CN117467327A - 一种中低温固化耐高温吸波材料及其制备方法 - Google Patents
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Abstract
本发明公开一种中低温固化耐高温吸波材料及其制备方法,涉及电磁波吸收材料领域,将吸收剂、四缩水甘油胺型环氧树脂及聚醚改性聚硅氧烷类消泡剂混合均匀,得到A组份;)将二乙基甲苯二胺、三氟化硼单乙胺及丁基缩水甘油醚混合均匀,得到B组份;使用时,将A组分与B组份混合均匀,浇筑于所用部位,在75‑120℃温度下固化,得到中低温固化耐高温吸波材料。本发明所制备的吸波材料满足“即用即灌封”及中低温固化要求,且玻璃化转变温度>200℃,满足航空航天器复杂腔体结构对吸波材料的使用需求。
Description
技术领域
本发明涉及电磁波吸收材料领域,特别涉及一种中低温固化耐高温吸波材料及其制备方法。
背景技术
吸波材料是一种能吸收、衰减入射的电磁波能量,并通过材料的介质损耗将电磁波能量转换成为其他形式的能量(如机械能、电能和热能等)而耗散掉,或使电磁波因干涉而消失,而反射、散射和投射都很小的功能材料,是各种型号航天器在天线、合成分路器、微波部组件等位置上广泛采用的材料。随着航空航天领域中电磁隐身技术的发展需要以及日常生活中电磁干扰、电磁污染问题的日趋严重,使得微波吸收材料逐渐成为功能材料领域的研究热点。
各类探测卫星是吸波材料常用的装备,其对吸波材料的性能及精度要求较高,特别是对于一些临近大功率天线附近的复杂腔体结构,其既需要所用吸波材料能够精确匹配的填满腔体,又要求吸波材料在大功率天线工作时能够承受功率发射所导致的高温环境(>200℃)。此外,由于常规的刚性吸波材料为规则块料,主要根据所需规格尺寸进行加工使用,但对于一些复杂腔体结构(如内腔大、开口小),刚性材料无法安装,因此要求吸波材料还能够满足“即用即灌封”的要求。
目前常用的低粘度树脂复合吸收剂即可制备浇筑型吸波材料,从而满足“即用即灌封”要求,但该类吸波材料受树脂特性限定,中低温固化(固化温度≤130℃)的材料其玻璃化转变温度较低(玻璃化转变温度≤160℃),无法满足大功率下的耐高温需求;而高温固化的材料其固化温度(>200℃)又会影响装备电子元器件性能,无法使用。
发明内容
本发明的目的是提供一种中低温固化耐高温吸波材料及其制备方法,该吸波材料满足“即用即灌封”及中低温固化要求(固化温度≤130℃),且玻璃化转变温度>200℃。
为实现上述目的,本发明采用的技术方案如下:
第一方面,本发明提供了一种中低温固化耐高温吸波材料的制备方法,其包括如下步骤:
(1)将吸收剂、四缩水甘油胺型环氧树脂及聚醚改性聚硅氧烷类消泡剂混合均匀,得到A组份;
(2)将二乙基甲苯二胺、三氟化硼单乙胺及丁基缩水甘油醚混合均匀,得到B组份;
(3)使用时,将A组分与B组份混合均匀,浇筑于所用部位,在75-120℃温度下固化,得到中低温固化耐高温吸波材料。
优选地,步骤(1)中吸收剂为羰基铁粉、铁硅铝合金粉、铁硅铬合金粉、碳化硅粉、石墨烯粉中的一种或几种。
优选地,步骤(1)中吸收剂与四缩水甘油胺型环氧树脂的质量比为7:3-8:2。
优选地,步骤(1)中聚醚改性聚硅氧烷类消泡剂用量为吸收剂与四缩水甘油胺型树脂总质量的0.3%-0.6%。
优选地,步骤(2)中的二乙基甲苯二胺、三氟化硼单乙胺与步骤(1)中的四缩水甘油胺型环氧树脂的质量比为35:3:100。
优选地,步骤(2)中丁基缩水甘油醚与三氟化硼单乙胺的质量比为(1-1.5):1。
优选地,步骤(3)中固化时间与固化温度对应,为75℃/12h、90℃/10h、100℃/6h、110℃/4h或120℃/2h中的一种。
第二方面,本发明提供了一种中低温固化耐高温吸波材料,采用上述制备方法制备得到。
本发明与现有技术相比至少具有如下有益效果:
(1)二乙基甲苯二胺为芳香胺类环氧固化剂,其常温下为液体,便于与其余组分的均匀混合。三氟化硼单乙胺(固体粉末)为助催化剂,可有效降低芳香胺类固化剂的固化温度(芳香胺类环氧固化剂常规固化温度需达到150℃以上)。丁基缩水甘油醚为活性稀释剂,可有效降低混合体系的黏度,便于混合组分浇筑,同时,其可以有效溶解三氟化硼单乙胺,从而保障三氟化硼单乙胺在混合组分内的均匀分散。
(2)本发明所制备的吸波材料满足“即用即灌封”及中低温固化要求(固化温度≤130℃),且玻璃化转变温度>200℃,满足航空航天器复杂腔体结构对吸波材料的使用需求。
附图说明
图1是实施例1所得吸波材料固化后的玻璃化转变温度测试结果。
具体实施方式
为使本发明的上述技术方案中各项技术特征和各项优点或技术效果能更明显易懂,下文配合附图进行详细说明。
实施例1
(1)将羰基铁粉(80g)、四缩水甘油胺型环氧树脂(20g)及聚醚改性聚硅氧烷类消泡剂(0.3g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(7g)、三氟化硼单乙胺(0.6g)及丁基缩水甘油醚(0.6g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用75℃固化,时间12小时,得到所需吸波材料。
实施例2
实施例2与实施例1基本相同,不同之处在于:吸收剂种类为铁硅铬合金粉,聚醚改性聚硅氧烷类消泡剂0.5g。
