石墨烯增强FeSiAl-MoS<sub>2</sub>/PLA复合材料吸波性能

叶喜葱; 杨超; 欧阳宾; 高琦; 吴海华; 何恩义; 叶永盛

doi:10.13801/j.cnki.fhclxb.20220415.004

石墨烯增强FeSiAl-MoS₂/PLA复合材料吸波性能

doi: 10.13801/j.cnki.fhclxb.20220415.004

叶喜葱^{1, 2, ,},
杨超²,
欧阳宾²,
高琦²,
吴海华^{1, 2},
何恩义^{1, 2},
叶永盛^{1, 2}

1.
三峡大学　石墨增材制造技术与装备湖北省工程研究中心，宜昌 443002
2.
三峡大学　机械与动力学院，宜昌 443002

基金项目: 国家自然科学基金(51575313)；三峡大学石墨增材制造技术与装备湖北省工程研究中心开放基金(HRCGAM202101)

详细信息

通讯作者:
叶喜葱，博士，教授，硕士生导师，研究方向为先进材料成形制造 E-mail: yexc@ctgu.edu.cn

中图分类号: TB333
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出版历程
- 收稿日期: 2022-01-14
- 修回日期: 2022-04-02
- 录用日期: 2022-04-06
- 网络出版日期: 2022-04-19
- 刊出日期: 2023-02-01

Graphene-enhanced electromagnetic wave absorbing properties of FeSiAl-MoS₂/PLA composites

YE Xicong^{1, 2
, ,},
YANG Chao²,
OUYANG Bin²,
GAO Qi²,
WU Haihua^{1, 2},
HE Enyi^{1, 2},
YE Yongsheng^{1, 2}

1.
Hubei Engineering Research Center for Graphite Additive Manufacturing Technology and Equipment, China Three Gorges University, Yichang 443002, China
2.
College of Mechanical & Power Engineering, China Three Gorges University, Yichang 443002, China

Funds: National Natural Science Foundation of China (51575313); Open Fund of Hubei Engineering Research Center for Graphite Additive Manufacturing Technology and Equipment of China Three Gorges University (HRCGAM202101)

摘要

摘要: 多元材料复合是制备轻质、宽频和强吸收吸波材料的有效方法。以聚乳酸(PLA)为基体，FeSiAl、MoS₂和石墨烯(GN)为填料，通过球磨和熔融挤出两步法制备了可用于熔融沉积成形(FDM)的FeSiAl-MoS₂-GN/PLA复合材料。采用XRD、拉曼光谱、SEM和矢量网络分析仪分别对复合材料的物相结构、微观形貌和电磁特性进行了表征，并研究了石墨烯含量对复合材料吸波性能的影响。研究表明：石墨烯、FeSiAl和MoS₂随机分散在PLA基体中，形成了复杂的导电网络；多元材料复合构筑了丰富的介电/磁异质界面，有利于促进界面极化；当石墨烯含量增加时，复合材料的吸波性能随之增强，当石墨烯含量为5wt%时，复合材料的吸波性能最佳，在厚度为1.7 mm时最小反射损耗为−27.90 dB，在厚度为1.9 mm时有效吸收带宽为4.96 GHz(12.64~17.60 GHz)。其优异的吸波性能归因于良好的阻抗匹配及介电损耗和磁损耗之间的协同作用。
- 复合材料 /
- FeSiAl /
- MoS₂ /
- 石墨烯 /
- 阻抗匹配 /
- 吸波性能
Abstract: Multi-material composite is an effective method to prepare light-weight, broadband and strong absorbing materials. In this paper, polylactic acid (PLA) was used as the matrix material, and FeSiAl, MoS₂ and graphene (GN) were used as fillers. FeSiAl-MoS₂-GN/PLA composites, which were used for fused deposition modeling (FDM), prepared by the two-step process of ball milling and melt extrusion. The phase structure, microscopic morphology and electromagnetic properties of composites were characterized by XRD, Raman spectroscopy, SEM and vector network analyzer, respectively. And the effect of graphene content on the electromagnetic wave absorbing properties of composites was also investigated. The research shows that graphene, FeSiAl and MoS₂ are randomly dispersed in the PLA matrix and form a complex conductive network; Multi-material composites build rich dielectric/magnetic heterointerfaces, which are beneficial to promote interface polarization; The higher the graphene content, the stronger the electromagnetic wave absorbing properties of composites; When the graphene content is 5wt%, the minimum reflection loss is −27.90 dB at a thickness of 1.7 mm, and the effective absorption bandwidth is 4.96 GHz (12.64-17.60 GHz) at a thickness of 1.9 mm. Its excellent absorbing properties are attributed to the perfect impedance matching and the synergy between dielectric and magnetic losses.
- composites /
- FeSiAl /
- MoS₂ /
- graphene /
- impedance matching /
- electromagnetic wave absorbing pro-perties

