CN108779033B - 用于通过将加载浆料加压注入到多孔模具中来制造陶瓷复合材料部件的方法 - Google Patents

用于通过将加载浆料加压注入到多孔模具中来制造陶瓷复合材料部件的方法 Download PDF

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CN108779033B
CN108779033B CN201680070989.0A CN201680070989A CN108779033B CN 108779033 B CN108779033 B CN 108779033B CN 201680070989 A CN201680070989 A CN 201680070989A CN 108779033 B CN108779033 B CN 108779033B
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slurry
fibrous texture
porous
texture
refractory ceramic
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CN108779033A (zh
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N·德罗兹
L·P·利埃斯
A·派克斯奥
M·泊德格斯奇
S·海费
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Safran Aircraft Engines SAS
Safran SA
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Safran SA
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Abstract

一种制造复合材料部件的方法，所述方法包括以下步骤：将含有耐火陶瓷颗粒(1500)的粉末的浆料(150)压力注射入纤维结构；使得通过纤维结构(10)的浆料(150)的液体(1501)排出，同时将耐火陶瓷颗粒的粉末保持在所述结构内，以获得加载有耐火陶瓷颗粒(1500)的纤维预制件(15)。注入工具包括由多孔材料(110)制造的模具，其具有内部放置纤维结构的内部壳体(113)，所述浆料(150)经由存在于注入工具中并通向由多孔材料(110)制造的模具的内部壳体(113)的至少一个注入端口(134)注入所述纤维结构(10)。所述工具还包括由刚性材料制成的外室(130)，多孔材料制成的模具(110)被保持在该外室中，当在压力下注入浆料(150)并且在排出所述浆料的液体(1501)的同时，浆料的液体(1501)经由存在于刚性材料制成的外室中的至少一个出口(135)排出。

Description

用于通过将加载浆料加压注入到多孔模具中来制造陶瓷复合 材料部件的方法
技术领域
本发明涉及用于由复合材料制造部件的方法，特别是由氧化物/氧化物型或陶瓷基质复合物(CMC)类型的复合材料制造部件的方法，即，其包含由耐火陶瓷材料纤维制成的纤维增强物并且通过同样由耐火陶瓷材料制成的基质进行致密化。
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备：在模具中铺设多个纤维层，该层由耐火氧化物纤维制成，并且每个层预先用填充有耐火氧化物颗粒的浆料进行浸渍。然后通过使用夹模(countermold)或真空盖(vacuum cover)并通过高压釜将以该方式排列的层组压实。然后，将所获得的经填充的预制件进行烧结，以在所述预制件内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。该技术也可用于由陶瓷基质复合物(CMC)材料制造部件。在这种情况下，纤维层由碳纤维或碳化硅(SiC)纤维制成，并且用填充有碳化物(例如SiC)颗粒、硼化物(例如TiB2)颗粒或氮化物(例如Si3N4)颗粒的浆料进行浸渍。
