SiC包覆过渡金属纳米吸波材料的制备与研究
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摘要
本文采用等离子电弧法,通过改变阳极合金组成和成分、反应气体组成和比例以及控制电弧电流等手段,制备了Fe(χ-C-Fe-Si/SiC)纳米胶囊、Ni(SiC)纳米胶囊。利用X射线粉末衍射(XRD)、高分辨透射电镜(HRTEM)、X光电子能谱(XPS)等测试技术,系统研究了各种纳米胶囊的相组成、颗粒形貌、尺寸分布、微观组织结构以及其元素的价态以及聚集体的结构特征。利用振动样品磁强计(VSM)、网络矢量分析仪研究了所制备纳米胶囊的磁性质和电磁性能,并初步探讨了纳米胶囊具有优秀电磁吸收性能的物理机制。
结果表明,利用直流电弧法成功地制备了Fe(χ-C-Fe-Si/SiC)纳米胶囊。高分辨电镜显示所制备的粒子具有清晰的壳核结构,粒径尺寸分布在10-50nm左右,壳层厚度在4-8nm范围内。通过XPS光电子谱表面分析确定所制备纳米胶囊的核成分是由Fe组成,同时壳层是由χ-C-Fe-Si,SiC以及一小部分的SiOx,FeOx,C所组成。电磁测试表明,以Fe(χ-C-Fe-Si/SiC)纳米胶囊最大吸收峰值达-37.2dB,对应的涂层厚度为4.5mm,在3.14GHz-13.5GHz频率范围内,吸收率低于-20dB。
利用直流电弧法成功地制备了Ni(SiC)纳米胶囊,粒径尺寸分布在20-50nm,壳层厚度在4-8nm范围内。XRD及XPS光电子谱分析可以得到,所制备的样品是以Ni为内核,SiC/C为外壳的纳米胶囊。磁性研究表明,与块体金属Ni相比,纳米胶囊的饱和磁化强度减小,而矫顽力增加。利用实验所得到的电磁参数数据模拟Ni(SiC)纳米胶囊/固体石蜡复合材料在不同厚度的电磁损耗能力。当涂层厚度为3.5mm时,该纳米胶囊/固体石蜡复合材料在7.38GHz反射系数达到-33.4dB。在3.88GHz-10.9GHz频率范围反射系数均小于-20dB。而且随着厚度的增加,最大反射损耗移至低频段。
Fe(χ-C-Fe-Si/SiC) and Ni(SiC) nanocapsules were prepared by arc-discharging technique, by changing constitution and composition of the anode, constitution and ratio of the discharging atmosphere and the arc current magnitude. The phase constitution, particles morphologies, size distributions, microstructure and the binding energy of the elements of these different kinds of nanocapsules and the structure characteristics of the aggregates have been studied by means of X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) in details. The magnetic characteristics and electromagnetic (EM) properties of the nanocapsules were measured by Vibrating sample magnetism (VSM), network vector analyzer. The physical mechanism of the good EM absorption properties in these nanocapsules was discussed.
The result reveals Fe(χ-C-Fe-Si/SiC) nanocapsules were successfully prepared by arc discharge. HRTEM studies revealed the particles have a distinct shell/core structure, the size of the nanocapsules ranges from 10 to 50 nm and the thickness of shell is in 4-8nm. Based on X-ray photoelectron spectroscopy investigation, the core of the as-prepared nanocapsules is Fe, while the shell is mainly composed ofχ-C-Fe-Si and SiC as well as a small amount of SiOx, FeOx, C. The results of microwave absorbing capability indicated that the maximum reflection loss of Fe(χ-C-Fe-Si/SiC) nanocapsules reached -32.3dB with 4.5mm and the absorption is less than -20 dB in the range of 3.14-13.5GHz.
