体颗粒进行热处理，以便在所述预制件中形成耐火陶瓷基质；
穿孔的刚性元件插入模具的底部和多孔材料零件之间；
该方法的特征在于，穿孔的刚性元件在其底面包括与模具底部的内表面接触的凹口或切口。
通过使用多孔材料零件来排出浆料的液体，本发明的方法使得可以消除引入纤维织构中的液体而不消除也存在于织构中的耐火陶瓷固体颗粒或耐火陶瓷前体颗粒。另外，通过在模具的底部和多孔材料零件之间插入穿孔的刚性元件，可以在多孔材料零件的底面上获得平衡的压力，液体通过该面排出。由于在模具底部和多孔材料零件之间存在穿孔的刚性元件，液体可以在多孔材料零件和模具的底部之间流动并且可以容易地到达排放口，而不管液体在哪里离开多孔材料零件。另外，在穿孔的刚性元件的底面中与模具底部的内表面接触的凹口或切口用于促进液体朝向排放口的流动。
利用本发明的方法，通过不会干扰在纤维织构内颗粒分布的排放而消除液体，因此，可以获得在整个纤维增强材料中具有均匀分布的基质的复合材料零件。因此，热结构复合材料零件具有改善的机械性能。
在本发明方法的第一个特定方面，穿孔的刚性元件具有多个孔眼，每个孔眼呈现矩形形状或圆形形状，所述矩形形状的边延伸距离小于或等于5毫米(mm)，所述圆形形状的直径小于或等于5mm。
在本发明方法的第二个特定方面，该穿孔的刚性元件具有约1mm的厚度。
在本发明方法的第四个特定方面，该穿孔的刚性元件由选自以下材料的材料制成：聚四氟乙烯(PTFE)；金属材料；聚合物等等。
在本发明方法的一种实施方式中，其中放置纤维织构的模具包括浸渍室，该浸渍室在其底部包括多孔材料零件，所述织构的第一面支撑在所述多孔材料零件上，该浸渍室在其顶部用面向纤维织构的第二面放置的可变形不可渗透的隔膜封闭，所述隔膜将该浸渍室与压实室分开，含有耐火陶瓷颗粒或耐火陶瓷前体颗粒的液体被注入纤维织构的第二面和隔膜之间的浸渍室中，压实流体被注入压实室中，该流体在隔膜上施加压力以迫使含有耐火陶瓷颗粒粉末或耐火陶瓷前体颗粒粉末的填充液体穿过纤维织构。在形成纤维织构的步骤期间，纱线可以采用三维编织或多层编织来编织。纤维织构同样可以通过堆叠使用二维编织而编织的层来制造，该织构具有至少0.5mm的厚度，优选至少1mm。
预制件的纱线可以由以下材料中的一种或多种构成的纤维制成：氧化铝；莫来石；二氧化硅；硅酸铝；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；硅酸铝；磷酸铝；氧化锆；碳化物；硼化物和氮化物。
在一种实施方式中，所得到的复合材料零件可以构成涡轮发动机叶片或实际上是后体零件、燃烧室、襟翼或加力燃烧室臂等。
附图说明
根据作为非限制性实施例给出的本发明特定实施方式的以下描述，并参考附图，本发明的其他特征和优点显而易见，其中：
-图1是根据本发明的实施方式的工具的示意性分解透视图；
-图2是用位于其中的纤维织构封闭的图1所示的工具的示意性剖视图；
-图3是图2工具中用填充浆料浸渍纤维织构的步骤的示意性剖视图；
-图4是根据本发明另一个实施方式的工具的示意性分解透视图；
-图5是用位于其中的纤维织构封闭的图4所示的工具的示意性剖视图；和
-图6和7是在图5的工具中用填充的浆料浸渍纤维织构的步骤的示意性剖视图。
具体实施方式
根据本发明的用于制造复合材料，特别是氧化物/氧化物或CMC类型的复合材料的方法，首先制造纤维织构，以形成零件的加强件。
