CN111850821A - 一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法 - Google Patents
一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法 Download PDFInfo
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Abstract
本发明公开了一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法。本发明利用同轴静电纺丝技术，制备外层掺杂水滑石生长种源、芯层掺杂碳纳米管的聚合物纤维膜，通过水热法制备负载水滑石的具有多级结构的复合纤维膜，然后经过预氧化和焙烧制备得到电磁波吸收材料。本发明将碳纳米纤维、碳纳米管和金属纳米粒子结合，形成具有三维导电网络结构的电磁波材料，其电磁波吸收性能优异，显著优于单一电磁波吸收剂，且具有质轻、体薄、电磁参数可调的优点。
Description
技术领域
本发明属于电磁波吸收材料制备技术领域，特别涉及一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法。
背景技术
近年来，由于日益严重的电磁辐射污染问题以及现代军事隐身技术的发展需要，电磁波吸收材料引起了广泛关注。碳材料如碳纳米管(CNTs)具有优异的导电性、较高的机械强度和较低的密度，是一种良好的介电损耗型吸波材料；磁性金属化合物如水滑石焙烧产物具有优良的磁性能，是一种良好的磁损耗型吸波材料。具有优异吸波性能的材料需要兼具厚度薄、频带宽、质量轻、吸收强等特点，而往往单一的组分难以同时满足，复合材料成为很有应用前景的吸波材料。纤维复合材料因其较小的密度和较强的电磁波吸收能力吸引了很多研究者的研究兴趣。
静电纺丝是一种特殊的制备纳米纤维的方式。聚合物溶液在高压静电场力的作用下形成纤维被接收器收集，层层堆叠形成纤维膜。利用静电纺丝技术，将聚合物纤维、碳纳米管和水滑石相结合，通过高温处理，可以得到兼具介电损耗、磁损耗的水滑石基碳纤维复合吸波材料，形成三维导电网络，有利于克服单一的电介质型或磁介质型吸波材料吸收频带窄的缺点。
发明内容
基于上述现有技术中存在的问题，本发明目的在于提供一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法。
本发明利用同轴静电纺丝技术，制备外层掺杂水滑石生长种源、芯层掺杂碳纳米管的聚合物纤维膜，通过水热法制备负载水滑石的具有多级结构的复合纤维膜，通过预氧化和焙烧制备电磁波吸收材料。
本发明由水滑石基复合纳米纤维制备的电磁波吸收材料为纤维结构，纤维的平均直径为200-500nm，纤维的芯层掺杂碳纳米管，铁镍合金及尖晶石纳米颗粒均匀分布于纤维内部和表面。
本发明所述的由水滑石基复合纳米纤维制备电磁波吸收材料的方法为：
1)配制浓度为0.08-0.2g/mL的聚合物溶液；将FeOOH分散到聚合物溶液中得到外层溶液，FeOOH的添加量是聚合物质量的5-50％；将碳纳米管按0.005-0.05g/mL添加量均匀分散到聚合物溶液中，得到芯层溶液；将两种溶液分别加入到注射器中，使用同轴针头，内针头与芯层溶液连接，外针头与外层溶液连接，设定电场电压为8-25kV，优选12-20kV，溶液流速为0.5-2mL/h，针头与接收器之间距离设定为8-20cm，优选12-18cm，纺丝所得纤维膜于50-100℃真空干燥6-12h，优选60-80℃真空干燥8h，得到种源掺杂的聚合物纤维膜；
2)采用水热法在种源掺杂的聚合物纤维膜上原位生长水滑石片状结构；