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图 1 FeSiAl的物理性能：(a) 粒径分布；(b) 磁滞回线

D_v(50)—Particle size at 50vol% volume fraction; M_S—Saturation magnetization; M_r—Residual magnetization; H_C—Coercivity

Figure 1. Physical properties of FeSiAl: (a) Particle size distribution; (b) Hysteresis loop

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图 2 复合粉末的堆积密度

Figure 2. Bulk density of composite powders

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图 3 (a) FeSiAl-MoS₂-GN/PLA复合线材；(b)测试用同轴环

Figure 3. (a) FeSiAl-MoS₂-GN/PLA composite filaments; (b) Coaxial rings for testing

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图 4 FeSiAl-MoS₂/PLA复合材料的反射损耗曲线：(a) 26%FeSiAl-4%MoS₂/PLA；(b) 22%FeSiAl-8%MoS₂/PLA；(c) 18%FeSiAl-12%MoS₂/PLA

Figure 4. Reflection loss curves of FeSiAl-MoS₂/PLA composites: (a) 26%FeSiAl-4%MoS₂/PLA; (b) 22%FeSiAl-8%MoS₂/PLA; (c) 18%FeSiAl-12%MoS₂/PLA

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图 5 FeSiAl-MoS₂-GN/PLA复合材料的结构表征：(a) XRD图谱；(b) Raman光谱

I_D/I_G—Intensity ratio of D peak and G peak

Figure 5. Structural characterizations of FeSiAl-MoS₂-GN/PLA composites: (a) XRD patterns; (b) Raman spectra

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图 6 3种吸波剂的SEM图像：(a) FeSiAl；(b) MoS₂；(c) 石墨烯

Figure 6. SEM images of 3 absorbers: (a) FeSiAl; (b) MoS₂; (c) Graphene

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图 7 FeSiAl-MoS₂-GN/PLA复合材料的SEM图像：(a) 22%FeSiAl-8%MoS₂/PLA；(b) 22%FeSiAl-8%MoS₂-3%GN/PLA；(c) 22%FeSiAl-8%MoS₂-4%GN/PLA；(d) 22%FeSiAl-8%MoS₂-5%GN/PLA；((e), (f)) 22%FeSiAl-8%MoS₂-5%GN/PLA的EDS图谱

Figure 7. SEM images of FeSiAl-MoS₂-GN/PLA composites: (a) 22%FeSiAl-8%MoS₂/PLA; (b) 22%FeSiAl-8%MoS₂-3%GN/PLA; (c) 22%FeSiAl-8%MoS₂-4%GN/PLA; (d) 22%FeSiAl-8%MoS₂-5%GN/PLA; ((e), (f)) EDS mapping of 22%FeSiAl-8%MoS₂-5%GN/PLA

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图 8 FeSiAl-MoS₂-GN/PLA复合材料的电磁参数：(a)复介电常数实部；(b)复介电常数虚部；(c)介电损耗角正切；(d)复磁导率实部；(e)复磁导率虚部；(f)磁损耗角正切