纤维织构通过使用提花型织机以已知的方式进行编织而制成，该提花织机具有布置成多层的经纱或股线的束，经纱通过纬纱相互连接，或反之亦然。纤维织构可以通过堆叠通过二维(2D)编织获得的层来制成。纤维织构也可以通过三维(3D)编织直接制成单个零件。术语“二维编织”在本文中用于表示传统的编织技术，其中每根纬纱在单层经纱中从一侧穿过到另一侧纱线，或反之亦然。本发明的方法特别适合于使填充的浆料能够被引入到2D纤维织构中，即通过堆叠2D层而获得的织构，并且所述2D纤维织构具有相当大的厚度，即具有至少0.5mm厚度的2D纤维织构，并且优选至少1mm。
术语“三维编织”或“3D编织”，或实际上“多层编织”在本文中用于表示如下的编织技术：其中至少一些纬纱在多个经纱层上连接经纱，或反之亦然，使用可特别选自以下编织类型的编织：互锁、多平纹、多缎纹和多斜纹。
术语“互锁编织或织构”在本文中用于表示如下3D编织：其中每层经纱连接多层纬纱，而给定经线列中的所有纱线在编织平面中具有相同的运动。
术语“多平纹编织或织构”在本文中用于表示如下的具有多层纬纱的3D编织：其中每层的基础编织等同于传统的平纹编织，但编织的某些点连接纬纱层。
术语“多缎纹编织或织构”在本文中用于表示如下的具有多层纬纱的3D编织：其中每层的基础编织相当于传统的缎纹编织，但编织的某些点连接纬纱层。
术语“多斜纹编织或织构”在本文中用于表示如下的具有多层纬纱的3D编织：其中每层的基础编织等同于传统的斜纹编织，但编织的某些点连接纬纱层。
3D织构呈现复杂的构造，并且难以将悬浮液中的固体颗粒引入到3D织构中并以均匀的方式分布它们。本发明的方法也非常适合于将填充的浆料引入3D编织纤维织构中。
用于编织形成复合材料零件的纤维增强件的纤维织构的纱线，可以特别地由以下任何材料构成的纤维制成：氧化铝、莫来石、二氧化硅、硅酸铝、硼硅酸盐、碳化硅、碳或多种这些材料的混合物。
一旦纤维织构被制成，就将其放置在根据本发明的工具中，如下所述，该工具用于在纤维织构内沉积耐火陶瓷颗粒或耐火陶瓷前体颗粒。为此目的，并且如图1和2所示，将纤维织构10放置在工具100中。在当前描述的实施例中，使用上面定义的技术之一(堆叠2D层或3D编织)使用由Nextel 610TM氧化铝制成的纱线制造纤维织构10。该实施例中的纤维织构10用于形成氧化物/氧化物复合材料叶片的纤维增强件。
工具100包括模具110和模具盖120。模具110具有带有排放口112的底部111。模具110还具有侧壁113，侧壁113与底部111配合以形成模腔114。在所示的实施例中，其中存在纤维织构10的工具100在其底部由模具110封闭，并且在其顶部由模具盖120封闭，模具盖120形成封闭工具100的盖子。模具110和模具盖120用于确定预制件的尺寸并因此确定要获得的零件的尺寸，并且还用于调节要获得的零件中的纤维体积分数。
模具盖120具有多个注入口121，通过该注入口121注入填充有耐火陶瓷颗粒或耐火陶瓷前体颗粒的液体，以便通过纤维织构1的第一面10a渗透到纤维织构10的孔中。在图1和2所示的实施例中，填充的液体用于通过多个注入口121注入，注入口121通向模腔的不同区域。然而，通过单个注入孔注入液体不会超出本发明的范围。
模具110具有用于液体的单个排放口112。自然地，使用多个出口排放口不会超出本发明的范围。
多孔材料零件130存在于模具110和纤维织构10之间的模腔114中。多孔材料零件130具有与纤维织构10的第二面10b接触的顶面130a，液体通过该顶面130a被排出。在图1和2所示的实施例中，纤维织构10的第二面10b位于第一面10a的对面，浆料通过该第一面10a渗透到织构1中。填充有耐火陶瓷颗粒的液体也可以经由预制件的侧面被注入。
