CN113185299A - 一种多层吸波陶瓷基复合材料的制备方法 - Google Patents
一种多层吸波陶瓷基复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种多层吸波陶瓷基复合材料的制备方法,本发明采用混合不同电磁纳米粒子的陶瓷先驱体,处理纤维织物使其具有不同电磁性能,将调控后的不同电磁性能的纤维织物按吸波结构设计铺层排布,通过热压固化、浸渍裂解循环工艺,制备出多层吸波陶瓷基复合材料。本发明可以通过改变电磁纳米粒子的种类和含量实现对多层纤维织物不同电磁性能的调控,达到调节陶瓷基复合材料吸波性能的目的,满足不同用途的使用需求,并且工艺操作简单,适合成型大尺寸复杂构件。
Description
技术领域
本发明涉及雷达吸波陶瓷基复合材料技术领域,特别是涉及一种多层吸波陶瓷基复合材料的制备方法。
背景技术
陶瓷基复合材料因其具有优异的力学性能,热物理性能和环境性能等,成为航空航天领域迅速发展的材料体系。随着雷达侦察技术的提升,发展吸波陶瓷基复合材料成为提高航空航天武器装备生存能力的关键。
陶瓷基复合材料主要由纤维预制体、界面层和基体等组成,现有技术的吸波复合材料的制备方法主要集中于纤维预制体设计,对纤维的电性能要求较高,因目前可选纤维种类较少,所以难以灵活调节复合材料吸波性能。专利CN201811199009.4开展了复合材料基体设计,结合多种工艺,制备出由外而内Si3N4/SiC/C的电磁阻抗渐变基体的吸波陶瓷基复合材料,但其存在基体成分设计单一且工艺制备复杂的问题,较难成型大尺寸复杂吸波陶瓷基复合材料构件。
综上,目前吸波陶瓷基复合材料制备方法主要存在以下问题:(1)吸波纤维预制体设计对纤维的电性能要求较高,纤维可选种类较少且电性能调节困难;(2)电磁阻抗渐变基体成分设计单一且制备工艺复杂,较难成型大尺寸复杂吸波陶瓷基复合材料构件。
因此,发明人提供了一种多层吸波陶瓷基复合材料的制备方法。
发明内容
(1)要解决的技术问题
本发明实施例提供了一种多层吸波陶瓷基复合材料的制备方法,解决了现有技术的吸波纤维可选种类少且电性能调节困难,难以调控陶瓷基复合材料吸波性能的技术问题。
(2)技术方案
本发明的实施例提出了一种多层吸波陶瓷基复合材料的制备方法,该制备方法至少包括以下步骤(1)~步骤(7):
步骤(1),选取连续纤维编织的二维织物,在真空烘箱中烘干2~5h,取出后置于800~1000℃高温真空或惰性气氛处理0.5~1h除去纤维织物表面上的浆剂。
步骤(2),在经步骤(1)处理后的纤维织物表面制备氮化硼界面层,通过控制沉积时间使得氮化硼界面层厚度在100~1000nm。
步骤(3),取黏度为20~200cP的陶瓷先驱体,通过搅拌、球磨的混合方式将电磁纳米粒子分散在先驱体中,改变电磁纳米粒子的种类和含量,制得具有不同电磁性能的混合先驱体,以实现混合先驱体不同电磁性能的调控。
步骤(4),将步骤(2)制得的带有氮化硼界面层的纤维织物浸渍于步骤(3)制得的不同电磁性能的混合陶瓷先驱体中6~10h,得到不同电磁性能的纤维织物。
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的不同电磁性能的纤维织物进行多层铺层叠加,再将其置于模具中热压完成固化。
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为20~200cP的陶瓷先驱体中6~10h,之后在800~1200℃高温真空或惰性气氛下保持0.5~2h完成裂解。
步骤(7),按照步骤(6)的方法采用黏度20~200cP的陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重小于2wt%,完成致密化,制备出多层吸波陶瓷基复合材料。
进一步地,所述步骤(1)中,所述连续纤维编织的二维织物采用吸波SiC纤维、透波SiC纤维、透波Si3N4纤维或透波Al2O3纤维的平纹或缎纹织物。
进一步地,所述步骤(3)、(6)、(7)中,所述陶瓷先驱体为采用适用浸渍裂解工艺的聚碳硅烷、聚硅氮烷或聚硅硼氮烷的陶瓷先驱体。
进一步地,所述步骤(3)中,所述电磁纳米粒子的种类包括但电性能调节的电导纳米粒子、介电纳米粒子以及磁性能调节的磁性纳米粒子。
进一步地,所述电导纳米粒子包括碳纳米管、炭黑、石墨烯纳米粒子。
进一步地,所述介电纳米粒子包括SiC、SiO2、Al2O3、Ti3SiC2纳米粒子。
进一步地,所述磁性能调节的磁性纳米粒子包括铁磁性金属粉末、铁氧体Fe2O3。
进一步地,所述步骤(3)中,所述电磁纳米粒子在所述混合先驱体中的含量范围在1wt%~20wt%。
进一步地,在所述步骤(5)中,所述多层吸波复合材料结构设计采用磁性能层、介电性能层、电导性能层的不同电磁性能的纤维织物实现多种组合设计。
