CN112549687A - 一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构及其制备方法 - Google Patents

一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构及其制备方法 Download PDF

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CN112549687A
CN112549687A CN202011304541.5A CN202011304541A CN112549687A CN 112549687 A CN112549687 A CN 112549687A CN 202011304541 A CN202011304541 A CN 202011304541A CN 112549687 A CN112549687 A CN 112549687A
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modified
polyimide
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absorbing material
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罗正权
胡渊
李英章
伍鑫
杨云鹏
夏林灿
骆金科
王建
李怀柱
黄春洪
伍小季
朱伟
官忠臣
杨军
李小东
朱宇翔
朱丽娟
梁鹏志
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Guizhou Aerospace Construction Engineering Co ltd
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Abstract

一种基于改性聚酰亚胺基的微波暗室用吸波材料由聚酰亚胺发泡前驱体复合吸波材料和改性泡沫铝共同构成；由聚酰亚胺发泡前驱体复合吸波材料制成吸波角锥，所述吸波角锥通过粘接剂粘附于改性泡沫铝板上，所述改性泡沫铝板的另一面通过长钉固定有泡沫铝板且改性泡沫铝板与泡沫铝板之间存在空隙，所述空隙内填充气凝胶。有益效果在于：采用多种吸波介质材料共同形成吸波角锥，有效提高复合材料在各频率上的吸波性能；采用吸波介质对泡沫铝进行改性，提高吸波能力，同时泡沫铝具备优异的隔声性能；采用气凝胶填充改性泡沫铝与普通泡沫铝间的夹层，提高了隔热保温性能。

Description

一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构 及其制备方法
技术领域
本发明属于吸波材料领域，具涉及一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构及其制备方法。
背景技术
微波暗室就是用吸波材料来制造一个封闭空间，创造出纯净的电磁环境，排除外界电磁干扰，是进行天线、雷达等无线通讯产品和电子产品测试的场所，可用测试产品免受杂波干扰，提高被测设备的测试精度和效率。现阶段的微波暗室，多采用铁氧体磁/发泡聚苯乙烯、铁氧体/发泡聚丙烯等作为吸波角锥材料，材料多为B2级阻燃材料，安全性欠佳。同时，单一吸波介质的吸波性能无法完全满足测试要求。