实施例3
实施例3与实施例1基本相同,不同之处在于:羰基铁粉75g,四缩水甘油胺型环氧树脂25g,聚醚改性聚硅氧烷类消泡剂0.6g,二乙基甲苯二胺8.75g,三氟化硼单乙胺0.8g,丁基缩水甘油醚1.0g。
实施例4
(1)将羰基铁粉(70g)、四缩水甘油胺型环氧树脂(30g)及聚醚改性聚硅氧烷类消泡剂(0.3g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(10.5g)、三氟化硼单乙胺(0.9g)及丁基缩水甘油醚(0.9g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用100℃固化,时间6小时,得到所需吸波材料。
实施例5
实施例5与实施例1基本相同,不同之处在于:丁基缩水甘油醚为0.9g。
实施例6
实施例6与实施例1基本相同,不同之处在于:采用120℃固化,时间2小时。
对比例1(针对吸收剂与环氧树脂的质量比)
(1)将羰基铁粉(90g)、四缩水甘油胺型环氧树脂(10g)及聚醚改性聚硅氧烷类消泡剂(0.3g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(7g)、三氟化硼单乙胺(0.6g)及丁基缩水甘油醚(0.6g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用75℃固化,时间12小时,得到所需吸波材料。
对比例2(针对消泡剂用量)
(1)将羰基铁粉(80g)、四缩水甘油胺型环氧树脂(20g)及聚醚改性聚硅氧烷类消泡剂(0.1g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(7g)、三氟化硼单乙胺(0.6g)及丁基缩水甘油醚(0.6g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用75℃固化,时间12小时,得到所需吸波材料。
对比例3(针对稀释剂用量)
(1)将羰基铁粉(80g)、四缩水甘油胺型环氧树脂(20g)及聚醚改性聚硅氧烷类消泡剂(0.3g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(7g)、三氟化硼单乙胺(0.6g)及丁基缩水甘油醚(1.2g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用75℃固化,时间12小时,得到所需吸波材料。
对比例4(针对固化时间)
(1)将羰基铁粉(80g)、四缩水甘油胺型环氧树脂(20g)及聚醚改性聚硅氧烷类消泡剂(0.3g)混合均匀,得到A组份;
(2)将二乙基甲苯二胺(7g)、三氟化硼单乙胺(0.6g)及丁基缩水甘油醚(0.6g)混合均匀,得到B组份;
(3)将A、B组份混合均匀,浇筑于所用部位,采用75℃固化,时间2小时,得到所需吸波材料。
将上述实施例1至6以及对比例1至4所得到的吸波材料分别测试其玻璃化转变温度。具体地,玻璃化转变温度的测试:按照标准机加成80×10×4mm试样,采用动态力学分析DMA测试玻璃化转变温度,通过测量材料在恒定外力下的弹性模量及损耗模量变化,从而进行玻璃化转变温度的测定。图1中材料在255℃时损耗模量最高,即为材料的玻璃化转变温度。全部测试结果见表1。
表1吸波材料的固化温度及玻璃化转变温度
虽然本发明已以实施例公开如上,然其并非用以限定本发明,本领域的普通技术人员对本发明的技术方案进行的适当修改或者等同替换,均应涵盖于本发明的保护范围内,本发明的保护范围以权利要求所限定者为准。
Claims (8)
1.一种中低温固化耐高温吸波材料的制备方法,其特征在于,包括如下步骤:
(1)将吸收剂、四缩水甘油胺型环氧树脂及聚醚改性聚硅氧烷类消泡剂混合均匀,得到A组份;
(2)将二乙基甲苯二胺、三氟化硼单乙胺及丁基缩水甘油醚混合均匀,得到B组份;
(3)使用时,将A组分与B组份混合均匀,浇筑于所用部位,在75-120℃温度下固化,得到中低温固化耐高温吸波材料。
2.如权利要求1所述的制备方法,其特征在于,步骤(1)中吸收剂为羰基铁粉、铁硅铝合金粉、铁硅铬合金粉、碳化硅粉、石墨烯粉中的一种或几种。
3.如权利要求1所述的制备方法,其特征在于,步骤(1)中吸收剂与四缩水甘油胺型环氧树脂的质量比为7:3-8:2。
4.如权利要求1所述的制备方法,其特征在于,步骤(1)中聚醚改性聚硅氧烷类消泡剂用量为吸收剂与四缩水甘油胺型树脂总质量的0.3%-0.6%。
5.如权利要求1所述的制备方法,其特征在于,步骤(2)中的二乙基甲苯二胺、三氟化硼单乙胺与步骤(1)中的四缩水甘油胺型环氧树脂的质量比为35:3:100。
6.如权利要求1所述的制备方法,其特征在于,步骤(2)中丁基缩水甘油醚与三氟化硼单乙胺的质量比为(1-1.5):1。
7.如权利要求1所述的制备方法,其特征在于,步骤(3)中固化时间与固化温度对应,为75℃/12h、90℃/10h、100℃/6h、110℃/4h或120℃/2h中的一种。
8.一种中低温固化耐高温吸波材料,其特征在于,采用权利要求1-7任一项所述的制备方法制备得到。
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