epoxy electromagnetic interference shielding nanocomposites

epoxy electromagnetic interference shielding nanocomposites

Composites Part A 121 (2019) 265–272 Contents lists available at ScienceDirect Composites Part A journal homepage: www.elsevier.com/locate/composite...

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Composites Part A 121 (2019) 265–272

Contents lists available at ScienceDirect

Composites Part A journal homepage: www.elsevier.com/locate/compositesa

Fabrication and investigation on the PANI/MWCNT/thermally annealed graphene aerogel/epoxy electromagnetic interference shielding nanocomposites

T



Yiming Huangfu, Kunpeng Ruan, Hua Qiu, Yuanjin Lu, Chaobo Liang, Jie Kong, Junwei Gu

MOE Key Laboratory of Material Physics and Chemistry Under Extraordinary Conditions, Shaanxi Key Laboratory of Macromolecular Science and Technology, Department of Applied Chemistry, School of Science, Northwestern Polytechnical University, Xi’ an, Shaanxi 710072, PR China

A R T I C LE I N FO

A B S T R A C T

Keywords: A. Polymer-matrix composites (PMCs) B. Electrical properties D. Electron microscopy E. Casting

After ultrasonic dispersion of graphene oxide (GO) prepared by modified Hummers method and surface carboxylated multi-walled carbon nanotubes (f-MWCNT), L-ascorbic acid was added and the MWCNT/thermally annealed graphene aerogel (MWCNT/TAGA) was obtained by thermal annealing. Polyaniline/MWCNT/TAGA (PANI/MWCNT/TAGA) was prepared by slow adding ammonium persulfate into aniline/hydrochloric acid solution containing MWCNT/TAGA. The corresponding PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites were successfully fabricated via template-casting method. Results revealed that when the mass ratio of GO to f-MWCNT was 3:1 and the total loading of PANI/MWCNT/TAGA was 4.61 wt% (2.58 wt % PANI + 0.83 wt% MWCNT + 1.20 wt% TAGA), the obtained PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites presented the highest electromagnetic interference shielding effectiveness (EMI SE, 42 dB). Meanwhile, the corresponding PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites showed electrical conductivity of 52.1 S/cm heat resistance index (THRI) of 171.3 °C, and reduced modulus of 5.35 GPa & hardness of 0.39 GPa.

1. Introduction Now, electromagnetic pollution caused by mobile phones, computers and radar systems has seriously interfered with people’s life and the use of other electronic products [1–5]. It has become another kind of pollution that can be compared with water pollution and air pollution in modern life. Therefore, it is imperative to solve the above problems [6–10]. To the best knowledge of us, conductive polymer composites have the advantages of low density and excellent electromagnetic interference shielding performance, and can meet the requirements of novel electromagnetic interference shielding materials (thin, light, wide and strong, etc) [11–14]. In comparison to other carbon materials (carbon black [15], carbon fibers [16] and graphite nanoplatelets [17]), graphene has large specific surface area and excellent electrical conductivities, and can be widely used for electromagnetic interference shielding materials [18–22]. However, the strong Van der Waal’s force between graphene sheets makes them prone to agglomeration inner polymer matrix, which seriously affects the final properties of the polymer composites [23–26]. To overcome the abovementioned



limitations, graphene is constructed to a three-dimensional structure (aerogel or foam) [27,28] and the corresponding composites are prepared by template-casting method, which can not only uniformly disperse graphene inner polymer matrix, but also achieve high electrical conductivities with relatively lower filler content [29]. And the obtained composites with high porosity have more interfaces, beneficial to the improvement of EMI SE. Chen et al. [30] prepared graphene foam/ epoxy composites. When the graphene foam loading only accounted for 2.5 vol%, the electrical conductivity of the epoxy composites reached 196 S/m. Jia et al. [31] fabricated graphene foam (by chemical vapor deposition)/epoxy composites, and the electrical conductivity reached 300 S/m, while the graphene foam loading only accounted for 0.2 wt%. To further enhance the EMI SE values of the graphene aerogel (foam)/polymer composites, secondary conductive fillers, such as silver (Ag), carbon nanofiber (CNF) and carbon nanotube (CNT) [32], can be further introduced into the composites. CNT is an ideal electromagnetic interference shielding material for their excellent good electrical conductivity, light weight and corrosion resistance [33–36]. Sun et al. [37] prepared graphene foam/multi-walled carbon nanotube (MWCNT)/ poly(dimethyl siloxane) composites. When the loading of graphene

Corresponding author. E-mail address: [email protected] (J. Gu).

https://doi.org/10.1016/j.compositesa.2019.03.041 Received 8 March 2019; Received in revised form 24 March 2019; Accepted 26 March 2019 Available online 26 March 2019 1359-835X/ © 2019 Elsevier Ltd. All rights reserved.

