Preparation and properties of multifunctional MXene-CCNT/polyimide electromagnetic shielding films
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摘要: 导电聚合物复合材料(CPC)因其耐腐蚀性好、比强度高、成本低和易加工等良好的综合性能,被广泛用于制备电磁屏蔽材料。本文采用简单的刮膜法和热酰亚胺化法制备了综合性能良好的MXene-羧基化碳纳米管(CCNT)/聚酰亚胺(MXene-CCNT/PI)复合薄膜。MXene和CCNT协同作用构筑了良好的导电网络,赋予薄膜高效的电磁屏蔽效能(EMI SE),当MXene和CCNT含量均为12.5wt%,膜厚度为80 μm时,电导率和EMI SE分别为5.88 S/cm和26.49 dB,电磁屏蔽效能与厚度的比值(EMI SE/t)为331.13 dB/mm。并且在极端恶劣环境下(酸-碱处理、高低温处理和重复弯曲)显示出持久而稳定的EMI SE。与此同时,MXene-CCNT/PI薄膜仍具有53.17 MPa的拉伸强度、优异的热稳定性(>500 ℃)和阻燃性能。实现了聚合物基电磁屏蔽复合材料的便捷、高效制备,同时兼顾其优异的力学性能和耐热性能。Abstract: Conductive polymer composites (CPCs) are widely used for the preparation of electromagnetic shielding materials due to their good comprehensive performance such as good corrosion resistance, high specific strength, low cost and easy processing. In this paper, MXene-carboxylated carbon nanotube (CCNT)/polyimide (MXene-CCNT/PI) composite films with good comprehensive performance were prepared by a simple scraping and thermal imidization method. The synergistic action of MXene and CCNT constructed a good conductive network, which gave the films high efficient electromagnetic shielding performance (EMI SE). When the contents of both MXene and CCNT were 12.5wt%, the film thickness was 80 μm, the conductivity was 5.88 S/cm, the EMI SE was 26.49 dB, and the ratio of electromagnetic shielding effectiveness to thickness (EMI SE/t) was 331.13 dB/mm. Moreover, the film showed long-lasting and stable EMI SE under extreme environments (acid-alkali treatment, high and low temperature treatment, and repetitive bending). At the same time, the MXene-CCNT/PI film still have a tensile strength of 53.17 MPa, excellent thermal stability (>500 ℃), and flame retardancy. Convenient and efficient preparation of polymer-based EMI shielding composites is realized, taking into account their excellent mechanical properties and heat resistance.
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Key words:
- polyimide /
- MXene /
- carboxylated carbon nanotube /
- electromagnetic interference shielding /
- film
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图 5 PI薄膜(a),5wt%MXene-CCNT/PI薄膜(b),10wt%MXene-CCNT/PI薄膜(c),15wt%MXene-CCNT/PI薄膜(d),20wt%MXene-CCNT/PI薄膜(e),25wt%MXene-CCNT/PI薄膜(f)经拉断后的截面SEM图
Figure 5. SEM image of cross-section of PI film (a), 5wt%MXene-CCNT/PI film (b), 10wt%MXene-CCNT/PI film (c), 15wt%MXene-CCNT/PI film (d), 20wt%MXene-CCNT/PI film (e), 25wt%MXene-CCNT/PI film (f) after pull-off
图 6 MXene-CCNT/PI膜的电导率曲线图(a),5wt%MXene-CCNT/PI薄膜连接在电路两端(b),10wt%MXene-CCNT/PI薄膜连接在电路两端(c),15wt%MXene-CCNT/PI薄膜连接在电路两端(d),20wt%MXene-CCNT/PI薄膜连接在电路两端(e),25wt%MXene-CCNT/PI薄膜连接在电路两端(f)灯泡亮度示意图
Figure 6. Electrical conductivity of MXene-CCNT/PI films (a), 5wt%MXene-CCNT/PI film (b), 10wt%MXene-CCNT/PI film (c), 15wt%MXene-CCNT/PI film (d), 20wt%MXene-CCNT/PI film (e), 25wt%MXene-CCNT/PI film connected to the circuit at both ends of the light bulb (f) brightness schematic diagram
图 7 MXene-CCNT/PI膜在X波段的EMI SET(a),EMI SER(b)和EMI SEA(c),MXene-CCNT/PI膜的平均SET、SEA和SER(d),MXene-CCNT/PI膜的T−R−A系数(e),SE/t与先前报告比较(f)
