CN114619718A - 一种宽频吸波复合材料及其制备方法 - Google Patents
一种宽频吸波复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种宽频吸波复合材料,由耐低温反射层、耐中温损耗层、耐高温匹配层依次叠层而成,匹配层是具有周期性结构的金属或碳纤维、氧化物复合材料,损耗层为改性碳化硅陶瓷基复合材料,反射层为低气孔率的金属复合材料。该复合材料的制备方法包括:纤维预制体除胶处理、界面制备、改性碳化硅基体制备、表面金属层制备、周期性结构制备及填充。该发明方法制备的复合材料的结构强度高,在吸波的同时可以实现承载功能,有效减少部件的重量,同时吸波性能稳定,即使在高温承载环境下也具有较为稳定的电磁波吸收能力,厚度薄,吸收频带宽,对电磁波的吸收具有可调谐性,具有较高的应用价值。
Description
技术领域
本发明涉及一种吸波材料及其制备方法,尤其涉及一种宽频吸波复合材料及其制备方法。
背景技术
电子通讯技术的飞速发展对于高超声速飞行器、舰艇的结构部件提出了更多的要求,在保证其结构强度的前提下,对于各部位的隐身性能需求也随之提高,不仅要求对电磁波的吸收能力强,同时要尽可能地拓宽其吸收带宽。
目前使用较多的隐身材料为吸波涂料,对于带宽的拓展及吸收频率的控制借助于周期性结构的吸波器来实现,两者独立性较大,就算将其进行结合,材料的结构强度与耐温性能十分有限。
申请公告号为CN110423506A的中国发明专利公开了一种可低温快速固化雷达吸波涂料,该可低温快速固化雷达吸波涂料由A、B两组分组成,其中A组分的组成及质量百分比为:树脂基体7.2~35.0%,雷达波吸收剂40.0~64.0%,分散剂0.5~2.0%,抗沉剂0.4~1.0%,触变剂1.5~5.0%,稀释剂17.0~21.8%;所述B组分为胺类固化剂,A、B组分质量比为7~ 36∶1。发明提供的可低温快速固化雷达吸波涂料在低温(-25℃~-5℃)条件下可2天内快速固化、施工周期短,同时具有雷达波吸波性能好,力学性能优异等特点,且雷达吸波涂料固化后电性能和力学性能随时间波动小,性能一致性强。
申请公告号为CN106572622A的中国发明专利公开了一种宽频段吸波体,包括介电层、电阻层和反射层,其中电阻层位于介电层表面,所述反射层位于所述宽频段吸波体的底层,介电层位于反射层上方;所述电阻层为连续层或者由周期性结构重复组成的阵列,所述周期性结构的尺寸为0.01mm~50mm,周期性结构的形状为点、线段、三角形、四边形、多边形、圆形、椭圆中的一种或多种的组合。该发明提出的宽频段吸波体通过合理的结构设计与计算,厚度薄,吸收频段宽。
申请公告号为CN106868676B的中国发明专利公开了一种宽带轻质超材料吸波结构。该超材料的结构单元为蚊香形镂空图案,尺寸为1~3cm,在180×180mm的基板上呈5×5、8 ×8、14×14的二维阵列分布。吸收剂与石蜡按一定的质量分数混合而成的微波吸收材料,将其填充到具有超材料的FR4或聚四氟乙烯基板的镂空缝隙中。该超材料吸波结构具有显著的宽频-轻质微波吸收效应;在1~40GHz频率范围内,小于-10dB的有效带宽为3.5~16.8GHz;面密度为0.081~0.932kg·m2;厚度为0.5~2mm。本发明的设计思路新颖,具有宽带-轻质吸波特性,制备过程简单、原料廉价易得,成本低、易于应用推广,所得的超材料在微波隐身技术、天线、安检、热辐射探测、热辐射成像和无损探测等领域具有广阔的应用前景。
