CN111039681A - 一种制备莫来石纤维基多孔隔热瓦的简易方法 - Google Patents
一种制备莫来石纤维基多孔隔热瓦的简易方法 Download PDFInfo
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Abstract
一种制备莫来石纤维基多孔隔热瓦的简易方法,首先多晶莫来石纤维进行剪切和除渣,得到短切莫来石纤维,将聚二甲基硅油和聚二甲基硅橡胶混合,得到前驱体溶液;向前驱体溶液滴加表面活性剂油酸以达到更好的纤维分散效果,然后缓慢地加入短切莫来石纤维且边加入边搅拌;加入固化剂二丙烯三胺(DPTA)后模压成型;坯体室温下固化后在高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦;本发明克服了莫来石陶瓷纤维隔热瓦粘结剂热迁移的技术问题并且优化了生产工艺,制备的莫来石纤维隔热瓦能承受1500℃高温且有高回弹性,可用于高超声速航天飞行器。
Description
技术领域
本发明属于高温隔热材料制备领域,主要涉及一种制备莫来石纤维基多孔隔热瓦的简易方法。
背景技术
近空间高超声速飞行器航空航天技术不仅是21世纪高端科技的典型代表,也是目前国际竞相争夺空间技术的焦点之一。由于空间飞行器的工作环境极其特殊,其热防护系统所用材料高温隔热问题已成为制约其发展的主要问题之一。莫来石纤维多孔材料具有轻质、隔热、抗氧化、抗腐蚀及耐热性优良等优点且基体具有一定抗弯强度,在各类空间飞行器的热防护系统中的作用十分重大。
在满足可重复使用的需求下,烧蚀型热防护材料逐渐不在考虑范围之内。无机纤维制品在热防护系统中研究最为广泛的是石英纤维和氧化铝纤维,但是石英纤维最高只能耐温1200℃,无法满足高马赫数航天器的耐温要求。而作为氧化铝大家族中的重要成员,莫来石纤维由于其卓越的性能迅速成为了国内外最新型的超轻质高温耐火纤维,最高使用温度可达1600℃左右。
粘结剂在制备莫来石纤维多孔材料过程中的作用是最关重要的,是决定纤维骨架稳固程度的关键。传统的粘结剂是硅溶胶及其改性溶胶及其复合体系。硅溶胶粘结剂在莫来石纤维表面的铺展效果很差,而且在干燥处理过程中容易出现热迁移现象,即硅溶胶随着水分的蒸发从节点往纤维表面发生扩散,导致内部节点无法形成有效连接,且制品内外不均。
发明内容
针对现有技术存在的问题,本发明提供一种制备莫来石纤维基多孔隔热瓦的简易方法,选用了多晶莫来石纤维作为基体,聚硅氧烷混合物作为室温及高温两用粘结剂,采用模压工艺,通过有机粘结剂原位交联固化的方法来制备空间结构优良的三维同相莫来石纤维隔热材料。该方法简化了制备工艺,使材料的力学性能显著提高。
一种制备莫来石纤维基多孔隔热瓦的简易方法,其制备过程包括以下步骤:
(1)利用纤维粉碎机对多晶莫来石纤维进行剪切和除渣,剪切时间为4min~8min,得到长度为400μm~600μm且长径比为40:1~60:1的短切莫来石纤维,干燥;
(2)将聚二甲基硅油和聚二甲基硅橡胶以4:1的质量比均匀混合,得到前驱体溶液;
(3)称取100g步骤(2)中得到的前驱体溶液,滴加2wt%的表面活性剂油酸,然后缓慢地加入15wt%~45wt%的短切莫来石纤维,边加入边搅拌,待纤维添加完后继续搅拌2min~4min,直至纤维均匀地分散在浆料中,得到分散好的纤维浆料;
(4)将步骤(3)中得到的浆料从搅拌器上取下,对浆料继续进行搅拌,同时按照比例向浆料中加入1wt%~2wt%的固化剂二丙烯三胺(DPTA),继续搅拌30s左右,将浆料倒入模具中,在0.1MPa压力下成型;
