CN111039686A - 一种含原位孔的连续纤维增强陶瓷基复合材料制备方法 - Google Patents

一种含原位孔的连续纤维增强陶瓷基复合材料制备方法 Download PDF

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CN111039686A
CN111039686A CN201911283878.XA CN201911283878A CN111039686A CN 111039686 A CN111039686 A CN 111039686A CN 201911283878 A CN201911283878 A CN 201911283878A CN 111039686 A CN111039686 A CN 111039686A
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谢巍杰
邱海鹏
陈明伟
赵禹良
罗文东
王晓猛
王岭
刘善华
张冰玉
马新
刘时剑
梁艳媛
关宏
王启明
李秀倩
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
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Abstract

本发明是一种含原位孔的连续纤维增强陶瓷基复合材料制备方法，本发明提供的含原位孔的连续纤维增强陶瓷基复合材料制备方法通过含原位孔结构的连续纤维预制体制备、原位孔结构的固定、陶瓷基体填充等过程控制，实现在获得孔结构的同时保持连续纤维增强陶瓷基复合材料结构完整性，与现有后加工制孔方法相比，不会对连续纤维和基体造成破坏损伤且高效低成本，能够使含孔结构的连续纤维增强陶瓷基复合材料的力学性能提升10％～60％。

Description

一种含原位孔的连续纤维增强陶瓷基复合材料制备方法
技术领域
本发明是一种含原位孔的连续纤维增强陶瓷基复合材料制备方法，属于陶瓷基复合材料的制备技术领域。
背景技术
连续纤维增强陶瓷基复合材料具有陶瓷材料耐高温、抗氧化、耐磨损、耐腐蚀等优点，同时因连续纤维的增强增韧作用而具有优异的抗外部冲击载荷性能。连续纤维增强陶瓷基复合材料凭借良好的高温稳定性和高温力学性能，在先进航空发动机热端部件、先进飞行器热防护***等领域得到越来越广泛的应用。
连续纤维增强陶瓷基复合材料在实际应用中通常包含孔结构，用于连接、装配、作为冷却通道等。目前常用的制孔方式为采用后加工方式在完整材料上制孔，如机械加工钻削制孔、激光制孔、水切割制孔、线切割制孔等，以上方式均会造成材料中的连续纤维与基体受到破坏损伤，从而使材料力学性能降低，进而影响构件整体使用性能。另外，陶瓷基复合材料由于超高的硬度和材料本身的不均匀性以及较大的脆性而属于典型的难加工材料，后加工方式制孔难度大且成本高。典型的在先进航空发动机领域，燃烧室等部位的部分热端构件需要进行数以千计甚至数以万计的阵列气膜孔制备，气膜孔孔径小、数量多，加工难度很大且成本很高，另外对于连续纤维增强陶瓷基复合材料热端构件，大量的气膜孔会对连续纤维和基体造成严重损伤，使构件力学性能大幅下降。如何获得孔结构的同时保持连续纤维增强陶瓷基复合材料结构的完整性，如何高效低成本获得孔结构，是连续纤维增强陶瓷基复合材料应用领域亟待解决的问题。
发明内容
本发明正是针对上述现有技术状况而设计提供了一种含原位孔的连续纤维增强陶瓷基复合材料制备方法，其目的是为含孔结构的连续纤维增强陶瓷基复合材料的制备提供有效解决方案，所述原位孔是指在完成连续纤维增强陶瓷基复合材料制备的同时无需通过加工即可获得的孔结构，实现了孔结构高效、低成本的制备，且在获得孔结构的同时不对连续纤维增强陶瓷基复合材料结构造成损伤，从而提升了含孔结构的连续纤维增强陶瓷基复合材料的力学性能。
本发明的技术解决方案是：
该种含原位孔的连续纤维增强陶瓷基复合材料制备方法的步骤如下：
步骤一、依据孔的尺寸及位置要求，制备含原位孔结构的连续纤维预制体，所述原位孔由连续纤维包围的不含连续纤维的空腔构成；
步骤二、固定原位孔结构，固定方式根据连续纤维预制体的特征采用以下方式之一：
第一种方式：针对预浸料类型的连续纤维预制体，对预制体进行热处理，使树脂固化或碳化，使原位孔结构固定；
第二种方式：针对非预浸料类型的连续纤维预制体，在连续纤维预制体表面制备固定层，使原位孔结构固定，固定层材料为热解炭、氮化硼、碳化硅、有机聚合物；
