碳纳米管改性CF/PEEK复合材料的力学与电磁屏蔽性能

瞿明城; 张礼颖; 周剑锋; 刘旋; 章嘉豪; 杨丽丽; 朱姝

doi:10.13801/j.cnki.fhclxb.20211126.001

碳纳米管改性CF/PEEK复合材料的力学与电磁屏蔽性能

doi: 10.13801/j.cnki.fhclxb.20211126.001

瞿明城^{1, 2},
张礼颖^{1, 2},
周剑锋^{1, 3},
刘旋^{1, 2},
章嘉豪^{1, 2},
杨丽丽¹,
朱姝^{1, 2, ,}

1.
东华大学　纤维材料改性国家重点实验室，高性能纤维及制品教育部重点实验室(B类)，材料科学与工程学院，上海 201620
2.
东华大学　上海市高性能纤维复合材料省部共建协同创新中心，上海市轻质结构复合材料重点实验室，民用航空复合材料东华大学协同创新中心，上海 201620
3.
东华大学　分析测试中心，上海 201620

基金项目: 国家自然科学基金面上项目(52173247)；上海市科委科研计划项目(20511107200)；国家大学生创新创业训练项目(202110255086)

详细信息

通讯作者:
朱姝，博士，副教授，硕士生导师，研究方向为航空级热塑性复合材料、结构功能一体化复合材料　E-mail: zhushu@dhu.edu.cn

中图分类号: TB332；V261.97
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- 文章访问数: 1931
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- 被引次数: 0
出版历程
- 收稿日期: 2021-09-30
- 修回日期: 2021-11-15
- 录用日期: 2021-11-17
- 网络出版日期: 2021-11-26
- 刊出日期: 2022-07-30

Effect of carbon nanotube reinforcement on the mechanical and EMI shielding properties of CF/PEEK composites

QU Mingcheng^{1, 2},
ZHANG Liying^{1, 2},
ZHOU Jianfeng^{1, 3},
LIU Xuan^{1, 2},
ZHANG Jiahao^{1, 2},
YANG Lili¹,
ZHU Shu^{1, 2
, ,}

1.
State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, Key Laboratory of High Performance Fibers & Products, Ministry of Education, College of Material Science and Engineering, Donghua University, Shanghai 201620, China
2.
Shanghai Collaborative Innovation Center for High Performance Fiber Composites, Shanghai Key Laboratory of Lightweight Composite, Center for Civil Aviation Composites, Donghua University, Shanghai 201620, China
3.
Research Center for Analysis and Measurement, Donghua University, Shanghai 201620, China

摘要

摘要: 为了制备兼具优异力学性能和电磁干扰屏蔽效能的结构功能一体化耐高温热塑性复合材料，对添加不同组分碳纳米管(CNT)的连续碳纤维增强聚醚醚酮复合材料(CF-CNT/PEEK)的力学性能、电导率以及电磁干扰屏蔽效能(EMI SE)进行了研究。考察用上浆后的CNT (SCNT)作为导电填料制备的SCF-SCNT/PEEK层合板力学性能、界面形貌和屏蔽效能，并与不进行表面修饰、仅活化的CNT (ACNT)的效果做对比实验。结果表明，适量的CNT会使CF/PEEK层合板的力学性能、电导率和EMI SE得到提高；SCNT比ACNT更容易在PEEK中均匀分散，且与SCF和PEEK的结合更好。所有样品中，仅添加1wt%SCNT的SCF-SCNT/PEEK层合板与不添加CNT的层合板相比，拉伸强度提高了20.8%，达到778 MPa；弯曲强度提高了25.9%，达到1684 MPa；电导率提升5倍，达到0.15 S/cm；电磁干扰屏蔽效能提升69.76%，平均值达到34.97 dB。
- 碳纤维 /
- 聚醚醚酮(PEEK) /
- 复合材料 /
- 电磁屏蔽(EMI SE) /
- 界面改性 /
- 力学性能
Abstract: In order to prepare a high temperature resistant thermoplastic composite material with integrated structure and function, which has excellent mechanical properties and electromagnetic interference shielding effectiveness at the same time, the mechanical properties, electrical conductivity and electromagnetic interference shielding effectiveness (EMI SE) of continuous carbon fiber reinforced polyether ether ketone composites (CF-CNT/PEEK) with different components of carbon nanotubes (CNT) were studied. The mechanical properties, interface morphology and shielding effectiveness of SCF-SCNT/PEEK laminates prepared with CNT modified PEEK sizing agent (SCNT) as conductive fillers were investigated, and the effect of the CNT (ACNT) without surface modification and only activation comparative experiment were compared. The results show that an appropriate amount of CNT will improve the mechanical properties, electrical conductivity and shielding effectiveness of the CF/PEEK laminate. SCNT is easier to uniformly disperse in PEEK than ACNT, and has a better combination with SCF and PEEK. In all samples, the tensile strength of SCF-SCNT/PEEK laminates with only 1wt%SCNT increased by 20.8% to 778 MPa compared with laminates without CNTs. Bending strength is increased by 25.9% to 1684 MPa. The conductivity is increased by 5 times, reaching 0.15 S/cm. The electromagnetic interference shielding efficiency is increased by 69.76%, with an average value of 34.97 dB.
- carbon fiber /
- polyether ether ketone (PEEK) /
- composite material /
- electromagnetic interference shielding effectiveness (EMI SE) /
- interface modification /
- mechanical property