专利CN103700410A提供了一种电磁兼容电波暗室用难燃型吸波材料及其制备方法，专利CN109788728A提供一种轻质吸波暗室尖锥材料及其制备方法。上述专利或只采用单一的吸波介质，或只针对吸波角锥进行改善。目前仍未能得到一种综合性能优秀，且对电磁波和声波均有较高的吸收率的吸波材料。
发明内容
本发明针对现有技术的不足，提出了一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构及其制备方法。
一种基于改性聚酰亚胺基的微波暗室用吸波材料由聚酰亚胺发泡前驱体复合吸波材料和改性泡沫铝共同构成；
所述聚酰亚胺发泡前驱体复合吸波材料包括聚酰亚胺发泡前驱体、四氢呋喃、改性碳纳米管、磁性铁纳米粉体材料、黄基席夫碱金属盐配合物；按质量份计：聚酰亚胺发泡前驱体85-95%，四氢呋喃0.2-1%，改性碳纳米管占1-8%，磁性铁纳米材料0.5-6%，视黄基席夫碱金属盐配合物0.1-4%，共计100%；
所述改性泡沫铝包括铝粉、改性碳纳米管、磁性铁纳米磁珠、碳化硅和氢化钛，按质量份计：铝粉90-95%，改性碳纳米管2-4%、磁性铁纳米磁珠0.8-3%、碳化硅0.7-3%、氢化钛0.5-2%，共计100%。
优选的，所述聚酰亚胺前驱体粉末过筛后粒径为45-200目。
优选的，所述改性碳纳米管为管径不大于30nm的羟基化多壁改性碳纳米管、羧基化多壁改性碳纳米管、短多壁改性碳纳米管、羧基化-羟基化短多壁改性碳纳米管、石墨化多壁改性碳纳米管中的一种或几种组成。
优选的，所述磁性铁纳米粉体材料为尺寸不大于25nm的纳米Fe3O4粉体材料。
优选的，所述视黄基席夫碱金属盐配合物中的金属盐为银、锌、铜中的一种。
优选的，所述改性碳纳米管为石墨化多壁改性碳纳米管。
优选的，所述磁性铁纳米磁珠为氧化硅-四氧化三铁磁珠、镍-四氧化三铁磁珠的一种或两种组成。
优选的，所述碳化硅为含SiC约97%以上的绿碳化硅。
优选的，所述改性泡沫铝气孔直径2-7mm，气孔率不低于75%。
一种基于改性聚酰亚胺基的微波暗室用吸波材料制备方法包括聚酰亚胺发泡前驱体复合吸波材料吸波角锥的制备及改性泡沫铝板的制备，具体制备方法为：
1. 聚酰亚胺发泡前驱体复合吸波材料吸波角锥的制备
1.1按质量份数，将聚酰亚胺发泡前驱体、四氢呋喃、改性碳纳米管、磁性铁纳米粉体材料、黄基席夫碱金属盐配合物复合粉末充分混合形成混合物；
1.2将步骤1.1中的混合物放置到第一预热温度80-100℃的角锥形发泡模具中保温0.1-0.5h；
1.3将温度升至第二发泡温度140-150℃，保温2-3h；
1.4将温度升到第三酰亚胺化温度300-330℃，保温1-2h；
1.5保温结束后降至室温即形成聚酰亚胺发泡前驱体复合吸波材料吸波角锥。
2改性泡沫铝的制备
2.1按质量份数，将铝粉、改性碳纳米管、磁性铁纳米材料、碳化硅、氢化钛进行充分混合形成混合物；
2.2将步骤2.1中的混合物使用液压机在200-500MPa的压力下保持压力5-10min，得到发泡毛坯；
2.3将发泡毛坯在惰性气体的保护下放入发泡炉模具中逐渐升温到600-800℃，升温时间30-60min，保温1-2min后取出模具进行冷却定型；
2.4切割得到厚度6-10cm的改性泡沫铝板。
一种基于改性聚酰亚胺基的微波暗室用吸波结构包括聚酰亚胺发泡前驱体复合吸波材料吸波角锥、改性泡沫铝板、泡沫铝板、气凝胶及粘接剂；所述聚酰亚胺发泡前驱体复合吸波材料吸波角锥通过粘接剂粘附于改性泡沫铝板上，所述改性泡沫铝板的另一面通过长钉固定有泡沫铝板且改性泡沫铝板与泡沫铝板之间存在空隙，所述空隙内填充气凝胶。
优选的，所述泡沫铝为闭孔泡沫铝，气孔直径2-7mm，气孔率不低于75%，厚度6-10cm。