授权公告号CN108148461B的中国发明专利公开了具有周期性结构中涂的吸波涂层,属于涂料技术领域。解决了现有涂层技术中由于纤维布的连续性带来的中间层存在扩展性破坏风险的问题。本发明的吸波涂层,由从内至外依次紧密排列的底涂、吸波层、中涂和面涂组成;底涂由环氧底漆与环氧底漆固化剂组成,吸收层由环氧树脂、低分子聚酰胺固化剂、磁性吸收剂、分散剂、增韧剂、消泡剂和流平剂组成,中涂上具有周期性开孔单元,主要材料为浸润环氧树脂、聚酰胺树脂固化剂、增韧剂和填充剂的混合液的玻璃纤维布,面涂由耐磨涂料和防腐涂料组成。该涂层各层综合作用,具备优异的防腐蚀性,耐磨性和抗冲击性,正拉伸强度可达到16MPa以上,高于不含有周期性结构中涂的涂层力学强度。
目前,所公布的吸波材料的性能较为单一,吸波性能与结构强度、耐温性能等通常只能取其一,要么为吸波涂覆材料,要么为吸波器的结构研究,就算涉及周期性结构,也通常将其使用在涂覆材料中,应用条件十分有限,所以研究开发具有周期性结构的耐高温结构吸波材料具有十分重要的实用价值。
发明内容
为解决上述问题,本发明提出一种宽频吸波复合材料,由耐低温反射层、耐中温损耗层、耐高温匹配层依次叠层而成,所述反射层位于复合材料的底部,为气孔率0~10%的金属材料,厚度为0.01~3mm;所述损耗层位于复合材料的中部,为碳/碳化硅复合材料、碳化硅/碳化硅复合材料,厚度为1~5mm;所述匹配层位于复合材料的表面,为金属或碳纤维、氧化物复合材料,具有周期性结构,厚度为0.01~2mm。
进一步地,所述的损耗层为纤维预制体增强复合材料,纤维的电阻率为10-1~102Ω·cm,纤维预制体外具有氮化硼界面层,基体为改性的碳化硅基体,复合材料的体积电阻率为 0.01~500Ω·m。
更进一步地,所述的匹配层的周期性结构为圆形图案、环形图案、多边形图案中的1~3 种,周期性图案的间距为5~50mm,图案部分为金属复合材料、碳纤维复合材料,图案上部使用二氧化硅进行填充。
一种宽频吸波复合材料的制备方法,其特征在于包括以下顺序的步骤:
步骤1,对纤维预制体在真空或惰性气氛、600℃~1200℃进行除胶处理;
步骤2,使用硼酸和尿素对除胶后的纤维预制体进行浸渍涂覆制备氮化硼界面,硼酸尿素的摩尔分数比为1∶12~1∶1;
步骤3,通过浸渍-热解对纤维预制体制备改性碳化硅基体;
步骤4,加工复合材料介质层的表面,对复合材料的上下表面分别通过真空浸渗或者电镀制备金属化层;
步骤5,加工金属化层,针对外表面通过电化学刻蚀、激光雕刻、数控加工制备周期性结构,并在周期性结构外使用硅溶胶制备二氧化硅填充物。
进一步地,所述步骤3中,改性碳化硅基体的制备方法为第一个周期使用聚碳硅烷的二甲苯溶液(二者的质量比为1∶1),采用聚合物浸渍裂解法制备,对复合材料称重,测量增重率;第二个周期进行改性,具体为使用硝酸铁、硫酸铝铵水溶液对复合材料进行真空浸渍低温裂解;之后重复第一个周期过程,直至复合材料的增重0.5%~1.5%。
更进一步地,所述的用于改性的硝酸铁、硫酸铝铵水溶液中硝酸铁的质量占溶液的 20%~30%,硫酸铝铵质量占溶液的10%~20%。
与现有材料及技术相比,本发明具有如下有益效果:(1)复合材料的结构强度高,在吸波的同时可以实现承载功能,有效减少部件的重量;(2)复合材料的耐高温性能优异;(3) 复合材料的吸波性能稳定,即使在高温承载环境下也具有较为稳定的电磁波吸收能力;(4) 材料厚度薄,吸收频带宽,对电磁波的吸收具有可调谐性。
附图说明
图1是本发明实施例1提供的一种宽频吸波复合材料示意图。
