CN107042661B - 一种耐高温热防护材料及其制备方法 - Google Patents

一种耐高温热防护材料及其制备方法 Download PDF

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CN107042661B
CN107042661B CN201611107668.1A CN201611107668A CN107042661B CN 107042661 B CN107042661 B CN 107042661B CN 201611107668 A CN201611107668 A CN 201611107668A CN 107042661 B CN107042661 B CN 107042661B
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fabric
fiber
high temperature
ceramic
resistant protective
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CN107042661A (zh
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裴雨辰
周玉贵
李文静
苏力军
刘斌
赵英民
鲁胜
权�成
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

本发明提出一种耐高温热防护材料及其制备方法，通过纤维框架织物制备、辅助支撑的制备、纤维框架织物陶瓷化、陶瓷基框架结构与隔热填料复合等步骤得到耐高温热防护材料。本发明采用辅助支撑与纤维框架结构结合，得到陶瓷基框架结构，最终得到轻质、防热、隔热、承载一体化的耐高温热防护材料。

Description

一种耐高温热防护材料及其制备方法
技术领域
本发明涉及一种耐高温热防护材料及其制备方法，属于热防护材料技术领域。
背景技术
先进航空航天技术飞跃发展，飞行器独特的力学结构和功能性要求对材料提出更多技术挑战：结构轻质化和多功能化。轻质夹层结构材料具有高比强度、高比刚度等特点，如金属蜂窝、泡沫和波纹板夹层结构等，在航空航天中广泛应用。
在热防护系统轻质多功能化方面，有以下两种结构材料：
以承载-隔热双层防热结构为特点的金属面板TPS，采用轻质金属蜂窝结构，起承载作用；内层使用saffil氧化铝纤维等多层绝热层，起隔热作用。该结构通常较重、耐温低，结构轻量化与结构力学可靠性已成为航天飞行器亟待解决的一项难题。
以四面体点阵夹层结构为特点的盖板式TPS，其结构将轻质化、承载能力和热防护设计相结合，其上层点阵夹层板、中间隔热层、下面板及侧面板组成。上层点阵夹层板由耐高温金属冲压成型，中间隔热层由氧化铝纤维、超细玻璃纤维等两层隔热纤维层组成。该结构存在材料种类多、成型装配工艺复杂、耐温等级低等缺点。
在树脂基复合材料中使用框架结构进行减重和承载，框架结构一般为立体织物浸胶固化得到，但由于树脂基复合材料的耐温、隔热性能无法达到热防护领域的要求，采用陶瓷基体可以提供其耐温、隔热性能，但在陶瓷化过程中，立体织物由于编织特点，能适应前驱体真空或压力浸渍的，立体织物面密度太大，前驱体无法顺利浸渍织物；而要满足前驱体顺利浸渍织物，在前驱体真空或压力浸渍时，立体织物又无法维形。
发明内容
本发明的目的在于克服现有技术不足，提供一种轻质、防热、隔热、承载一体化的耐高温热防护材料及其制备方法。
本发明的技术解决方案：一种耐高温热防护材料，由陶瓷基框架结构及填充在陶瓷基框架结构内的隔热填料构成，所述的陶瓷基框架结构为纤维框架织物在辅助支撑的作用下浸渍陶瓷前驱体后陶瓷化得到；
所述的纤维框架织物由上下表面结构层织物和中间波纹支撑层织物进行锁式缝合制成。
所述的辅助支撑在前驱体陶瓷化温度下能裂解成气体或粉末等物质，并具有在浸渍陶瓷前驱体过程中维形的强度。具体种类没有特殊限制，只要能满足上述要求即可，一般使用有机泡沫、石墨材料、纸板等。
本发明对纤维框架织物的纤维种类没有特殊限制，只要能满足耐温等级要求即可，可以采用常见的石英纤维织物、氧化铝纤维织物、碳纤维织物等。织物形式为纤维平纹布、纤维斜纹布、纤维2.5D编织布等。
陶瓷基框架结构单元形状可以为三角形结构、方形或矩形结构、梯形结构等中的任意一种，如图2所示。
所述的隔热填料为陶瓷纤维棉、气凝胶材料、纤维增强气凝胶材料等中的一种或任意几种。
所述的陶瓷前驱体为本领域常用陶瓷前驱体，根据耐温等级进行具体种类选择，如可采用常见的硅溶胶、硅树脂等。
本发明框架结构空隙填充隔热填料，采用框架结构化的热防护材料改善了结构强度，除满足热防护需求，并提高对垂直方向载荷具有抗压及承载强度。