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Fig. 1. Schematic diagram of the fabrication for the PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

2. Experiment section

foam/MWCNT was 2.7/2 wt%, the obtained EMI SE value of the composites reached 75 dB, 25 dB higher than that of the composites without MWCNT. Zhao et al. [32] also fabricated graphene aerogel/singlewalled carbon nanotube (SWCNT)/polydimethylsilane composites with EMI SE value of 31 dB (0.28 wt% graphene aerogel/SWCNT), 4 dB higher than that of the composites without SWCNT. Polyaniline (PANI), which has excellent electrical conductivity and easy fabrication, has been widely used in the electromagnetic interference shielding field [38]. Movassagh-Alanagh et al. [39] prepared [email protected]@carbon fiber/epoxy composites, and the EMI SE value reached 29 dB when [email protected]@carbon fiber only accounted for 1.5 wt%. Zhao et al. [40] fabricated layer-structured fabric-supported polyaniline/cobalt-nickel coatings (PANI/Co-Ni, 2.86/3.99 mg/cm−2) with EMI SE value of 46 dB, increased by 13 dB compared with that of uncoated fabric. At present, there are few reports on the simultaneous addition of MWCNT and PANI to three-dimensional graphene aerogels. The combination of ternary mixtures for TAGA, MWCNT and PANI endows the epoxy nanocomposites with a synergistically reinforced triple conductive network. In our present work, after ultrasonic dispersion of graphene oxide (GO) prepared by modified Hummers method and surface carboxylated multi-walled carbon nanotubes (f-MWCNT), L-ascorbic acid was added and the MWCNT/thermally annealed graphene aerogel (MWCNT/ TAGA) was obtained by thermal annealing. Polyaniline/MWCNT/TAGA (PANI/MWCNT/TAGA) was prepared by slow adding ammonium persulfate into aniline/hydrochloric acid solution containing MWCNT/ TAGA. The corresponding PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites were fabricated via template-casting method. PANI, MWCNT, f-MWCNT, MWCNT/GA, MWCNT/TAGA and PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites were analyzed and characterized by Fourier transform infrared (FTIR) spectra, X-ray photoelectron spectroscopy (XPS), X-ray diffractometer (XRD), scanning electron microscope (SEM), thermal gravimetric analyses (TGA) and nanoindenter. Mass ratio of GO/f-MWCNT and loading of PANI influencing on the electrical conductivities, EMI SE values, mechanical properties and thermal properties of the obtained epoxy nanocomposites were investigated and discussed in detail.

2.1. Materials Graphite flake (325 mesh) was provided by Alfa Aesar Co. Ltd. (Shanghai, China). Ammonium persulfate ((NH4)2S2O8, ≥99%), potassium persulfate (K2S2O8, ≥99%), phosphorus pentoxide (P2O5, ≥98%), potassium permanganate (KMnO4, ≥99%), sulfuric acid (H2SO4, 98%), hydrochloric acid (HCl, 37%), nitric acid (HNO3, 65%), hydrogen peroxide (H2O2, 30%) were all purchased from Beijing Chemical Factory (Beijing, China). L-ascorbic acid (C6H8O6, ≥99.99%) and aniline (C6H7N, ≥99.99%) were both supplied by Macklin (Shanghai, China). Multi-walled carbon nanotubes (MWCNT) by CVD method were obtained from Chengdu Organic Chemicals Co. Ltd. (Sichuan, China). Bisphenol F epoxy (Epon 862) and the curing agent of 2, 4-diethyl-6-methylbenzene-1,3-diamine (EK 3402) were both provided by Hexion Inc (Columbus, USA). All the chemicals were as-received without further treatment. 2.2. Fabrication of MWCNT/TAGA and PANI/MWCNT/TAGA GO was prepared by modified Hummers method [41] and MWCNT was surface functionalized by H2SO4/HNO3 (3/1, v/v) to obtain fMWCNT [42]. A certain mass of GO and f-MWCNT were ultrasonically dispersed in the deionized water for 10 min (10 mg/mL GO, GO/fMWCNT, 6/1, 3/1 and 2/1, w/w). Then L-ascorbic acid (GO/L-ascorbic acid, 1/2, w/w) was added under the ultrasonication for 10 min and the solution was heated to 40 °C for another 12 hrs to obtain MWCNT/GO hydrogel. The obtained hydrogel was then frozen in liquid nitrogen, freeze-dried for 48 hrs, and thermally annealed at 800 °C for 30 min under nitrogen atmosphere to obtain MWCNT/TAGA. A certain mass of aniline (0.125 mol/L, 0.187 mol/L and 0.25 mol/ L) was dispersed in 1 mol/L hydrochloric acid and then MWCNT/TAGA was placed in the above solution. After stirring for 30 min, ammonium persulfate was slowly added in the above mixtures in an ice bath. The reaction was carried out for 1 hr and the product was freeze-dried to obtain the PANI/MWCNT/TAGA. 2.3. Fabrication of MWCNT/TAGA/epoxy and PANI/MWCNT/TAGA/ epoxy electromagnetic interference shielding nanocomposites Epon 862 and EK 3402 (100/26.5, w/w) were stirred at 70 °C for 1 hr and poured into the above MWCNT/TAGA and PANI/MWCNT/ 266

