CN107521176B - 一种具有夹芯结构的雷达隐身复合薄膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种具有夹芯结构的雷达隐身复合薄膜及其制备方法，属于复合材料技术领域。本发明的复合薄膜是由芯材以及芯材两侧的蒙皮构成的一体化夹芯结构体，所述蒙皮为石墨烯，所述芯材包括纳米纤维构成的无纺布和导电高分子，所述纳米纤维及包覆在纳米纤维上的导电高分子组成核壳结构；具体是按下述步骤进行的：一、静电纺丝法制备无纺布；二、然后采用氧化反应在构成无纺布的纳米纤维上包覆导电高分子；三、然后浸渍石墨烯并致密化处理。本发明的方法能够替代现有吸波涂料，广泛应用于飞机、水面舰艇和地面装甲等对雷达波需要隐身的部位。
Description
技术领域
本发明属于复合材料技术领域；具体涉及一种具有夹芯结构的雷达隐身复合薄膜及其制备方法。
背景技术
传统吸波材料主要为涂料型或者结构型吸波材料。涂料一般由铁氧体、金属粉或碳粉与树脂体系组成，特点是厚度小，但是密度大、屏蔽或吸收的频带较窄，同时在使用时面临易脱落等问题；结构型吸波材料对毫米雷达波和厘米雷达波同时有宽频吸收作用，但是其厚度大，密度待优化。
发明内容
本发明的目的是为了提供一种厚度薄、柔韧性好并对毫米雷达波和厘米雷达波同时具有吸收作用的复合薄膜。
为解决上述技术问题，本发明的一种具有夹芯结构的雷达隐身复合薄膜是由芯材以及芯材两侧的蒙皮构成的一体化夹芯结构体，所述蒙皮为石墨烯，所述芯材包括纳米纤维构成的无纺布和导电高分子，所述纳米纤维及包覆在纳米纤维上的导电高分子组成核壳结构；具体是按下述步骤进行的：
步骤一、静电纺丝法制备无纺布；
步骤二、然后采用氧化反应在构成无纺布的纳米纤维上包覆导电高分子；
步骤三、然后浸渍石墨烯并致密化处理；即得到具有夹芯结构的雷达隐身复合薄膜。
进一步地限定，所述无纺布的材料为Fe3O4@SiO2。
进一步地限定，所述导电高分子为聚吡咯。
进一步地限定，步骤一中Fe3O4@SiO2无纺布是将0.3mg～0.8mgFeCl3溶于20mL～50mL乙二醇溶液中，再加入0.36g～0.6g柠檬酸钠，磁力搅拌不少于10min，然后缓慢加入到反应釜中，再在120℃～160℃条件下反应2～5h，即得到Fe3O4@SiO2凝胶；然后将Fe3O4@SiO2凝胶放入静电纺丝装置的注射泵，注射泵上设置2个针头，将铝箔固定在热台上，在针头加上高压电，铝箔接地，将铝箔和针头之间距离控制在5cm～10cm(以此调整无纺布厚度)，即在铝箔和针头之间形成静电场，湿度小于30％～50％环境下，将Fe3O4@SiO2凝胶在5kV～13kV高压电下注射形成喷雾，逐渐沉积在铝箔上；喷射完成后，将铝箔上膜揭下，即得到Fe3O4@SiO2无纺布。
进一步地限定，步骤二中将Fe3O4@SiO2无纺布置于Py溶液中5min～10min，取出，置于浓度为0.5mol/L～2mol/L的FeCl3溶液中10min～20min后干燥。
进一步地限定，步骤二中所述干燥是在60℃～80℃下保温12h～24h。
进一步地限定，步骤三中浸渍石墨烯溶液中10min～20min后取出，干燥，即得到雷达隐身电纺布/导电高分子/石墨烯复合薄膜。
进一步地限定，步骤三所述石墨烯溶液是单层率大于99％和含氧官能团含量小于10％的石墨烯浆料，浓度为1mg/mL～20mg/mL。
进一步地限定，步骤三中所述干燥是在60℃～80℃下保温12h～24h。
本发明的复合薄膜具有良好的柔韧性，又能对毫米雷达波和厘米雷达波同时具有宽频隐身作用，同时能够满足高低温、耐酸碱等环境要求。
本发明的方法能够替代现有吸波涂料，广泛应用于飞机、水面舰艇和地面装甲等对雷达波需要隐身的部位。
附图说明
图1是夹芯结构的雷达隐身复合薄膜示意图，图1a为薄膜正面示意图，图1b为复合薄膜的截面照片图，图1c为薄膜在螺旋状态下的示意图；
图2是夹芯结构的雷达隐身复合薄膜照片：(a)原始状态；(b)-40℃～140℃高低温试验后薄膜；(c)1MNaOH溶液浸渍24小时后取出烘干薄膜；
图3是夹芯结构的雷达隐身复合薄膜在2～18GHz的电磁反射损耗数据。
具体实施方式
具体实施方式一：本实施方式中具有夹芯结构的雷达隐身复合薄膜是按下述步骤进行的：
步骤一、制备Fe3O4@SiO2无纺布：
1)制备Fe3O4@SiO2凝胶：将0.32mgFeCl3溶于20ml乙二醇溶液中，再向该溶液中加入0.369g柠檬酸钠，磁力搅拌10min；用注射泵将混合溶液缓慢加入到反应釜中，160℃下反应2.5h，即得到Fe3O4@SiO2凝胶；