举例来说，多孔材料零件130可以由微孔聚四氟乙烯(PTFE)制成，诸如由供应商出售的“微孔PTFE”产品。举例来说，为了制造多孔材料零件130，可以使用由供应商销售的PM 0130材料，并且孔的尺寸在1微米(μm)至2μm范围内。
多孔材料零件130使得液体能够从纤维织构10中被排出，并且由于在出口排放口112和注入口121之间施加压力梯度而经由出口排放口112排出。
举例来说，多孔材料零件130可具有大于或等于1mm的厚度，或实际上几毫米的厚度。多孔材料零件130的平均孔隙率可为约30％。多孔材料零件的孔的平均尺寸(D50)可以在例如1μm至2μm的范围内。
在一种实施方式中，多孔材料零件130可以是刚性的并且呈现与预制件和将要获得的复合材料零件的形状相对应的形状。举例来说，在这种情况下，多孔材料零件可以通过热成型制成。在一个变型中，多孔材料零件可以是可变形的并且可以呈现模具的形状，模具的形状对应于预制件的形状加上要获得的复合材料零件的形状。
根据本发明，穿孔的刚性元件140插入模具110的底部111和多孔材料零件130之间。更确切地说，穿孔的刚性元件140具有与多孔材料零件130的底面130b接触的顶面140a和与模具110的底部111的内表面111a接触的底面140b。
在当前描述的实施例中，穿孔的刚性元件140呈现由垂直交叉的壁142和壁143构成的网格形式，壁142和143在它们之间限定了矩形形状的孔眼141。孔眼141优选地具有长度小于或等于5mm的边，以避免多孔材料零件130的任何局部变形。举例来说，穿孔的刚性元件140可以呈现小于或等于1mm的厚度E140。
穿孔的刚性元件由与注入纤维织构的液体和多孔材料零件的化学和/或机械相容的材料制成。在当前描述的实施例中，穿孔的刚性元件140由聚四氟乙烯(PTFE)制成，类似于多孔材料零件130。
根据本发明的特征，与模具110的底部111的内表面111a接触的刚性元件140的底面140b具有与壁142和143相关联的凹口或切口1420和1430，以便促使液体流向出口排放口112。
在将浆料注入纤维织构10之前，用于压实模具110和模具盖120之间的纤维织构10的压实压力，可以通过夹紧模具或通过压力施加，在注入期间可以保持压实压力。
在一个变型中，可以在开始注入填充的液体之后施加压实压力，然后可以保持压实压力。施加压实压力可以用于压实织构，以便有助于排出液体并达到纤维预制件的目标厚度而不损坏纤维预制件。
在目前描述的实施例中，填充的液体对应于含有耐火陶瓷颗粒的浆料。图3示出了在注入浆料150并排出液体介质时获得的构造。浆料150在压力下经由注入口121被注入，以便通过纤维织构10的第一面10a渗透到纤维织构10中。存在于浆料150中的耐火陶瓷颗粒1500使得能够在纤维织构10的孔中形成耐火陶瓷基质。在一种实施方式中，耐火陶瓷基质可以是耐火氧化物基质。
举例来说，浆料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0.3μm的范围内。所用的氧化铝粉末可以是由供应商Baikowski以名称SM8销售的阿尔法氧化铝粉末。
