CN108439410A - 一种B4C/SiC纳米线复合微波吸收材料 - Google Patents
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Abstract
本发明公开了一种B4C/SiC纳米线复合微波吸收材料,该材料是以石墨、碳纳米管、棉纤维等作为碳源,硼粉为硼源,与SiO2以及催化剂(硝酸铁或硝酸镍)充分混合后,在惰性气氛保护下加热反应,即得到B4C/SiC纳米线复合微波吸收材料。本发明所采用的原料简单易得、操作简单可控,制备的B4C/SiC纳米线复合材料结晶度好、形貌规则、尺寸均匀,具有良好的微波吸收性能。
Description
技术领域
本发明属于微波吸收材料技术领域,具体涉及一种B4C/SiC纳米线复合微波吸收材料。
背景技术
B4C的晶体结构为二十面体,构成B4C的C原子和B原子均属于非金属元素,而且原子半径小,所以两者形成了强共价键,使得B4C表现出了高熔点、高硬度、低密度、中子吸收性能等物理特性。与此同时,B4C材料在毫米波阶段的吸波性能已经得到实际运用(W.Bin,A.Bruschi.Absorbing coatings for high power millimeter-wave devices andmatched.Fusion Engineering and design[J].2013,2510-2514.)。研究表明,B4C块体材料可以通过2.45GHz微波辐射加热到2000℃,烧结密度为理论密度的95%。这项实验证明了B4C材料在2.45GHz的频率具有一定的吸波性能(J.D.Kate,R.D.Blake,J.J.Petrovic,H.Sheinberg.Microwave sintering of boron carbide[J].MRS Proceedings.1988,10(1557):124-219.)。然而,B4C材料在更宽微波频段下的吸收性能则鲜有报道。
近年来,一维无机纳米材料中的碳化物,如碳化硅、碳化硼等,由于其具有较强的量子尺寸效应,常常表现出比传统块体材料更好的力学、光学及电学性能,在构造纳米器件方面也具有很好的应用前景,受到了极大关注。如一维SiC纳米材料有着优异的介电性质,SiC纳米线的加入能够提高复合材料介电损耗能力,获得优异的吸波性能。一维B4C纳米材料具有比块体材料更为优良的力学性能,能够承受多次高应变弯曲循环试验,最高应变可达45%。单个纳米线在高应变弯曲循环下也表现出优异的阴极射线性质,证明了一维B4C纳米材料具有良好的电学性质(Yuan Huang,Fei Liu,Qiang Luo,Yuan Tian.Fabricationof patterned boron carbide nanowires and their electrical,filed emission,andflexibility properties.Nano Research[J].2012,Vol.5(12):896-902.)。然而,有关B4C纳米线的吸波性能未见报道。
目前已存在多种纳米线的制备方法,其中包括基于气-液-固生长机制的化学气相沉积法,基于氧化物辅助生长机理的热蒸发法,以及使用一维材料作为模板通过覆盖或替换制备纳米线的模板法。其中,模板法原料简单易得,工艺相对简单实用。
发明内容
本发明的目的是提供一种结晶度好、形貌规则、尺寸均匀、具有良好的微波吸收性能的B4C/SiC纳米线复合材料。
本发明的B4C/SiC纳米线复合微波吸收材料由下述方法制备得到:
以石墨或碳纳米管或脱脂棉作为碳源,硼粉为硼源,SiO2为硅源,硝酸铁或硝酸镍为催化剂,按照硼碳摩尔比为1:4、SiO2与碳的摩尔百分比为15%~55%、催化剂与碳的摩尔百分比为10%~15%,将原料充分依次加入无水乙醇中,超声0.5~2小时,加热搅拌直至干燥,然后将干燥产物在惰性气氛保护下1200~1400℃反应,得到B4C/SiC纳米线复合微波吸收材料。
上述制备方法中,优选SiO2与碳的摩尔百分比为30%~45%。
上述制备方法中,进一步优选将干燥产物在惰性气氛保护下1300℃反应2~3小时。
本发明复合微波吸收材料的纳米线长度为1~50μm,长径比为20~1000。
本发明的优点是:
(1)原料价格便宜,制备工艺简单,容易实现。
(2)所制备B4C/SiC纳米线复合微波吸收材料组分可调,显微结构均匀。
(3)所制备B4C/SiC纳米线复合微波吸收材料结晶度好、形貌规则、尺寸均匀。
(4)所B4C/SiC纳米线复合微波吸收材料在2GHz~18GHz的频率范围内具有良好的吸波性能。
附图说明
图1是实施例1制备的B4C/SiC纳米线复合微波吸收材料的SEM图。
图2是实施例4制备的B4C/SiC纳米线复合微波吸收材料的SEM图。
图3是对比例1制备的B4C纳米线(曲线a)以及实施例1(曲线b)和实施例4(曲线c)制备的B4C/SiC纳米线复合微波吸收材料的XRD图。
图4是对比例1制备的B4C纳米线不同厚度下的反射系数随频率变化曲线。
图5是实施例1制备的B4C/SiC纳米线复合微波吸收材料不同厚度下的反射系数随频率变化曲线。
图6是实施例4制备的B4C/SiC纳米线复合微波吸收材料不同厚度下的反射系数随频率变化曲线。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
按照硼碳摩尔比为1:4,SiO2相对于碳的摩尔百分比为16%,硝酸镍相对于碳的摩尔百分比为12%,将脱脂棉置于管式炉中,在氩气气氛中700℃煅烧3小时,得到碳纤维;将0.0780g(6.5mmol)碳纤维、0.2811g(26mmol)硼粉、0.0625g(1mmol)SiO2、0.1405g(0.8mmol)硝酸镍依次加入20mL无水乙醇中,超声0.5小时,加热搅拌直至干燥。将干燥后的粉体放在石墨模具中,置于管式炉中,在氩气气氛中1300℃加热2小时,得到B4C/SiC纳米线复合微波吸收材料(见图1),纳米线长度为5~10μm,长径比为50~125。
实施例2
按照硼碳摩尔比为1:4,SiO2相对于碳的摩尔百分比为16%,硝酸镍相对于碳的摩尔百分比为12%,将0.1200g(10.0mmol)粒径为100目的石墨、0.4324g(40.0mmol)硼粉、0.0961g(1.6mmol)SiO2、0.2162g(1.2mmol)硝酸镍依次加入30mL无水乙醇中,超声0.5小时,加热搅拌直至干燥。将干燥后的粉体放在石墨模具中,置于管式炉中,在氩气气氛中1300℃加热2小时,得到B4C/SiC纳米线复合微波吸收材料。
实施例3
本实施例中,用等摩尔碳纳米管替换实施例2中的石墨,其他步骤与实施例2相同,得到B4C/SiC纳米线复合微波吸收材料。
实施例4
按照硼碳摩尔比为1:4,SiO2相对于碳的摩尔百分比为36%,硝酸镍相对于碳的摩尔百分比为12%,将脱脂棉置于管式炉中,在氩气气氛中700℃煅烧3小时,得到碳纤维;将0.1536g(12.8mmol)碳纤维、0.5535g(5.12mmol)硼粉、0.2767g(4.6mmol)SiO2、0.2767g(1.5mmol)硝酸镍依次加入30mL无水乙醇中,超声0.5小时,加热搅拌直至干燥。将干燥后的粉体放在石墨模具中,置于管式炉中,在氩气气氛中1300℃加热2小时,得到B4C/SiC纳米线复合微波吸收材料(见图2),纳米线长度为10~30μm,长径比为100~600。
