石墨烯-铁镍合金-聚乳酸复合材料的制备及其吸波性能

胡正浪; 吴海华; 杨增辉; 姜建堂; 周建新

doi:10.13801/j.cnki.fhclxb.20210903.004

石墨烯-铁镍合金-聚乳酸复合材料的制备及其吸波性能

胡正浪^{1, 2},
吴海华^{1, 2, ,},
杨增辉^{1, 2},
姜建堂³,
周建新⁴

1.
三峡大学　机械与动力学院，宜昌 443002
2.
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
3.
哈尔滨工业大学　材料科学与工程学院，哈尔滨 150001
4.
华中科技大学　材料成形与模具技术国家重点实验室，武汉 430074

基金项目: 国家自然科学基金(51575313)；华中科技大学材料成形与模具技术国家重点实验室开放课题研究基金(P2020-003)

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3D打印吸波材料及其工程应用技术　E-mail: wuhaihua@ctgu.edu.cn

中图分类号: TB34；TP391.73
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出版历程
- 收稿日期: 2021-07-12
- 修回日期: 2021-08-09
- 录用日期: 2021-08-16
- 网络出版日期: 2021-09-02
- 刊出日期: 2022-07-29

Preparation of graphene-iron-nickel alloy-polylactic acid composites and their microwave absorption properties

HU Zhenglang^{1, 2},
WU Haihua^{1, 2, ,},
YANG Zenghui^{1, 2},
JIANG Jiantang³,
ZHOU Jianxin⁴

1.
College of Mechanical and Power Engineering, China Three Gorges University, Yichang 443002, China
2.
Hubei Engineering Research Center for Graphite Additive Manufacturing Technology and Equipment, China Three Gorges University, Yichang 443002, China
3.
School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001, China
4.
State Key Laboratory of Material Processing and Die & Mould Technology, Huazhong University of Science and Technology, Wuhan 430074, China

摘要

摘要: 发展轻量化、宽频带的微波吸收材料来应对严重的电磁污染是一个巨大的挑战。本文通过熔融沉积成形(FDM)工艺制备出石墨烯(GR)-铁镍合金(FeNi50)-聚乳酸(PLA)复合材料，采用XRD、Raman、SEM和矢量网络分析仪(VNA)对复合材料的物相结构、微观形貌和电磁性能进行表征分析，并讨论了GR-FeNi50质量比对复合材料吸波性能的影响。结果表明，与未添加GR的复合材料相比，复合材料内部形成了触发极化损耗的异质界面，并产生了丰富的褶皱和孔隙，从而增强了微波的多次反射和散射；随着GR-FeNi50质量比的增加，吸波性能先增强、后减弱，当GR-FeNi50质量比为4∶20时，吸波性能最佳，最小反射损耗达到−40.5 dB，有效吸收带宽为4.7 GHz(13.28~18 GHz)。其优异的吸波性能归因于良好的阻抗匹配和界面极化损耗、偶极极化损耗、电导损耗、磁损耗之间的协同作用。此外，与湿化学法制备的吸波材料相比，GR-FeNi50-PLA复合材料在环保、易加工和规模化生产方面具有优势。
- 复合材料 /
- 介电损耗 /
- 磁损耗 /
- 微波吸收 /
- 阻抗匹配 /
- 吸波材料
Abstract: The development of lightweight, broadband microwave absorbing materials to cope with severe electromagnetic pollution is a great challenge. In this paper, graphene (GR)-iron-nickel alloy (FeNi50)-polylactic acid (PLA) composites were prepared by fused deposition modeling (FDM) process, and the physical structure, micromorphology and electromagnetic properties of the composites were characterized by XRD, Raman, SEM and vector network analyzer (VNA). The effects of the GR-FeNi50 mass ratio on the microwave absorption properties of the composites were discussed. The results show that, compared with the composites without GR addition, heterogeneous interfaces triggering polarization loss are formed inside the composites, and abundant folds and pores are generated, which enhance the multiple reflections and scattering of microwaves. The minimum reflection loss reaches −40.5 dB and the effective absorption bandwidth is 4.7 GHz (13.28-18 GHz). The excellent absorption performance is attributed to the good impedance matching and the synergy between interfacial polarisation loss, dipole polarisation loss, conductivity loss and magnetic loss. In addition, the GR-FeNi50-PLA composite has advantages in terms of environmental friendliness, ease of processing and scale production compared to the absorbing materials prepared by wet chemical methods.
- composites /
- dielectric loss /
- magnetic loss /
- microwave absorption /
- impedance matching /
- absorbing materials