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图 1 SCF-SCNT/PEEK层合板模压成型流程图

Figure 1. Schematic diagram for process of SCF-SCNT/PEEK Laminates

CF—Carbon fiber; PEEK—Poly(ether-ether-ketone); CNT—Carbon nanotube; DMSO—Dimethyl sulfoxide; SPEEK—Sulfonated poly(ether-ether-ketone); SCF—Sized carbon fiber; SCNT—Sized carbon nanotube

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图 2 SPEEK和PEEK的FTIR图谱

Figure 2. FTIR spectras of SPEEK and PEEK

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图 3 CNT和ACNT的XPS图谱

Figure 3. XPS patterns of CNT and ACNT

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图 4 ACNT (a)以及ACNT与SCNT联合(b)的热重分析曲线

Figure 4. TGA curves of ACNT (a) and ACNT with SCNT (b)

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图 5 SPEEK热重分析图谱(a)以及ACNT与SCNT联合的FTIR图谱(b)

Figure 5. TGA spectra of SPEEK (a) and FTIR spectra of ACNT and SCNT (b)

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图 6 不同CNT组分的SCF-CNT/PEEK层合板的力学性能

Figure 6. Mechanical properties of SCF-CNT/PEEK laminates with different CNT contents

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图 7 不同CNT组分层合板拉伸断裂后断面SEM图像：(a) SCF-0wt%ACNT/PEEK；(b) SCF-1wt%ACNT/PEEK；(c) SCF-1wt%SCNT/PEEK；(d) SCF-3wt%SCNT/PEEK；(e) SCF-5wt%SCNT/PEEK

Figure 7. SEM images of the laminates with different contents of CNT：(a) SCF-0wt%ACNT/PEEK; (b) SCF-1wt%ACNT/PEEK; (c) SCF-1wt%SCNT/PEEK; (d) SCF-3wt%SCNT/PEEK; (e) SCF-5wt%SCNT/PEEK

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图 8 不同CNT组分层合板金相显微镜图像：(a) SCF-0wt%ACNT/PEEK；(b) SCF-1wt%ACNT/PEEK；(c) SCF-1wt%SCNT/PEEK；(d) SCF-3wt%SCNT/PEEK；(e) SCF-5wt%SCNT/PEEK

Figure 8. Metallurgical microscope images of the laminates with different contents of CNT：(a) SCF-0wt% ACNT/PEEK; (b) SCF-1wt%ACNT/PEEK; (c) SCF-1wt%SCNT/PEEK; (d) SCF-3wt%SCNT/PEEK; (e) SCF-5wt%SCNT/PEEK

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图 9 SCF-SCNT/PEEK中不同部位的FESEM图像：SCF与SCNT的排布((a)、(b) )；PEEK中团聚的SCNT((c)、(d))

Figure 9. FESEM images of different parts of SCF-SCNT/PEEK: SCNT around the SCF ((a), (b)); SCNT agglomerates within the PEEK ((c), (d) )

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图 10 (a)不同CNT组分层合板的总屏蔽效能值(E_Total)；(b) SCF-1wt% SCNT/PEEK层合板的反射率(R)、透射率(T)、吸收率(A)参数与电磁干扰屏蔽效能(EMI SE)组成

Figure 10. (a) Total shielding effectiveness (E_Total) spectra of the laminates with different contents of CNT; (b) Reflected (R), transmitted (T), absorbed (A) index and the component of the electromagnetic interference shielding effectiveness (EMI SE) of SCF-1wt% SCNT/PEEK

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表 1 不同组分SCF-CNT/PEEK层合板中原料的质量

Table 1. The mass of raw materials in SCF-CNT/PEEK laminates with different components

No.	Sample	Mass of SCNT/g	Mass of ACNT/g	Mass of PEEK/g
1	SCF-0wt%ACNT/PEEK	0	0	25.00
2	SCF-1wt%ACNT/PEEK	0	0.25	24.75
3	SCF-1wt%SCNT/PEEK	0.25	0	24.75
4	SCF-3wt%SCNT/PEEK	0.75	0	24.25
5	SCF-5wt%SCNT/PEEK	1.25	0	23.75
Notes: PEEK—Poly(ether-ether-ketone); SCF—Sized carbon fiber; SCNT—Sized carbon nanotube; ACNT—Activated carbon nanotube.

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表 2 SPEEK磺化度酸碱滴定法测定结果

Table 2. Sulfonation degree of SPEEK measured by acid-base titration

No.	1	2	3	4	5
Sulfonation degree/%	7.9	7.6	7.8	7.7	7.5

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表 3 CNT酸化前后表面C与O元素相对原子数分数

Table 3. Relative atomic fractions of C and O elements on the surface of CNT before and after acidification

Name	C/at%	O/at%	O/C
CNT	98.82	1.18	0.012
ACNT	86.32	13.68	0.158
Notes：O/C—Relative atomic fractions of C is divided by the relative atomic fractions of O.

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