更一般地，浆料可以是具有耐火陶瓷颗粒的悬浮液，其平均粒径在0.1μm至10μm的范围内。注入前浆料中耐火陶瓷颗粒的体积分数可在20％至40％的范围内。耐火陶瓷颗粒可包括选自以下的材料：氧化铝，莫来石，二氧化硅，硅酸铝，磷酸铝，氧化锆，碳化物，硼化物和氮化物。取决于它们的基本组成，耐火陶瓷颗粒也可以与氧化铝、氧化锆、硅酸铝、稀土氧化物、稀土硅酸盐(其可以用于例如环境屏障或热障)中的颗粒混合，或者与用于使要获得的复合材料零件功能化的任何其他填料混合，诸如与炭黑、石墨或碳化硅混合。
举例来说，浆料的液体介质可包含呈现酸性pH(即pH小于7)和/或醇相的水相，例如包含乙醇。浆料可以包括酸化剂诸如硝酸，并且液体介质的pH可以在例如1.5至4的范围内。浆料还可包括有机粘合剂，诸如聚乙烯醇(PVA)，特别是其可溶于水。
如图3所示，在将浆料150注入纤维织构10的孔中之后，会出现耐火陶瓷颗粒1500。箭头151表示浆料150注入纤维织构10中的运动。箭头152表示由多孔材料零件130排出的浆液的液相或介质的移动。
模具盖120在注入步骤期间和之后在纤维织构10上施加压力。
在排出期间，还可以经由出口排放口112施加泵送P，例如通过使用主真空泵。进行这种泵送可以改善排液并更快地干燥纤维织构。
作为另外一种选择或组合，在排出期间，可以加热仍然存在于纤维织构的孔中的液体介质，以使通过纤维织构的第二面和多孔材料零件的液体蒸发。例如，液体介质的温度可以升高到80℃至105℃的范围内。
在这种配置中，多孔材料零件130用于在纤维织构10内保留最初存在于浆料中的耐火陶瓷颗粒1500，并确保这些颗粒中的一些或全部通过在纤维织构10中过滤而沉积。
一旦进行了注入和排出步骤，就得到纤维预制件15，它填充有耐火陶瓷颗粒，例如耐火陶瓷氧化物颗粒，例如氧化铝颗粒。
然后将所得的预制件干燥然后脱模，并且由于在浆料中存在粘合剂诸如PVA，在脱模之后，预制件能够保留其在模腔中采用的形状，例如，在模具和模具盖之间压实后采用的形状。
此后，对预制件进行热处理，在本实施例中烧结，例如在温度为1000℃至1200℃范围内的空气中，烧结耐火陶瓷颗粒，从而在纤维预制件的孔中形成耐火陶瓷基质。由此获得复合材料零件，例如由氧化物/氧化物复合材料制成的零件，具有由纤维预制件形成的纤维增强件，并且具有高基质体积分数，耐火陶瓷基质均匀地分布在整个纤维增强件中。
由氧化物/氧化物材料以外的CMC材料制成的零件可以通过用碳化硅纤维和/或碳纤维制成的纤维织构，并且通过使用填充有碳化物(例如SiC)、硼化物(例如TiB2)或氮化物(Si3N4)颗粒的浆料以相同的方式获得。
在一个变型中，注入预制件中的填充液体可包括耐火陶瓷前体的颗粒，例如溶胶-凝胶或聚合物类型的颗粒。在这种情况下，热处理包括至少一个将耐火陶瓷前体转变成陶瓷材料的步骤(被称为“陶瓷化”步骤)，可选地随后进行另外的烧结步骤，以进一步致密化复合材料零件。
图4至7示出了在本发明的另一个实施方式中制造复合材料零件的方法。如图4和5所示，纤维织构20放置在工具200中。在当前描述的实施例中，使用上面定义的任何一种技术(堆叠2D层或3D编织)使用由Nextel 610TM氧化铝制成的纱线制造纤维织构20。在该实施例中，纤维织构20用于形成氧化物/氧化物复合材料叶片的纤维增强件。