3)将步骤2)得到的负载水滑石的聚合物纤维膜先在空气中预氧化，再进行焙烧处理，即得电磁波吸收材料。
所述步骤2)的具体操作方法为：配制含Ni2+和Fe3+的混合盐溶液，其中Ni2+和Fe3+的摩尔比为1-4，Ni2+浓度为0.001-0.2mol/L，优选0.01-0.1mol/L；然后向混合盐溶液中加入尿素，加入尿素的物质的量为溶液中金属盐的阴离子总物质的量的1-4倍；搅拌均匀后将混合溶液转移至聚四氟乙烯反应釜中；将种源掺杂的聚合物纤维膜加入聚四氟乙烯反应釜中，于90-160℃下水热反应6-24h，优选8-16h；将聚合物纤维膜取出，先用去离子水冲洗，然后用去离子水超声清洗5-30min，再用去离子水和乙醇冲洗后，于50-100℃真空干燥4-12h，优选60-80℃真空干燥8h。
所述的金属盐的阴离子为硝酸根或氯离子。
所述的预氧化的温度为200-280℃，保温时间1-3h，升温速率为1-5℃/min。
所述的焙烧的温度为400-900℃，气氛为氮气或氩气，保温时间3-8h，升温速率为1-10℃/min。
一种电磁波吸收体，由上述制备得到的电磁波吸收材料和石蜡混合配制而成。
所述电磁波吸收体厚度为1.4mm，频率为16.8GHz时达到最大吸收强度，其反射损耗为-49.5dB。
所述电磁波吸收体厚度为1.5mm，有效吸收频带宽度为4.72GHz。
将上述制备的电磁波吸收材料和/或电磁波吸收体应用在无线电通讯系统、防高频、微波加热设备、构造微波暗室、或隐身技术中。
本发明利用静电纺丝技术，将碳纳米纤维、碳纳米管和金属纳米粒子结合，形成具有三维导电网络结构的电磁波材料，其电磁波吸收性能优异，显著优于单一电磁波吸收剂，且具有质轻、体薄、电磁参数可调的优点。
附图说明
图1是本发明实施例1制备的镍铁水滑石-聚丙烯腈的XRD谱图。
图2是本发明实施例1制备的镍铁水滑石-聚丙烯腈的扫描电镜图。
图3是本发明实施例1制备的电磁波吸收材料的XRD谱图。
图4是本发明实施例1制备的电磁波吸收材料的扫描电镜图。
图5是本发明实施例1制备的不同厚度电磁波吸收材料的电磁波吸收曲线。
具体实施方式
下面结合附图对本发明进行详细说明，以令本领域技术人员参照说明文字能够实施。
实施例1
(1)量取10mL的N,N-二甲基甲酰胺，向其中加入0.8g聚丙烯腈以及0.08g FeOOH，配制成溶液，该溶液为外层溶液；量取10mL N,N-二甲基甲酰胺，向其中加入0.8g聚丙烯腈以及0.05g碳纳米管，配制成溶液，该溶液为芯层溶液；将两种溶液分别加入到注射器中，使用同轴针头，内针头与芯层溶液连接，外针头与外层溶液连接，设置电场电压为18kV，接收距离为15cm，溶液流速为1.5mL/h；纺丝所得纤维膜置于60℃真空干燥箱中干燥8h，得到FeOOH掺杂的聚丙烯腈纤维膜；
(2)配制氯化镍和氯化铁的混合盐溶液，Ni2+和Fe3+的摩尔比为3:1，Ni2+的浓度为0.015mol/L，尿素的物质的量为溶液中氯离子物质的量的2倍，搅拌10min，注入聚四氟乙烯反应釜中；裁取FeOOH掺杂的聚丙烯腈纤维膜为边长5cm的正方形，加入反应釜中，140℃水热反应8h；冷却至室温后取出膜，去离子水冲洗后，置于盛有去离子水的烧杯中，超声清洗15min，再用去离子水和乙醇冲洗，真空干燥箱中60℃干燥8h，制得镍铁水滑石-聚丙烯腈复合纤维膜；
(3)将镍铁水滑石-聚丙烯腈复合纤维膜在200℃下预氧化处理3h后，置于氮气气氛的马弗炉中，在900℃下焙烧3h。
性能测试：
将实施例1制备的电磁波吸收材料与石蜡按照质量比3:7的比例混合后压成环状的吸收体样品(D外×d内×h＝7×3×2mm)，进行电磁波吸收性能的测试，曲线如图5所示，1.4mm厚度下吸收峰最小值为-49.5dB，1.5mm厚度下吸收率小于-10dB的带宽为4.72GHz。
