多功能MXene-CCNT/聚酰亚胺电磁屏蔽薄膜的制备与性能

储娜; 骆春佳; 晁敏; 杨雪雪; 颜录科

doi:10.13801/j.cnki.fhclxb.20231214.002

多功能MXene-CCNT/聚酰亚胺电磁屏蔽薄膜的制备与性能

doi: 10.13801/j.cnki.fhclxb.20231214.002

长安大学　材料科学与工程学院，西安 710018

基金项目: 国家自然科学基金 (22005039)；陕西省重点研发计划(2022GY-403)；陕西省创新能力支撑计划(2023-CX-TD-43)；长安大学中央高校基本科研业务费专项资金(300102312403；300102313208)

详细信息

通讯作者:
晁敏，博士，副教授，研究方向为树脂基复合材料和先进纳米功能材料的设计与制备　E-mail: chaominchd@163.com

中图分类号: TB34；TB332
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出版历程
- 收稿日期: 2023-10-11
- 修回日期: 2023-11-20
- 录用日期: 2023-12-07
- 网络出版日期: 2023-12-14
- 刊出日期: 2024-08-15

Preparation and properties of multifunctional MXene-CCNT/polyimide electromagnetic shielding films

School of Materials Science & Engineering, Chang'an University, Xi'an 710064, China

Funds: National Natural Science Foundation of China (22005039); Shaanxi Key Research & Development Project (2022GY-403); Innovation Capability Support Program of Shaanxi (2023-CX-TD-43); Fundamental Research Funds for the Central Universities, CHD (300102312403; 300102313208)

摘要

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/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。
- 聚酰亚胺 /
- MXene /
- 羧基化碳纳米管 /
- 电磁屏蔽 /
- 薄膜
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.
- polyimide /
- MXene /
- carboxylated carbon nanotube /
- electromagnetic interference shielding /
- film

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图 1 MXene (a) 和MXene-羧基化碳纳米管/聚酰亚胺(MXene-CCNT/PI) (b) 薄膜的制备过程示意图

ODA—4, 4'-diaminodiphenyl ether; PMDA—Pyromellitic dianhydride

Figure 1. Schematic diagram of preparation process of MXene (a) and MXene-carboxylated carbon nanotube/polyimide (MXene-CCNT/PI) films (b)

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图 2 MAX相(a)和MXene (b)的SEM图像；(c) MAX相和MXene的XRD图谱

Figure 2. SEM images of MAX (a) and MXene (b); (c) XRD patterns of MAX and MXene

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图 3 MXene-CCNT/PI薄膜的FTIR图谱(a)和XRD图谱(b)；25wt%MXene-CCNT/PI薄膜的TEM图像(c)和相应的EDS图像(d)

Figure 3. FTIR spectra (a) and XRD patterns (b) of MXene-CCNT/PI films; TEM image (c) and corresponding EDS image (d) of 25wt%MXene-CCNT/PI film

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图 4 MXene-CCNT/PI薄膜的力学性能：(a)拉伸强度和断裂伸长率；(b)薄膜弯折成任意形状的照片

Figure 4. Mechanical properties of MXene-CCNT/PI films: (a) Tensile strength and elongation at break; (b) Photographs of films bent into arbitrary shapes

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图 5 PI (a)、5wt%MXene-CCNT/PI (b)、10wt%MXene-CCNT/PI (c)、15wt%MXene-CCNT/PI (d)、20wt%MXene-CCNT/PI (e)、25wt%MXene-CCNT/PI (f)薄膜经拉断后的截面SEM图像

Figure 5. SEM images of cross-section of PI (a), 5wt%MXene-CCNT/PI (b), 10wt%MXene-CCNT/PI (c), 15wt%MXene-CCNT/PI (d), 20wt%MXene-CCNT/PI (e), 25wt%MXene-CCNT/PI (f) film after pull-off