步骤三、针对连续纤维预制体中除原位孔结构之外的孔隙填充陶瓷基体，原位孔不被陶瓷基体填充，其它孔隙被陶瓷基体填充，完成含原位孔的连续纤维增强陶瓷基复合材料的致密化，得到含原位孔的连续纤维增强陶瓷基复合材料。
在一种实施中，步骤二的第二种方式中，所述固定层的厚度为500nm～100μm。
在一种实施中，所述原位孔孔径不小于0.1mm。
在一种实施中，所述原位孔的分布为阵列分布。
在一种实施中，所述连续纤维为碳纤维、碳化硅纤维、氮化物纤维、氧化物纤维。
在一种实施中，所述连续纤维预制体制备方式为铺丝、铺带、铺层、机织、手工编织，连续纤维预制体结构为单向带、2D铺层、2.5D编织、3D编织。
在一种实施中，所述固定层的制备方式为化学气相渗透、液相浸渍。
在一种实施中，所述陶瓷基体为碳化硅、氮化物陶瓷、氧化物陶瓷。
在一种实施中，采用液相浸渍填充陶瓷基体时，特别针对薄壁结构连续纤维增强陶瓷基复合材料，使连续纤维预制体表面与液相浸渍剂接触且不被液相浸渍剂浸没，根据毛细管作用原理，通过调整液相浸渍剂粘度实现对临界孔隙尺寸的控制，使浸渍剂对应的临界孔隙尺寸大于连续纤维预制体中除原位孔结构之外的孔隙尺寸，这样液相浸渍剂就能够通过毛细管作用充分填充除原位孔结构之外的孔隙，原位孔的尺寸大于临界孔隙尺寸而不会被填充，最终得到保留并形成连续纤维增强陶瓷基复合材料中的原位孔，其它孔隙尺寸小于临界孔隙尺寸而被浸渍剂填充，最终被陶瓷基体填充而致密化，临界孔隙尺寸为直径0.05mm～5mm，浸渍剂为有机树脂、无机溶液、液相金属。对于壁厚较厚的连续纤维增强陶瓷基复合材料，连续纤维预制体需要部分或全部浸没于液相浸渍剂中使孔隙被充分填充，随后连续纤维预制体离开液相浸渍剂，原位孔中的浸渍剂会因缺少毛细管作用而在重力作用下排出，其它孔隙中的浸渍剂会因毛细管作用而保持填充状态，若原位孔中仍有液相浸渍剂残留，可进一步通过物理、化学方式对残留的液相浸渍剂进行清除，实现原位孔结构的保留，清除方式为真空吸除、高速气流吹除、溶解清除、反应清除。
在一种实施中，采用气相先驱体填充陶瓷基体时，利用化学气相渗透过程中对气体流场进行控制而在原位孔中不发生沉积，使原位孔不被填充而得到保留并形成连续纤维增强陶瓷基复合材料中的原位孔，其它孔隙中发生沉积而被填充，最终被陶瓷基体填充而致密化，气体流场控制方式为设置导流装置、控制工艺气体组分与浓度。
本发明具有的优点和有益效果是：本发明提供的含原位孔的连续纤维增强陶瓷基复合材料制备方法通过含原位孔结构的连续纤维预制体制备、原位孔结构的固定、陶瓷基体填充等过程控制，实现在获得孔结构的同时保持连续纤维增强陶瓷基复合材料结构完整性，与现有后加工制孔方法相比，不会对连续纤维和基体造成破坏损伤且高效低成本，能够使含孔结构的连续纤维增强陶瓷基复合材料的力学性能提升10％～60％。
附图说明：
图1为实施例中含原位孔结构的连续纤维预制体示意图；
图2为实施例中连续纤维与固定层的示意图；
图3为实施例中陶瓷基体填充示意图。
具体实施方式：
以下结合附图和下述实施方案对本发明做进一步的详细说明：
参见附图1～3所示，制备具有阵列气膜孔结构的连续碳化硅纤维增强碳化硅陶瓷基复合材料航空发动机热端部件，气膜孔径向尺寸为0.8mm，气膜孔呈矩阵分布，相邻列间距为3mm，相邻行间距为2mm，该种含原位孔的连续纤维增强陶瓷基复合材料制备方法的步骤如下：
步骤一、依据孔的尺寸及位置要求，制备含原位孔结构的连续纤维预制体：依据原位孔2的尺寸及位置要求，进行含原位孔2结构的连续纤维预制体1制备，采用连续碳化硅纤维进行2.5D结构预制体的机织，通过编织机对经纱与纬纱的空间位置进行排布，获得含原位孔2和其它孔隙3的连续碳化硅纤维预制体1，原位孔2的径向尺寸为0.9mm，其它孔隙3的尺寸小于0.1mm，原位孔2呈矩阵分布，相邻列间距为3mm，相邻行间距为2mm；
步骤二、固定原位孔结构：采用化学气相渗透工艺在连续碳化硅纤维4表面制备固定层5，使原位孔2结构固定，固定层5材料为热解炭，固定层5厚度为50μm；
步骤三、针对连续纤维预制体1中除原位孔2结构之外的孔隙3填充陶瓷基体6：采用聚碳硅烷浸渍裂解工艺填充陶瓷基体，所用聚碳硅烷液态浸渍剂对应的临界孔隙尺寸为直径0.1mm，使连续纤维预制体1表面与液相浸渍剂接触且不被液相浸渍剂浸没，液相浸渍剂通过毛细管作用充分填充除原位孔2结构之外的孔隙3，原位孔2的尺寸大于临界孔隙尺寸而不会被填充，最终得到保留并形成连续碳化硅纤维增强碳化硅陶瓷基复合材料7中的原位孔2，其它孔隙3尺寸小于临界孔隙尺寸而被浸渍剂填充，最终经裂解被碳化硅陶瓷基体6填充而致密化，得到含原位孔2的连续碳化硅纤维增强碳化硅陶瓷基复合材料7。

