Robustly Superhydrophobic Conductive Textile for Efficient

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Surfaces, Interfaces, and Applications

Robustly Superhydrophobic Conductive Textile for Efficient Electromagnetic Interference Shielding Li-Chuan Jia, Guoqiang Zhang, Ling Xu, Wen-Jin Sun, GanJi Zhong, Jun Lei, Ding-Xiang Yan, and Zhong-Ming Li ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b18459 • Publication Date (Web): 06 Dec 2018 Downloaded from http://pubs.acs.org on December 8, 2018

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ACS Applied Materials & Interfaces

Robustly

Superhydrophobic

Conductive

Textile

for

Efficient

Electromagnetic Interference Shielding

Li-Chuan Jia,† Guoqiang Zhang,‡ Ling Xu,† Wen-Jin Sun,† Gan-Ji Zhong,† Jun Lei,† DingXiang Yan,*,†,§ Zhong-Ming Li*,†

†College

of Polymer Science and Engineering, State Key Laboratory of Polymer Materials

Engineering, Sichuan University, Chengdu 610065, P. R. China. ‡Department

of Macromolecular Science and Engineering, Case Western Reserve University,

Cleveland, Ohio 44106-7202, United States §School

of Aeronautics and Astronautics, Sichuan University, Chengdu 610065, China

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ABSTRACT: Superhydrophobic electromagnetic interference (EMI) shielding textile (EMIST) is of great significance to the safety and long-term service of all-weather outdoor equipment. However, it is still challenging to achieve long-term durability and stability under external mechanical deformations or other harsh service conditions. Herein, by designing and implementing silver nanowire (AgNW) networks and a superhydrophobic coating onto a commercial textile, we demonstrate a highly robust superhydrophobic EMIST. The resultant EMIST shows a synergy of high water contact angle (160.8°), low sliding angle (2.9°), and superior EMI shielding effectiveness (51.5 dB). Remarkably, the EMIST still maintains its superhydrophobic feature and high EMI shielding level (42.6 dB) even after 5000 stretchingreleasing cycles. Moreover, the EMIST exhibits strong resistance to ultrasonic treatment up to 60 min, peeling test up to 100 cycles, strong acidic/alkaline solutions and different organic solvents, indicating its outstanding mechanical robustness and chemical durability. These attractive features of the EMIST are mainly a result of the joint action of AgNWs, carbon nanotubes, polytetrafluoroethylene nanoparticles and fluoroacrylic polymer. This work offers a promising approach for the design of future durable, superhydrophobic EMISTs, which are capable of remaining fully functional against long-time exposure to extreme conditions, e.g. wet and corrosive environments.

KEYWORDS: superhydrophobic, conductive textile, EMI shielding, mechanical robustness, chemical durability


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1. INTRODUCTION Electromagnetic interference (EMI) shielding textiles (EMISTs) have gained extensive attention for protecting human beings and sensitive electronic devices from electromagnetic radiation because of their lightweight, good flexibility and conformability.1-9 However, conventional EMISTs fabricated by interweaving metal fibers with polymer fibers or coating a conductive layer on original textiles generally lack enough stretchability and exhibit poor EMI shielding reliability under large mechanical deformation. Besides being stretchable, ideal EMISTs are also asked to show strong water repellency to guarantee long-term usage under harsh environments (wet or corrosive conditions). This is of significance for their practical applications, especially for being used in all-weather outdoor equipment, such as signal station, mobile communication devices, and antiradiation clothing. The importation of superhydrophobic coating has emerged as a prospective avenue to improve water repellency of a textile, which offers exciting promise for prolonging the service life of a textile under wet or corrosive conditions. Inspired by the natural superhydrophobic surfaces including lotus leaves, butterfly wings, and gecko feet, the combination of hierarchical micro/nanostructures with low-surface-energy materials is essential to realize superhydrophobic surface.10-13 Being guided by the wisdom of “learning from mother nature’’, great efforts have been made towards the development of superhydrophobic textiles by utilizing fibrous micro-structured textures and further coating fibers with nanoparticles (e.g., SiO2, TiO2, ZnO) and low-surface-energy materials.14-18 Though superhydrophobicity was achieved, these surface structures suffered from poor fastness and were easily damaged under harsh physicochemical conditions. Additionally, these superhydrophobic textiles could only be suitable for applications that require low deformation, due to the fragility of the superhydrophobic surface to a large mechanical deformation such as stretching. Until now, successful examples on developing stretchable superhydrophobic textiles are still scarce.19 The establishment of covalent bonding between 3 ACS Paragon Plus Environment