优选的，所述气凝胶为二氧化硅气凝胶，导热系数不高于0.02W/（m·K），填充厚度3-5cm。
优选的，所述粘接剂为硅酮胶。
优选的，所述改性泡沫铝板与聚酰亚胺发泡前驱体复合吸波材料吸波角锥采用齿状结构相互啮合固定。
本发明所述技术方案的有益效果在于：相较于现有技术，本发明所述的一种微波暗室泡沫铝-改性聚酰亚胺基复合吸波材料及其制备方法具有以下优势:
1.本发明采用改性碳纳米管、磁性铁纳米粉体材料、手性高分子材料视黄基席夫碱金属盐配合物填充改性聚酰亚胺，制得的吸波角锥体可调节各吸波材料组分配比，灵活调控性能，提高复合材料的在多个频段上的吸波性能。
2.本发明采用改性聚酰亚胺能作为制备吸波角锥的基质，利用其抗温变性能强特点制备保温耐燃的吸波功能材料，提高安全系数。
3.本发明采用泡沫铝作为基底材料，利用其隔声性能好并兼具吸波性能的特点，提高复合吸波材料的综合性能；本发明采用改性碳纳米管、磁性铁纳米磁珠对中间层泡沫铝进行改性，提高泡沫铝吸波性能的同时，提高泡沫铝板的力学性能。
4.本发明采用气凝胶填充改性泡沫铝及普通泡沫铝间的孔隙，提高吸波材料隔热效果，利于保持微波暗室的温度恒定。
附图说明
图1为本发明所述一种基于改性聚酰亚胺基的微波暗室用吸波结构的整体示意图；
图2为本发明所述一种基于改性聚酰亚胺基的微波暗室用吸波结构的整体示意图2；
图中:1、聚酰亚胺发泡前驱体复合吸波材料吸波角锥、2改性泡沫铝板、3气凝胶、4泡沫铝板、5长钉。
具体实施方式
为了使本领域技术人员更好地理解本发明的技术方案，下面结合具体实施例对本发明作进一步的详细说明。
如图1所示，一种基于改性聚酰亚胺基的微波暗室用吸波结构包括聚酰亚胺发泡前驱体复合吸波材料吸波角锥1、改性泡沫铝板2、泡沫铝板4、气凝胶3及粘接剂；所述聚酰亚胺发泡前驱体复合吸波材料吸波角锥1通过粘接剂粘附于改性泡沫铝板2上，所述改性泡沫铝板2的另一面通过长钉5固定有泡沫铝板4且改性泡沫铝板2与泡沫铝板4之间存在空隙，所述空隙内填充气凝胶3。
为增加稳固性，如图2所示，与实施例1相比，进一步改进的是，所述聚酰亚胺发泡前驱体复合吸波材料吸波角锥1及改性泡沫铝板2设有齿状结构，与之对应的改性泡沫铝板板2也设置为齿状，两者相互啮合。
为进一步验证本发明所述一种基于改性聚酰亚胺基的微波暗室用吸波材料性能，如下通过实施例进行进一步分析，具体如下：
一种基于改性聚酰亚胺基的微波暗室用吸波结构按如下步骤制备:
实施例1
1）聚酰亚胺发泡前驱体复合吸波材料吸波角锥制备
按质量份计，将85%的聚酰亚胺发泡前驱体，0.2%的四氢呋喃，8%的改性碳纳米管，2.8%的磁性铁纳米材料，4%的视黄基席夫碱金属盐配合物，共计100%，充分混合后进行烘干，放置到第一预热温度80℃的角锥形发泡模具中保温0.5h，然后将温度升至第二发泡温度140℃，保温3h；之后将温度升到第三酰亚胺化温度300℃，保温2h；保温结束后降至室温，即制得一种聚酰亚胺发泡前驱体复合吸波材料吸波角锥。
2）改性泡沫铝制备
按质量份计，将90%的铝粉，4%的改性碳纳米管、3%的磁性铁纳米磁珠、1%的碳化硅、2%的氢化钛，共计100%，进行充分混合后在使用液压机在200MPa的压力下保持压力10min，得到发泡毛坯；然后在惰性气体的保护下将发泡毛坯放入发泡炉模具中逐渐升温到600℃，升温时间60min，保温2min后取出模具进行冷却定型。
3）粘贴及组装
使用粘接剂将聚酰亚胺发泡前驱体复合吸波材料吸波角锥粘附于改性泡沫铝板上，使用长钉固定改性泡沫铝及泡沫铝，改性泡沫铝及泡沫铝之间使用气凝胶填充，改性泡沫铝板厚度6cm，泡沫铝板厚度6cm，两者间隙即气凝胶填充厚度5cm。最终获得一种基于改性聚酰亚胺基的微波暗室用吸波结构。
