CN116217253A - 一种阻抗渐变层状梯度复合气凝胶及其制备方法和应用 - Google Patents
一种阻抗渐变层状梯度复合气凝胶及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种阻抗渐变层状梯度复合气凝胶及其制备方法和应用，属于吸波材料的制备领域，该阻抗渐变层状梯度复合气凝胶由不同阻抗的SiC/Si3N4复合气凝胶堆叠排列组成，SiC/Si3N4复合气凝胶具有SiC纳米线和Si3N4(微)纳米带相互搭接形成的多层不均匀界面的可调控孔隙的独特三维网络多孔结构。将不同阻抗的SiC/Si3N4复合气凝胶堆叠排列进行组装，进行气凝胶自粘接组装，以外层高阻抗的SiC/Si3N4复合气凝胶提升气凝胶的阻抗匹配。以内层高衰减的SiC/Si3N4复合气凝胶进行衰减，形成阻抗匹配由高到低的阻抗渐变层状梯度复合气凝胶，使电磁波能够以“之”字形的方式被不断缓慢逐层衰减，即将电磁波限制在层状气凝胶的内部被耗散，从而提高电磁波吸收性能。
Description
技术领域
本发明属于吸波材料的制备领域，具体涉及一种阻抗渐变层状梯度复合气凝胶及其制备方法和应用。
背景技术
电磁波技术广泛应用于信息通讯、医疗健康、交通运输、电子器件等国基民生的众多领域。然而，大功率射频发射器的普及使得电磁波在传输过程中会产生大量的电磁泄漏，从而导致不利的电磁干扰、电磁辐射和信息泄漏，造成了电子设备的失灵失控。同时研究表明，长期处在过量电磁辐射的环境中，人体各项机能都会下降，甚至诱发癌变，在无形中对人体健康产生威胁。不仅如此，在国防领域中各种先进雷达探测设备的诞生加剧了各国在军事领域的博弈，一系列高精尖侦察和打击系统成为未来战场的主要威胁，“发现即被摧毁”是武器装备面临的最大风险。因此，研究吸波材料的电磁参数并获得高性能吸波材料是亟待突破的科学问题。
吸波材料是一种将入射的电磁波吸收掉的功能材料，主要是通过将电磁能转化为热能或其他形式的能耗散掉，减少电磁波的反射及透射。理想的吸波材料应该具备厚度薄、质量轻、吸收频带宽、吸收能力强的特点，此外为了满足一些特殊情况的使用，还需具备一定的力学强度、耐腐蚀、耐高温、抗氧化等特点。目前典型的吸波材料主要有介电陶瓷、磁性材料及其复合材料，碳基材料及其复合材料等，这些材料大多都存在密度高，吸收强度低，吸波频段窄，较低的磁转变温度，以及高温下严重的氧化作用等缺点，从而限制了其应用。SiC由于其具有低密度，优异的热稳定性及化学稳定性的特点，成为了在极端环境下很有前途的电磁波吸收材料，但由于SiC阻抗匹配较差，导致其对电磁波的吸收效果并不令人满意。目前主要通过结构设计(多孔、核壳、层状或三维网络结构)，以及材料复合(介电陶瓷、磁性材料或碳基材料)的方法来对其进行改善，以提供丰富的异质界面以触发极化损失或提供大量用于EM散射的孔。
到目前为止，基于上述策略制备了大量的高性能电磁波吸收器。例如石墨烯/Si3N4、SiC/SiO2、SiCNWs/C/Si3N4、CNT/TiO2等复合材料。然而，这些材料还局限于研究阶段，材料的有效吸收带宽(EAB)有待扩大，材料的制备过程也相对复杂。因此，如何简单制备出具备薄、轻、宽、强特性的吸波性能，以及拥有优异的高温稳定性和隔热性能的吸波材料，仍然是本领域存在的一个技术困难点。同时，透波材料的引入虽然提高了阻抗匹配，但也牺牲了对电磁波的衰减能力。因此，如何制备同时具备高阻抗和高损耗的吸波材料，实现阻抗渐变，以让电磁波在材料内部缓慢衰减，是获得宽频吸波材料的关键，这也是本领域存在的一个技术困难点。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种阻抗渐变层状梯度复合气凝胶及其制备方法和应用，以解决现有的透波材料无法实现阻抗渐变，电磁波在材料内部不能缓慢衰减，因而无法获得宽频吸波材料的技术问题。