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图 6 (a) MXene-CCNT/PI膜的电导率曲线图；5wt%MXene-CCNT/PI (b)、10wt%MXene-CCNT/PI (c)、15wt%MXene-CCNT/PI (d)、20wt%MXene-CCNT/PI (e)、25wt%MXene-CCNT/PI (f)薄膜连接在电路两端时灯泡亮度示意图

Figure 6. (a) Electrical conductivity of MXene-CCNT/PI films; Light bulb brightness schematic diagram of 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) connected to the circuit at both ends

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图 7 MXene-CCNT/PI膜在X波段的EMI SE_T(a)、EMI SE_R(b)和EMI SE_A(c)；(d) MXene-CCNT/PI膜的平均SE_T、SE_A和SE_R；(e) MXene-CCNT/PI膜的T/R/A系数；(f) SE/t与文献[7, 33-45]比较

Figure 7. EMI SE_T (a), EMI SE_R(b) and EMI SE_A (c) of MXene-CCNT/PI films in X-band; (d) Average SE_T, SE_A and SE_R of MXene-CCNT/PI films; (e) T/R/A coefficients of MXene-CCNT/PI films; (f) Comparison of SE/t with previous reports [7, 33-45]

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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)及在液氮(−196℃)中浸泡2 h后在300℃下处理2 h (f)前后的EMI SE

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)

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图 9 25wt%MXene-CCNT/PI薄膜在不同环境中处理前后的平均SE_T (a)和MXene-CCNT/PI膜中电磁微波耗散示意图(b)

Figure 9. Average SE_T of 25wt%MXene-CCNT/PI film before and after treatment in different environments (a) and schematic diagram of electromagnetic microwave dissipation in MXene-CCNT/PI films (b)

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图 10 MXene-CCNT/PI薄膜在氮气气氛中的TG曲线

Figure 10. TG curves of MXene-CCNT/PI films in nitrogen atmosphere

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图 11 MXene-CCNT/PI薄膜的阻燃性：PI薄膜(a)、5wt%MXene-CCNT/PI薄膜(b)和25wt%MXene-CCNT/PI薄膜(c)在火焰上燃烧

Figure 11. Flame retardancy of MXene-CCNT/PI films: PI film (a), 5wt%MXene-CCNT/PI film (b) and 25wt%MXene-CCNT/PI film (c) burning on flame

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表 1 MXene-CCNT/PI薄膜各组分的比例

Table 1. Proportions of components in MXene-CCNT/PI films

Sample	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
Note: DMAc—N, N-dimethylacetamide.

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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	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

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表 3 MXene-CCNT/PI膜的EMI SE/t与以往文献对比

Table 3. EMI SE/t of MXene-CCNT/PI films compared with previously reported literature

Polymer	Conductive filler	Filler content	Thickness/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	MWCNT	80wt%	0.30	41.70	139.00	[35]
WPU	Ti₃C₂T_x	7wt%	0.50	50.00	100.00	[36]
ANF	Ti₃C₂T_x	21wt%	1.90	56.80	29.89	[37]
Epoxy	Graphene	19.5vol%	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	140.00	[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	This work
Notes: PIF—Polyimide fiber; ANF—Aramid nanofibers; WPU—Waterborne polyurethane; CNF—Cellulose nanofibrils; PCL—Poly(ε-caprolactone); PVDF—Polyvinylidene fluoride.

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表 4 MXene-CCNT/PI膜的热性能

Table 4. Thermal properties of MXene-CCNT/PI films

Sample	T_5%/℃	T_10%/℃	R_W/%
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: T_5%,T_10%—Temperatures corresponding to the first 5wt% mass loss and the first 10wt% mass loss; R_W—Final carbon residue.

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表 5 MXene-CCNT/PI薄膜的极限氧指数(LOI)

Table 5. Limiting oxygen index (LOI) values of MXene-CCNT/PI films

Sample	LOI/%
PI	42
5wt%MXene-CCNT/PI	44
25wt%MXene-CCNT/PI	47

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