CN112757727A - 一种耐海洋环境结构功能一体化透波复合材料及其制备方法 - Google Patents
一种耐海洋环境结构功能一体化透波复合材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种耐海洋环境结构功能一体化透波复合材料及其制备方法;是由上下两层耐海洋环境透波层蒙皮和位于上下两层透波层蒙皮之间的高模量透波层芯材复合而成的耐海洋环境结构功能一体化透波夹芯复合材料;耐海洋环境透波层蒙皮能够有效保护内部高模量透波层芯材免受外部潮湿、盐雾和太阳暴晒等海洋环境的影响,高模量透波层芯材又可赋予材料非常优异的力学性能;通过调节蒙皮和芯材的厚度,可以得到满足不同海洋环境使用要求的结构功能一体化透波复合材料。本发明的透波复合材料具有质量轻、模量高、耐海水腐蚀、透波性能好等优点;可广泛应用于水下潜水器、各种舰船雷达天线罩等部位,能够有效保护海洋环境中的雷达天线设备不被破坏并提供优异的透波窗口。
Description
技术领域
本发明属于纤维/树脂基功能复合材料技术领域,具体涉及一种耐海洋环境结构功能一体化透波复合材料及其制备方法。
背景技术
随着现代通信技术的发展,雷达天线广泛运用。为保证雷达天线免受大风、盐雾和暴雨等恶劣环境的影响,通常在雷达天线外部加装具有优异介电性能和力学性能的天线罩,以达到延长天线使用寿命、提高系统可靠性和保障雷达天线全天候工作的目的。目前,雷达天线罩多采用增强纤维和树脂基体组成的复合材料并采用特定的工艺或成型方法制备。
海洋环境具有高盐度、高温度、高湿度特点,此外还具有极强的腐蚀性,这些环境和工况特点对海洋用材料的可靠性和耐久性会产生严重的影响。由于海水是一种腐蚀性很强的天然电解质,含有多种盐分,当异种金属接触时会造成显著的腐蚀效应。因此,金属及合金材料在海洋环境中的腐蚀不可避免,而纤维增强树脂基复合材料在海洋环境中具有金属材料无可比拟的优势。
在海洋这种恶劣的工作环境中,除保障雷达天线免受海洋恶劣环境的影响,还要求天线罩材料在具有良好透波性能的同时具有良好的力学性能和耐腐蚀性能。
发明内容
为解决上述问题,本发明提供了一种耐海洋环境结构功能一体化透波复合材料。
为解决上述技术问题,本发明所采用的技术方案为:一种耐海洋环境结构功能一体化透波复合材料,是由上下两层耐海洋环境透波层蒙皮和位于上下两层透波层蒙皮之间的高模量透波层芯材复合而成的耐海洋环境结构功能一体化透波夹芯复合材料;其中,高模量透波层芯材由热固性树脂、树脂改性剂、高模量透波纤维布、界面改性剂制备而成;耐海洋环境透波层蒙皮由热固性树脂、树脂改性剂、超高分子量聚乙烯纤维布制成。
高模量透波层芯材,选用兼具高模量和透波性能的纤维布及热固性树脂,并通过适当的界面改性剂对纤维布进行改性,可以提升其与热固性树脂的界面相容性,从而使该芯材能够提供可靠的结构、优秀的力学性能和优异的透波性能。耐海洋环境透波层蒙皮,选用具有极低介电常数和介电损耗以及极低吸水率的超高分子量聚乙烯纤维布,其与热固性树脂复合以后,在恶劣的海洋环境中可以有效阻止水分向复合材料内部的渗透,从而赋予整个复合材料优异的耐海洋环境性能,同时还可赋予复合材料优异的透波性能。
另外,本发明还提供上述耐海洋环境结构功能一体化透波复合材料的制备方法,通过模压成型工艺一体成型,制备方法包括手糊制备预浸料,然后模压成型;具体步骤为:
(1)高模量透波层预浸料和耐海洋环境透波层预浸料的制备:
除去纤维布表面的杂质,之后放入真空烘箱中干燥至恒重,得到干净纤维布;将质量分数为95%的乙醇水溶液调节pH至3~4左右,加入界面改性剂,混合均匀后,在60℃水解1h,然后将得到的干净纤维布浸入到水解后的混合液中4h,取出纤维布后用无水乙醇清洗,以除去表面未反应的界面改性剂,在真空烘箱中干燥至恒重后,得到改性纤维布;
在热固性树脂中加入树脂改性剂并搅拌均匀,加入固化剂,再次混合均匀,然后使用真空烘箱对树脂在常温下进行脱泡处理,真空负压控制在0.095~0.1MPa,得到配制好的混合树脂胶液;
将数层改性纤维布进行浸渍,则得到高模量透波层预浸料或者耐海洋环境透波层预浸料(若纤维布选择高模量透波纤维布,则得到高模量透波层预浸料,若纤维布选择用于作为耐海洋环境透波层蒙皮中的超高分子量聚乙烯纤维布,则得到耐海洋环境透波层预浸料);
(2)耐海洋环境结构功能一体化透波复合材料的制备:
将步骤(1)制备的耐海洋环境透波层预浸料按照设计的厚度铺放在涂有脱模剂的模具中,然后在其上铺放设计厚度的步骤(1)制备的高模量透波层预浸料,最后再铺放设计厚度的步骤(1)制备的耐海洋环境透波层预浸料,铺放完毕后在一定温度和压力下固化一定时间,然后自然冷却到室温,拆模,则得到耐海洋环境结构功能一体化透波复合材料。
进一步的,所述热固性树脂选用任何耐腐蚀且透波的热固性树脂。
优选的,所述热固性树脂为环氧树脂。
进一步的,所述高模量透波纤维布为石英纤维布、高强玻璃纤维布、高硅氧纤维布及超高分子量聚乙烯纤维布中的任一种或是任意两种的组合物;所述石英纤维布、高强玻璃纤维布、高硅氧纤维布及超高分子量聚乙烯纤维布或为单向布,或为多轴向织物,或为平纹布,或为斜纹布,或为缎纹布。
进一步的,树脂改性剂为笼型倍半硅氧烷、介孔二氧化硅和纳米级氮化硼中的一种。
进一步的,所述界面改性剂选用钛酸酯偶联剂或者硅烷偶联剂。
进一步的,所述固化剂为自胺类固化剂、酰胺类固化剂和酸酐类固化剂中的一种。
进一步的,步骤(1)中,热固性树脂与固化剂的重量配比为100:55,树脂改性剂与固化剂的重量配比为100:66;界面改性剂加入量为纤维布质量的5% ;
步骤(1)中,除去纤维布表面的杂质,放入真空烘箱中进行干燥的温度为120℃;除去表面未反应的界面改性剂的纤维布在真空烘箱中处理温度为120℃。
另外,本发明还提供上述耐海洋环境结构功能一体化透波复合材料在透波结构件中的应用,在水下潜水器以及海洋环境中各种型号天线罩中的应用。
与现有技术相比本发明具有以下有益效果:
(1)本发明通过高模量透波复合材料层芯材和耐海洋腐蚀透波复合材料层蒙皮复合而成的夹芯结构,制备了一种可以同时满足耐海洋环境腐蚀和透波功能的结构-功能一体化复合材料。耐海洋环境透波层蒙皮能够有效保护内部高模量透波层芯材免受外部潮湿、盐雾和太阳暴晒等海洋环境的影响,而高模量透波层芯材又可赋予材料非常优异的力学性能。尤其是,通过调节蒙皮和芯材的厚度,可以得到满足不同海洋环境使用要求的结构功能一体化透波复合材料。
(2)本发明采用操作简单和设备投入不高的模压成型工艺,制备的耐海洋环境透波复合材料具有质量轻、模量高、耐海水腐蚀、透波性能好等优点。
(3)复合材料使用操作简单的模压成型工艺,制备得到的复合材料具有性能稳定、缺陷少等特点,本发明的耐海洋环境透波复合材料可以制备成各种透波结构件,广泛应用于水下潜水器以及海洋环境中各种型号天线罩中。
附图说明
图1是本发明的耐海洋环境结构功能一体化透波复合材料的结构示意图。
图2是实施例1制备的复合材料Ku波段传输损耗图。该复合材料可以应用于海洋环境深海及水下潜水器透波设备中。