工具200包括具有底部211的模具210，底部211设置有排放口212。模具210还具有侧壁213，侧壁213包括装配有阀门2150的注入口215。多孔材料零件230放置在纤维织构20下面，多孔材料零件120具有用于接收纤维织构20的顶面230a。在当前描述的实施例中，零件230由可变形材料制成，以便能够紧密贴合对应于由模具210限定的待制造的最终零件形状的形状或轮廓，特别是航空发动机叶片。通过成形，零件230呈现其顶面230a的形状，其类似于待制造的零件的形状。举例来说，零件120可以由微孔聚四氟乙烯(PTFE)制成，诸如由供应商出售的“微孔PTFE”产品。在变型的实施方式中，多孔材料零件是刚性的并且具有与要制造的最终零件的形状对应的形状的顶面。在这种情况下，该零件尤其可以通过热成型制成。举例来说，微孔零件可以具有几毫米的厚度和约30％的平均孔隙率。多孔材料零件的平均孔径(D50)可以在例如1μm至2μm的范围内。
根据本发明，穿孔的刚性元件240插入模具210的底部211和多孔材料零件230之间。更确切地说，穿孔的刚性元件240具有与多孔材料零件230的底面230b接触的顶面240a和与模具210的底部211的内表面211a接触的底面240b。
在当前描述的实施例中，并且与图1中所示的穿孔的刚性元件140类似，穿孔的刚性元件240呈现由垂直交叉的壁242和243构成的网格形式，壁242和243在它们之间限定了矩形形状的孔眼。孔眼优选地具有长度小于或等于5mm的边，以避免多孔材料零件230的局部变形。举例来说，穿孔的刚性元件240可以呈现小于或等于1mm的厚度E240。穿孔的刚性元件240还成形为具有与由模具210的211的表面211a呈现的曲率对应的曲率。
穿孔的刚性元件由与注入纤维织构的填充液体和多孔材料零件的化学和/或机械相容的材料制成。在当前描述的实施例中，穿孔的刚性元件240由聚四氟乙烯(PTFE)制成，类似于多孔材料零件230。
根据本发明的特征，与模具210的底部211的内表面211a接触的刚性元件240的底面240b在其壁243中包括凹口或切口2430，以便于液相朝向出口排放孔212流动。壁242还包括凹口或切口(图4至7中未示出)。
工具200还包括盖子220，盖子220包括装配有阀门2210的注入口221和可变形隔膜280，一旦工具已经封闭(图5)，该可变形隔膜280用于分离其中存在纤维织构20的浸渍室201与位于隔膜280上方的压实室202。举例来说，隔膜280可以由硅树脂制成。
在将织构20放置在多孔材料零件230的顶面230a上之后，用盖子230封闭模具210(图5)。然后将填充的液体，特别是浆料250经由注入口215注入浸渍室201中，同时其阀门2150打开(图6)。在该实施例中，浆料250用于在织构中形成耐火氧化物基质。浆料250对应于含有耐火氧化物颗粒粉末的悬浮液，该颗粒的平均粒径在0.1μm至10μm的范围内。浆料的液相可以特别地由水(具有酸性pH)、由乙醇或由任何其他液体构成，其中可以将所需的粉末置于悬浮液中。还可以加入有机粘合剂(例如PVA，其可溶于水)。粘合剂用于确保在干燥之后和烧结之前生坯部分保持在一起。
举例来说，浆料250可以对应于由氧化铝粉末构成的水性悬浮液，氧化铝粉末平均粒径(D50)在0.1μm至0.3μm的范围内，并且体积分数在20％至40％的范围内，悬浮液用硝酸酸化(pH值在1.5至4范围内)。除氧化铝外，耐火氧化物颗粒同样可以选自氧化铝、莫来石、二氧化硅、硅酸铝、磷酸铝、氧化锆、碳化物、硼化物和氮化物。取决于它们的基本组成，耐火氧化物颗粒还可以与氧化铝、氧化锆、硅酸铝、稀土氧化物、稀土二硅酸盐(例如用于环境屏障或热障)中的颗粒混合，或与用于为最终材料(炭黑、石墨、碳化硅等)添加特定功能的任何其他填料混合。