Figure 8. Electromagnetic parameters of FeSiAl-MoS₂-GN/PLA composites: (a) Real part of complex permittivity; (b) Imaginary part of complex permittivity; (c) Dielectric loss tangent; (d) Real part of complex permeability; (e) Imaginary part of complex permeability; (f) Magnetic loss tangent

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图 9 FeSiAl-MoS₂-GN/PLA复合材料的反射损耗曲线图与3D颜色映射曲面图：((a), (b)) 22%FeSiAl-8%MoS₂/PLA；((c), (d)) 22%FeSiAl-8%MoS₂-3%GN/PLA；((e), (f)) 22%FeSiAl-8%MoS₂-4%GN/PLA；((g), (h)) 22%FeSiAl-8%MoS₂-5%GN/PLA

R_Lmin—Minimum reflection loss; EAB—Effective absorption bandwidth; d—Thickness

Figure 9. Reflection loss curves and 3D color mapping surfaces of FeSiAl-MoS₂-GN/PLA composites: ((a), (b)) 22%FeSiAl-8%MoS₂/PLA; ((c), (d)) 22%FeSiAl-8%MoS₂-3%GN/PLA; ((e), (f)) 22%FeSiAl-8%MoS₂-4%GN/PLA; ((g), (h)) 22%FeSiAl-8%MoS₂-5%GN/PLA

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图 10 22%FeSiAl-8%MoS₂-5%GN/PLA在不同厚度时的有效吸收带宽

Figure 10. Effective absorption bandwidth of 22%FeSiAl-8%MoS₂-5%GN/PLA composite material in different thicknesses

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图 11 本文中吸波材料与文献中填充量相近的吸波材料吸波性能对比^[40-48]

Figure 11. Comparison of the absorbing properties of the absorbing material in this paper with the absorbing materials with similar filling amount in other literatures^[40-48]

RGO—Reduced graphene oxide; BNSF—BaNd_0.2Sm_0.2Fe_11.6O₁₉; ZNCF—Co-doped ZnNi ferrite; PANI—Polyaniline; CNT—Carbon nanotubes; WPC/MNPs—Porous carbon/magnetic nanoparticles composite

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图 12 FeSiAl-MoS₂-GN/PLA复合材料厚度为2.0 mm时的阻抗匹配特性(a)和衰减常数(b)；(c) 22%FeSiAl-8%MoS₂-5%GN/PLA复合材料的反射损耗、阻抗匹配和衰减常数的对应关系图

Figure 12. Impedance matching characteristics in the 2.0 mm (a) and attenuation constants (b) of FeSiAl-MoS₂-GN/PLA composites; (c) Correspondence diagram of reflection loss, impedance matching and attenuation constant of 22%FeSiAl-8%MoS₂-5%GN/PLA composite

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图 13 FeSiAl-MoS₂-GN/PLA复合材料的Cole-Cole曲线：(a) 22%FeSiAl-8%MoS₂/PLA；(b) 22%FeSiAl-8%MoS₂-3%GN/PLA；(c) 22%FeSiAl-8%MoS₂-4%GN/PLA；(d) 22%FeSiAl-8%MoS₂-5%GN/PLA

Figure 13. Cole-Cole curves of FeSiAl-MoS₂-GN/PLA composites: (a) 22%FeSiAl-8%MoS₂/PLA; (b) 22%FeSiAl-8%MoS₂-3%GN/PLA; (c) 22%FeSiAl-8%MoS₂-4%GN/PLA; (d) 22%FeSiAl-8%MoS₂-5%GN/PLA

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图 14 FeSiAl-MoS₂-GN/PLA复合材料的电导率

Figure 14. Conductivity of FeSiAl-MoS₂-GN/PLA composites

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图 15 (a) FeSiAl-MoS₂-GN/PLA复合材料的涡流(C₀)值；(b) 22%FeSiAl-8%MoS₂-5%GN/PLA的四分之一波长模型