图3是实施例2制备的复合材料Ku波段传输损耗图。该复合材料可以应用于海洋环境浅水区及水上透波设备中。
图中标记如下:
1-耐海洋环境透波层,2-高模量透波层。
具体实施方式
本发明的耐海洋环境结构功能一体化透波复合材料采用模压成型工艺,整体操作简便、制备的复合材料具有质量轻、具有质量轻、模量高、耐海水腐蚀、透波性能好等等优点。
高模量透波复合材料层芯材采用模量较高同时透波性能优异的石英纤维布、高强玻璃纤维布、高硅氧纤维布中的一种或者多种,可为制备的天线罩或者潜水器提供可靠的结构,更好地保护内部的仪器设备。
界面改性剂主要用于对纤维表面进行改性,在纤维和基体树脂之间形成“桥梁”作用,改善界面相容性的同时大幅提高界面强度。界面强度的提升可以有效降低湿热、盐雾对界面作用形成界面空洞。
耐海洋腐蚀透波层蒙皮采用具有极低吸水率同时介电性能非常优异的超高分子量聚乙烯纤维,能够有效保护内部高模量透波层免受外部潮湿、盐雾和太阳暴晒的海洋环境的影响。
氧树脂或者兼具耐腐蚀和透波性的树脂,除具有良好的粘结性能以外,还具有良好的耐海洋环境性能。
固化剂用于热固性树脂的固化,胺类固化剂、酰胺类固化剂或者酸酐类固化剂与热固性树脂进行开环聚合反应,使其固化。
树脂改性剂用于改善热固性树脂的介电性能,从而提升复合材料的透波性能;此外,树脂改性剂POSS可以提供与热固性树脂生成化学交联键的基团,介孔二氧化硅可以提供孔洞,它们都可以提高热固性树脂的交联密度,提升树脂体系的介电性能。
加入的树脂改性剂可以占据热固性树脂固化过程中形成的空隙,降低其体积收缩率,减少水分的进入,从而有效提升复合材料的耐海洋环境性能。
以下结合具体实施例对本发明作进一步说明。
实施例1
耐海洋透波复合材料的总厚度为7mm,中间的高模量透波层芯材6mm,耐海洋环境透波层蒙皮各0.5mm。高模量透波层的增强材料采用平纹石英纤维布,耐海洋环境透波层的增强材料采用超高分子量聚乙烯纤维布,热固性树脂选用E51环氧树脂,树脂改性剂选用缩水甘油醚基笼型倍半硅氧烷(EP-POSS),固化剂选择胺类固化剂聚醚氨D400,界面改性剂为硅烷偶联剂KH550。树脂和固化剂重量配比100:55,加入5%质量分数的树脂改性剂,制备的复合材料整体的胶含量控制在35%左右。
(1)高模量透波层预浸料和耐海洋环境透波层预浸料的制备
除去平纹石英纤维布和超高分子量聚乙烯纤维布表面的杂质,之后放入120℃的真空烘箱中干燥至恒重,得到干净纤维布;将质量分数为95%的乙醇水溶液调节pH至3~4左右,加入纤维布质量5 wt. %的界面改性剂硅烷偶联剂KH550,混合均匀后,在60℃水解1h,然后将得到的干净纤维布浸入到水解后的混合液中4h,取出纤维布后用无水乙醇清洗,以除去表面未反应的界面改性剂,在120℃真空烘箱中干燥至恒重,得到改性纤维布;
在E51环氧树脂中加入树脂改性剂EP-POSS,搅拌均匀,然后加入胺类固化剂聚醚氨D400,再次混合均匀,使环氧树脂和固化剂的重量配比为100:55,EP-POSS和固化剂质量配比为100:66,然后使用真空烘箱对树脂在常温下进行脱泡处理,真空负压控制在0.095~0.1MPa,得到配制好的混合树脂胶液;
将数层改性的石英纤维布或超高分子量聚乙烯纤维布进行浸渍,则得到高模量透波层预浸料或者耐海洋环境透波层预浸料;
(2)耐海洋环境结构功能一体化透波复合材料的制备