然而，该类型的制备方法仅适于制造仅具有较薄厚度和二维(2D)纤维强化物的氧化物/氧化物或CMC复合材料部件。这些类型的复合材料的机械特性在某些方向上仍然受限。特别地，这些材料的分层耐受性不良，并且它们无法良好地经受剪切力。
在连续的经纱和纬纱之间三维编织而获得的制造纤维织构能够增加材料的机械强度，并且特别是能够增强其分层耐受性。在该情况下，对于厚的2D纤维织构，仅通过利用压力梯度的方法(例如有灌注型方法、树脂传递模塑(RTM)的方法，或亚微米粉末吸入的方法)就能够使填充浆料渗透进入纤维织构的厚度，所述纤维织构的厚度取决于目标应用可达数十毫米。
尽管如此，注入填充浆料的纤维织构的一部分与要排出浆料液相的纤维织构的另一部分之间的压力梯度难以在整个纤维织构上进行控制。如果在面向具有一个或多个排放出口的模具端部的纤维织构的整个表面积上压力不均匀，则在靠近出口的区域和远离的区域之间产生压力差，其中浆料的液相通过所述排放出口进行排放。在此情况下，难以排放所述液相，因为需要从织构中除去液相而不妨碍已通过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。特别地，在进行排放时，液相可以带走颗粒，并且/或者可能改变纤维织构中颗粒的分布以及由此可能由于在某些位置缺少基质而导致最终材料中产生大孔。
发明内容
本发明的目的在于改进上述缺点并提出能够由厚的和/或形状复杂的纤维织构用复合材料(特别是用氧化物/氧化物型或CMC型复合材料)制造部件的方案，并且以快速且可靠的方式实施，同时对固体颗粒在纤维织构中的沉积和分布进行良好的控制以获得具有非常少量的大孔的材料。
为此，本发明提供了一种由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；
·将纤维织构置于注入工具中；
·在压力下将含有耐火陶瓷颗粒的粉末的浆料注射入纤维织构；
·使得通过纤维织构的浆料的液体排出，同时将耐火陶瓷颗粒的粉末保持在所述织构内，以获得填充有陶瓷颗粒的纤维预制件；
·将所述纤维预制件干燥；
·将所述纤维预制件脱模；以及
·对所述纤维预制件中存在的耐火陶瓷颗粒进行烧结，以在所述预制件中形成耐火基质；
所述方法的特征在于，注入工具包括多孔材料的模具，其具有在内部放置纤维织构的内部壳体，所述浆料经由存在于注入工具中并通向多孔材料模具的内部壳体的至少一个注入端口来注入所述纤维织构，所述工具还包括由刚性材料制成的外壳，其中当在压力下注入浆料并且在排出所述浆料的液体的同时，多孔材料模具被保持在该外壳中，浆料的液体经由存在于刚性材料外壳中的至少一个出口排出。
通过使用由多孔材料制成的模具，本发明的方法能够从已经引入纤维织构的浆料中除去液相，而不会除去也存在于织构中的耐火固体颗粒。而且，因为多孔材料模具围绕整个纤维织构，浆料的液体可以在所有方向上从所述织构中排出，即，通过织构和模具之间界面的任意点排出。这用于通过使得纤维织构中耐火陶瓷颗粒均匀且致密沉淀来提高沉积，并因此在最终复合材料部件中获得了高基质体积分数，并且显著增加了排液时间。因此，复合材料部件具有改进的机械性质。
而且，因为多孔材料模具保持在由刚性材料制成的外壳中，其可以耐受将填充浆料注入织构的压力以及泵送所施加的压力，从而排出浆料的液体介质。
根据本发明方法的具体特征，所述多孔材料模具具有尺寸小于刚性材料外壳的内部体积，并且多孔材料模具和刚性材料外壳之间存在的体积用致密的多孔介质进行填充。多孔介质的使用特别用于通过与任何类型的模具形状(即使是复杂的)紧密贴合而有助于将多孔材料模具集成在注入模具中，同时确保力在模具和注入工具的外壳之间良好地传递。该传递使得能够提高压力而不会使得多孔模具变形。因此，大幅减少了密封问题。此外，模具周围存在的多孔介质能够使得浆料的液体更好地从多孔材料模具中排出，由此使得在每次注入后更易于清洁，并且因此有利于其再使用。
存在于多孔介质中的空的体积优选大于注入到纤维织构中的浆料的液相体积。