Figure 7. EMI SET (a) EMI SER(b) and EMI SEA (c) of MXene-CCNT/PI films in X-band, Average SET, SEA and SER of MXene-CCNT/PI films (d), T-R-A coefficients of MXene-CCNT/PI films (e), Comparison of SE/t with previous reports (f)
图 8 25wt%MXene-CCNT/PI薄膜在HCl中浸泡12 h (a),在碱液中浸泡12 h (b),重复弯曲100次(c),在300℃下处理2 h (d),在液氮中浸泡2 h (e),以及在液氮(−196℃)中浸泡2 h后在300℃下处理2 h前后的EMI SE (f)
Figure 8. EMI SE of 25wt%MXene-CCNT/PI films before and after immersion in HCl for 12 h (a), immersion in lye for 12 h (b), repetitive bending for 100 times (c), treatment at 300℃ for 2 h (d), immersion in liquid nitrogen (−196℃) for 2 h (e), and treatment at 300℃ for 2 h after 2 h in liquid nitrogen (-196℃) (f)
表 1 MXene-羧基化碳纳米管/聚酰亚胺(MXene-CCNT/PI)薄膜各组分的比例
Table 1. Proportions of components in MXene-carboxylated carbon nanotube/polyimide (MXene-CCNT/PI) Films
Sample name ODA/g PMDA/g MXene/g CCNT/g DMAc/g PI 2.27 2.53 0 0 43.20 5wt%MXene-CCNT/PI 2.27 2.53 0.13(2.5wt%) 0.13(2.5wt%) 45.47 10wt%MXene-CCNT/PI 2.27 2.53 0.27(5.0wt%) 0.27(5.0wt%) 48.00 15wt%MXene-CCNT/PI 2.27 2.53 0.42(7.5wt%) 0.42(7.5wt%) 50.82 20wt%MXene-CCNT/PI 2.27 2.53 0.60(10.0wt%) 0.60(10.0wt%) 54.00 25wt%MXene-CCNT/PI 2.27 2.53 0.80(12.5wt%) 0.80(12.5wt%) 57.60 表 2 MXene-CCNT/PI薄膜的拉伸强度和断裂伸长率
Table 2. Tensile strength and elongation at break of MXene-CCNT/PI films
Sample name Average tensile strength/MPa Average elongation
at break/%PI 121.18 25.95 5wt%MXene-CCNT/PI 119.27 14.75 10wt%MXene-CCNT/PI 92.69 5.91 15wt%MXene-CCNT/PI 65.87 3.31 20wt%MXene-CCNT/PI 64.06 2.20 25wt%MXene-CCNT/PI 53.17 2.03 表 3 MXene-CCNT/PI膜的EMI SE/t与以往报道文献对比
Table 3. EMI SE/t of MXene-CCNT/PI films compared with previously reported literature
Polymer Conductive filler Filler content Thicknesses/mm EMI SE/dB SE/t/(dB·mm−1) Ref. PIF MXene 49.1wt% 0.26 49.90 87.40 [7] PI CB 40wt% 1.00 35.00 35.00 [33] PI MXene 25wt% 0.14 29.12 208.00 [34] ANF MWCNTs 80wt% 0.30 41.70 139.00 [35] WPU Ti3C2Tx 7 wt % 0.50 50.00 100.00 [36] ANF Ti3C2Tx 21wt% 1.90 56.80 29.89 [37] Epoxy Graphene 19.5 vol% 1.00 65.00 65.00 [38] CNF MXene 17wt% 2.00 74.56 37.28 [39] PCL MWCNT 15wt% 0.50 61.50 123.00 [40] Epoxy GNP /CNT 1:1 0.25 35.00 140 [41] PVDF CNT:ZnONW 5.0:2.5wt% 1.10 41.00 37.27 [42] - Vertical graphene/SiC - 1.50 38.00 25.33 [43] - Fe3O4/MWCNT/SiO2 - 0.60 40.00 66.67 [44] - MXene/CNT - 3.00 103.90 34.63 [45] PI MXene-CNT 12.5/12.5wt% 0.08 26.49 331.10 本文 Notes: polyimide fiber (PIF); aramid nanofibers (ANF); waterborne polyurethane (WPU); cellulose nanofibrils (CNF); Poly(ε-caprolactone) (PCL); polyvinylidene fluoride (PVDF) 表 4 MXene-CCNT/PI膜的热性能
Table 4. Thermal properties of MXene-CCNT/PI films
Sample name T5%/℃ T10/℃ RW/% PI 532 570 52 5wt%MXene-CCNT/PI 540 564 61 10wt%MXene-CCNT/PI 523 558 63 15wt%MXene-CCNT/PI 540 566 61 20wt%MXene-CCNT/PI 519 564 63 25wt%MXene-CCNT/PI 531 571 68 MXene - - 96 CCNT 635 - 91 Notes: T5% and T10% are the temperatures corresponding to the first 5% weight loss and the first 10% weight loss; RW is the final carbon residue. 表 5 MXene-CCNT/PI薄膜的LOI
Table 5. LOI values of MXene-CCNT/PI films
Sample name LOI/% PI 42 5wt%MXene-CCNT/PI 44 25wt%MXene-CCNT/PI 47 -
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