实施例2
1）聚酰亚胺发泡前驱体复合吸波材料吸波角锥制备
按质量份计，将88%的聚酰亚胺发泡前驱体，0.5%的四氢呋喃，2.5%的改性碳纳米管，6%的磁性铁纳米材料，3%的视黄基席夫碱金属盐配合物，共计100%，充分混合后进行烘干，放置到第一预热温度85℃的角锥形发泡模具中保温0.4h，然后将温度升至第二发泡温度142℃，保温2.7h；之后将温度升到第三酰亚胺化温度305℃，保温1.8h；保温结束后降至室温，即制得一种聚酰亚胺发泡前驱体复合吸波材料吸波角锥。
2）改性泡沫铝制备
按质量份计，将91%的铝粉，3%的改性碳纳米管、1.5%的磁性铁纳米磁珠、3%的碳化硅、1.5%的氢化钛，共计100%，进行充分混合后在使用液压机在300MPa的压力下保持压力8min，得到发泡毛坯；然后在惰性气体的保护下将发泡毛坯放入发泡炉模具中逐渐升温到700℃，升温时间50min，保温1.8min后取出模具进行冷却定型。
3）粘贴及组装
使用粘接剂将聚酰亚胺发泡前驱体复合吸波材料吸波角锥粘附于改性泡沫铝板上，使用长钉固定改性泡沫铝及泡沫铝，改性泡沫铝及泡沫铝之间使用气凝胶填充，改性泡沫铝板厚度10cm，泡沫铝板厚度10cm，两者间隙即气凝胶填充厚度3cm。最终获得一种基于改性聚酰亚胺基的微波暗室用吸波结构。
实施例3
1）聚酰亚胺发泡前驱体复合吸波材料吸波角锥制备
按质量份计，将93%的聚酰亚胺发泡前驱体，0.8%的四氢呋喃，5.6%的改性碳纳米管，0.5%的磁性铁纳米材料，0.1%的视黄基席夫碱金属盐配合物，共计100%，充分混合后进行烘干，放置到第一预热温度95℃的角锥形发泡模具中保温0.2h，然后将温度升至第二发泡温度145℃，保温2.5h；之后将温度升到第三酰亚胺化温度315℃，保温1.5h；保温结束后降至室温，即制得一种聚酰亚胺发泡前驱体复合吸波材料吸波角锥。
2）改性泡沫铝制备
按质量份计，将93%的铝粉，2.5%的改性碳纳米管、2%的磁性铁纳米磁珠、1.5%的碳化硅、1%的氢化钛，共计100%，进行充分混合后在使用液压机在400MPa的压力下保持压力6min，得到发泡毛坯；然后在惰性气体的保护下将发泡毛坯放入发泡炉模具中逐渐升温到750℃，升温时间40min，保温1.5min后取出模具进行冷却定型。
3）粘贴及组装
使用粘接剂将聚酰亚胺发泡前驱体复合吸波材料吸波角锥粘附于改性泡沫铝板上，使用长钉固定改性泡沫铝及泡沫铝，改性泡沫铝及泡沫铝之间使用气凝胶填充，改性泡沫铝板厚度8cm，泡沫铝板厚度7cm，两者间隙即气凝胶填充厚度4cm。最终获得一种基于改性聚酰亚胺基的微波暗室用吸波结构。
实施例4
1）聚酰亚胺发泡前驱体复合吸波材料吸波角锥制备
按质量份计，将95%的聚酰亚胺发泡前驱体，1%的四氢呋喃，1%的改性碳纳米管，2.5%的磁性铁纳米材料，0.5%的视黄基席夫碱金属盐配合物，共计100%，充分混合后进行烘干，放置到第一预热温度100℃的角锥形发泡模具中保温0.1h，然后将温度升至第二发泡温度150℃，保温3h；之后将温度升到第三酰亚胺化温度330℃，保温1h；保温结束后降至室温，即制得一种聚酰亚胺发泡前驱体复合吸波材料吸波角锥。
2）改性泡沫铝制备
按质量份计，将95%的铝粉，2%的改性碳纳米管、0.8%的磁性铁纳米磁珠、0.7%的碳化硅、0.5%的氢化钛，共计100%，进行充分混合后在使用液压机在500MPa的压力下保持压力5min，得到发泡毛坯；然后在惰性气体的保护下将发泡毛坯放入发泡炉模具中逐渐升温到800℃，升温时间30min，保温1min后取出模具进行冷却定型。
