CN112391833B - 轻质高效吸波材料SnFe2O4/C复合纳米纤维、吸波涂层及制备方法 - Google Patents
轻质高效吸波材料SnFe2O4/C复合纳米纤维、吸波涂层及制备方法 Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 42
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- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 10
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Abstract
本发明公开了轻质高效吸波材料SnFe2O4/C复合纳米纤维、吸波涂层及制备方法。该复合材料包括碳纳米纤维，碳纳米纤维表面附有尖晶石铁氧体SnFe2O4纳米颗粒。采用静电纺丝结合后期溶剂热法处理制得。本发明复合纤维不仅厚度薄、频带宽、吸收强，几乎在整个2～18GHz频段内都有强烈的吸收，且其电磁参数及微波吸收特性可方便地通过改变金属盐含量以及热处理过程参数进行宽范围调控。
Description
技术领域
本发明涉及吸波材料及制备方法，特别涉及轻质高效吸波材料SnFe2O4/C复合纳米纤维、吸波涂层及制备方法。
背景技术
随着GHz频段电磁波在电子通讯领域如移动电话、无线局域网、雷达系统等方面的广泛应用，电磁辐射污染问题也越来越突出，这不仅对人类健康带来潜在危害，而且还可能造成信息泄露和系统故障等问题；另一方面，提高现代及未来战争中武器装备的生存能力和突防能力要求尽可能降低雷达反射截面以实现其电磁隐身。于是为了解决电磁干扰和污染，以及军事装备隐身问题，高性能电磁波吸收材料的研制与开发一直受到各国的高度重视。众所周知，理想的吸波材料应该兼具很高的相对介电常数虚部值和相对磁导率虚部值，一个材料要获得好的吸波效果必须同时满足2个条件：一是阻抗匹配要好，入射电磁波能有效进入吸波体内部而不被反射；二是衰减能力要强，进入到材料内部的电磁波能被迅速地衰减吸收。根据衰减机制，吸波材料可分为磁损耗型和介电损耗型两大类。然而由于单个介电型材料或者磁性吸波材料的阻抗匹配较差，通常很难同时满足这两个要求。因此，将不同种类的材料以适当的形式制备成复合材料，有望在一定程度上实现理想吸波材料所要求的特性。
目前，在众多磁性吸波材料中，铁氧体因其吸波性能较好、成本低、制备工艺简单等优势是研究较多且已被广泛应用的一种传统微波吸收材料。其中，尖晶石铁氧体研究较为广泛，通式为MFe2O4，M通常指过渡元素，常见的有Co、Ni、Fe、Mn、Mg、Zn 等。而作为吸波材料的锡铁氧体(SnFe2O4)却由于Sn的不稳定难以制备而研究较少。是目前吸波材料的一大空白，鲜有人报道。
碳系材料，如碳纳米纤维(CNFs)、碳纳米管(CNTs)、碳纳米球、石墨烯等，由于其密度低、比表面积大、导电性好、化学稳定性好等特点，常被用作吸波材料的载体，因而在吸波材料方面应用广泛。但由于碳系材料的介电常数远大于磁导率，导致其阻抗匹配特性较差，因此一般将其与磁性物质进行复合，通过磁损耗与介电损耗的协同效应来有效改善吸波材料与自由空间之间的阻抗匹配特性，大大提高微波吸收性能。然而至今，人们对尖晶石铁氧体/碳复合吸收材料的研究主要集中在碳与尖晶石钴铁氧体、镍铁氧体、锰铁氧体和锌铁氧体复合上，而关于尖晶石锡铁氧体与一维碳纳米复合材料及其制备技术与应用还鲜有报道。
近年来，一维或者准一维纳米结构材料如纳米线、纳米纤维、纳米管和纳米棒等因其独特的形状各向异性提供了不同于各向同性微粒的损耗机制而在吸波材料方面展示出独到的优势，已成为一种很有发展前途的新型吸波材料。一维纳米结构还具有显著的空间限域效应，可使各组分在微观尺度上实现均匀分布，能够解决三维块体、二维薄膜和零维粉体中常易出现的颗粒团聚以及非均相分布问题，大大提高组分间的接触面积，不仅有利于加强锡铁氧体/碳纳米纤维复合体系中表面/界面效应以及介电损耗与磁损耗间的协同效应，而且还可在纳米尺度范围内形成良好的电磁匹配。