多孔介质可以具体由沙子、泡沫、或具有堆叠部分的任何粒状材料构成，所述堆叠部分可以为滤液提供壳体或通道。
在本发明方法的一个具体方面，模具可以由选自以下材料的至少一种材料制成：多孔树脂和灰泥。
在形成纤维织构的步骤中，纱线可以使用三维编织或多层编织进行编织。所述纤维织构还可以通过堆叠用二维编织所编织的层来制造，所述织构的厚度为至少0.5毫米(mm)，优选为至少1mm。
所述预制件的纱线可由纤维制成，所述纤维由以下材料中的一种或多种构成：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；硼硅酸盐；碳化硅；和碳。
所述耐火陶瓷颗粒可由选自以下的材料制成：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；铝磷酸盐；二氧化锆；碳化物；硼化物；和氮化物。
在一实施方式中，由复合材料制成的所获得的部件可以构成涡轮发动机叶片。
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进行显示，所述具体实施方式以非限制示例的形式给出，附图中：
图1是根据本发明的一实施方式中注射工具的示意性分解透视图；
图2是显示当由位于其中的纤维织构密闭时，图1的工具的示意性截面图；和
图3是显示图2的工具中用填充浆料对纤维织构进行浸渍的步骤的示意性截面图。
具体实施方式
本发明的用于制造复合材料部件(特别是氧化物/氧化物型或CMC型的复合材料部件)的方法首先制造用于形成部件的增强物的纤维织构。
纤维结构以常规方式通过使用提花织机(Jacquard type loom)以多个层用设置于其上的一束经纱或股线进行编织，所述经纱通过纬纱相互连接，或者也可正好相反。所述纤维织构可通过堆叠由二维(2D)编织获得的层来制造。所述纤维织构也可通过三维(3D)编织来直接制造成单一部件。本文所用的术语“二维编织”是指常规的编织方法，其中，各纬纱从单层经纱的一侧穿至另一侧，或者也可正好相反。本发明的方法特别适合将填充浆料引入2D纤维织构，即，通过堆叠2D层而获得的较大厚度的织构，即，厚度为至少0.5mm、优选至少1mm的2D纤维结构。
本文所用的术语“三维编织”或“3D编织”、或实际上的“多层编织”是指一种编织技术，其中，纬纱中的至少一些与多层经纱相互连接，或者也可正好相反，使用可通过具体选自以下编织方法的编织方法来进行：互锁编织(interlock)；多平纹编织(multi-plain)；多缎纹编织(multi-satin)；和多斜纹编织(multi-twill)。
本文所用术语"互锁编织或织物"指的是3D编织，其中各经纱层与多层纬纱层互连，并且给定经列中的所有纱线在编织平面中同样地移动。
本文所用术语"多平纹编织或织物"指的是使用多层纬纱的3D编织，其中各层的基本花纹与常规的平纹类型花纹等同，但是花纹的某些点与纬纱层彼此互连在一起。
本文所用术语"多缎纹编织或织物"指的是使用多层纬纱的3D编织，其中各层的基本花纹与常规的缎纹类型花纹等同，但是花纹的某些点与纬纱层彼此互连在一起。
本文所用术语"多斜纹编织或织物"指的是使用多层纬纱的3D编织，其中各层的基本花纹与常规的斜纹类型花纹等同，但是花纹的某些点与纬纱层彼此互连在一起。
3D织构具有复杂的构型，难以向其中引入悬浮液的固体颗粒并将其均匀分散。本发明的方法也非常适合将填充的粉浆引入3D编织纤维织构。
用于编织将要形成复合材料部件的纤维增强物的纤维织构的纱线可由纤维制成，所述纤维由以下材料中的一种构成：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；硼硅酸盐；碳化硅；碳；或这些材料中多种的混合物。
一旦制成了纤维织构，则将其放入根据本发明的注入工具中，使得能够将耐火颗粒沉积在纤维织构内，如以下所说明的。为此，如图1和图2所示，将纤维织构10置于注入工具100中。在当前描述的示例中，纤维织构10使用如上所述技术(堆叠2D层或3D编织)中的一种技术和由Nextel 610TM氧化铝制成的纱线来制造。在该示例中，纤维织构10用于形成叶片的纤维增强物，所述叶片由氧化物/氧化物复合材料制成。