(5)将步骤(4)中得到的坯体放置2h直至完全固化,之后将坯体放入高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦。烧结制度控制为在290℃~340℃之间升温4h,再以5℃/min~7℃/min的升温速率加热到1300℃~1500℃,保温2h。
一种制备莫来石纤维基多孔隔热瓦的简易方法,用有机粘结剂替代了传统的溶胶粘结体系,利用聚硅氧烷的原位交联固化及高温裂解的特性来确保纤维骨架的稳定及制品的均一性,且采用一步模压成型方法,简化了制备工艺。本发明克服了莫来石陶瓷纤维隔热瓦粘结剂热迁移的技术问题并且优化了生产工艺。聚硅氧烷粘结剂的采用相比传统氧化硅氧化硼粘结剂使隔热瓦耐温性能由1200℃提高到1500℃,同时使粘结剂对莫来石纤维有了很好的包覆,力学性能显著提高。本发明制备的莫来石纤维多孔隔热瓦能承受1500℃高温且具有高的压缩回弹性,可用于高超声速航天飞行器机身的较高温区及热密封领域。
附图说明
图1为实施例1制备的莫来石纤维多孔隔热瓦的电子扫描图片;
图2为实施例1制备的莫来石纤维多孔隔热瓦纤维搭接点处的电子扫描图片。
具体实施方式
为了更好地理解本发明,下面结合实施实例进一步阐明本发明的内容,但本发明的内容不仅仅局限于所述实施实例。
实施例1:
一种制备莫来石纤维基多孔隔热瓦的简易方法,具体是按照以下步骤进行的:
(1)利用纤维粉碎机对多晶莫来石纤维进行剪切和除渣,剪切时间为4min,得到长度为600μm且长径比为60:1的短切莫来石纤维,干燥;
(2)将聚二甲基硅油和聚二甲基硅橡胶以4:1的质量比均匀混合,得到前驱体溶液;
(3)称取100g步骤(2)中得到的前驱体溶液,滴加2wt%的表面活性剂油酸,然后缓慢地加入15wt%的短切莫来石纤维,边加入边搅拌,待纤维添加完后继续搅拌2min,直至纤维均匀地分散在浆料中,得到分散好的纤维浆料;
(4)将步骤(3)中得到的浆料从搅拌器上取下,对浆料继续进行搅拌,同时按照比例向浆料中加入2wt%的固化剂二丙烯三胺(DPTA),继续搅拌30s,将浆料倒入模具中,在0.1MPa压力下成型;
(5)将步骤(4)中得到的坯体在室温下放置2h直至完全固化,之后将坯体放入高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦。烧结制度控制为排胶4h,再以5℃/min的升温速率加热到1500℃,保温2h。
得到的莫来石纤维多孔隔热瓦试样密度为0.396g/cm3,抗压强度达到1.1Mpa,耐温达到1500℃,粘结剂对纤维有较好的包覆(见附图1、2)。
本实施例制备的莫来石纤维多孔隔热瓦的电子扫描图片如图1所示。
本实施例制备的莫来石纤维多孔隔热瓦纤维搭接点处的电子扫描图片如图2所示。
实施例2:
一种制备莫来石纤维基多孔隔热瓦的简易方法,具体是按照以下步骤进行的:
(1)利用纤维粉碎机对多晶莫来石纤维进行剪切和除渣,剪切时间为8min,得到长度为400μm且长径比为40:1的短切莫来石纤维,干燥;
(2)将聚二甲基硅油和聚二甲基硅橡胶以4:1的质量比均匀混合,得到前驱体溶液;
(3)称取100g步骤(2)中得到的前驱体溶液液,滴加2wt%的表面活性剂油酸,然后缓慢地加入45wt%的短切莫来石纤维,边加入边搅拌,待纤维添加完后继续搅拌4min,直至纤维均匀地分散在浆料中,得到分散好的纤维浆料;
(4)将步骤(3)中得到的浆料从搅拌器上取下,对浆料继续进行搅拌,同时按照比例向浆料中加入1wt%的固化剂二丙烯三胺(DPTA),继续搅拌30s,将浆料倒入模具中,在0.1MPa压力下成型;
(5)将步骤(4)中得到的坯体放置2h直至完全固化,之后将坯体放入高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦。烧结制度控制为排胶4h,再以7℃/min的升温速率加热到1300℃,保温2h。