Figure 15. (a) Eddy currents (C₀) values of FeSiAl-MoS₂-GN/PLA composites; (b) Quarter-wavelength model of 22%FeSiAl-8%MoS₂-5%GN/PLA composite

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图 16 FeSiAl-MoS₂-GN/PLA复合材料中的电磁波衰减过程示意图

R—Resistance

Figure 16. Schematic illustration of the electromagnetic wave attenuation process in the FeSiAl-MoS₂-GN/PLA composites

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表 1 FeSiAl-MoS₂-GN/聚乳酸(PLA)复合材料的成分

Table 1. Ingredients of FeSiAl-MoS₂-GN/polylactic acid (PLA) composites

Sample	Mass fraction/wt%
Sample	GN	FeSiAl	MoS₂	PLA
26%FeSiAl-4%MoS₂/PLA	0	26	4	70
22%FeSiAl-8%MoS₂/PLA	0	22	8	70
18%FeSiAl-12%MoS₂/PLA	0	18	12	70
22%FeSiAl-8%MoS₂-3%GN/PLA	3	22	8	67
22%FeSiAl-8%MoS₂-4%GN/PLA	4	22	8	66
22%FeSiAl-8%MoS₂-5%GN/PLA	5	22	8	65
Note: GN—Graphene.

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表 2 近五年文献中报道的FeSiAl复合材料与本文制备的复合材料吸波性能对比

Table 2. Comparison of the absorbing properties of FeSiAl composites reported in the literature in the past five years and the composites prepared in this paper

Materials	Loading/wt%	Matrix	R_L_min (Thickness)	EAB/GHz	Ref.
FeSiAl/nitrides	50	Paraffin	−34.50 dB (2.50 mm)	8.11	[5]
FeSiAl/MgO	80	Paraffin	−33.00 dB (1.50 mm)	4.93	[6]
FeSiAl@SiO₂	80	Paraffin	−21.40 dB (2.10 mm)	3.80	[7]
FeSiAl@SiO₂@C	80	Paraffin	−46.75 dB (3.50 mm)	7.73	[9]
FeSiAl hollow microspheres	60	Paraffin	−22.10 dB (5.00 mm)	3.30	[30]
FeSiAl@C	50	Paraffin	−15.68 dB (4.00 mm)	2.00	[31]
FeSiAl/rGO/Al₂O₃	5	Al₂O₃	−35.42 dB (1.40 mm)	1.12	[32]
FeSiAl/MnZnFe₂O₄	80	Paraffin	−16.50 dB (1.50 mm)	4.60	[33]
Flaky FeSiAl/MnZnFe₂O₄	80	Paraffin	−24.30 dB (1.50 mm)	3.60	[34]
Flakey FeSiAl/NiZnFe₂O₄	60	Paraffin	−29.20 dB (2.50 mm)	4.00	[35]
FeSiAl/ZnO/epoxy resin	55	Epoxy	−40.50 dB (2.20 mm)	3.50	[36]
FeSiAl@ZnO₂@Al₂O₃	80	Paraffin	−50.60 dB (3.72 mm)	1.50	[37]
FeSiAl@SiO₂@PUA	80	Paraffin	−49.00 dB (4.50 mm)	7.80	[38]
FeSiAl@Al₂O₃@SiO₂	80	Paraffin	−46.29 dB (2.50 mm)	7.33	[39]
22%FeSiAl-8%MoS₂-4%GN/PLA	34	PLA	−15.24 dB (1.60 mm)	3.12	This work
22%FeSiAl-8%MoS₂-5%GN/PLA	35	PLA	−27.90 dB (1.70 mm)	4.96	This work
Notes: EAB—Effective absorption bandwidth (R_L≤–10 dB); PUA—Polyurethane-acrylic; GN—Graphene, rGO—Reduced graphene oxide.

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