为了达到上述目的，本发明采用以下技术方案予以实现：
本发明公开了一种阻抗渐变层状梯度复合气凝胶，该阻抗渐变层状梯度复合气凝胶为层状结构，从电磁波入射方向到复合凝胶的底层是由阻抗由低到高的不同含量占比的SiC/Si3N4复合气凝胶堆叠而成；
其中，阻抗从低到高的SiC/Si3N4复合气凝胶通过纳米构筑基元的自粘性完成层状结构的组装，且阻抗匹配最好的SiC/Si3N4复合气凝胶放置在电磁波入射的表面层。
优选地，所述SiC/Si3N4复合气凝胶是由SiC纳米线和Si3N4微米/纳米带相互缠绕构筑的三维网络多孔结构，密度为5mg/cm3～100mg/cm3；其中，SiC纳米线的长度为100μm～1000μm，直径为20nm～0.5μm；Si3N4微米/纳米带的长度为100μm～1000μm，宽度为300nm～5μm。
进一步优选地，当SiC/Si3N4复合气凝胶的厚度为2mm时，SiC/Si3N4复合气凝胶具有7.36GHz的有效吸波带宽，能够覆盖整个Ku波段。
优选地，该阻抗渐变层状梯度复合气凝胶的密度为20～200mg/cm3，有效吸波带宽为2.6GHz～8.32GHz。
本发明还公开了上述的阻抗渐变层状梯度复合气凝胶的制备方法，包括以下步骤：
1)以多孔碳材料为骨架，通过负压浸渍向其内部浸入聚硅氧烷溶胶，得到浸渍试样；
2)将浸渍试样处理至溶胶完全凝胶化，然后先在氩气气氛中加热发生裂解反应，随后通入0.2～0.5MPa的氮气继续反应，反应完后随炉冷却至室温；
3)将步骤2)反应后的试样氧化除去碳纤维，制得SiC/Si3N4复合气凝胶；
4)将不同阻抗的SiC/Si3N4复合气凝胶在氩气环境下进行热压处理，以形成自粘接组装，获得阻抗渐变层状梯度复合气凝胶。
优选地，步骤1)中，负压浸渍处理的压力≥0.6MPa。
优选地，步骤2)中，先在0.2MPa氩气气氛中加热至1450℃发生裂解反应，保温2h，通入氮气后继续加热至1550℃并保温3h进行反应。
优选地，步骤2)中，通过调控通入氮气的含量调控SiC纳米线和Si3N4微米/纳米带的相对含量，从而调控SiC/Si3N4复合气凝胶的吸波性能，获得不同阻抗的SiC/Si3N4复合气凝胶。
优选地，步骤4)中，热压处理是在1000℃、氩气气氛下保温处理1h。
本发明还公开了上述的阻抗渐变层状梯度复合气凝胶在制备吸波材料中的应用。
与现有技术相比，本发明具有以下有益效果：
本发明公开的阻抗渐变层状梯度复合气凝胶，将不同阻抗的SiC/Si3N4复合气凝胶堆叠排列进行组装，进行气凝胶自粘接组装，以获得阻抗渐变层状梯度复合气凝胶，以外层高阻抗的SiC/Si3N4复合气凝胶提升气凝胶的阻抗匹配；以内层高衰减的SiC/Si3N4复合气凝胶进行衰减，形成阻抗匹配由高到低的阻抗渐变层状梯度复合气凝胶，使电磁波能够以“之”字形的方式被不断缓慢逐层衰减，即将电磁波限制在层状气凝胶的内部被耗散，从而提高电磁波吸收性能。本发明的阻抗渐变层状梯度复合气凝胶能够有效实现阻抗渐变，同时由于电磁波限制在层状气凝胶的内部被耗散，所以能够实现缓慢衰减从而获得宽频吸波材料。