工具100包括由多孔材料制成的模具110，其由两个部分111和112组成，所述部分各自具有相应的凹部1110或1120。当两个部分111和112相对于彼此组装在一起时，凹部1110和1120限定了模腔113(图2)，所述腔接收纤维织构。凹部1110和1120具有与由纤维织构所制造部件形状相对应的形状。两个部分111和112用于确定预制件的尺寸，以及由此获得的部件的尺寸，并用于调整所获得部件中的纤维含量。
在当前描述的示例中，多孔材料模具110的部分111包括用于将填充浆料注入纤维织构的通道1111，如下文详述。
注入工具100还具有其中保持多孔材料模具110的刚性材料外壳130。外壳130具有底部131、固定到底部131的侧壁132、和盖子133。外壳130可以由满足以下条件的材料中的任一类型制成：具有足够刚性以耐受将浆料注入的压力和真空泵送以排出其液相的压力。特别是，外壳可以由金属或塑料材料制成。
盖子133包括注入端口134，浆料通过所述注入端口134注入以渗入纤维织构10的孔中。在如图1和图2所示的示例中，通过通向模腔113的注入端口134将浆料注入。然而，通过多个通向模腔的注入端口将浆料注入不会超出本发明的范围。
外壳130具有用于排放浆料的液体介质的单独排放出口135，出口在该示例中存在于底部131附近的侧壁132中。当然，如果在外壳的不同位置使用多个排出口，也不会超出本发明的范围。
在当前描述的实施方式中，多孔材料模具110的尺寸小于由金属材料制成的外壳130的内部体积。在该情况下，由多孔材料制成的模具和由金属材料制成的外壳之间存在的体积用多孔介质120填充，以使得浆料的液相流动并排出。特别是，多孔介质120可以由沙子、泡沫或粒状材料构成。如果使用泡沫，则具有允许浆料的液体介质通过的孔阵列的任何刚性或柔性类型的泡沫可用作多孔介质。类似地，任何类型的具有与通过浆液的液相相容的填充分数的粒状材料可以用作多孔介质。多孔介质120包括与外壳130的注入端口134和多孔材料模具110的通道1111连通的导管121。
多孔介质中存在的空的体积优选大于注入到纤维织构中的浆料的液相体积。当通过一个或多个排放出口抽真空和/或在通过注入端口施加压力时，这可以将所有液相从多孔模具的壁中排出。
在实施方式的一个变体中，多孔材料模具具有与外壳内部体积相当的外部尺寸。在该情况下，多孔材料模具与外壳内壁直接接触。在该情况下，优选选择多孔材料模具的尺寸，使得其具有大于注入到纤维织构中浆料的液相的量或体积的空隙体积。当通过一个或多个出口抽真空时，这可以优化纤维织构的填充。
例如，多孔材料模具110可以由多孔树脂制成。在该情况下，模具110的部分111和112本身通过在模具和夹模之间注塑并使得树脂聚合来制备，如果凹部是相同的，模具具有与部分111和112的凹部1110和1120相同的形状。否则，各部分111和112使用不同的模具，以在每个部分中形成不同的凹部。模具中的孔阵列的特征、特别是孔径和孔隙度(空隙分数)可以通过调整聚合周期随所用树脂的变化关系进行控制。因此，孔阵列的选择与可用的多孔树脂一样多。作为非限制性示例，以下多孔树脂可以用于制造多孔材料模具：
·孔尺寸范围8微米(μm)至13μm的
Figure GDA0003021757470000072
T；
·孔尺寸范围4μm至7μm的
Figure GDA0003021757470000073
F+；
·孔尺寸范围3μm至10μm的SamaPore；以及
·孔的平均孔径为7μm的Microplast Fine。
模具110、或者更精确地构成模具110的部分111和112可以由刚性多孔材料制成，例如，微孔聚四氟乙烯(PTFE)，例如，供应商Porex公司出售的产品“微孔PTFE”。为了制造模具110，例如，可以使用供应商
Figure GDA0003021757470000071