实施例2
同实施例1，区别在于：步骤(1)中，碳纳米管的用量为0.1g；步骤(2)中，用硝酸镍和硝酸铁替代氯化镍和氯化铁；步骤(3)中，预氧化处理的时间和温度为：300℃预氧化处理2h。
实施例3
同实施例1，区别在于：步骤(1)中，FeOOH的用量为0.1g，所述高压静电纺丝法的电压为15kV；步骤(2)中，所述反应的温度为100℃，反应时间为14h；步骤(3)中，焙烧处理的时间和温度为：900℃焙烧处理3h。
Claims (10)
1.一种由水滑石基复合纳米纤维制备的电磁波吸收材料，其特征在于，所述的电磁波吸收材料为纤维结构，纤维的平均直径为200-500nm，纤维的芯层掺杂碳纳米管，铁镍合金及尖晶石纳米颗粒均匀分布于纤维内部和表面。
2.一种由水滑石基复合纳米纤维制备电磁波吸收材料的方法，其特征在于，所述的方法的操作步骤为：
1)配制浓度为0.08-0.2g/mL的聚合物溶液；将FeOOH分散到聚合物溶液中得到外层溶液，FeOOH的添加量是聚合物质量的5-50％；将碳纳米管按0.005-0.05g/mL添加量均匀分散到聚合物溶液中，得到芯层溶液；将两种溶液分别加入到注射器中，使用同轴针头，内针头与芯层溶液连接，外针头与外层溶液连接，设定电场电压为8-25kV，优选12-20kV，溶液流速为0.5-2mL/h，针头与接收器之间距离设定为8-20cm，优选12-18cm，纺丝所得纤维膜于50-100℃真空干燥6-12h，优选60-80℃真空干燥8h，得到种源掺杂的聚合物纤维膜；
2)采用水热法在种源掺杂的聚合物纤维膜上原位生长水滑石片状结构；
3)将步骤2)得到的负载水滑石的聚合物纤维膜先在空气中预氧化，再进行焙烧处理，即得电磁波吸收材料。
3.根据权利要求2所述的方法，其特征在于，所述步骤2)的具体操作方法为：配制含Ni2+和Fe3+的混合盐溶液，其中Ni2+和Fe3+的摩尔比为1-4，Ni2+浓度为0.001-0.2mol/L，优选0.01-0.1mol/L；然后向混合盐溶液中加入尿素，加入尿素的物质的量为溶液中金属盐的阴离子总物质的量的1-4倍；搅拌均匀后将混合溶液转移至聚四氟乙烯反应釜中；将种源掺杂的聚合物纤维膜加入聚四氟乙烯反应釜中，于90-160℃下水热反应6-24h，优选8-16h；将聚合物纤维膜取出，先用去离子水冲洗，然后用去离子水超声清洗5-30min，再用去离子水和乙醇冲洗后，于50-100℃真空干燥4-12h，优选60-80℃真空干燥8h。
4.根据权利要求3所述的方法，其特征在于，所述的预氧化的温度为200-280℃，保温时间1-3h，升温速率为1-5℃/min。
5.根据权利要求3所述的方法，其特征在于，所述的焙烧的温度为400-900℃，气氛为氮气或氩气，保温时间3-8h，升温速率为1-10℃/min。
6.一种电磁波吸收体，其特征在于，由权利要求2-6任一项所述的方法制备得到的电磁波吸收材料和石蜡混合配制而成。
7.根据权利要求6所述的电磁波吸收体，其特征在于，所述电磁波吸收体厚度为1.4mm，频率为16.8GHz时达到最大吸收强度，其反射损耗为-49.5dB。
8.根据权利要求6所述的电磁波吸收体，其特征在于，所述电磁波吸收体厚度为1.5mm，有效吸收频带宽度为4.72GHz。
9.根据权利要求2-5任一项所述的方法制备得到的电磁波吸收材料在无线电通讯系统、防高频、微波加热设备、构造微波暗室、或隐身技术中的应用。
10.根据权利要6所述的电磁波吸收体在无线电通讯系统、防高频、微波加热设备、构造微波暗室、或隐身技术中的应用。
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