注入浸渍室201中的浆料250的量被确定为待浸渍的纤维织构20的体积的函数。最初引入的粉末量决定了凝固厚度，从而决定了纤维体积分数(FVF)和基质体积分数(MVF)。
一旦将浆料注入浸渍室201中，就通过注入压实流体260，例如油来进行压实操作，当阀门2210打开时，压实流体经由注入口221进入压实室202，注入口215的阀门2150预先关闭(图7)。压实流体260通过隔膜280对浆料250施加压力，从而迫使浆料250渗透到纤维织构20中。流体260对整个隔膜280施加压力，并因此对织构20上存在的所有浆料施加压力。由隔膜280施加在浆料上和纤维织构上的压力优选小于15巴，例如7巴，以使浆料渗透到织构中，从而使织构充分压实，使浆料的液相能够经由多孔材料零件排出，而不会使所得的预制件劣化。
位于纤维织构的面20b旁边的多孔材料零件230用于执行多种功能，纤维织构的面20b与面20a相对，浆料通过面20a渗透到织构中。具体地，零件230允许浆料的液体从纤维织构中排出，这样排出的液体在该实施例中经由排放口212排出。在压实操作期间和之后进行排液。一旦没有液体通过排放口212流出，就终止排液。结合借助于压实流体对浆料施加压力，可以进行泵送P，例如经由排放口212借助于主真空泵(图4至图7中未示出)。这种泵送是可选的。加热可能就足够了。相反，不加热泵送就足够了。然而，结合泵送和加热用于加速干燥。
此外，工具可以设置有加热器装置，诸如结合在工具的壁中的电阻器元件，以便提高压实室中的温度并且有助于通过蒸发排空浆料的液体。压实室中的温度可以设置在80℃至105℃的温度范围内。
多孔材料零件220用于保持浆料中存在的固体耐火氧化物颗粒，因此耐火氧化物颗粒逐渐沉积在纤维织构中。随后这用于获得基质(例如在烧结后)。
零件220还用于在压实操作期间保持纤维织构的形状，因为其顶面220a再现了与要制造的最终零件的形状相对应的模具210的底部211的形状。
由此获得纤维预制件30，其填充有耐火氧化物颗粒，特别是上述类型的氧化铝颗粒。此后，通过从压实室202中排空压实流体来脱模预制件，由于浆料中存在诸如PVA的粘合剂，预制件在脱模后保持其压实形状。
此后，从工具中取出预制件，并在1000℃至1200℃的温度范围内在空气中进行烧结热处理，以便将耐火氧化物颗粒烧结在一起，从而形成预制件中的耐火氧化物基质。由此获得氧化物/氧化物复合材料零件，其具有通过3D编织获得的纤维增强件和基质在整个纤维增强件中的均匀分布。
CMC材料零件可以通过用碳化硅或碳纤维制成纤维织构并通过使用填充有碳化物(例如SiC)、硼化物(例如TiB2)或氮化物(Si3N4)颗粒的浆料以相同方式获得。
在一个变型中，注入预制件中的填充液体可包括耐火陶瓷前体的颗粒，例如溶胶-凝胶或聚合物类型的颗粒。在这种情况下，热处理包括至少一个将耐火陶瓷前体转变成陶瓷材料的步骤(被称为“陶瓷化”步骤)，可选地随后进行另外的烧结步骤，以进一步致密化复合材料零件。
本发明的穿孔的刚性元件可具有各种形式。特别地，它可以是具有如上所述的矩形孔眼的网格的形式，具有多个圆形孔眼的板的形式，或者实际上是蜂巢状的蜂窝结构(例如)类型的形式，其中蜂窝构成孔眼。
如上所述，穿孔的刚性元件优选地由与注入纤维织构的浆料和多孔材料零件的化学和/或机械相容的材料制成。特别地，穿孔的刚性元件可以由以下任何材料制成：聚四氟乙烯(PTFE)；金属材料；聚合物。

Claims (9)

1.一种制造复合材料零件的方法，该方法包括以下步骤：
-由耐火陶瓷纤维形成纤维织构(10)；