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图 1 石墨烯(GR)的SEM (a) 和TEM (b) 图像；铁镍合金(FeNi50) (c) 和聚乳酸(PLA) (d) 的SEM图像

Figure 1. SEM image (a) and TEM image (b) of graphene (GR); SEM images of Fe-Ni alloy (FeNi50) (c) and polylactic acid (PLA) (d)

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图 2 (a) GR的N₂吸附-脱附等温线；(b) PLA的TG和DSC曲线

Figure 2. (a) N₂ adsorption-desorption isothermals of GR; (b) TG and DSC curves of PLA

S_g—Specific surface area of the tested sample; v_m—Saturated adsorption capacity of N₂ molecule monolayer in standard state; T_m—Melting temperature; T_d—Decomposition temperature

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图 3 (a) GR-FeNi50-PLA复合粉末；(b) GR-FeNi50-PLA复合线材；(c) 测试用的同轴环

Figure 3. (a) GR-FeNi50-PLA composite powders; (b) GR-FeNi50-PLA composite filaments; (c) Coaxial rings of testing

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图 4 不同GR质量分数GR-FeNi50-PLA复合材料的XRD图谱

Figure 4. XRD patterns of GR-FeNi50-PLA composites with different GR mass fraction

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图 5 不同GR质量分数GR-FeNi50-PLA复合材料的拉曼光谱

Figure 5. Raman spectra of GR-FeNi50-PLA composites with different GR mass fraction

I_D/I_G—Intensity ratio of the D band to the G band

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图 6 不同GR-FeNi50质量比GR-FeNi50-PLA复合材料的SEM图像

Figure 6. SEM images of GR-FeNi50-PLA composites with different GR-FeNi50 mass ratio

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图 7 6个不同GR-FeNi50质量比同轴环的电磁参数：在2~18 GHz频率范围内，复介电常数的实部(a)、虚部(b)和介电损耗角正切(c)；复磁导率的实部(d)、虚部(e)和磁损耗角正切(f)

Figure 7. Electromagnetic parameters of six coaxial rings with different GR-FeNi50 mass ratio: Real part (a), imaginary part (b); tangent dielectric loss (c) of the complex permittivity; Real part (d), imaginary part (e), tangent magnetic loss (f) of the complex permeability in the frequency range of 2–18 GHz

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图 8 不同GR-FeNi50质量比GR-FeNi50-PLA复合材料的的Cole–Cole曲线

Figure 8. Cole–Cole curves of GR-FeNi50-PLA composites with different GR-FeNi50 mass ratios

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图 9 不同GR-FeNi50质量比GR-FeNi50-PLA复合材料的的电导率

Figure 9. Conductivity of GR-FeNi50-PLA composites with different GR-FeNi50 mass ratios

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图 10 GR-FeNi50-PLA复合材料的电磁损耗机制示意图

Figure 10. Schematic illustration of electromagnetic loss mechanism of GR-FeNi50-PLA composites

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图 11 不同GR-FeNi50质量比GR-FeNi50-PLA复合材料的 $\mu ''{(\mu \prime )}^{-2}{f}^{-1}$ 计算值

Figure 11. Calculated $\mu ''{(\mu \prime )}^{-2}{f}^{-1}$ for GR-FeNi50-PLA composites with different GR-FeNi50 mass ratios