1为匹配层,2为损耗层,3为反射层。
图2是本发明实施例1提供的宽频吸波复合材料的周期性结构示意图。
1为金属铝,2为二氧化硅填充物。
具体实施方式
下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
参见图1为一种宽频吸波复合材料,由耐低温反射层、耐中温损耗层、耐高温匹配层依次叠层而成,所述反射层位于复合材料的底部,为气孔率2%的金属铝,厚度为0.5mm;所述损耗层位于复合材料的中部,为碳/碳化硅复合材料,厚度为3.4mm;所述匹配层位于复合材料的表面,为金属铝与二氧化硅复合材料,具有周期性结构,厚度为0.5mm,参见图2。
进一步地,所述的损耗层为纤维预制体增强复合材料,纤维的电阻率为10-1Ω·cm,纤维预制体外具有氮化硼界面层,基体为改性的碳化硅基体,复合材料的体积电阻率为50Ω·m。
更进一步地,所述的匹配层的周期性结构为圆形图案和边数为12的十字形图案,周期性图案的间距为8mm,图案部分为金属复合材料、碳纤维复合材料,图案上部使用二氧化硅进行填充。
一种宽频吸波复合材料的制备方法,其特征在于包括以下顺序的步骤:
步骤1,对纤维预制体在惰性气氛、700℃进行除胶处理;
步骤2,使用硼酸和尿素对除胶后的纤维预制体进行浸渍涂覆制备氮化硼界面,硼酸尿素的摩尔分数比为1∶12~1∶1;
步骤3,通过浸渍-热解对纤维预制体制备改性碳化硅基体;
步骤4,加工复合材料介质层的表面,对复合材料的上下表面分别通过真空浸渗金属化铝层;
步骤5,加工金属化层,针对外表面通过激光雕刻制备周期性结构,并在周期性结构外使用硅溶胶制备二氧化硅填充物。
进一步地,所述步骤3中,改性碳化硅基体的制备方法为第一个周期使用聚碳硅烷的二甲苯溶液(二者的质量比为1∶1),采用聚合物浸渍裂解法制备,对复合材料称重,测量增重率;第二个周期进行改性,具体为使用硝酸铁、硫酸铝铵水溶液对复合材料进行真空浸渍低温裂解;之后重复第一个周期过程,直至复合材料的增重小于1%。
更进一步地,所述的用于改性的硝酸铁、硫酸铝铵水溶液中硝酸铁的质量占溶液的30%,硫酸铝铵质量占溶液的10%。
制备的上述复合材料在8.2-18.0GHz频段电磁波的介电损耗正切值为0.2-0.5,在X波段的最高反射率可达-20.1dB,复合材料的弯曲强度可达266MPa,由于吸波性能和弯曲强度表现优异,同时材料具有较好的耐温性能,在耐高温结构吸波领域有重要应用价值。
实施例2
一种宽频吸波复合材料,由耐低温反射层、耐中温损耗层、耐高温匹配层依次叠层而成,所述反射层位于复合材料的底部,为气孔率1%的金属材料,厚度为0.6mm;所述损耗层位于复合材料的中部,为碳化硅/碳化硅复合材料,厚度为4.5mm;所述匹配层位于复合材料的表面,为金属镍与二氧化硅复合材料,具有周期性结构,厚度为0.01~2mm。
进一步地,所述的损耗层为纤维预制体增强复合材料,纤维的电阻率为102Ω·cm,纤维预制体外具有氮化硼界面层,基体为改性的碳化硅基体,复合材料的体积电阻率为150Ω·m。
更进一步地,所述的匹配层的周期性结构为六边形图案,边长为8mm,周期性图案的间距为10mm,图案部分为金属镍,图案上部使用二氧化硅进行填充。
一种宽频吸波复合材料的制备方法,其特征在于包括以下顺序的步骤:
步骤1,对纤维预制体在真空或惰性气氛、900℃进行除胶处理;
步骤2,使用硼酸和尿素对除胶后的纤维预制体进行浸渍涂覆制备氮化硼界面,硼酸尿素的摩尔分数比为1∶11;
步骤3,通过浸渍-热解对纤维预制体制备改性碳化硅基体;