售卖的平均孔径范围为1μm～2μm的材料PM 0130。各凹部1110和1120分别通过多孔材料的热成型或机械加工制成。
作为非限制性示例，模具110也可以由灰泥制成。
由于在出口135和注入端口134之间施加压力梯度，多孔材料模具110能够使得浆料的液体介质从纤维织构10排出，并且通过出口135排放。
例如，多孔材料模具的平均孔径(D50)范围可以是例如1μm至10μm。
图3显示了在注入浆料150并排出其液相或液体介质时获得的构型。在将浆料注入工具之前，在多孔材料模具中抽真空，以使得纤维织构随后可以最大程度填充浆料。可以通过泵送通过排放出口135来抽真空。
图3中，在压力下通过注入端口121将浆料150注入，并且通过管道121和通道1111输送到纤维织构10，以渗透到纤维织构10中。存在于浆料150中的耐火颗粒1500用于形成纤维织构10的孔中的耐火陶瓷基质。在一实施方式中，该耐火陶瓷基质可以是耐火氧化物基质。
例如，浆料可以是氧化铝粉末在水中的悬浮液。所用的氧化铝粉末可以是销售商Baikowski以商品名SM8售卖的α-氧化铝粉末。
更一般地，浆料可以是包含具体平均粒度范围为0.1μm至10μm的耐火陶瓷颗粒的悬浮液。在注入前，浆料中耐火陶瓷颗粒的体积分数范围为15％至40％。所述耐火陶瓷颗粒可包含选自以下的材料：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；铝磷酸盐；碳化物；硼化物；氮化物；和这些材料的混合物。取决于它们的基础成分，耐火陶瓷颗粒也可与氧化铝颗粒、氧化锆颗粒、铝硅酸盐颗粒、稀土氧化物颗粒、稀土硅酸盐的颗粒(例如可以用于环境屏障或热屏障)、或适用于为所获得的复合材料部件提供功能的任意其它填料(例如，碳黑、石墨、碳化硅等)混合。
例如，浆料的液相或体液介质可以包含具有酸性pH(即，小于7的pH)的水相和/或醇相(例如，包括乙醇)。浆料可以包含酸化剂，例如，硝酸，并且，例如，液体介质的pH范围可以为1.5至4。此外，浆料可以包括有机粘合剂，例如，特别是可溶于水的聚乙烯醇(PVA)。
如图3所示，在注入浆料150之后，耐火陶瓷颗粒1500存在于纤维织构10的孔中。箭头1501表示通过多孔材料模具110排出的浆料液相或液体介质1501的移动。
还可以在排液的同时向排出口135施加泵送作用P，例如使用初级真空泵来施加。实施该泵送用于改进排水并使得纤维织构更快干燥。
在该构造中，多孔材料模具110用于将用于将最初存在于浆料中的耐火陶瓷颗粒1500保持在纤维织构10内，使得这些颗粒中的一些或全部通过过滤而沉积在纤维织构10中。
通过使用多孔材料模具110，浆料的液相或液体介质1501可以在所有方向上从纤维织构10排出，并且液相或液体介质1501随后流动通过多孔介质120到达出口135，其通过出口135从注入工具100排放出来。液体介质在所有方向上的这样排出使得纤维织构10中均匀且致密沉淀来提高耐火陶瓷颗粒1500的沉积，并因此在最终部件中获得了高基质体积分数。
而且，因为多孔材料模具110保持在由刚性材料制成的外壳130中，其可以经受将填充浆料注入织构的压力以及泵送所施加的压力，从而排放浆料的液体介质。
一旦实施了注入和排放步骤，获得了填充有耐火陶瓷颗粒、例如耐火陶瓷氧化物颗粒或氧化铝颗粒的纤维预制件15。
所获得的预制件随后进行干燥，然后脱模，经脱模的预制件保持其在模腔中所采用的形状。
然后，对预制件进行烧结热处理，例如在1000℃至1200℃的温度范围下在空气中进行烧结热处理，从而烧结耐火陶瓷颗粒，由此在纤维预制件的孔中形成耐火陶瓷基质。这生产出了复合材料部件，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物并呈现出均匀分布在整个纤维增强物中的耐火陶瓷基质的高基质体积分数。
除了氧化物/氧化物部件之外，CMC复合材料部件可以通过如下以相同的方式获得：由碳化硅纤维和/或碳纤维制成纤维织构，并使用填充有碳化物颗粒(例如SiC)、硼化物颗粒(例如TiB2)或氮化物颗粒(例如Si3N4)的浆料。