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284.0 eV and 530.0 eV is assigned to the C 1s and O 1s element, respectively. Compared with that of MWCNT, the oxygen content of fMWCNT is greatly increased, ascribed to the introduced carboxyl groups on MWCNT after surface functionalization. Compared with that of MWCNT at 800 °C (7.1 wt%), the corresponding thermal weight loss of f-MWCNT at 800 °C (Fig. 2(b)) reaches 16.7 wt%, mainly attributed to the introduction of carboxyl groups on MWCNT. Above results show that MWCNT has been successfully carboxylated [43]. Fig. 3(a) is the FTIR spectrum of PANI. Representative peaks at 1570 cm−1 and 1490 cm−1 are corresponded to C]C stretching vibration of benzenoid and quinoid rings, respectively. Peaks at 1298 cm−1 and 1238 cm−1 indicate CeN stretching vibration of benzenoid unit. Peak at 1144 cm−1 and 874 cm−1 is associated with inplane and out-plane CeH bending vibration, respectively. Characteristic vibration peak at 796 cm−1 is assigned to the para-disubstituted aromatic ring, indicating the formation of polymer chains. It can be found that there are two peaks (Fig. 3(b)) at 2θ of 20° and 25°, caused by the parallel and vertical periodicity of PANI [44–46], further indicating that PANI has been successfully prepared. XPS spectra of the GA, MWCNT/GA, MWCNT/TAGA and PANI/ MWCNT/TAGA are depicted in Fig. 4. XPS curves of the C 1s for GA and MWCNT/GA contain four characteristic peaks: ∼284.6 eV (CeC), 285.6 eV (CeO), 287.0 eV (C]O) and 288.6 eV (OeC]O) [47,48]. MWCNT/TAGA displays a substantial decline in the O 1s peak intensity and the characteristic peaks of the CeO, C]O and OeC]O bonds are weakened, suggesting the efficient removal of vast majority of oxygen functional groups in MWCNT/GA [49]. Compared with that of MWCNT/TAGA, the XPS curve of C 1s for PANI/MWCNT/TAGA shows a characteristic peak of CeN bond at 285.5 eV, indicating the presence of PANI on the surface of MWCNT/TAGA. Fig. 5(a) shows the SEM image of PANI/MWCNT/TAGA. It can be seen that PANI/MWCNT/TAGA has an obvious pore structure and PANI is distributed on the surface of TAGA and MWCNT (a’), beneficial to the absorption and reflection of electromagnetic waves. Fig. 5(b) is the SEM image of the PCGE4 nanocomposites. It can be seen that continuous and porous 3D aerogel architectures are well retained and epoxy resin is dispersed in the pores of PANI/MWCNT/TAGA, which is beneficial to achieving high electrical conductivity and EMI SE value of the PCGE nanocomposites. Electrical conductivities of the CGE and PCGE nanocomposites are shown in Fig. 6, where the electrical conductivities are increased with the increase of MWCNT loading. With the further increase of MWCNT (GO:MWCNT = 3:1), the obtained electrical conductivities of the CGE nanocomposites are decreased because the excessive MWCNT will agglomerate in the GO solution and finally affect the electrical

Table 1 Fillers contents of the epoxy electromagnetic interference shielding nanocomposites. Samples