3）粘贴及组装
使用粘接剂将聚酰亚胺发泡前驱体复合吸波材料吸波角锥粘附于改性泡沫铝板上，使用长钉固定改性泡沫铝及泡沫铝，改性泡沫铝及泡沫铝之间使用气凝胶填充，改性泡沫铝板厚度7cm，泡沫铝板厚度9cm，两者间隙即气凝胶填充厚度4.5cm。最终获得一种基于改性聚酰亚胺基的微波暗室用吸波结构。
测试
分别测试上述实施例1-4的一种微波暗室泡沫铝-改性聚酰亚胺基复合吸波材料同等环境下的电磁屏蔽性能，依据国家军用标准 GJB 2038-9进行电磁性能测试；再分别测试其导热系数、燃烧性能、耐功率等，测试情况见表1所示。对比例为普通市售铁氧体磁/发泡聚苯乙烯损耗型吸波材料。
表1 性能测试
Figure 998409DEST_PATH_IMAGE001
根据上表，在同等情况下，实施例1-4组的电磁性能测试数值整体优于对比例，同时在导热系数、燃烧性能、耐功率、隔声量方面则优于对比例，说明本发明的泡沫铝-改性聚酰亚胺基复合吸波材料电磁屏蔽效果良好，同时保温隔热效果好，利于保持微波暗室的温度稳定，并显著提高了材料的防火性能、耐功率、隔声性能等。综上所述，该泡沫铝-改性聚酰亚胺基复合吸波材料电磁屏蔽性能好，应用安全系数高，绿色环保，综合性能优异。
本发明采用多种吸波介质材料填充聚酰亚胺基质，提高吸波性能，利用碳纳米管造成介电损耗、磁性铁纳米材料产生的磁损耗、视黄基席夫碱金属盐配合物电磁波交叉极化作用等提高复合材料在各频率上的吸波性能。本发明采用吸波介质对泡沫铝进行改性，提高吸波能力，同时泡沫铝具备优异的隔声性能；采用气凝胶填充改性泡沫铝与普通泡沫铝间的夹层，提高了隔热保温性能。
以上对本发明所提供的一种基于改性聚酰亚胺基的微波暗室用吸波材料、吸波结构及其制备方法进行了详细介绍，本文中应用了实施例对本申请的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本申请的方法及其核心思想；同时，对于本领域的一般技术人员，依据本申请的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本申请的限制。

Claims (15)

1.一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述微波暗室用吸波材料由聚酰亚胺发泡前驱体复合吸波材料和改性泡沫铝共同构成；
所述聚酰亚胺发泡前驱体复合吸波材料包括聚酰亚胺发泡前驱体、四氢呋喃、改性碳纳米管、磁性铁纳米粉体材料、黄基席夫碱金属盐配合物；按质量份计：聚酰亚胺发泡前驱体85-95%，四氢呋喃0.2-1%，改性碳纳米管占1-8%，磁性铁纳米材料0.5-6%，视黄基席夫碱金属盐配合物0.1-4%，共计100%；
所述改性泡沫铝包括铝粉、改性碳纳米管、磁性铁纳米磁珠、碳化硅和氢化钛，按质量份计：铝粉90-95%，改性碳纳米管2-4%、磁性铁纳米磁珠0.8-3%、碳化硅0.7-3%、氢化钛0.5-2%，共计100%。
2.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述聚酰亚胺前驱体粉末过筛后粒径为45-200目。
3.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述改性碳纳米管为管径不大于30nm的羟基化多壁改性碳纳米管、羧基化多壁改性碳纳米管、短多壁改性碳纳米管、羧基化-羟基化短多壁改性碳纳米管、石墨化多壁改性碳纳米管中的一种或几种组成。