得到的莫来石纤维多孔隔热瓦试样密度为0.441g/cm3,抗压强度达到0.96Mpa,粘结剂对纤维有较好的包覆。
实施例3:
一种制备莫来石纤维基多孔隔热瓦的简易方法,具体是按照以下步骤进行的:
(1)利用纤维粉碎机对多晶莫来石纤维进行剪切和除渣,剪切时间为6min,得到长度为500μm且长径比为50:1的短切莫来石纤维,干燥;
(2)将聚二甲基硅油和聚二甲基硅橡胶以4:1的质量比均匀混合,得到前驱体溶液;
(3)称取100g步骤(2)中得到的前驱体溶液,滴加2wt%的表面活性剂油酸,然后缓慢地加入30wt%的短切莫来石纤维,边加入边搅拌,待纤维添加完后继续搅拌3min,直至纤维均匀地分散在浆料中,得到分散好的纤维浆料;
(4)将步骤(3)中得到的浆料从搅拌器上取下,对浆料继续进行搅拌,同时按照比例向浆料中加入1.5wt%的固化剂二丙烯三胺(DPTA),继续搅拌30s,将浆料倒入模具中,在0.1MPa压力下成型;
(5)将步骤(4)中得到的坯体在室温下放置2h直至完全固化,之后将坯体放入高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦。烧结制度控制为排胶4h,再以7℃/min的升温速率加热到1400℃,保温2h。
得到的莫来石纤维多孔隔热瓦试样密度为0.416g/cm3,抗压强度达到1.21Mpa,粘结剂对纤维有较好的包覆。
Claims (6)
1.一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:制备过程包括以下步骤:
(1)利用纤维粉碎机对多晶莫来石纤维进行剪切和除渣,得到短切莫来石纤维,干燥;
(2)将聚二甲基硅油和聚二甲基硅橡胶均匀混合,得到前驱体溶液;
(3)称取步骤(2)中得到的前驱体溶液,滴加表面活性剂油酸,然后缓慢地加入短切莫来石纤维,边加入边搅拌,待纤维添加完后继续搅拌,直至纤维均匀地分散在浆料中,得到分散好的纤维浆料;
(4)将步骤(3)中得到的浆料从搅拌器上取下,对浆料继续进行搅拌,同时按照比例向浆料中加入固化剂二丙烯三胺(DPTA),继续搅拌30s,将浆料倒入模具中,在压力下成型;
(5)将步骤(4)中得到的坯体在室温下放置2h直至完全固化,之后将坯体放入高温炉中进行排胶和烧结,得到莫来石纤维多孔隔热瓦。
2.根据权利要求1所述的一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:步骤(1)中的剪切时间为4min~8min,短切纤维的长度为400μm~600μm且长径比为40:1~60:1。
3.根据权利要求1所述的一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:步骤(2)中的前驱体溶液由质量比为聚二甲基硅油:聚二甲基硅橡胶=4:1的组分组成。
4.根据权利要求1所述的一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:步骤(3)中称取100g前驱体溶液,表面活性剂为2%质量分数的油酸,加入的多晶莫来石纤维质量百分比为15%~45%。
5.根据权利要求1所述的一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:步骤(4)中固化剂添加量为1wt%~2wt%,成型压力为0.1MPa。
6.根据权利要求1所述的一种制备莫来石纤维基多孔隔热瓦的简易方法,其特征在于:步骤(5)中的烧结制度控制为在290℃~340℃之间升温4h,再以5℃/min~7℃/min的升温速率加热到1300℃~1500℃,保温2h。
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