CGE1 CGE2 CGE3 CGE4 PCGE1 PCGE2 PCGE3 PCGE4

Filler contents (wt%) TAGA

MWCNT

PANI

1.20 1.20 1.20 1.20 1.20 1.20 1.20 1.20

0 0.41 0.83 1.24 0.83 0.83 0.83 0.83

0 0 0 0 0 1.34 1.96 2.58

TAGA. MWCNT/TAGA/epoxy and PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites were then obtained after being cured in an oven at 120 °C for 5 hrs and cooled to room temperature (as shown in Fig. 1). The fillers' contents of the epoxy nanocomposites were shown in Table 1. 2.4. Characterizations Fourier transform infrared (FTIR) spectra of the samples were obtained on a Bruker Tensor 27 equipment (Bruker Corp., Germany). Xray photoelectron spectroscopy (XPS) analyses of the samples were carried out using PHI5400 equipment (PE Corp., England). X-ray diffractometer (XRD) analyses of the samples were carried out using D2 PHASER X equipment (Bruker Corp., Germany). Morphologies of the samples were analyzed by scanning electron microscope (SEM, VEGA3LMH, ESCAN Corporation, Czech Republic). Thermal gravimetric analyses (TGA) of the samples were carried out using STA 449F3 (Netzsch C Corp., Germany) at 10 °C/min−1 (argon condition), over the entire temperature range (40–800 °C). Direct current (DC) electrical conductivities of the samples were measured by a four-probe method at room temperature. Indentation experiment was performed with an using a G200 nanoindenter from Agilent. Characteristic EMI shielding parameters of the samples were tested by VNA (MS4644A, Anritsu) using the wave-guide method at X-band according to ASTM D5568-08, and the corresponding dimensions of the samples are 22.86 mm in length, 10.16 mm in width, and 3 mm in thickness. 3. Results and discussion Fig. 2(a) is the XPS spectra of MWCNT and f-MWCNT. Peaks at

Fig. 2. XPS (a) spectra and TGA (b) curves of the MWCNT and f-MWCNT. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.) 267

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Fig. 3. FTIR (a) spectra and XRD (b) pattern of the PANI. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 4. XPS spectra of the GA, MWCNT/GA, MWCNT/TAGA and PANI/MWCNT/TAGA. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 5. SEM images of the PANI/MWCNT/TAGA (a), (a’) and PCGE4 nanocomposites (b). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

suggest that MWCNT and PANI can both enhance the electrical conductivities of epoxy nanocomposites. Fig. 7(a) and (b) depict the EMI SE values at X-band of the CGE and PCGE nanocomposites. It can be seen that with the increase of MWCNT loading, the EMI SE value of the CGE nanocomposites is increased from 28 dB to 36 dB. The EMI SE value of the CGE nanocomposites no longer

conductivities [32]. Compared with that of CGE nanocomposites, the electrical conductivities of the PCGE nanocomposites are improved due to the addition of PANI. While the loading of PANI is 2.58 wt%, the electrical conductivity of the PCGE nanocomposites is improved from 42.0 S/m to 52.1 S/m, mainly attributed to the further improvement of the conductive networks of the PCGE nanocomposites. These results

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Fig. 6. Electrical conductivities of the CGE (a) and PCGE (b) nanocomposites. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 7. EMI SE values of the CGE (a) and PCGE (b), (b’) nanocomposites. Schematic illustration of EMI shielding mechanism (c). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

surface of MWCNT/TAGA. The impedance mismatch between the surfaces of the PCGE nanocomposites and the external environment is further increased, which results in the increase of SER value. Due to addition of PANI with high electrical conductivity and the more perfect conductive networks, the final electrical conductivity of PCGE nanocomposites is further improved and the SEA value is also increased from 31 dB to 35 dB. Just like the influence on electrical conductivity, both MWCNT and PANI play important roles in the improvement of EMI SE value. The representative load-displacement curves of the CGE and PCGE

increase while the loading of MWCNT is further increased (GO:MWCNT = 3:1), mainly attributed that MWCNT exceeds the highest concentration where it can be uniformly dispersed and results in a decrease in electrical conductivity. After PANI is grown on MWCNT/TAGA, the EMI SE value of the PCGE nanocomposites with 2.58 wt% PANI is further improved to 42 dB. Fig. 7(b’) shows the absorption shielding effectiveness (SEA) and reflection shielding effectiveness (SER) of the PCGE at X-band. SER value of the PCGE nanocomposites is increased from 5 dB to 7 dB, because of forming new interfaces duo to the growth of PANI on the 269