superhydrophobic coating and textile is promising, however, the relatively complicated and time-consuming process severely limits its usage for practical applications. Apart from this, integration of electrical conductivity onto stretchable superhydrophobic textiles is deemed valuable to further expand their application horizons. To date, researches about the exploitation of stretchable superhydrophobic conductive textile have been seldom reported, let alone achieving a stretchable superhydrophobic EMIST. Herein, for the first time, a superhydrophobic EMIST with high stretchability and reliability was fabricated via a highly efficient and facile drop-coating method. The superhydrophobic EMIST is composed of an original textile with a silver nanowire (AgNW) conductive layer and a superhydrophobic layer comprising carbon nanotubes (CNT), polytetrafluoroethylene (PTFE) nanoparticles and fluoroacrylic polymer (Capstone ST-110). The resultant EMIST exhibited superhydrophobic properties with a water contact angle (CA) of 160.8° and a sliding angle (SA) of 2.9°, which are desired to endow self-cleaning feature. The EMIST also showed an extraordinary EMI shielding effectiveness (EMI SE) of 51.5 dB at a thickness of only 0.6 mm. Remarkably, the superhydrophobicity and high EMI SE were highly reliable when the EMIST was subjected to large mechanical deformations (30% stretching-releasing and kneading-releasing up to 5000 cycles). The EMIST also maintained excellent superhydrophobic and EMI shielding durability against ultrasonic treatment up to 60 min, peeling test up to 100 cycles, strong acid/alkaline solutions, and different organic solvents. The facile drop-coating method combined with an excellent multifunctionality makes our EMIST an easy-fabricated, non-wetting EMI shielding materials desirable for applications under harsh environment. We envision that our findings will be helpful to design innovative and valuable textiles to extend their lifespan for practical applications.


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2. RESULTS AND DISCUSSION The superhydrophobic EMIST (CPC-AgNW/Textile) was prepared via a facile drop-coating method, as shown in Figure 1a. Briefly, the pre-determined AgNW dispersion was first dropped on the 100% pre-strained textile. After dried at 25 °C for 120 min, the released AgNW/Textile was further decorated with superhydrophobic coating (denoted as CPC) dispersion by the same drop-coating method. More detailed information on the CPC dispersion was provided in the Experimental Section and Supporting Information (Figure S1). AgNW was chosen as conductive nanomaterial to construct highly conductive networks due to its large aspect ratio (Figure S2), excellent intrinsic conductivity and low contact resistance between each other. The superhydrophobic coating consisted of CNT, PTFE and Capstone ST-110, based on the following considerations. (1) CNT has been regarded as an ideal rough template for tailoring surface roughness (Figure S3).20 Moreover, CNT can form additional conductive paths, which would contribute to further improve electrical conductivity of the CPC-AgNW/Textile. (2) Submicron PTFE particles (Figure S4 and S5), as hydrophobic fillers, can reduce surface energy and surface adhesion simultaneously. (3) Capstone ST-110 is fluoroacrylic polymer which would further reduce the surface energy of the textile. Moreover, Capstone ST-110 owns good adhesive property, which can play a key role in stabilizing the conductive and superhydrophobic coatings. Figure 1b-e showed the surface wettability of the pure textile, AgNW/Textile, and CPCAgNW/Textile. Commercially available tricot-weave textile was selected as the substrate due to high stretchability, which was woven by 82 wt% polyester yarns and 18 wt% spandex yarns. Note that the spandex yarns ran through the textile interior and the polyester yarns were exposed to the upper and lower surfaces, as shown in Figure S6. Thus, the hydrophobic nature of polyester fibers gave rise to a high initial CA of 122.6° for pure textile. The water droplets gradually spread over the textile and completely wet the surface within 100 s (Figure 1c, Video S1). After depositing AgNWs, the textile surface was hydrophilic and easily infiltrated 5 ACS Paragon Plus Environment


by water droplets due to the presence of polyvinyl pyrrolidone (PVP) as surfactant in AgNW dispersion (Figure 1d, Video S2). Once subjected to CPC coating, the coated textile again became very hydrophobic. Water droplet spheres were formed on top of the textile and held still over time (Figure 1e), indicating the effectiveness of CPC on improving the hydrophobicity of AgNW/Textile. The CA measurement revealed that the CPCAgNW/Textile held a very high CA of 160.8° (Figure 1e inset), demonstrating the achievement of superhydrophobicity. In addition, SA was employed as an indicator of CA hysteresis to further characterize the superhydrophobicity of the CPC-AgNW/textile. The SA was only 2.9° (Figure S7, Video S3), indicating excellent water repellency of CPCAgNW/Textile. To explore the mechanism underlying the evolution of surface wettability, SEM were performed and shown in Figure 1f-h. The pure textile was made of twisted yarns comprising bundles of smooth microfibers (about 12 μm in diameter) in a typical tricot-weave pattern. (Figure 1f and Figure S8a). After the AgNW coating, it was found that the fiber surface of the textile was randomly covered with interconnected AgNW networks (Figure 1g and Figure S8b). For the CPC-AgNW/Textile, a dual-scaled surface structure with micro and nanoscale roughness was observed (Figure 1h and Figure S8c). CNT bundles and PTFE particles were banded together by the Capstone ST-110 on the fiber surface, which provided nanoscale roughness to compliment the inherent microscale roughness of the textile fibers. Atomic force microscopy (AFM) was further used to evaluate surface morphology and the results were shown in Figure S9. The fibers of pure textile were relatively smooth, and the root-meansquare roughness (RMS) was 25.4 nm (Figure S9a and b). In contrast, the fibers of CPCAgNW/Textile became rough, with zonal and particulate protrusions scattered on the surface, resulting in an obvious increase of RMS to 66.7 nm (Figure S9c and d). The AFM results verified that the fibers significantly increased surface roughness after coating CPC, which was consist with SEM results. It is considered that creation of hierarchical roughness by micro and 6 ACS Paragon Plus Environment