因此，借助于一维纳米结构材料所具有的独特结构和性能特征将锡铁氧体与碳纳米纤维复合形成一维纤维状纳米复合材料，有望进一步加强该复合体系的微波吸收性能，对于发展新型高性能一维结构纳米复合吸波材料科学与技术，促进锡铁氧体与碳纳米纤维复合材料在电磁波吸收与屏蔽领域的应用具有重要的意义和价值。
发明内容
发明目的：本发明目的是提供一种具有良好的吸波效果，且厚度薄、频带宽、吸收强以及电磁参数与吸波特性可宽范围调控的SnFe2O4/C复合纳米纤维。
本发明另一目的是提供所述SnFe2O4/C复合纳米纤维的制备方法。
技术方案：本发明提供一种轻质高效吸波材料SnFe2O4/C复合纳米纤维，包括碳纳米纤维，碳纳米纤维表面附有尖晶石铁氧体SnFe2O4纳米颗粒。
进一步地，当填充量为10％(质量分数)、厚度为1.7mm时，相应吸波涂层的最小反射损耗达到-29.0dB，低于-10dB的有效吸收带宽为7.2GHz，频率范围为10.8～18 GHz。
进一步地，当厚度为3.0mm时，有效吸收带宽为12.7GHz(5.3～18GHz)。
所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，包括如下步骤：
(1)碳纳米纤维的制备：在N，N-二甲基甲酰胺(DMF)中加入聚丙烯腈(PAN)，搅拌至完全溶解，得到纺丝溶液(PAN/DMF溶液)，采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维，干燥；在惰性气体条件下，前驱体纤维预氧化后，再经过碳化处理、硝酸酸化处理得到碳纳米纤维；
(2)SnFe2O4/C复合纳米纤维的制备：向乙二醇溶剂中依次加入反应物料氯化铁和氯化锡，待反应物料完全溶解后，再加入氢氧化钠，氨水，水浴加热搅拌后，将步骤(1) 得到的碳纳米纤维置入溶液后进行溶剂热反应；反应后产物经水和乙醇洗涤、干燥，即可。
进一步地，所述步骤(1)中，纺丝溶液(PAN/DMF溶液)中PAN的质量分数为 8～12％。
一种吸波涂层，以石蜡为基体，SnFe2O4/C复合纳米纤维匀分散在石蜡中。
进一步地，所述吸波涂层中SnFe2O4/C复合纳米纤维质量分数为5～20wt％。
进一步地，所述静电纺丝工艺参数为：电压15～20kV，溶液推进速率0.3～0.5ml/h，固化距离为15～20cm，温度为15～30℃，湿度小于40％。所述预氧化具体参数为：温度为180～280℃，保温时间1～3h，升温速率为1～5℃/min。所述碳化处理具体参数为：温度为600～1200℃，保温时间1～5h，升温速率为1～5℃/min。所述硝酸酸化处理具体参数为：处理时间为8～20h。
进一步地，在50ml乙二醇中，氯化铁的加入量为0.07～1.41g，氯化锡的加入量为0.03～0.59g，氢氧化钠的加入量为0.15g；氨水的加入体积为8～10ml，其中，氨水的浓度为12.9～14.8mol/L。溶剂热反应的反应温度为180～250℃，溶剂热反应的反应时间为 10～48h。
有益效果：本发明复合纤维不仅厚度薄、频带宽、吸收强，几乎在整个2～18GHz 频段内都有强烈的吸收，且其电磁参数及微波吸收特性可方便地通过改变金属盐含量以及热处理过程参数进行宽范围调控；同时，在制备时，采用静电纺丝技术结合溶剂热法合成出SnFe2O4/C复合纳米纤维微波吸收剂，工艺简单、操作方便、成本低、产率高，可连续大量制备SnFe2O4/C复合纳米纤维。此外，采用该纤维制备的吸波涂层，各涂层几乎在整个2～18GHz频段内均有较强烈的吸收，最小反射损耗达到-29.0dB，反射损耗在-10dB以下(即吸收率超过90％)的吸收带宽达到约12.7GHz，可覆盖一大半C波段和整个X至Ku波段。
附图说明
图1为本发明实施例1制备的SnFe2O4/C复合纳米纤维的SEM照片；
图2为本发明实施例1制备的SnFe2O4/C复合纳米纤维的XRD谱图；