2)制备Fe3O4@SiO2无纺布：将Fe3O4@SiO2凝胶放入注射泵，湿度小于50％环境下，用注射泵注射，注射器的针头数量为2个；将铝箔固定在热台上，在针头加上13kV高压电，铝箔接地，即在铝箔和针头之间形成静电场；将混合溶液在高压下注射形成喷雾，逐渐沉积在铝箔上；喷射完成后，将铝箔上膜揭下，即得到Fe3O4@SiO2无纺布，通过控制针头的数目和基底的面积可控制无纺布的尺寸；
步骤一制备的Fe3O4@SiO2无纺布是纤维多孔结构的；所述的Fe3O4@SiO2无纺布密度为0.076g/cm3；
步骤二、包覆导电高分子：
1)Fe3O4@SiO2无纺布与Py溶液混合：将Fe3O4@SiO2无纺布与Py溶液低温下混合5min；
所述的过程中Py溶液需要将Fe3O4@SiO2无纺布漫过；
2)Fe3O4@SiO2无纺布Py的聚合反应：将Fe3O4@SiO2无纺布从Py溶液中取出，置于0.5MFeCl3溶液中10min，在80℃下保温干燥12h；
步骤二、包覆石墨烯：将上述制备的复合薄膜后浸入石墨烯溶液10min后，取出在80℃下保温干燥12h，即得到雷达隐身复合薄膜；
步骤三所述石墨烯溶液是石墨烯溶液是由单层率大于99％和含氧官能团含量小于10％的石墨烯浆料，浓度为1～20mg/ml。
本实施方式中基于Fe3O4@SiO2@PPy核壳结构以及Fe3O4@SiO2@PPy作为芯，石墨烯作为蒙皮的夹芯结构的吸波复合材料薄膜的制备方法。在第一步中，通过采用静电纺丝方法制得Fe3O4@SiO2支撑网络纤维材料，随后在Fe3O4@SiO2支撑网络上通过氧化反应将吡咯单体Py(浓度大于50％)包覆导电聚合物PPy，最终通过石墨烯浸渍并致密化处理，石墨烯或者氧化石墨烯浓度介于1mg/ml与20mg/ml之间。通过上述材料复合组成的复合材料薄膜既具有良好的柔韧性和强度，如图1所示；，又能对毫米雷达波和厘米雷达波同时具有隐身作用，还能满足高低温和酸碱等环境条件，如图2所示。
由图3可知，本实施例通过测试样品的拉伸强度大于1.50MPa，在4.5～18GHz范围内电磁反射损耗均小于-10dB，2～4.5GHz频段内电磁反射损耗均值小于-5dB，具有优异的宽频隐身效果。
Claims (7)
1.一种具有夹芯结构的雷达隐身复合薄膜的制备方法，所述复合薄膜是由芯材以及芯材两侧的蒙皮构成的一体化夹芯结构体，所述蒙皮为石墨烯，所述芯材包括纳米纤维构成的无纺布和导电高分子，所述纳米纤维及包覆在纳米纤维上的导电高分子组成核壳结构；其中，无纺布的材料为Fe3O4@SiO2；所述导电高分子为聚吡咯；其特征在于所述制备方法是按下述步骤进行的：
步骤一、静电纺丝法制备无纺布；
步骤二、然后采用氧化反应在构成无纺布的纳米纤维上包覆导电高分子；
步骤三、然后浸渍石墨烯并致密化处理；即得到具有夹芯结构的雷达隐身复合薄膜。
2.根据权利要求1所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤一中Fe3O4@SiO2无纺布是将Fe3O4@SiO2凝胶放入静电纺丝装置的注射泵，注射泵上设置2个针头，将铝箔固定在热台上，在针头加上高压电，铝箔接地，将铝箔和针头之间距离控制在5cm~10 cm，即在铝箔和针头之间形成静电场，湿度30%~50%环境下，将Fe3O4@SiO2凝胶在5kV~13kV高压电下注射形成喷雾，逐渐沉积在铝箔上；喷射完成后，将铝箔上膜揭下，即得到Fe3O4@SiO2无纺布。
3.根据权利要求2所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤二中将Fe3O4@SiO2无纺布置于Py溶液中5 min ~10min，取出，置于浓度为0.5mol/L~2mol/L的FeCl3溶液中10 min~20 min后干燥。
4.根据权利要求3所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤二中所述干燥是在60℃~80℃下保温12 h ~24 h。
5.根据权利要求3或4所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤三中浸渍石墨烯溶液中10 min~20 min后取出，干燥，即得到雷达隐身无纺布/导电高分子/石墨烯复合薄膜。
6.根据权利要求5所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤三所述石墨烯溶液是单层率大于99%和含氧官能团含量小于10%的石墨烯浆料，浓度为1 mg/mL ~ 20mg/mL。
7.根据权利要求5所述一种具有夹芯结构的雷达隐身复合薄膜的制备方法，其特征在于步骤三中所述干燥是在60℃~80℃下保温12h ~24h。
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