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图 12 0wt GR-FeNi50-PLA (a)、 1wt%GR-FeNi50-PLA (b)、 2wt%GR-FeNi50-PLA (c)、3wt%GR-FeNi50-PLA (d)、4wt%GR-FeNi50-PLA (e) 和5wt%GR-FeNi50-PLA (f) 的反射损耗三维图和吸波曲线

Figure 12. 3D maps of reflection loss and microwave absorption curves of 0wt%GR-FeNi50-PLA (a), 1wt%GR-FeNi50-PLA (b),2wt%GR-FeNi50-PLA (c), 3wt%GR-FeNi50-PLA (d), 4wt%GR-FeNi50-PLA (e) and 5wt%GR-FeNi50-PLA (f)

R_{L_min}—Minimum reflection loss; E_AB—Electromagnetic wave absorption bandwidth

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图 13 (a) 不同GR-FeNi50质量比GR-FeNi50-PLA复合材料的衰减常数；(b) 4wt% GR-FeNi50-PLA的delta值二维图；(c) 5wt% GR-FeNi50-PLA的delta值二维图

Figure 13. (a) Attenuation constant of GR-FeNi50-PLA composites with different GR-FeNi50 mass ratio; Calculated delta value 2D maps: (b) 4wt% GR-FeNi50-PLA and (c) 5wt% GR-FeNi50-PLA

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表 1 GR-FeNi50-PLA复合材料的组分

Table 1 Components of GR-FeNi50-PLA composites

Sample	Mass fraction/wt%
Sample	GR	FeNi50	PLA
0wt%GR-FeNi50-PLA	0	20	80
1wt%GR-FeNi50-PLA	1	20	79
2wt%GR-FeNi50-PLA	2	20	78
3wt%GR-FeNi50-PLA	3	20	77
4wt%GR-FeNi50-PLA	4	20	76
5wt%GR-FeNi50-PLA	5	20	75

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表 2 近3年其他文献GR基磁性复合材料吸波性能比较

Table 2 Comparison of microwave absorption performance of GR-based magnetic composites in other literature in the last 3 years

Material	Matrix	${\text{R}}{{\text{L}}_{{\text{min}}}}$ /dB (mm)	Bandwidth/GHz	Ref.
FeNi₃/N-GN	Paraffin	−57.2(1.45)	3.4	[10]
KH550@Fe₃O₄/rGO	Paraffin	−49.32(1.48)	9.52	[39]
ZnCO₂O₄/C/MG	Paraffin	−52.9(3.5)	4.48	[42]
Fe₃O₄@SiO₂−rGO	Paraffin	−55.4(3.7)	6.24	[43]
SiC/Fe₃O₄/rGO	Paraffin	−30.3(2.0)	6.65	[44]
Fe-Co/NC/rGO	Paraffin	−43.26(2.5)	9.29	[45]
CoFe₂O₄/graphene	Paraffin	−55.2(1.7)	5.4	[46]
Co/NPC@ZnO/rGO	Paraffin	−25.4(2.0)	5.4	[47]
SGN/Fe₃O₄	Paraffin	−41(2.0)	5.3	[48]
Fe₃O₄−doped graphene	Paraffin	−53.6(1.8)	5.0	[49]
GR-FeNi50-PLA	PLA	−40.5(1.5)	4.7	This work
Notes: SGN—Sulfide doped graphene; MG—Magnetic graphene; GN—Graphene nanocrystals.

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石墨烯-铁镍合金-聚乳酸复合材料的制备及其吸波性能

通讯作者: 吴海华，博士，教授，博士生导师，研究方向为3D打印吸波材料及其工程应用技术 E-mail: wuhaihua@ctgu.edu.cn

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Preparation of graphene-iron-nickel alloy-polylactic acid composites and their microwave absorption properties

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通讯作者:
吴海华，博士，教授，博士生导师，研究方向为3D打印吸波材料及其工程应用技术　E-mail: wuhaihua@ctgu.edu.cn