进一步地，本发明采用前驱体裂解结合化学气相反应的方法，成功制备出具有独特三维网络结构的SiC/Si3N4复合气凝胶。利用其独特的三维网络结构骨架和Si3N4本身的低介电常数，实现吸波材料与环境间的阻抗匹配，引入了界面极化和多重散射等多种电磁波损耗机制，得到了具有优异吸波性能的超低密度复合气凝胶。
更近一步地，当厚度为2mm时，SiC/Si3N4复合气凝胶的最小反射损耗达到-48.62dB，实现了99.99％的电磁波吸收，-10dB以下的吸收频带宽度具有7.36GHz，能够覆盖整个Ku波段，具有优异的吸波性能。
本发明公开的上述阻抗渐变层状梯度复合气凝胶的制备方法简单易行、对设备要求低、可量产；采用该方法制得的复合气凝胶具有密度超轻、厚度薄，吸收强度高，吸波频段宽的特性、以及能在高温下使用，有望成为服务于极端环境的新一代复合吸波材料，并在工业上的推广使用。
附图说明
图1为实施例1制得的SiC/Si3N4复合气凝胶的宏观照片；
图2为实施例1制得的SiC/Si3N4复合气凝胶的微观扫描照片；
图3为实施例1制得的SiC/Si3N4复合气凝胶的XRD图；
图4为实施例1制得的SiC/Si3N4复合气凝胶的吸波性能曲线；其中，(a)为纯碳化硅；(b)为氮气压力0.1MPa；(c)为氮气压力0.2MPa；(d)为氮气压力0.3MPa；(e)为氮气压力0.4MPa；(f)为氮气压力0.5MP制备气凝胶的反射损失；
图5为实施例1制得的SiC/Si3N4复合气凝胶的高温稳定性；
图6为实施例3制得的阻抗渐变层状梯度复合气凝胶的微观照片；
图7为实施例3制得的阻抗渐变层状梯度复合气凝胶的吸波性能曲线。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分的实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。
需要说明的是，本发明的说明书和权利要求书及上述附图中的术语“第一”、“第二”等是用于区别类似的对象，而不必用于描述特定的顺序或先后次序。应该理解这样使用的数据在适当情况下可以互换，以便这里描述的本发明的实施例能够以除了在这里图示或描述的那些以外的顺序实施。此外，术语“包括”和“具有”以及他们的任何变形，意图在于覆盖不排他的包含，例如，包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元，而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备固有的其它步骤或单元。
下面结合附图对本发明做进一步详细描述：
实施例1
一种SiC/Si3N4复合气凝胶的制备方法，按照如下步骤进行：
1)以多孔碳材料或多孔碳纤维材料为骨架，通过负压浸渍向其内部浸入聚硅氧烷溶胶(聚硅氧烷溶胶如专利号为ZL201811626203.6公开的方法制备得到：以硅氧烷为原料，无水乙醇为溶剂，水为交联剂，制备聚硅氧烷溶胶。其中，以质量百分比计，制备聚硅氧烷溶胶所用硅氧烷为10～70％，水为10％～70％，无水乙醇为10％～80％)；
2)将步骤1)浸渍后的试样静置，形成陶瓷前驱体，然后将陶瓷前驱体放入真空干燥箱中持续处理至溶胶完全凝胶化，随后在0.2MPa氩气加热至1450℃裂解，保温2h，继续通入0.4MPa氮气加热至1550℃并保温3h进行反应，随后随炉冷却至室温；