图3为本发明实施例1制备的SnFe2O4/C复合纳米纤维/石蜡吸波涂层在2～18GHz频率范围内的微波吸收性能曲线。
具体实施方式
实施例1
本发明SnFe2O4/C复合纳米纤维的制备方法，包括如下步骤：
步骤1，碳纳米纤维的制备：将2g聚丙烯腈(PAN)加入到18g N，N-二甲基甲酰胺(DMF)中，并在60℃水浴搅拌2h至PAN完全溶解后再在室温下搅拌3h得到PAN/DMF 溶液，然后采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维。温度为20℃，湿度小于40％，工艺参数为：电压15kV、接收距离15cm、溶液推进速率0.5mL·h-1。收集到的PAN纤维经充分干燥后先在空气中加热至250℃预氧化2h，升温速率为2℃·min-1，然后再在氮气气氛下以5℃·min-1的速率升温到800℃碳化3h，最后随炉自然冷却至室温获得碳纤维，然后将其在硝酸溶液里浸泡12h，经去离子水和乙醇洗涤干燥后得到酸化后的碳纳米纤维。
步骤2，SnFe2O4/C复合纳米纤维的制备：在50mL乙二醇溶剂中依次加入0.7054g 氯化铁和0.2946g氯化锡，完全溶解后，加入0.15g氢氧化钠固体，搅拌至氢氧化钠完全溶解后，缓慢加入10mL 12.9mol/L氨水，60℃水浴加热搅拌2h后，取0.2g步骤1得到的碳纳米纤维置入溶液，将上述混合液转移到高压反应釜中，置于鼓风干燥箱中加热到200℃，保温15h；自然冷却至室温后将所得碳纤维经水和乙醇洗涤、干燥后，得到最终产物SnFe2O4/C复合纳米纤维，标记为SFO/C。
以石蜡为基体，将SFO/C复合纳米纤维匀分散在石蜡中，当吸收剂填充量为10％(质量分数，下同)，涂层厚度为1.7mm时，SFO/C-石蜡吸波涂层的最小反射率在17.6GHz 处达到-29.0dB，低于-10dB的有效吸收带宽为7.2GHz，频率范围为10.8～18GHz。
实施例2
步骤1，碳纳米纤维的制备：将2g聚丙烯腈(PAN)加入到18g N，N-二甲基甲酰胺(DMF)中，并在60℃水浴搅拌2h至PAN完全溶解后再在室温下搅拌3h得到PAN/DMF 溶液，然后采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维。温度为20℃，湿度小于40％，工艺参数为：电压15kV、接收距离15cm、溶液推进速率0.5mL·h-1。收集到的PAN纤维经充分干燥后先在空气中加热至250℃预氧化1h，升温速率为1℃·min-1，然后再在氮气气氛下以5℃·min-1的速率升温到800℃碳化3h，最后随炉自然冷却至室温获得碳纤维，然后将其在硝酸溶液里浸泡12h，经去离子水和乙醇洗涤干燥后得到酸化后的碳纳米纤维。
步骤2，SnFe2O4/C复合纳米纤维的制备：在50mL乙二醇溶剂中依次加入0.07g氯化铁和0.03g氯化锡，完全溶解后，加入0.15g氢氧化钠固体，搅拌至氢氧化钠完全溶解后，缓慢加入10mL 12.9mol/L氨水，60℃水浴加热搅拌2h后，取0.2g步骤1得到的碳纳米纤维置入溶液，将上述混合液转移到高压反应釜中，置于鼓风干燥箱中加热到 200℃，保温15h；自然冷却至室温后将所得碳纤维经水和乙醇洗涤、干燥后，得到最终产物SnFe2O4/C复合纳米纤维，标记为SFO/C(I)。
以石蜡为基体，将SFO/C(I)复合纳米纤维匀分散在石蜡中，当吸收剂填充量为5％，涂层厚度为2.7mm时，SFO/C(I)-石蜡吸波涂层的最小反射率在17.8GHz处达到-32.9dB，低于-10dB的有效吸收带宽为8.2GHz，频率范围为9.8～18GHz。
实施例3
步骤1，碳纳米纤维的制备：将1.6g聚丙烯腈(PAN)加入到18.4g N，N-二甲基甲酰胺(DMF)中，并在60℃水浴搅拌2h至PAN完全溶解后再在室温下搅拌3h得到 PAN/DMF溶液，然后采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维。温度为15℃，湿度小于40％，工艺参数为：电压20kV、接收距离20cm、溶液推进速率0.3mL·h-1。收集到的PAN纤维经充分干燥后先在空气中加热至180℃预氧化3h，升温速率为 5℃·min-1，然后再在氮气气氛下以1℃·min-1的速率升温到600℃碳化5h，最后随炉自然冷却至室温获得碳纤维，然后将其在硝酸溶液里浸泡20h，经去离子水和乙醇洗涤干燥后得到酸化后的碳纳米纤维。