步骤4,加工复合材料介质层的表面,对复合材料的上下表面分别通过电镀制备金属化镍层;
步骤5,加工金属化层,针对外表面通过数控加工制备周期性结构,并在周期性结构外使用硅溶胶制备二氧化硅填充物。
进一步地,所述步骤3中,改性碳化硅基体的制备方法为第一个周期使用聚碳硅烷的二甲苯溶液(二者的质量比为1∶1),采用聚合物浸渍裂解法制备,对复合材料称重,测量增重率;第二个周期进行改性,具体为使用硝酸铁、硫酸铝铵水溶液对复合材料进行真空浸渍低温裂解;之后重复第一个周期过程,直至复合材料的增重小于1%。
更进一步地,所述的用于改性的硝酸铁、硫酸铝铵水溶液中硝酸铁的质量占溶液的25%,硫酸铝铵质量占溶液的20%。
制备的上述复合材料的密度低于2.6g/cm3,耐高温性能好(高达1200℃),高温下抗弯强度可达280MPa,抗氧化性能优异,同时具有较好的反射率(低至-13.4dB),吸波带宽达5.5GHz。
上述仅为本发明的具体实施方式,但本发明的设计构思并不局限于此,凡利用此构思对本发明进行非实质性的改动,均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (6)
1.一种宽频吸波复合材料,由耐低温反射层、耐中温损耗层、耐高温匹配层依次叠层而成,所述反射层位于复合材料的底部,为气孔率0~10%的金属材料,厚度为0.01~3mm;所述损耗层位于复合材料的中部,为碳/碳化硅复合材料、碳化硅/碳化硅复合材料,厚度为1~5mm;所述匹配层位于复合材料的表面,为金属或碳纤维、氧化物复合材料,具有周期性结构,厚度为0.01~2mm。
2.根据权利要求1所述的宽频吸波复合材料,其特征在于所述的损耗层为纤维预制体增强复合材料,纤维的电阻率为10-1~102Ω·cm,纤维预制体外具有氮化硼界面层,基体为改性的碳化硅基体,复合材料的体积电阻率为0.01~500Ω·m。
3.根据权利要求1所述的宽频吸波复合材料,其特征在于所述的匹配层的周期性结构为圆形图案、环形图案、多边形图案中的1~3种,周期性图案的间距为5~50mm,图案部分为金属复合材料、碳纤维复合材料,图案上部使用二氧化硅进行填充。
4.一种宽频吸波复合材料的制备方法,其特征在于包括以下顺序的步骤:
步骤1,对纤维预制体在真空或惰性气氛、600℃~1200℃进行除胶处理;
步骤2,使用硼酸和尿素对除胶后的纤维预制体进行浸渍涂覆制备氮化硼界面,硼酸尿素的摩尔分数比为1∶12~1∶1;
步骤3,通过浸渍-热解对纤维预制体制备改性碳化硅基体;
步骤4,加工复合材料介质层的表面,对复合材料的上下表面分别通过真空浸渗或者电镀制备金属化层;
步骤5,加工金属化层,针对外表面通过电化学刻蚀、激光雕刻、数控加工制备周期性结构,并在周期性结构外使用硅溶胶制备二氧化硅填充物。
5.根据权利要求4所述的制备方法,其特征在于所述步骤3中,改性碳化硅基体的制备方法为第一个周期使用聚碳硅烷的二甲苯溶液(二者的质量比为1∶1),采用聚合物浸渍裂解法制备,对复合材料称重,测量增重率;第二个周期进行改性,具体为使用硝酸铁、硫酸铝铵水溶液对复合材料进行真空浸渍低温裂解;之后重复第一个周期过程,直至复合材料的增重0.5%~1.5%。
6.根据权利要求5所述的改性碳化硅基体制备方法,其特征在于所述的用于改性的硝酸铁、硫酸铝铵水溶液中硝酸铁的质量占溶液的20%~30%,硫酸铝铵质量占溶液的10%~20%。
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