熔融沉积成型Fe<sub>3</sub>O<sub>4</sub>-MWCNTs/PLA微波吸收材料性能

黄才华; 黄陈; 吴海华; 高琦; 叶喜葱

doi:10.13801/j.cnki.fhclxb.20230902.001

熔融沉积成型Fe₃O₄-MWCNTs/PLA微波吸收材料性能

doi: 10.13801/j.cnki.fhclxb.20230902.001

黄才华^{1, 2},
黄陈²,
吴海华^{1, 2, ,},
高琦²,
叶喜葱^{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: 湖北省技术创新专项重大项目(2019AAA164)−高性能石墨烯基材料制备关键技术研究

详细信息

通讯作者:
吴海华，博士，教授，博士生导师，研究方向为石墨/石墨烯3D打印及其应用技术　E-mail: wuhaihua@ctgu.edu.cn

中图分类号: TB333
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- 文章访问数: 488
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- 被引次数: 0
出版历程
- 收稿日期: 2023-05-29
- 修回日期: 2023-07-24
- 录用日期: 2023-08-24
- 网络出版日期: 2023-09-04
- 刊出日期: 2024-04-01

Properties of microwave absorbers formed by fused deposition modeling with Fe₃O₄-MWCNTs/PLA composite wire

HUANG Caihua^{1, 2},
HUANG Chen²,
WU Haihua^{1, 2
, ,},
GAO Qi²,
YE Xicong^{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: Major Technological Innovation Project of Hubei Science and Technology Department (2019AAA164)—Research on Key Technologies for the Preparation of High-performance Graphene-based Materials

摘要

摘要: 具有轻质高强、宽吸收带、薄厚度和热稳定性的电磁吸收材料是实现微波吸收应用的核心要求。本文以聚乳酸(PLA)为基体，Fe₃O₄和多壁碳纳米管(MWCNTs)为填料，通过球磨混合和熔融挤出法制备出Fe₃O₄-MWCNTs/PLA复合线材，利用熔融沉积成型(FDM)制备出Fe₃O₄-MWCNTs/PLA复合材料。采用XRD、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Fe₃O₄含量对复合材料吸波性能的影响。Fe₃O₄与MWCNTs-PLA复合形成的复合吸波材料质量轻、稳定性好、介电性能可调，因其良好的阻抗匹配和电磁波衰减能力而表现出优异的宽带吸收能力。实验结果表明：Fe₃O₄含量达到25wt%，厚度为1.4 mm时，反射损耗达到−48.5 dB，有效吸收带宽达到6.78 GHz (10.38~17.16 GHz)，表现出优异的微波吸收性能。
- 介电损耗 /
- 磁损耗 /
- Fe₃O₄ /
- 碳纳米管 /
- 阻抗匹配
Abstract: Electromagnetic absorbing materials with light weight, high strength, wide absorption band, thin thickness and thermal stability are the core requirements for microwave absorption applications. In this paper, Fe₃O₄-MWCNTs/PLA composite wires were prepared by ball milling mixing and melt extrusion using polylactic acid (PLA) as matrix, Fe₃O₄ and multi-walled carbon nanotubes (MWCNTs) as fillers, and Fe₃O₄-MWCNTs/PLA composites were prepared by melt deposition molding (FDM). The phase structure, microstructure and electromagnetic properties of the composites were characterized by XRD, SEM and vector network analyzer, respectively. The composite absorbing material of Fe₃O₄-MWCNTs/PLA has light weight, good stability, and adjustable dielectric properties, which exhibits excellent broadband absorption ability due to its good impedance matching and electromagnetic wave attenuation ability. The experimental results show that when the Fe₃O₄ content reaches 25wt% and the thickness is 1.4 mm, the reflection loss reaches −48.5 dB and the effective absorption bandwidth reaches 6.78 GHz (10.38-17.16 GHz), showing excellent microwave absorption performance.
- dielectric loss /
- magnetic loss /
- Fe₃O₄ /
- carbon nanotube /
- impedance matching

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图 1 Fe₃O₄-MWCNTs/PLA复合粉末的DSC曲线

Figure 1. DSC curves of Fe₃O₄-MWCNTs/PLA composite powders

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图 2 (a) Fe₃O₄-MWCNTs/PLA复合线材；(b) 同轴环；(c) 拉伸试样

Figure 2. (a) Fe₃O₄-MWCNTs/PLA composite filaments; (b) Coaxial rings; (c) Tensile specimen

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图 3 Fe₃O₄-MWCNTs/PLA复合材料的XRD图谱

Figure 3. XRD patterns of Fe₃O₄-MWCNTs/PLA composites

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图 4 MWCNTs/PLA和Fe₃O₄-MWCNTs/PLA复合材料的热重分析曲线

Figure 4. Thermogravimetric (TG) curves of MWCNTs/PLA and Fe₃O₄-MWCNTs/PLA composites

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图 5 不同Fe₃O₄含量的Fe₃O₄-MWCNTs/PLA复合材料SEM图像：(a) 6%MWCNTs/PLA；(b) 10%Fe₃O₄-6%MWCNTs/PLA；(c) 15%Fe₃O₄-6%MWCNTs/PLA；(d) 20%Fe₃O₄-6%MWCNTs/PLA；((e), (f)) 25%Fe₃O₄-6%MWCNTs/PLA

Figure 5. SEM images of Fe₃O₄-MWCNTs/PLA composites with different Fe₃O₄ contents: (a) 6%MWCNTs/PLA; (b) 10%Fe₃O₄-6%MWCNTs/PLA; (c) 15%Fe₃O₄-6%MWCNTs/PLA; (d) 20%Fe₃O₄-6%MWCNTs/PLA; ((e), (f)) 25%Fe₃O₄-6%MWCNTs/PLA