(3)有益效果
1、本发明采用陶瓷先驱体混合电磁纳米粒子的方式,通过控制电磁纳米粒子的种类和含量,实现对多层纤维织物不同电磁性能的调控,可调节范围大。
2、本发明通过不同电磁性能纤维织物的叠加组合,实现磁性能、介电性能、电导性能等不同电磁性能纤维织物的多层结构设计,达到灵活调控陶瓷基复合材料的吸波性能的目的,满足不同的使用需求。
3、本发明采用先驱体浸渍裂解工艺,通过浸渍-裂解循环实现复合材料致密化,其操作简单,适合成型大尺寸复杂构件,满足航空航天隐身构件的研制需求。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对本发明实施例中所需要使用的附图作简单地介绍,显而易见地,下面所描述的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是本发明实施例的一种多层吸波陶瓷基复合材料结构示意图;
图2是本发明实施例的一种多层吸波陶瓷基复合材料平板试样。
具体实施方式
下面结合附图和实施例对本发明的实施方式作进一步详细描述。以下实施例的详细描述和附图用于示例性地说明本发明的原理,但不能用来限制本发明的范围,即本发明不限于所描述的实施例,在不脱离本发明的精神的前提下覆盖了零件、部件和操作方式的任何修改、替换和改进。
需要说明的是,在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。下面将参照附图并结合实施例来详细说明本申请。
实施例1
请参照图1和图2所示,实施例1提供了一种多层吸波陶瓷基复合材料的制备方法,该制备方法至少包括以下步骤(1)~步骤(7):
步骤(1),选取10层连续SiC纤维编织的平纹二维织物,在100℃真空烘箱中烘干2h,取出后置于800℃高温下真空处理0.5h除去纤维织物表面上的浆剂。
步骤(2),在经步骤(1)处理后的纤维织物表面通过沉积4h制备厚度为300nm的氮化硼界面层。
步骤(3),取黏度为20cP的聚碳硅烷陶瓷先驱体两份,通过搅拌或球磨的混合方式,分别将10wt%质量分数的SiO2纳米粒子和20wt%质量分数的Fe2O3纳米粒子分散在前述的两份聚碳硅烷陶瓷先驱体中,因SiO2粒子的低介电性和Fe2O3粒子的磁性,使得混合先驱体分别具有低介电性能和磁损耗性能。
步骤(4),将步骤(2)制得的带有氮化硼界面层的5层纤维织物浸渍于步骤(3)制得的混合SiO2纳米粒子的陶瓷先驱体中10h,其余5层浸渍于混合Fe2O3纳米粒子的陶瓷先驱体中10h,分别得到具有介电性能和磁性能的两种电磁性能的纤维织物。
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的两种电磁性能的纤维织物进行多层铺层叠加,再将其置于模具中,在压力4MPa,温度180℃,热压1h条件下完成热压固化。
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为20cP的聚碳硅烷陶瓷先驱体中10h,之后在800℃高温真空下保持0.5h完成裂解。
步骤(7),按照步骤(6)的方法采用黏度20cP的聚碳硅烷陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重为1wt%,完成致密化,制备出多层吸波陶瓷基复合材料。
经分析,实施例1最终吸波陶瓷基复合材料为介电性能、磁性能组合的多层结构,反射率8~18GHz≤-3dB,最大吸波峰值为-5dB。
实施例2
请参照图1和图2所示,实施例2提供了一种多层吸波陶瓷基复合材料的制备方法,该制备方法至少包括以下步骤(1)~步骤(7):
步骤(1),选取10层连续SiC纤维编织的平纹二维织物,在100℃真空烘箱中烘干2h,取出后置于1000℃高温下真空处理0.5h除去纤维织物表面上的浆剂。
步骤(2),在经步骤(1)处理后的纤维织物表面通过沉积2h制备厚度为100nm的氮化硼界面层。
步骤(3),取黏度为100cP的聚硅氮烷陶瓷先驱体两份,通过球磨的混合方式,分别将5wt%质量分数的SiO2纳米粒子和1wt%质量分数的碳纳米管纳米粒子分散在前述的两份聚碳硅烷陶瓷先驱体中,因SiO2粒子的低介电性和碳纳米管粒子的导电性,使得混合先驱体分别具有低介电性能和高电导性能。
步骤(4),将步骤(2)制得的带有氮化硼界面层的4层纤维织物浸渍于步骤(3)制得的混合SiO2纳米粒子的陶瓷先驱体中6h,其余6层浸渍于混合碳纳米管纳米粒子的陶瓷先驱体中6h,分别得到具有介电性能和电导性能的两种电磁性能的纤维织物。
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的两种性能的纤维织物进行多层铺层叠加,再将其置于模具中,在压力4MPa,温度220℃,热压2h条件下完成热压固化。