将步骤(1)制备的耐海洋环境透波层预浸料按照设计的厚度铺放在涂有脱模剂的模具中,厚度确定的依据是使最终复合材料中的耐海洋环境透波层下蒙皮为0.5mm,然后在其上铺放设计厚度的步骤(1)制备的高模量透波层预浸料,厚度确定的依据是使最终复合材料中的高模量透波层芯材为6mm,然后铺放一定厚度的步骤(1)制备的耐海洋环境透波层预浸料,厚度确定的依据是使最终复合材料中的耐海洋环境透波层上蒙皮为0.5mm;铺放完毕后,在80℃达到凝胶时间后,按照80℃/2h+130℃/2h、压力15MPa的固化工艺进行固化,最后自然冷却到室温,拆模,得到复合材料制品。
参照GJB 7954-2012雷达透波材料透波率测试方法在微波暗室中利用喇叭法对样品进行透波率的测试,同时通过矢量网络分析仪获得传输损耗,如图2所示,其传输损耗最大为-1.455dB,即透波率整体在71.5%及以上。
盐雾实验按照GB/T10125-97进行,实验前先按照标准配制质量分数为5%、pH在6.5~7.2之间的氯化钠溶液,试运行后将裁好的试验样件放置盐雾试验机内进行为期28天的盐雾老化试验。实验结果:经过28天的盐雾腐蚀后,其吸水率为0.78%。
复合材料弯曲性能的测试参考GB/T1456-2005,根据不同复合材料的厚度确定测试试样的长度,每组5个试样,测试结果求其平均值。采用万能试验机测试其室温弯曲强度为376.43 MPa,弯曲模量22.4 GPa。
该复合材料采用高强高模、透波性能优异的石英纤维,可为海洋环境深海及水下潜水器透波设备提供可靠的保护。
实施例2
耐海洋透波复合材料的总厚度为7mm,高模量透波层芯材4mm,耐海洋环境透波层蒙皮各1.5mm。高模量透波材料层增强材料采用平纹石英纤维布,耐海洋环境透波层增强材料采用超高分子量聚乙烯纤维,热固性树脂选用E51环氧树脂,树脂改性剂选用缩水甘油醚基笼型倍半硅氧烷(EP-POSS),固化剂选用胺类固化剂聚醚氨D400,界面改性剂为硅烷偶联剂KH550。树脂和固化剂重量配比100:55,EP-POSS和固化剂质量配比为100:66,加入5%质量分数的树脂改性剂,制备的复合材料整体的胶含量控制在35%左右。工艺参数按照实施例1所述进行。
参照GJB 7954-2012雷达透波材料透波率测试方法在微波暗室中利用喇叭法对样品进行透波率的测试,同时通过矢量网络分析仪获得传输损耗,如图3所示,其传输损耗最大损耗为-0.56dB,即整体透波率在87.8%及以上。
盐雾实验参考GB/T10125-97进行,实验前先按照标准配制质量分数为5%、pH在6.5~7.2之间的氯化钠溶液,试运行后将裁好的试验样件放置盐雾试验机内进行为期28天的盐雾老化试验。实验结果:经过28天的盐雾腐蚀后,其吸水率为0.08%。
复合材料弯曲性能的测试参考GB/T1456-2005。根据不同复合材料的厚度确定测试试样的长度,每组5个试样,测试结果求其平均值。采用万能试验机测试其室温弯曲强度为254.13 MPa,弯曲模量17.62 GPa。
此结构复合材料采用轻质的超高分子量聚乙烯纤维,具有质量轻、透波性能优异、耐海洋环境性能优异的特点,适用于海洋环境浅水低压及水上大中小型雷达天线罩。
Claims (10)
1.一种耐海洋环境结构功能一体化透波复合材料,其特征在于,是由上下两层耐海洋环境透波层蒙皮和位于上下两层透波层蒙皮之间的高模量透波层芯材复合而成的耐海洋环境结构功能一体化透波夹芯复合材料;其中,高模量透波层芯材由热固性树脂、树脂改性剂、高模量透波纤维布、界面改性剂制备而成;上下两层耐海洋环境透波层蒙皮由热固性树脂、树脂改性剂、超高分子量聚乙烯纤维布制成。
2.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料的制备方法,其特征在于,通过模压成型工艺一体成型,制备方法包括手糊制备预浸料,然后模压成型;具体步骤为:
(1)高模量透波层预浸料和耐海洋环境透波层预浸料的制备:
除去纤维布表面的杂质,之后放入真空烘箱中干燥至恒重,得到干净纤维布;将质量分数为95%的乙醇水溶液调节pH至3~4左右,加入界面改性剂,混合均匀后,在60℃水解1h,然后将得到的干净纤维布浸入到水解后的混合液中4h,取出纤维布后用无水乙醇清洗,以除去表面未反应的界面改性剂,在真空烘箱中干燥至恒重后,得到改性纤维布;
在热固性树脂中加入树脂改性剂并搅拌均匀,加入固化剂,再次混合均匀,然后使用真空烘箱对树脂在常温下进行脱泡处理,真空负压控制在0.095~0.1MPa,得到配制好的混合树脂胶液;
将数层改性纤维布进行浸渍,则得到高模量透波层预浸料或者耐海洋环境透波层预浸料;
(2)耐海洋环境结构功能一体化透波复合材料的制备:
将步骤(1)制备的耐海洋环境透波层预浸料按照设计的厚度铺放在涂有脱模剂的模具中,然后在其上铺放设计厚度的步骤(1)制备的高模量透波层预浸料,最后再铺放设计厚度的步骤(1)制备的耐海洋环境透波层预浸料,铺放完毕后在一定温度和压力下固化一定时间,然后自然冷却到室温,拆模,则得到耐海洋环境结构功能一体化透波复合材料。
3.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法,其特征在于,所述热固性树脂选用任何耐腐蚀且透波的热固性树脂。
4.根据权利要求3所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法,其特征在于,所述热固性树脂为环氧树脂。
5.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法,其特征在于,所述高模量透波纤维布为石英纤维布、高强玻璃纤维布、高硅氧纤维布及超高分子量聚乙烯纤维布中的任一种或是任意两种的组合物;所述石英纤维布、高强玻璃纤维布、高硅氧纤维布及超高分子量聚乙烯纤维布或为单向布,或为多轴向织物,或为平纹布,或为斜纹布,或为缎纹布。
6.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法,其特征在于,树脂改性剂为笼型倍半硅氧烷、介孔二氧化硅和纳米级氮化硼中的一种。
7.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法,其特征在于,所述界面改性剂选用钛酸酯偶联剂或者硅烷偶联剂。
8.根据权利要求2所述的一种耐海洋环境结构功能一体化透波复合材料的制备方法,其特征在于,所述固化剂为胺类固化剂、酰胺类固化剂和酸酐类固化剂中的一种。
9.根据权利要求2所述的一种耐海洋环境结构功能一体化透波复合材料的制备方法,其特征在于,步骤(1)中,热固性树脂与固化剂的重量配比为100:55,树脂改性剂与固化剂的重量配比为100:66;界面改性剂加入量为纤维布质量的5% ;
步骤(1)中,除去纤维布表面的杂质,放入真空烘箱中进行干燥的温度为120℃;除去表面未反应的界面改性剂的纤维布在真空烘箱中处理温度为120℃。
10.根据权利要求1所述的一种耐海洋环境结构功能一体化透波复合材料或权利要求2所述的制备方法得到的透波复合材料在透波结构件中的应用,在水下潜水器以及海洋环境中各种型号天线罩中的应用。
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