3)将裂解后的试样置于空气炉中，700℃下保温3h，制得由纳米线构筑的SiC/Si3N4复合气凝胶。
结果参见图1，为本实施例制得的SiC/Si3N4复合气凝胶的宏观照片，从图1中可以看出，采用本发明方法所制得的SiC/Si3N4复合气凝胶宏观上呈青灰色和白色，是一种具有独特三维网络多孔结构的超轻陶瓷气凝胶材料。
参见图4，为本实施例制得的SiC/Si3N4复合气凝胶的吸波性能曲线。从图4中可以看出，当吸波体厚度为2mm时，最大反射损耗达到-48.62dB，小于-10dB的有效吸波频带宽度为7.36GHz，覆盖了整个Ku波段。
实施例2
一种SiC/Si3N4复合气凝胶的制备方法，按照如下步骤进行：
1)以多孔碳材料或多孔碳纤维材料为骨架，通过负压浸渍向其内部浸入聚硅氧烷溶胶(聚硅氧烷溶胶如专利号为ZL201811626203.6公开的方法制备得到，同实施例1)；
2)将步骤1)浸渍后的试样静置，形成陶瓷前驱体，然后将陶瓷前驱体放入真空干燥箱中持续处理至溶胶完全凝胶化，随后在0.2MPa氩气加热至1450℃裂解，保温2h，继续通入0.5MPa氮气加热至1550℃裂解，保温4h，随后随炉冷却至室温；
3)将裂解后的试样置于空气炉中，700℃下保温3h，制得由纳米线构筑的SiC/Si3N4复合气凝胶。
在样品厚度为2.4mm时，最大反射损耗达到-39.82dB，小于-10dB的有效吸波频带宽度为6.04GHz。
实施例3
一种制备阻抗渐变层状梯度复合气凝胶的方法，包括以下步骤：
步骤一：分别在0.2MPa、0.3MPa、0.4MPa、0.5MPa氮气条件下，获得阻抗依次增大的SiC/Si3N4复合气凝胶；
步骤二：将上述不同阻抗的SiC/Si3N4复合气凝胶堆叠排列，阻抗由低到高，外层为高阻抗，依靠气凝胶的自粘结性对其进行组装，并在1000℃、氩气气氛、保温1小时后得到复合层状气凝胶，密度为40mg/cm3。图6为制得的复合层状气凝胶的截面微观扫描照片，说明不同SiC/Si3N4复合气凝胶组装成层状结构，并且层间结合紧密。如图7所示，此时厚度为4mm时，复合层状气凝胶吸收频带宽为11.6GHz，吸收强度为-25dB。
实施例4
一种制备阻抗渐变层状梯度复合气凝胶的方法，包括以下步骤：
步骤一：分别在0.4MPa、0.5MPa氮气条件下，获得阻抗依次增大的SiC/Si3N4复合气凝胶；
步骤二：将上述不同SiC/Si3N4复合气凝胶堆叠排列，阻抗由低到高，外层为高阻抗，依靠气凝胶的自粘结性对其进行组装，并在1000℃、氩气气氛、保温1小时后得到复合层状气凝胶，密度为55mg/cm3。此时的复合层状气凝胶吸收频带宽为8.32GHz，吸收强度为-30dB。
实施例5
一种制备阻抗渐变层状梯度复合气凝胶的方法，包括以下步骤：
步骤一：分别在0.3MPa、0.4MPa、0.5MPa氮气条件下，获得阻抗依次增大SiC/Si3N4复合气凝胶；
步骤二：将上述不同SiC/Si3N4复合气凝胶堆叠排列，阻抗由低到高，外层为高阻抗，依靠气凝胶的自粘结性对其进行组装，并在1000℃、氩气气氛、保温1小时后得到复合层状气凝胶，密度为42mg/cm3。此时的复合层状气凝胶吸收频带宽为7.1GHz，吸收强度为-25dB。
实施例6
一种制备阻抗渐变层状梯度复合气凝胶的方法，包括以下步骤：
步骤一：分别在0.3MPa、0.4MPa、0.5MPa氮气条件下，获得阻抗依次增大的SiC/Si3N4复合气凝胶；