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图 6 Fe₃O₄-MWCNTs/PLA复合材料的应力-应变柱状图

Figure 6. Stress-strain histogram of Fe₃O₄-MWCNTs/PLA composites

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图 7 Fe₃O₄-MWCNTs/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 7. Electromagnetic parameters of Fe₃O₄-MWCNTs/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 8 Fe₃O₄-MWCNTs/PLA复合材料的Colo-Colo曲线

Figure 8. Colo-Colo curves of Fe₃O₄-MWCNTs/PLA composites

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图 9 Fe₃O₄-MWCNTs/PLA复合材料的涡流值C₀

Figure 9. Eddy current data C₀ of Fe₃O₄-MWCNTs/PLA composites

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图 10 6%MWCNTs/PLA ((a), (a1))、10%Fe₃O₄-6%MWCNTs/PLA ((b), (b1))、15%Fe₃O₄-6%MWCNTs/PLA ((c), (c1))、20%Fe₃O₄-6%MWCNTs/PLA ((d), (d1))和25%Fe₃O₄-6%MWCNTs/PLA ((e), (e1))的反射损耗曲线图与3D颜色映射曲面图

Figure 10. Reflection loss curves and 3D color mapping surfaces of 6%MWCNTs/PLA ((a), (a1)), 10%Fe₃O₄-6%MWCNTs/PLA ((b), (b1)), 15%Fe₃O₄-6%MWCNTs/PLA ((c), (c1)), 20%Fe₃O₄-6%MWCNTs/PLA ((d), (d1)), 25%Fe₃O₄-6%MWCNTs/PLA ((e), (e1))

L_{R, min}—Minimal reflection loss; d—Thickness; EAB—Effective absorption bandwidth

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图 11 (a) 复合材料厚度为1.4 mm时的阻抗匹配特性；(b) Fe₃O₄-MWCNTs/PLA复合材料的衰减系数

Figure 11. (a) Impedance matching characteristics for the composites with the thickness of 1.4 mm; (b) Attenuation constants of Fe₃O₄-MWCNTs/PLA composites

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图 12 25%Fe₃O₄-6%MWCNTs/PLA的1/4波长(λ)模型

Figure 12. 1/4 wave length (λ) model of 25%Fe₃O₄-6%MWCNTs/PLA

t_m—Thickness between 1/4 and 3/4 wave length

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表 1 Fe₃O₄-多壁碳纳米管(MWCNTs)/聚乳酸(PLA)复合材料的成分

Table 1. Ingredients of Fe₃O₄-multi-walled carbon nanotubes (MWCNTs)/polylactic acid (PLA) composites

Sample	Mass fraction/wt%
Sample	PLA	MWCNTs	Fe₃O₄
6%MWCNTs/PLA	94	6	0
10%Fe₃O₄-6%MWCNTs/PLA	84	6	10
15%Fe₃O₄-6%MWCNTs/PLA	79	6	15
20%Fe₃O₄-6%MWCNTs/PLA	74	6	20
25%Fe₃O₄-6%MWCNTs/PLA	69	6	25

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表 2 Fe₃O₄-MWCNTs/PLA复合粉末DSC曲线对应的数据

Table 2. DSC data of Fe₃O₄-MWCNTs/PLA composite powders

Sample	T_m/℃	T_c/℃	T_g/℃
6%MWCNTs/PLA	113.2	98.88	86.48
10%Fe₃O₄-6%MWCNTs/PLA 15%Fe₃O₄-6%MWCNTs/PLA 20%Fe₃O₄-6%MWCNTs/PLA 25%Fe₃O₄-6%MWCNTs/PLA	112.6 112.8 112.7 112.7	98.47 98.37 98.34 98.37	85.67 85.68 85.65 85.45
Notes: T_m—Melting temperature; T_c—Crystallization temperature; T_g—Glass transition temperature.

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表 3 近3年文献中报道的Fe₃O₄复合材料与本文制备的复合材料吸波性能对比

Table 3. Comparison of the absorbing properties of Fe₃O₄ composites reported in the literature in the past three years and the composites prepared in this paper

Material	Loading/wt%	Matrix	L_{R, min}/dB (Thickness)	EAB/GHz	Ref.
Fe₃O₄@f-GNPs RGO-Fe₃O₄ CF/Fe₃O₄ Fe₃O₄/MDCF Palygorskite/Fe₃O₄ Fe₃O₄@Ti₃C₂T_x/CNTs Fe₃O₄/RGO@PANI Fe₃O₄@RGO Fe₃O₄@2H-MoS₂ ZnO/Fe₃O₄ 25%Fe₃O₄-6%MWCNTs/PLA	70 35 50 70 50 20 60 60 60 70 31	Paraffin Paraffin Paraffin Paraffin Paraffin Paraffin Paraffin Paraffin Paraffin Paraffin PLA	−25.00 (2 mm) −34.40 (1.6 mm) −19.00 (1.5 mm) −26.45 (5 mm) −40.41 (5.9 mm) −40.01 (2 mm) −46.49 (2.5 mm) −49.40 (1.75 mm) −50.00 (1.9 mm) −51.10 (2.2 mm) −48.50 (1.4 mm)	2.40 3.80 4.80 4.28 4.80 5.80 4.25 3.96 4.20 5.28 6.78	[34] [33] [35] [36] [38] [39] [40] [43] [47] [49] This work
Notes: EAB—Effective absorption bandwidth (L_{R, min}≤−10 dB); f-GNPs—Graphene nanosheets; RGO—Graphene; CF—Foamed carbon; MDCF—Reticulated foam carbon; CNTs—Carbon nanotubes; PANI—Polyaniline.

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