步骤2，SnFe2O4/C复合纳米纤维的制备：在50mL乙二醇溶剂中依次加入0.2820g 氯化铁和0.1180g氯化锡，完全溶解后，加入0.15g氢氧化钠固体，搅拌至氢氧化钠完全溶解后，缓慢加入8mL 14.8mol/L氨水，60℃水浴加热搅拌2h后，取0.2g步骤1得到的碳纳米纤维置入溶液，将上述混合液转移到高压反应釜中，置于鼓风干燥箱中加热到180℃，保温48h；自然冷却至室温后将所得碳纤维经水和乙醇洗涤、干燥后，得到最终产物SnFe2O4/C复合纳米纤维，标记为SFO/C(II)。
以石蜡为基体，将SFO/C(II)复合纳米纤维匀分散在石蜡中，当吸收剂填充量为20％，涂层厚度为1.4mm时，SnFe2O4/C-石蜡吸波涂层的最小反射率在16.9GHz处达到-18dB，低于-10dB的有效吸收带宽为7.3GHz，频率范围为10.7～18GHz。
实施例4
步骤1，碳纳米纤维的制备：将2.4g聚丙烯腈(PAN)加入到17.6g N，N-二甲基甲酰胺(DMF)中，并在60℃水浴搅拌2h至PAN完全溶解后再在室温下搅拌3h得到 PAN/DMF溶液，然后采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维。温度为30℃，湿度小于40％，工艺参数为：电压20kV、接收距离15cm、溶液推进速率0.5mL·h-1。收集到的PAN纤维经充分干燥后先在空气中加热至280℃预氧化1h，升温速率为 1℃·min-1，然后再在氮气气氛下以5℃·min-1的速率升温到1200℃碳化1h，最后随炉自然冷却至室温获得碳纤维，然后将其在硝酸溶液里浸泡8h，经去离子水和乙醇洗涤干燥后得到酸化后的碳纳米纤维。
步骤2，SnFe2O4/C复合纳米纤维的制备：在50mL乙二醇溶剂中依次加入1.41g氯化铁和0.59g氯化锡，完全溶解后，加入0.15g氢氧化钠固体，搅拌至氢氧化钠完全溶解后，缓慢加入10mL 14.8mol/L氨水，60℃水浴加热搅拌2h后，取0.2g步骤1得到的碳纳米纤维置入溶液，将上述混合液转移到高压反应釜中，置于鼓风干燥箱中加热到 250℃，保温10h；自然冷却至室温后将所得碳纤维经水和乙醇洗涤、干燥后，得到最终产物SnFe2O4/C复合纳米纤维，标记为SFO/C(III)。
以石蜡为基体，将SFO/C(III)复合纳米纤维匀分散在石蜡中，当吸收剂填充量为5％，涂层厚度为3mm时，SnFe2O4/C-石蜡吸波涂层的最小反射率在13.6GHz处达到-41.9 dB，低于-10dB的有效吸收带宽为9.4GHz，频率范围为8.6～18GHz。
图1为本发明实施例1制得的SFO/C的SEM照片，从图1可以看出，SFO/C复合材料保持良好的纤维织构，粗细较为均匀，平均直径约(200±20)nm，纤维表面附有 SnFe2O4纳米颗粒。纤维彼此相互交联和堆叠构成一个三维导电网络，电子可通过迁移、跳跃和隧穿等方式在该导电网络中传输，增强材料的导电损耗，进而有助于提高对电磁波的衰减能力。
图2为本发明实施例1制得的SFO/C的X射线衍射图，从图2可以看出，在所测范围之内有明显的多个衍射峰，对应于SnFe2O4的各个晶面。
图3为本发明实施例1制得的SFO/C的反射损耗图谱，从图3可以看出，SFO/C复合材料表现出优异的微波吸收性能，当填充量为10％(质量分数)、厚度为1.7mm时，相应吸波涂层的最小反射损耗达到-29.0dB，低于-10dB的有效吸收带宽为7.2GHz，频率范围为10.8～18GHz；当厚度为3.0mm时，有效吸收带宽可提高到12.7GHz(5.3～18 GHz)。优异的吸波性能表明将SnFe2O4纳米颗粒锚定在碳纤维表面是构筑轻质、宽频和高效吸波材料的一种有效方法。