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为100cP的聚硅氮烷陶瓷先驱体中8h,之后在1200℃高温真空下保持0.5h完成裂解。
步骤(7),按照步骤(6)的方法采用黏度100cP的聚硅氮烷陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重为1wt%,完成致密化,制备出多层吸波陶瓷基复合材料。
经分析,实施例2最终制备的吸波陶瓷基复合材料为介电性能、电导性能组合的多层结构,反射率8~18GHz≤-6dB,最大吸波峰值为-9dB。
实施例3
请参照图1和图2所示,实施例3提供了一种多层吸波陶瓷基复合材料的制备方法,该制备方法至少包括以下步骤(1)~步骤(7):
步骤(1),选取10层连续Si3N4纤维编织的平纹二维织物,在100℃真空烘箱中烘干5h,取出后置于800℃高温下真空处理1h除去纤维织物表面上的浆剂。
步骤(2),在经步骤(1)处理后的纤维织物表面通过沉积10h制备厚度为1000nm的氮化硼界面层。
步骤(3),取黏度为200cP的聚碳硅烷陶瓷先驱体三份,通过球磨混合方式,分别将3wt%质量分数的SiO2纳米粒子、1wt%质量分数的碳纳米管纳米粒子以及5wt%质量分数的Ti3SiC2纳米粒子分散在前述的三份聚碳硅烷陶瓷先驱体中,因SiO2粒子的低介电性、碳纳米管粒子的导电性和Ti3SiC2粒子的高介电性,使得混合先驱体分别具有低介电性能、高电导性能、高介电性能。
步骤(4),将步骤(2)制得的带有氮化硼界面层的2层纤维织物浸渍于步骤(3)制得的混合SiO2纳米粒子的陶瓷先驱体中8h,2层纤维织物浸渍于混合碳纳米管纳米粒子的陶瓷先驱体中8h,其余6层浸渍于混合Ti3SiC2纳米粒子的陶瓷先驱体中8h,对应地分别得到具有介电性能、电导性能和介电性能的三种电磁性能的纤维织物。
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的三种性能的纤维织物进行多层铺层叠加,以混合SiO2、碳纳米管、Ti3SiC2的顺序从上到下依次叠放成预制体置于模具中,再将其置于模具中,在压力4MPa,温度220℃,热压2h条件下完成热压固化。
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为200cP的聚碳硅烷陶瓷先驱体中6h,之后在800℃高温真空下保持2h完成裂解。
步骤(7),按照步骤(6)的方法采用黏度200cP的聚碳硅烷陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重为1wt%,完成致密化,制备出多层吸波陶瓷基复合材料。
经分析,实施例3最终制备的吸波陶瓷基复合材料为介电性能、电导性能、介电性能组合的多层结构,反射率8~18GHz≤-4dB,最大吸波峰值为-9dB。
实施例4
请参照图1和图2所示,实施例3提供了一种多层吸波陶瓷基复合材料的制备方法,该制备方法至少包括以下步骤(1)~步骤(7):
步骤(1),选取10层连续Al2O3纤维编织的平纹二维织物,在100℃真空烘箱中烘干1h,取出后置于800℃高温下真空处理0.5h除去纤维织物表面上的浆剂。
步骤(2),在经步骤(1)处理后的纤维织物表面通过沉积4h制备厚度为300nm的氮化硼界面层。
步骤(3),取黏度为50cP的聚硅硼氮烷陶瓷先驱体三份,通过球磨混合方式,分别将3wt%质量分数的Fe2O3纳米粒子、5wt%质量分数的SiO2纳米粒子以及10wt%质量分数的碳纳米管纳米粒子分散在前述的三份聚硅硼氮烷陶瓷先驱体中,因Fe2O3粒子的磁性、SiO2粒子的低介电性和碳纳米管粒子的导电性,使得混合先驱体分别具有磁损耗性能、低介电性能和高电导性能。
步骤(4),将步骤(2)制得的带有氮化硼界面层的3层纤维织物浸渍于步骤(3)制得的混合Fe2O3纳米粒子的陶瓷先驱体中8h,4层浸渍于混合SiO2纳米粒子的陶瓷先驱体中8h,其余3层浸渍于混合碳纳米管纳米粒子的陶瓷先驱体中8h,对应地分别得到具有磁性能、介电性能和电导性能的三种电磁性能的纤维织物。
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的三种性能的纤维织物进行多层铺层叠加,以混合Fe2O3、SiO2、碳纳米管的顺序从上到下依次叠放成预制体置于模具中,再将其置于模具中,在压力2MPa,温度150℃,热压1h条件下完成热压固化。
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为50cP的聚硅硼氮烷陶瓷先驱体中6h,之后在900℃高温真空下保持1h完成裂解。