实施例5
按照硼碳摩尔比为1:4,SiO2相对于碳的摩尔百分比为36%,硝酸镍相对于碳的摩尔百分比为12%,将0.1200g(10.0mmol)粒径为100目的石墨、0.4324g(40.0mmol)硼粉、0.2162g(3.6mmol)SiO2、0.2162g(1.2mmol)硝酸镍依次加入20mL无水乙醇中,超声0.5小时,加热搅拌直至干燥。将干燥后的粉体放在石墨模具中,置于管式炉中,在氩气气氛中1300℃加热2小时,得到B4C/SiC纳米线复合微波吸收材料。
实施例6
本实施例中,用等摩尔碳纳米管替换实施例5中的石墨,其他步骤与实施例5相同,得到B4C/SiC纳米线复合微波吸收材料。
对比例1
按照硼碳摩尔比为1:4,SiO2相对于碳的摩尔百分比为4%,硝酸镍相对于碳的摩尔百分比为12%,将脱脂棉置于管式炉中,在氩气气氛中700℃煅烧3小时,得到碳纤维;将0.0810g(6.8mmol)碳纤维、0.2919g(27.0mmol)硼粉、0.0162g(0.3mmol)SiO2、0.1459g(0.8mmol)硝酸镍依次加入20mL无水乙醇中,超声0.5小时,加热搅拌直至干燥。将干燥后的粉体放在石墨模具中,置于管式炉中,在氩气气氛中1300℃加热3小时,得到B4C纳米线。
为了证明本发明的有益效果,发明人将实施例1和实施例4制备的B4C/SiC纳米线复合微波吸收材料以及对比例1制备的B4C纳米线分别与石蜡按质量比为4:6混合,制备成环状样品,采用矢量网络分析仪测试样品的微波电磁参数,并计算出在2GHz~18GHz的频率范围内不同匹配厚度下的反射损失,结果见图4~6。
由图4~6可见,对比例1制备的B4C纳米线的匹配厚度为5mm时,反射损失在7.3GHz处达到最小值-13.4dB,有效吸收带宽为1.65GHz。而本发明实施例1制备的B4C/SiC纳米线复合微波吸收材料的匹配厚度为4mm时,反射损失在9.01GHz处达到最小值-14.9dB,有效吸收带宽为2.34GHz,实施例4制备的B4C/SiC纳米线复合微波吸收材料的匹配厚度为3.3mm时,反射损失在11.8GHz处达到最小值-50.8dB,有效吸收带宽为3.12GHz。由此可见,本发明的B4C/SiC纳米线复合微波吸收材料相对于B4C纳米线,具有更强的微波吸收损耗,且具有更大的有效吸收带宽,其中实施例4制备的B4C/SiC纳米线复合微波吸收材料相对于对比例1制备的B4C纳米线,微波吸收损耗提高了近3倍,有效吸收带宽也提高了约1倍。
Claims (4)
1.一种B4C/SiC纳米线复合微波吸收材料,其特征在于该材料由下述方法制备得到:以石墨或碳纳米管或脱脂棉作为碳源,硼粉为硼源,SiO2为硅源,硝酸铁或硝酸镍为催化剂,按照硼碳摩尔比为1:4、SiO2与碳的摩尔百分比为15%~55%、催化剂与碳的摩尔百分比为10%~15%,将原料充分依次加入无水乙醇中,超声0.5~2小时,加热搅拌直至干燥,然后将干燥产物在惰性气氛保护下1200~1400℃反应,得到B4C/SiC纳米线复合微波吸收材料。
2.根据权利要求1所述的B4C/SiC纳米线复合微波吸收材料,其特征在于:所述SiO2与碳的摩尔百分比为30%~45%。
3.根据权利要求1所述的B4C/SiC纳米线复合微波吸收材料,其特征在于:将干燥产物在惰性气氛保护下1300℃反应2~3小时。
4.根据权利要求1~3任意一项所述的B4C/SiC纳米线复合微波吸收材料,其特征在于:所述复合微波吸收材料的纳米线长度为1~50μm,长径比为20~1000。
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