步骤二：将上述不同SiC/Si3N4复合气凝胶的堆叠排列，阻抗由高到低，外层为低阻抗，依靠气凝胶的自粘结性对其进行组装，并在1000℃、氩气气氛、保温1小时后得到复合层状气凝胶，密度为50mg/cm3。此时的复合层状气凝胶吸收频带宽为1.6GHz，吸收强度为-21dB。
以上内容仅为说明本发明的技术思想，不能以此限定本发明的保护范围，凡是按照本发明提出的技术思想，在技术方案基础上所做的任何改动，均落入本发明权利要求书的保护范围之内。
Claims (10)
1.一种阻抗渐变层状梯度复合气凝胶，其特征在于，该阻抗渐变层状梯度复合气凝胶为层状结构，从电磁波入射方向到复合凝胶的底层是由阻抗由低到高的不同含量占比的SiC/Si3N4复合气凝胶堆叠而成；
其中，阻抗从低到高的SiC/Si3N4复合气凝胶通过纳米构筑基元的自粘性完成层状结构的组装，且阻抗匹配最好的SiC/Si3N4复合气凝胶放置在电磁波入射的表面层。
2.根据权利要求1所述的阻抗渐变层状梯度复合气凝胶，其特征在于，所述SiC/Si3N4复合气凝胶是由SiC纳米线和Si3N4微米/纳米带相互缠绕构筑的三维网络多孔结构，密度为5mg/cm3～100mg/cm3；其中，SiC纳米线的长度为100μm～1000μm，直径为20nm～0.5μm；Si3N4微米/纳米带的长度为100μm～1000μm，宽度为300nm～5μm。
3.根据权利要求2所述的阻抗渐变层状梯度复合气凝胶，其特征在于，当SiC/Si3N4复合气凝胶的厚度为2mm时，SiC/Si3N4复合气凝胶具有7.36GHz的有效吸波带宽，能够覆盖整个Ku波段。
4.根据权利要求1所述的阻抗渐变层状梯度复合气凝胶，其特征在于，该阻抗渐变层状梯度复合气凝胶的密度为20～200mg/cm3，有效吸波带宽为2.6GHz～8.32GHz。
5.权利要求1～4中任意一项所述的阻抗渐变层状梯度复合气凝胶的制备方法，其特征在于，包括以下步骤：
1)以多孔碳材料为骨架，通过负压浸渍向其内部浸入聚硅氧烷溶胶，得到浸渍试样；
2)将浸渍试样处理至溶胶完全凝胶化，然后先在氩气气氛中加热发生裂解反应，随后通入0.2～0.5MPa的氮气继续反应，反应完后随炉冷却至室温；
3)将步骤2)反应后的试样氧化除去碳纤维，制得SiC/Si3N4复合气凝胶；
4)将不同阻抗的SiC/Si3N4复合气凝胶在氩气环境下进行热压处理，以形成自粘接组装，获得阻抗渐变层状梯度复合气凝胶。
6.根据权利要求5所述的阻抗渐变层状梯度复合气凝胶的制备方法，其特征在于，步骤1)中，负压浸渍处理的压力≥0.6MPa。
7.根据权利要求5所述的阻抗渐变层状梯度复合气凝胶的制备方法，其特征在于，步骤2)中，先在0.2MPa氩气气氛中加热至1450℃发生裂解反应，保温2h，通入氮气后继续加热至1550℃并保温3h进行反应。
8.根据权利要求5所述的阻抗渐变层状梯度复合气凝胶的制备方法，其特征在于，步骤2)中，通过调控通入氮气的含量调控SiC纳米线和Si3N4微米/纳米带的相对含量，从而调控SiC/Si3N4复合气凝胶的吸波性能，获得不同阻抗的SiC/Si3N4复合气凝胶。
9.根据权利要求5所述的阻抗渐变层状梯度复合气凝胶的制备方法，其特征在于，步骤4)中，热压处理是在1000℃、氩气气氛下保温处理1h。
10.权利要求1～4中任意一项所述的阻抗渐变层状梯度复合气凝胶在制备吸波材料中的应用。
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