4.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述磁性铁纳米粉体材料为尺寸不大于25nm的纳米Fe3O4粉体材料。
5.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述视黄基席夫碱金属盐配合物中的金属盐为银、锌、铜中的一种。
6.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述改性碳纳米管为石墨化多壁改性碳纳米管。
7.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述磁性铁纳米磁珠为氧化硅-四氧化三铁磁珠、镍-四氧化三铁磁珠的一种或两种组成。
8.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述碳化硅为含SiC约97%以上的绿碳化硅。
9.如权利要求1所述的一种基于改性聚酰亚胺基的微波暗室用吸波材料，其特征在于：所述改性泡沫铝气孔直径2-7mm，气孔率不低于75%。
10.一种基于改性聚酰亚胺基的微波暗室用吸波材料制备方法，其特征在于：所述微波暗室用吸波材料制备方法包括聚酰亚胺发泡前驱体复合吸波材料吸波角锥的制备及改性泡沫铝板的制备，具体制备方法为：
聚酰亚胺发泡前驱体复合吸波材料吸波角锥的制备
1.1按质量份数，将聚酰亚胺发泡前驱体、四氢呋喃、改性碳纳米管、磁性铁纳米粉体材料、黄基席夫碱金属盐配合物复合粉末充分混合形成混合物；
1.2将步骤1.1中的混合物放置到第一预热温度80-100℃的角锥形发泡模具中保温0.1-0.5h；
1.3将温度升至第二发泡温度140-150℃，保温2-3h；
1.4将温度升到第三酰亚胺化温度300-330℃，保温1-2h；
1.5保温结束后降至室温即形成聚酰亚胺发泡前驱体复合吸波材料吸波角锥；
2改性泡沫铝的制备
2.1按质量份数，将铝粉、改性碳纳米管、磁性铁纳米材料、碳化硅、氢化钛进行充分混合形成混合物；
2.2将步骤2.1中的混合物使用液压机在200-500MPa的压力下保持压力5-10min，得到发泡毛坯；
2.3将发泡毛坯在惰性气体的保护下放入发泡炉模具中逐渐升温到600-800℃，升温时间30-60min，保温1-2min后取出模具进行冷却定型；
2.4切割得到厚度6-10cm的改性泡沫铝板。
11.一种基于改性聚酰亚胺基的微波暗室用吸波结构，其特征在于：所述微波暗室用吸波结构包括聚酰亚胺发泡前驱体复合吸波材料吸波角锥、改性泡沫铝板、泡沫铝板、气凝胶及粘接剂；所述聚酰亚胺发泡前驱体复合吸波材料吸波角锥通过粘接剂粘附于改性泡沫铝板上，所述改性泡沫铝板的另一面通过长钉固定有泡沫铝板且改性泡沫铝板与泡沫铝板之间存在空隙，所述空隙内填充气凝胶。
12.如权利要求11所述的一种基于改性聚酰亚胺基的微波暗室用吸波结构，其特征在于：所述泡沫铝为闭孔泡沫铝，气孔直径2-7mm，气孔率不低于75%，厚度6-10cm。
13.如权利要求11所述的一种基于改性聚酰亚胺基的微波暗室用吸波结构，其特征在于：所述气凝胶为二氧化硅气凝胶，导热系数不高于0.02W/（m·K），填充厚度3-5cm。
14.如权利要求11所述的一种基于改性聚酰亚胺基的微波暗室用吸波结构，其特征在于：所述粘接剂为硅酮胶。
15.如权利要求11所述的一种基于改性聚酰亚胺基的微波暗室用吸波结构，其特征在于：所述改性泡沫铝板与聚酰亚胺发泡前驱体复合吸波材料吸波角锥采用齿状结构相互啮合固定。
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