一种耐高温热防护材料的制备方法，通过以下步骤实现：
第一步，纤维框架织物制备，
纤维框架织物包括上下表面结构层织物和中间波纹支撑层织物，将上、下表面结构层织物依次与中间支撑层织物进行锁式缝合；
所述的上下表面结构层织物厚度为1mm～3mm，中间波纹支撑层纤维织物厚度为0.5mm～1.0mm。厚度的控制，确保结构力学稳定性。
锁式缝合为本领域公知技术，本领域技术人员根据实际生产进行缝合才是的选择，如纤维框架织物的缝合行距可以采用3mm～6mm，缝合针距可以采用5mm～8mm。
第二步，按照第一步制备的纤维框架织物的框架单元的结构尺寸，制备辅助支撑；
第三步，纤维框架织物陶瓷化，
将第二步制备的辅助支撑填充到第一步制备的纤维框架织物内，进行陶瓷前驱体浸渍，浸渍完成后，进行高温陶瓷化处理，得到陶瓷基框架结构；
陶瓷前驱体浸渍及陶瓷化处理为本领域公知技术，根据实际生产选择前驱体种类、浸渍次数、浸渍形式及将陶瓷化处理的温度、时间等。辅助支撑在陶瓷化处理过程中被氧化、裂解成气体或粉末等物质。
第四步，陶瓷基框架结构与隔热填料复合，得到耐高温热防护材料。
将第三步得到的陶瓷基框架结构与隔热填料进行复合，根据不同种类的隔热填料采用不同复合方法，制成耐高温热防护材料。
若使用陶瓷纤维棉，将陶瓷纤维棉填充到陶瓷基框架结构内的空隙中；若使用气凝胶材料，采用溶胶凝胶法对陶瓷基框架结构完成气凝胶材料填充；若使用纤维增强气凝胶材料，采用溶胶凝胶法等方法对陶瓷基框架结构完成纤维增强气凝胶材料填充。具体复合方法为本领域公知技术，本领域技术人员自行选择。
进一步，对第四步得到的耐高温热防护材料进行三防处理。
在第四步得到的耐高温热防护材料表面喷涂三防漆，增加其防潮、防霉菌、防盐雾的能力。三防处理为本领域公知技术，在此不一一赘述。
本发明与现有技术相比的有益效果：
(1)本发明采用辅助支撑与纤维框架结构结合，得到陶瓷基框架结构，最终得到轻质、防热、隔热、承载一体化的耐高温热防护材料；
(2)本发明框架结构改善了结构强度，具有耐高温、耐高温高压承载、高效隔热等特点，并提高对垂直方向载荷具有抗压及承载强度；
(3)本发明材料成本低、制备周期短、工艺适应性强，可制成平板和异型复杂构件；
(4)本发明集轻质、防热、隔热、承载、抗压等高性能多功能于一体，性能优异，成本低及制备周期短，应用推广价值大。
附图说明
图1为本发明流程图；
图2为本发明不同结构单元的陶瓷基框架结构，a为三角形、b为矩形、c为梯形。
具体实施方式
下面结合具体实例及附图对本发明进行详细说明。
本发明如图1所示，通过纤维框架织物制备、辅助支撑的制备、纤维框架织物陶瓷化、陶瓷基框架结构与隔热填料复合等步骤得到耐高温热防护材料。
实施例1
1mm和1mm厚的织物作为表面结构层织物，1mm厚织物作为中间波纹支撑层织物，将有机泡沫按照矩形框架结构单元尺寸加工成泡沫条，缝合行距3mm，针距5mm，制成纤维框架织物；将纤维框架织物置于模具内，与硅溶胶前驱体进行浸渍8次，浸渍完成后，经过800℃高温处理得到陶瓷基框架结构，如图2b所示；将陶瓷基框架结构与陶瓷纤维棉进行填充复合，隔热填料密度为0.05g.cm-3；在材料表面喷涂三防漆，最终制成耐高温热防护材料。
本实施例制备得到的材料密度0.35g.cm-3,室温热导率0.027W/m·K，室温压缩强度3.05MPa(10％形变)，平拉伸强度2.5MPa。
实施例2
1mm和3mm厚的织物作为表面结构层织物，0.5mm厚织物作为中间波纹支撑层织物，将有机泡沫按照三角形框架结构单元尺寸加工成泡沫条，缝合行距6mm，针距8mm，制成纤维框架织物；将纤维框架织物置于模具内，与硅树脂前驱体进行浸渍6次，浸渍完成后，经过1000℃高温处理得到陶瓷基框架结构，如图2a所示；将陶瓷基框架结构与气凝胶进行复合，填料密度为0.10g.cm-3；在材料表面喷涂三防漆，最终制成耐高温热防护材料。
本实施例制备得到的材料密度0.42g.cm-3,室温热导率0.025W/m·K，室温压缩强度3.4MPa(10％形变)，平拉伸强度2.6MPa。
实施例3
3mm和3mm厚的织物作为表面结构层织物，0.8mm厚织物作为中间波纹支撑层织物，将有机泡沫按照梯形框架结构单元尺寸加工成泡沫条，缝合行距5mm，针距7mm，制成纤维框架织物；将纤维框架织物置于模具内，与硅溶胶前驱体进行浸渍4次，浸渍完成后，经过900℃高温处理得到陶瓷基框架结构；将陶瓷基框架结构与陶瓷纤维棉及气凝胶材料进行复合，填料密度为0.20g.cm-3；在材料表面喷涂三防漆，最终制成耐高温热防护材料。
本实施例制备得到的材料密度0.45g.cm-3,室温热导率0.034W/m·K，室温压缩强度3.7MPa(10％形变)，平拉伸强度2.8MPa。
本发明未详细说明部分为本领域技术人员公知技术。