-将纤维织构(10)放置在模具(110)中，所述模具(110)在其底部包括由多孔材料制成的零件(130)，所述织构(10)的第一面(10b)支撑在所述零件(130)上；
-用面向纤维织构(10)的第二面(10a)放置的模具盖或盖子(120)封闭模具；
-在压力下将液体(150)注入纤维织构(10)中，该液体含有耐火陶瓷颗粒的粉末或耐火陶瓷前体颗粒的粉末；
-经由多孔材料零件(120)排出液体，该液体已经通过纤维织构(10)，而所述多孔材料零件(130)将耐火陶瓷颗粒的粉末或耐火陶瓷前体颗粒的粉末保留在所述织构内，以便获得填充有耐火陶瓷颗粒或耐火陶瓷前体颗粒的纤维预制件(15)，该液体经由存在于模具底部的至少一个排放口排出；
-干燥纤维预制件(15)；
-脱模纤维预制件(15)；和
-对纤维预制件中存在的耐火陶瓷颗粒或耐火陶瓷前体颗粒进行热处理，以便在所述预制件中形成耐火陶瓷基质；
穿孔的刚性元件(140)插入模具(110)的底部(111)和多孔材料零件(130)之间；
该方法的特征在于，穿孔的刚性元件(140)在其底面(140b)包括与模具(110)的底部(111)的内表面(111a)接触的凹口或切口(1420，1430)。
2.根据权利要求1所述的方法，其特征在于，该穿孔的刚性元件(140)具有多个孔眼(141)，每个孔眼呈现矩形形状或圆形形状，所述矩形形状的边延伸距离小于或等于5mm，所述圆形形状的直径小于或等于5mm。
3.根据权利要求2所述的方法，其特征在于，该穿孔的刚性元件(140)具有约1mm的厚度(E140)。
4.根据权利要求1至3中任一项所述的方法，其特征在于，该穿孔的刚性元件(140)由选自以下材料的材料制成：聚四氟乙烯(PTFE)；金属材料；聚合物。
5.根据权利要求1至4中任一项所述的方法，其特征在于，其中放置纤维织构的模具(210)包括浸渍室(201)，该浸渍室(201)在其底部包括多孔材料零件(230)，所述织构(20)的第一面(20b)支撑在所述多孔材料零件(230)上，该浸渍室(201)在其顶部用面向纤维织构(20)的第二面(20a)布置的可变形不可渗透隔膜(280)封闭，所述隔膜(280)将该浸渍室(201)与压实室(202)分开，含有耐火陶瓷颗粒粉末或耐火陶瓷前体颗粒粉末的液体(250)被注入纤维织构(20)的第二面(20a)和隔膜(280)之间的浸渍室中，压实流体(260)被注入压实室(202)中，该流体在隔膜(280)上施加压力以迫使含有耐火陶瓷颗粒粉末或耐火陶瓷前体颗粒粉末的液体(250)穿过纤维织构(20)。
6.根据权利要求1至5中任一项所述的方法，其特征在于，在形成纤维织构的步骤期间，纱线采用三维编织或多层编织来编织。
7.根据权利要求1至6中任一项所述的方法，其特征在于，该预制件的纱线由以下材料中的一种或多种构成的纤维制成：氧化铝；莫来石；二氧化硅；硅酸铝；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，其特征在于，该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；硅酸铝；磷酸铝；氧化锆；碳化物；硼化物和氮化物。
9.根据权利要求1至8中任一项所述的方法，其特征在于，所获得的复合材料零件构成涡轮发动机叶片、后体零件、燃烧室、襟翼或加力燃烧室臂。
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