低密度Fe3O4/中孔炭微球复合材料的可规模制备及吸波性能

doi:10.15541/jim20160689

摘要/Abstract

摘要：

采用喷雾干燥法制备出中孔炭微球(MCMSs), 进一步通过液相浸渍得到磁性Fe₃O₄/MCMSs纳米复合材料, 系统研究了复合材料的形貌结构和吸波性能。结果发现, Fe₃O₄/MCMSs复合材料具有优异的流动性和低密度(0.24~0.33 g/cm³)特征, 其中Fe₃O₄纳米颗粒高度分散在MCMSs中孔孔道内。复合材料具有较高的比表面积(548~735 m²/g), 可以促进多种介电弛豫的形成。在2~18 GHz范围内, 复合材料以介电损耗为主, 在12.6 GHz处具有最大反射率-25 dB, 小于-10 dB的带宽达4.7 GHz。复合材料优异的吸波性能可以归因于均相分布的Fe₃O₄纳米颗粒和中孔炭微球的协同作用, 在增大界面弛豫和电磁波散射的同时, 改善了阻抗匹配, 减少了电磁波在吸波层表面的反射。

关键词: 复合材料, 中孔炭微球, 四氧化三铁, 吸波性能

Abstract:

Fe₃O₄/mesoporous carbon microspheres (MCMSs) composites were prepared by a facile wet-impregnation method using spray-drying produced MCMSs as carbon substrates. The structure, morphology and microwave absorbing performance were investigated. Results indicate that the composites have good fluidity and low bulk density of 0.24- 0.33 g/m³. The Fe₃O₄nanoparticles are homogeneously dispersed in the mesoporous channels without blocking the porosity of MCMSs. The resulting Fe₃O₄/MCMSs composites have very high BET surface areas of 548-735 m²/g, which promote multiple relaxations. In the frequency range of 2-18 GHz, the microwave loss is primarily derived from dielectric loss. The composite with 40wt% Fe₃O₄ exhibits a maximum reflection loss of -25 dB at 12.6 GHz and a broad absorption band over 4.7 GHz. Such good microwave electromagnetic performances can be ascribed to the synergistic effects of highly dispersed Fe₃O₄nanoparticles and mesoporous channels, which can increase interfacial relaxation and microwave diffraction as well as reduce the reflection of microwave at the interface between air and absorber.

Key words: composites, mesoporous carbon microspheres, ferrites, microwave absorption properties

中图分类号:

TM25

刘克, 王际童, 龙东辉, 凌立成. 低密度Fe₃O₄/中孔炭微球复合材料的可规模制备及吸波性能[J]. 无机材料学报, 2017, 32(10): 1023-1028.

LIU Ke, WANG Ji-Tong, LONG Dong-Hui, LING Li-Cheng. Scalable Preparation and Microwave Absorption of Lightweight Fe₃O₄/Mesoporous Carbon Microsphere Composites[J]. Journal of Inorganic Materials, 2017, 32(10): 1023-1028.

图/表 7

图1 Fe3O4/MCMSs复合材料的热重曲线和XRD图谱

Fig. 1 (a) TG curves and (b) XRD patterns of Fe3O4/MCMSs composites

图2 40%-Fe3O4-MCMSs的SEM, TEM和SEM Mapping照片

Fig. 2 (a) SEM , (b), (c) TEM and (e)-(f) SEM mapping images of 40%-Fe3O4-MCMSs

图3 MCMSs和Fe3O4/MCMSs复合材料的氮气吸脱附等温线和孔径分布图

Fig. 3 (a) Nitrogen adsorption-desorption isotherms and (b) BJH pore size distributions of MCMSs and Fe3O4/MCMSs composites

表1 MCMSs和Fe3O4/MCMSs复合材料的孔结构参数

Table 1 Structure parameters of MCMSs and Fe3O4/MCMSs magnetic composites

Sample	S_BET^a/ (m²·g^-1)	V_total^b/ (cm³·g^-1)	Pore size /nm	Tap density /(g·m^-3)
MCMSs	1221	2.4	8.1	0.18
20%-Fe₃O₄-MCMSs	735	1.8	8.1	0.24
40%-Fe₃O₄-MCMSs	548	1.1	8.1	0.33

图4 Fe3O4/MCMSs复合材料在室温下的磁滞回线及低磁化场下的放大图

Fig. 4 Magnetic hysteresis loops at room temperature of Fe3O4/MCMSs composites. Inset is low field hysteresis curves

图5 MCMSs和Fe3O4/MCMSs复合材料的复介电常数, 复磁导率及对应磁损耗因子

Fig. 5 Permittivity, permeability and loss tangent of MCMSs and Fe3O4/MCMSs composites

图6 MCMSs和Fe3O4/MCMSs复合材料的反射率曲线

Fig.6 RL curves of (a) MCMSs, (b)20%-Fe3O4-MCMSs and (c) 40%-Fe3O4-MCMSs at different thickness (1-5 nm)

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低密度Fe₃O₄/中孔炭微球复合材料的可规模制备及吸波性能

Scalable Preparation and Microwave Absorption of Lightweight Fe₃O₄/Mesoporous Carbon Microsphere Composites

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