Claims (7)

1.一种耐高温热防护材料，其特征在于：由陶瓷基框架结构及填充在陶瓷基框架结构内的隔热填料构成，所述的陶瓷基框架结构为纤维框架织物在辅助支撑的作用下浸渍陶瓷前驱体后陶瓷化得到；
所述的纤维框架织物由上下表面结构层织物和中间波纹支撑层织物进行锁式缝合制成；
所述辅助支撑填充到所述纤维框架织物内。
2.根据权利要求1所述的一种耐高温热防护材料，其特征在于：所述的辅助支撑在前驱体陶瓷化温度下能裂解成气体或粉末，并具有在浸渍陶瓷前驱体过程中维形的强度。
3.根据权利要求1所述的一种耐高温热防护材料，其特征在于：所述的织物形式为纤维平纹布、纤维斜纹布或纤维2.5D编织布。
4.一种耐高温热防护材料的制备方法，其特征在于，通过以下步骤实现：
第一步，纤维框架织物制备，
纤维框架织物包括上下表面结构层织物和中间波纹支撑层织物，将上、下表面结构层织物依次与所述中间波纹支撑层织物进行锁式缝合；
第二步，按照第一步制备的纤维框架织物的框架单元的结构尺寸，制备辅助支撑；
第三步，纤维框架织物陶瓷化，
将第二步制备的辅助支撑填充到第一步制备的纤维框架织物内，进行陶瓷前驱体浸渍，浸渍完成后，进行高温陶瓷化处理，得到陶瓷基框架结构；
第四步，陶瓷基框架结构与隔热填料复合，得到耐高温热防护材料。
5.根据权利要求4所述的一种耐高温热防护材料的制备方法，其特征在于：所述第四步中若隔热填料为陶瓷纤维棉，将陶瓷纤维棉填充到陶瓷基框架结构内的空隙中；若隔热填料为气凝胶材料，采用溶胶凝胶法对陶瓷基框架结构完成气凝胶材料填充；若隔热填料为纤维增强气凝胶材料，采用溶胶凝胶法对陶瓷基框架结构完成纤维增强气凝胶材料填充。
6.根据权利要求4所述的一种耐高温热防护材料的制备方法，其特征在于：所述第四步得到的耐高温热防护材料进行三防处理。
7.根据权利要求4所述的一种耐高温热防护材料的制备方法，其特征在于：所述第一步中上下表面结构层织物厚度为lmm~3mm ，中间波纹支撑层纤维织物厚度为0.5mm~1.0mm 。
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