Claims (8)

1.一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(10)；
·将所述纤维织构(10)置于注入工具(100)中；
·在压力下将含有耐火陶瓷颗粒(1500)的粉末的浆料(150)注射入纤维织构(10)；
·使得通过纤维织构(10)的浆料(150)的液相(1501)排出，同时将耐火陶瓷颗粒的粉末保持在所述织构内，以获得填充有耐火陶瓷颗粒(1500)的纤维预制件(15)；
·将所述纤维预制件(15)干燥；
·将所述纤维预制件(15)脱模；以及
·对所述纤维预制件中存在的耐火陶瓷颗粒进行烧结，以在所述预制件中形成耐火基质；
所述方法的特征在于，注入工具包括多孔材料模具(110)，其具有其内放置纤维织构(10)的内部壳体(113)，所述浆料(150)经由存在于注入工具中并通向多孔材料模具(110)的内部壳体(113)的至少一个注入端口(134)注入所述纤维织构(10)，所述注入工具还包括由刚性材料制成的外壳(130)，其中当在压力下注入浆料(150)并且在排出所述浆料的液相(1501)的同时，多孔材料模具(110)被保持在该外壳中，浆料的液相(1501)通过存在于刚性材料外壳中的至少一个出口(135)排出，
其中，所述多孔材料模具(110)围绕整个纤维预制件(15)，
其中，所述多孔材料模具(110)的尺寸小于刚性材料外壳(130)的内部体积，并且多孔材料模具和刚性材料外壳之间存在的体积用多孔介质(120)进行填充。
2.如权利要求1所述的方法，其特征在于，多孔介质(120)至少由沙子或泡沫构成。
3.如权利要求1所述的方法，其特征在于，存在于多孔介质(120)中的空的体积大于注入纤维织构(10)的浆料(150)的液相(1501)的体积。
4.如权利要求1所述的方法，其特征在于，所述模具(110)由选自由以下材料中的一种材料制成：多孔树脂和灰泥。
5.如权利要求1所述的方法，其特征在于，在形成所述纤维织构(10)的步骤中，以三维编织或多层编织对纱线进行编织。
6.如权利要求1所述的方法，其特征在于，所述纤维织构(10)的纱线由纤维制成，所述纤维由一种或多种以下材料构成：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；硼硅酸盐；碳化硅；和碳。
7.如权利要求1所述的方法，其特征在于，所述耐火陶瓷颗粒(1500)由选自以下的材料制成：氧化铝；多铝红柱石；二氧化硅；铝硅酸盐；铝磷酸盐；二氧化锆；碳化物；硼化物；和氮化物。
8.如权利要求1所述的方法，其特征在于，由复合材料所制得的部件构成了涡轮发动机叶片。
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WO2017060601A8 (fr) 2017-12-21
FR3041890B1 (fr) 2017-11-24
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JP2018537378A (ja) 2018-12-20
BR112018006792A2 (pt) 2018-10-16
RU2721674C2 (ru) 2020-05-21
CA3000963A1 (fr) 2017-04-13
US20180297901A1 (en) 2018-10-18
EP3359506B1 (fr) 2022-02-09
RU2018116397A (ru) 2019-11-08
WO2017060601A1 (fr) 2017-04-13
FR3041890A1 (fr) 2017-04-07
RU2018116397A3 (zh) 2020-03-23
JP6878420B2 (ja) 2021-05-26
US10954169B2 (en) 2021-03-23

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