Claims (9)
1.一种轻质高效吸波材料SnFe2O4/C复合纳米纤维，其特征在于：包括碳纳米纤维，碳纳米纤维表面附有尖晶石铁氧体SnFe2O4纳米颗粒，
所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，包括如下步骤：
（1）碳纳米纤维的制备：在N,N-二甲基甲酰胺中加入聚丙烯腈，搅拌至完全溶解，得到纺丝溶液，采用静电纺丝工艺将纺丝溶液制备成前驱体纤维，干燥；在惰性气体条件下，前驱体纤维预氧化后，再经过碳化处理、硝酸酸化处理得到碳纳米纤维；
（2）SnFe2O4/C复合纳米纤维的制备：向乙二醇溶剂中依次加入反应物料氯化铁和氯化锡，待反应物料完全溶解后，再加入氢氧化钠，氨水，水浴加热搅拌后，将步骤（1）得到的碳纳米纤维置入溶液后进行溶剂热反应；反应后产物经水和乙醇洗涤、干燥，即可。
2.根据权利要求1所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维，其特征在于：当填充量以质量分数计为10%、厚度为1.7 mm时，相应吸波涂层的最小反射损耗达到–29.0 dB，低于–10 dB的有效吸收带宽为7.2 GHz，频率范围为10.8~18 GHz。
3.根据权利要求1所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维，其特征在于：当厚度为3.0 mm时，有效吸收带宽为12.7 GHz。
4.权利要求1所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，其特征在于：包括如下步骤：
（1）碳纳米纤维的制备：在N,N-二甲基甲酰胺中加入聚丙烯腈，搅拌至完全溶解，得到纺丝溶液，采用静电纺丝工艺将纺丝溶液制备成PAN前驱体纤维，干燥；在惰性气体条件下，前驱体纤维预氧化后，再经过碳化处理、硝酸酸化处理得到碳纳米纤维；
（2）SnFe2O4/C复合纳米纤维的制备：向乙二醇溶剂中依次加入反应物料氯化铁和氯化锡，待反应物料完全溶解后，再加入氢氧化钠，氨水，水浴加热搅拌后，将步骤（1）得到的碳纳米纤维置入溶液后进行溶剂热反应；反应后产物经水和乙醇洗涤、干燥，即可。
5.根据权利要求4所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，其特征在于：所述步骤（1）中，纺丝溶液中聚丙烯腈的质量分数为8~12%。
6.根据权利要求4所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，其特征在于：所述步骤（1）中，静电纺丝工艺参数为：电压15~20kV，溶液推进速率0.3~0.5ml/h，固化距离为15~20cm，温度为15~30℃，湿度小于40%；预氧化具体参数为：温度为180~280℃,保温时间1~3h，升温速率为1~5℃/min；碳化处理具体参数为：温度为600~1200℃,保温时间1~5h，升温速率为1~5℃/min；硝酸酸化处理具体参数为：处理时间为8~20h。
7.根据权利要求4所述的轻质高效吸波材料SnFe2O4/C复合纳米纤维的制备方法，其特征在于：所述步骤（2）中，在50ml乙二醇中，氯化铁的加入量为0.07~1.41g，氯化锡的加入量为0.03~0.59g，氢氧化钠的加入量为0.15g；氨水的加入体积为8~10ml，其中，氨水的浓度为12.9~14.8mol/L，溶剂热反应的反应温度为180~250℃，溶剂热反应的反应时间为10~48h。
8.一种吸波涂层，其特征在于：以石蜡为基体，将权利要求1所述的SnFe2O4/C复合纳米纤维均匀分散在石蜡中。
9.根据权利要求8所述的吸波涂层，其特征在于：所述吸波涂层中SnFe2O4/C复合纳米纤维质量分数为5~20wt%。
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