Claims (9)

1.一种含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：该方法的步骤如下：
步骤一、依据孔的尺寸及位置要求，制备含原位孔结构的连续纤维预制体，所述原位孔由连续纤维包围的不含连续纤维的空腔构成；
步骤二、固定原位孔结构，固定方式根据连续纤维预制体的特征采用以下方式之一：
第一种方式：针对预浸料类型的连续纤维预制体，对预制体进行热处理，使树脂固化或碳化，使原位孔结构固定；
第二种方式：针对非预浸料类型的连续纤维预制体，在连续纤维预制体表面制备固定层，使原位孔结构固定，固定层材料为热解炭、氮化硼、碳化硅、有机聚合物；
步骤三、针对连续纤维预制体中除原位孔结构之外的孔隙填充陶瓷基体，原位孔不被陶瓷基体填充，其它孔隙被陶瓷基体填充，完成含原位孔的连续纤维增强陶瓷基复合材料的致密化，得到含原位孔的连续纤维增强陶瓷基复合材料。
2.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：步骤二的第二种方式中，所述固定层的厚度为500nm～100μm。
3.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述原位孔孔径不小于0.1mm。
4.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述原位孔的分布为阵列分布。
5.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述连续纤维为碳纤维、碳化硅纤维、氮化物纤维、氧化物纤维。
6.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述连续纤维预制体制备方式为铺丝、铺带、铺层、机织、手工编织，连续纤维预制体结构为单向带、2D铺层、2.5D编织、3D编织。
7.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述固定层的制备方式为化学气相渗透、液相浸渍。
8.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：所述陶瓷基体为碳化硅、氮化物陶瓷、氧化物陶瓷。
9.根据权利要求1所述的含原位孔的连续纤维增强陶瓷基复合材料制备方法，其特征在于：采用液相浸渍填充陶瓷基体时，浸渍剂的临界孔隙尺寸应大于连续纤维预制体中除原位孔结构之外的孔隙尺寸。
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