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Fig. 8. Representative load-displacements curves of the CGE (a) and PCGE (c) nanocomposites. Hardness and reduced modulus of the CGE (b) and PCGE (d) nanocomposites. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 9. TGA curves of the CGE (a) and PCGE (b) nanocomposites. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

and 0.39 GPa, respectively. These results reveal that the addition of MWCNT and PANI enhances the Er and hardness of epoxy resin. Fig. 9 depicts the TGA curves of the CGE and PCGE nanocomposites at argon atmosphere and the corresponding thermal characteristics data are shown in Table 2. It can be concluded that the thermal decomposition of the CGE and PCGE nanocomposites takes place between 300 °C and 400 °C, mainly due to the pyrolysis of epoxy resin. The decomposition temperatures of the CGE nanocomposites with 5% and 30% weight loss (T5 and T30) and the heat resistance index (THRI) are all increased with the increase of MWCNT loading. It can be mainly attributed that MWCNT owns good heat resistance. Compared with that

nanocomposites are shown in Fig. 8(a) and (c). Indentation depth of the CGE nanocomposite is smaller than that of pure epoxy resin. With the increase of MWCNT and PANI, the indentation depth of the CGE and PCGE nanocomposites is decreased gradually, indicating that the addition of MWCNT and PANI enhances the ability of epoxy resin to resist indentation. Reduced modulus (Er) and hardness of the CGE nanocomposites are shown in Fig. 8(b). Along with the increase of MWCNT loading, both the Er and hardness are improved to 4.93 GPa and 0.31 GPa for CGE4 nanocomposite, compared to 4.03 GPa and 0.26 GPa for epoxy resin. As shown in Fig. 8(d), with the increase of PANI, the Er and hardness of the PCGE nanocomposites further increases to 5.35 GPa 270

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Table 2 Thermal characteristic data of the CGE and PCGE nanocomposites. [6] Samples

Epoxy CGE1 CGE2 CGE3 CGE4 PCGE1 PCGE2 PCGE3 PCGE4

Weight loss temperature (°C) T5

T30

342.5 344.7 348.9 351.3 356.0 351.3 332.8 323.0 304.8

371.8 377.7 379.6 382.4 383.9 382.4 376.5 377.2 379.5

THeat-resistance

index

(°C) [7]

176.4 178.3 179.9 181.3 182.6 181.3 175.9 174.2 171.3

[8] [9]

[10]

[11]

The sample’s heat-resistance index is calculated by Eq. (1). THeat-resistance index = 0.49 × [T5 + 0.6 × (T30 − T5)] (Eq. (1)).

[12]

[13]

of CGE nanocomposites, the obtained T5, T30 and THRI of the PCGE nanocomposites show a downward trend, mainly because the introduction of PANI can reduce the thermal stabilities of the PCGE nanocomposites [50–52]. However, THRI value of the all above nanocomposites is higher than 171.3 °C, still remaining at a relatively high level.

[14]

[15]

4. Conclusions

[16] [17]

PANI/MWCNT/TAGA nanocomposites with high electrical conductivities and EMI SE values were successfully prepared. The obtained nanocomposites had obvious pore structures, beneficial to the absorption and reflection of electromagnetic waves. When the mass ratio of GO to f-MWCNT was 3:1 and the total loading of the PANI/MWCNT/ TAGA was 4.61 wt% (2.58 wt% PANI + 0.83 wt% MWCNT + 1.2 wt% TAGA), the obtained PANI/MWCNT/TAGA/epoxy electromagnetic interference shielding nanocomposites presented the excellent electrical conductivity of 52.1 S/m and the highest EMI SE of 42 dB. At the same time, Er increased from 4.03 to 5.35 GPa and hardness increased from 0.26 to 0.39 GPa. Owing to outstanding electrical conductivity and EMI shielding performance at ultralow PANI/MWCNT/TAGA loading, as well as remarkable mechanical properties, PANI/MWCNT/TAGA nanocomposites would be used as electromagnetic interference shielding materials for many key fields.

[18]

[19]

[20]

[21]

[22]

[23]

Acknowledgments [24]

This work is supported by Space Supporting Fund from China Aerospace Science and Industry Corporation (Nos. 2019-HT-XG and 2018-HT-XG); Foundation of Aeronautics Science Fund (No. 2017ZF53071); Natural Science Basic Research Plan in Shaanxi Province of China (No. 2018JM5001); Y. Huangfu thanks for the Seed Foundation of Innovation and Creation for Graduate Students of Northwestern Polytechnical University (ZZ2019034); We would like to thank the Analytical & Testing Center of Northwestern Polytechnical University for SEM test.

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