步骤(7),按照步骤(6)的方法采用黏度50cP的聚硅硼氮烷陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重为1wt%,完成致密化,制备多层吸波陶瓷基复合材料。
经分析,实施例4最终制备的吸波陶瓷基复合材料为磁性能、介电性能、电导性能组合的多层结构,反射率8~18GHz≤-7dB,最大吸波峰值为-15dB。
需要说明的是,本发明的方法中的电导纳米粒子可选择的种类包括但不限于碳纳米管、炭黑、石墨烯纳米粒子等;介电纳米粒子可选择的种类包括但不限于SiC、SiO2、Al2O3、Ti3SiC2纳米粒子等;磁性纳米粒子可选择的种类包括但不限于铁磁性金属粉末、铁氧体Fe2O3等。
以上所述仅为本申请的实施例而已,并不限制于本申请。在不脱离本发明的范围的情况下对于本领域技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原理之内所作的任何修改、等同替换、改进等,均应包含在本申请的权利要求范围内。
Claims (9)
1.一种多层吸波陶瓷基复合材料的制备方法,其特征在于,包括:
步骤(1),选取连续纤维编织的二维织物,在真空烘箱中烘干2~5h,取出后置于800~1000℃高温真空或惰性气氛处理0.5~1h除去纤维织物表面上的浆剂;
步骤(2),在经步骤(1)处理后的纤维织物表面制备氮化硼界面层,通过控制沉积时间使得氮化硼界面层厚度在100~1000nm;
步骤(3),取黏度为20~200cP的陶瓷先驱体,通过搅拌、球磨的混合方式将电磁纳米粒子分散在先驱体中,改变电磁纳米粒子的种类和含量,制得具有不同电磁性能的混合先驱体,以实现混合先驱体不同电磁性能的调控;
步骤(4),将步骤(2)制得的带有氮化硼界面层的纤维织物浸渍于步骤(3)制得的不同电磁性能的混合陶瓷先驱体中6~10h,得到不同电磁性能的纤维织物;
步骤(5),根据多层吸波复合材料结构设计,通过将步骤(4)制得的不同电磁性能的纤维织物进行多层铺层叠加,再将其置于模具中热压完成固化;
步骤(6),将步骤(5)固化后的复合材料再次浸渍于黏度为20~200cP的陶瓷先驱体中6~10h,之后在800~1200℃高温真空或惰性气氛下保持0.5~2h完成裂解;
步骤(7),按照步骤(6)的方法采用黏度20~200cP的陶瓷先驱体对复合材料进行浸渍-裂解的循环操作,直到复合材料增重小于2wt%,完成致密化,制备出多层吸波陶瓷基复合材料。
2.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述步骤(1)中,所述连续纤维编织的二维织物采用吸波SiC纤维、透波SiC纤维、透波Si3N4纤维或透波Al2O3纤维的平纹或缎纹织物。
3.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述步骤(3)、(6)、(7)中,所述陶瓷先驱体为采用适用浸渍裂解工艺的聚碳硅烷、聚硅氮烷或聚硅硼氮烷的陶瓷先驱体。
4.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述步骤(3)中,所述电磁纳米粒子的种类包括电性能调节的电导纳米粒子、介电纳米粒子以及磁性能调节的磁性纳米粒子。
5.根据权利要求4所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述电导纳米粒子包括碳纳米管、炭黑、石墨烯纳米粒子。
6.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述介电纳米粒子包括SiC、SiO2、Al2O3、Ti3SiC2纳米粒子。
7.根据权利要求4所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述磁性能调节的磁性纳米粒子包括铁磁性金属粉末、铁氧体Fe2O3。
8.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,所述步骤(3)中,所述电磁纳米粒子在所述混合先驱体中的含量范围在1wt%~20wt%。
9.根据权利要求1所述的多层吸波陶瓷基复合材料的制备方法,其特征在于,在所述步骤(5)中,所述多层吸波复合材料结构设计采用磁性能层、介电性能层、电导性能层的不同电磁性能的纤维织物实现多种组合设计。
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CN113526973B (zh) * | 2021-09-07 | 2021-11-16 | 中国人民解放军国防科技大学 | 一种具有双界面相的透波陶瓷基复合材料及其制备方法 |
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