Ni(SiC) nanocapsules were successfully prepared by arc discharge, the size of which is 20-50 nm and the thickness is in 4-8nm. It is approved that the core is Ni and the shell is SiC/C measured by XRD and XPS photoelectron spectrum. Magnetism research shows that the saturation magnetization of nanocapsules decreases and the coercive force of nanocapsules increases, compared with pure bulk Ni. The reflection loss R(dB) of the nanocapsules were simulated with experimental date. The reflection loss R(dB) of the nanocapsules 3.5mm in thickness reaches to -33.4dB at 7.38GHz, and EM absorption properties (RL<-20dB) in the 3.88-10.9GHz range. In addition, the optimal RL obviously shifts to the lower-frequency range with increasing thickness of the layer.
结果表明,利用直流电弧法成功地制备了Fe(χ-C-Fe-Si/SiC)纳米胶囊。高分辨电镜显示所制备的粒子具有清晰的壳核结构,粒径尺寸分布在10-50nm左右,壳层厚度在4-8nm范围内。通过XPS光电子谱表面分析确定所制备纳米胶囊的核成分是由Fe组成,同时壳层是由χ-C-Fe-Si,SiC以及一小部分的SiOx,FeOx,C所组成。电磁测试表明,以Fe(χ-C-Fe-Si/SiC)纳米胶囊最大吸收峰值达-37.2dB,对应的涂层厚度为4.5mm,在3.14GHz-13.5GHz频率范围内,吸收率低于-20dB。
利用直流电弧法成功地制备了Ni(SiC)纳米胶囊,粒径尺寸分布在20-50nm,壳层厚度在4-8nm范围内。XRD及XPS光电子谱分析可以得到,所制备的样品是以Ni为内核,SiC/C为外壳的纳米胶囊。磁性研究表明,与块体金属Ni相比,纳米胶囊的饱和磁化强度减小,而矫顽力增加。利用实验所得到的电磁参数数据模拟Ni(SiC)纳米胶囊/固体石蜡复合材料在不同厚度的电磁损耗能力。当涂层厚度为3.5mm时,该纳米胶囊/固体石蜡复合材料在7.38GHz反射系数达到-33.4dB。在3.88GHz-10.9GHz频率范围反射系数均小于-20dB。而且随着厚度的增加,最大反射损耗移至低频段。
Fe(χ-C-Fe-Si/SiC) and Ni(SiC) nanocapsules were prepared by arc-discharging technique, by changing constitution and composition of the anode, constitution and ratio of the discharging atmosphere and the arc current magnitude. The phase constitution, particles morphologies, size distributions, microstructure and the binding energy of the elements of these different kinds of nanocapsules and the structure characteristics of the aggregates have been studied by means of X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS) in details. The magnetic characteristics and electromagnetic (EM) properties of the nanocapsules were measured by Vibrating sample magnetism (VSM), network vector analyzer. The physical mechanism of the good EM absorption properties in these nanocapsules was discussed.
The result reveals Fe(χ-C-Fe-Si/SiC) nanocapsules were successfully prepared by arc discharge. HRTEM studies revealed the particles have a distinct shell/core structure, the size of the nanocapsules ranges from 10 to 50 nm and the thickness of shell is in 4-8nm. Based on X-ray photoelectron spectroscopy investigation, the core of the as-prepared nanocapsules is Fe, while the shell is mainly composed ofχ-C-Fe-Si and SiC as well as a small amount of SiOx, FeOx, C. The results of microwave absorbing capability indicated that the maximum reflection loss of Fe(χ-C-Fe-Si/SiC) nanocapsules reached -32.3dB with 4.5mm and the absorption is less than -20 dB in the range of 3.14-13.5GHz.
Ni(SiC) nanocapsules were successfully prepared by arc discharge, the size of which is 20-50 nm and the thickness is in 4-8nm. It is approved that the core is Ni and the shell is SiC/C measured by XRD and XPS photoelectron spectrum. Magnetism research shows that the saturation magnetization of nanocapsules decreases and the coercive force of nanocapsules increases, compared with pure bulk Ni. The reflection loss R(dB) of the nanocapsules were simulated with experimental date. The reflection loss R(dB) of the nanocapsules 3.5mm in thickness reaches to -33.4dB at 7.38GHz, and EM absorption properties (RL<-20dB) in the 3.88-10.9GHz range. In addition, the optimal RL obviously shifts to the lower-frequency range with increasing thickness of the layer.
引文
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