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nanoscale structures contributed to the superhydrophobicity. The excellent water repellency of CPC-AgNW/Textile can be told from the water flow impacting test (Figure 1i, Video S4). Water flow can automatically roll away at a small slanting angle when it touched the superhydrophobic surface. In addition, the CPC-AgNW/Textile also exhibited excellent electrical conduction. As seen in Figure 1j, LED lamp emitted brilliant blue light with taking the CPC-AgNW/Textile as part of the circuit. Moreover, the brightness of LED lamp was unaffected at all even CPC-AgNW/Textile was immersed in water (Figure S10). Thus, it is nice to see that the great electrical conductivity can be extended to waterborne/underwater conditions. Figure 1k showed that the CPC-AgNW/Textile achieved an extraordinary EMI SE of 51.5 dB, which far surpassed the target for commercial EMI shielding application (20dB).21-23 The contribution of microwave absorption loss (SEA) to the EMI SE was much higher than that of microwave reflection loss (SER), indicating an absorption-dominant shielding mechanism in the CPC-AgNW/Textile. More details on the EMI shielding performance would be discussed in the following part. All the above features demonstrated the successful preparation of a highly conductive and superhydrophobic EMIST for effective EMI shielding application.



Figure 1. (a) Schematic illustration of the preparation of the CPC-AgNW/Textile. Dyed water droplets (10 μL) on (b) pure textile at initial status, (c) pure textile after 5 min, (d) AgNW/Textile at initial status, and (e) CPC-AgNW/Textile after 5 min. The insets showed the static contact angle of the water droplet. Scanning electron microscope (SEM) images of (f) pure textile, (g) AgNW/Textile with AgNW area density of 0.3 mg/cm2 and (h) CPCAgNW/Textile with AgNW area density of 0.3 mg/cm2 and CPC area density of 4 mg/cm2. (i) Water flow impacting the surface of CPC-AgNW/Textile. (j) Digital photograph showing a light emitting diode (LED) lamp under 9 V when the CPC-AgNW/Textile was used as electrically conductive elements (30 × 5 × 0.6 mm3). (k) EMI shielding performance of the CPC-AgNW/Textile with AgNW area density of 0.3 mg/cm2 and CPC area density of 4 mg/cm2. Generally, the area density of hydrophobic coating has great influence on the surface morphology and wettability of the coated textile. After being coated with CPC, the surface morphology of the CPC-AgNW/Textiles was endowed with hierarchical micro/nanoscale 8 ACS Paragon Plus Environment

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roughness (Figure S11). The coating was not only on the individual fiber surface, but also filled up the gaps between fibers with increasing CPC area density (Figure 2a-d). To study the effect of CPC area density on the hydrophobicity and electrical performance of the CPCAgNW/Textiles, CA and electrical conductivity were measured (Figure 2e). For the convenience of discussion, CPC-AgNW/Textiles with different CPC area densities were labeled as CPC-X (X=I, II, III and IV, representing the corresponding CPC area density of 1, 2, 3 and 4 mg/cm2, respectively). In contrast to the pure textile, the AgNW/Textile became quite hydrophilic due to the presence of PVP on the surfaces of AgNWs. Introduction of CPC coating imparted hydrophobicity to the CPC-AgNW/Textiles. For example, the CPC-I showed a CA of 135.2° at low area density of 1 mg/cm2. As the area density increases to 2 and 3 mg/cm2, accordingly higher CA of 143.7° and 148.5° were obtained for CPC-II and CPC-III. With furthering increasing to 4 mg/cm2, a CA of 160.8° was finally achieved for CPC-IV, and the corresponding SA was only 2.9°. Note that water droplets were tightly clung to the needle over the CA test of CPC-IV (Video S5), demonstrating low surface adhesion and remarkable water repellency of the coated textile. This allowed CPC-AgNW/Textile to selfclean the surface contaminants. In Figure 2f, the self-cleaning feature was demonstrated using CPC-IV sample. As can be seen, contaminants (soil particles from a flowerpot) on the surface came with running water droplets and quickly moved away from textile surface, leaving the surface contaminant-free. Beside the extraordinary water repellency, the CPC-AgNW/Textile also exhibited excellent electrical conductivity (Figure 2e), which is of great significance for EMI shielding applications. The effect of AgNW area density on the electrical conductivity of the AgNW/Textile was first investigated. As shown in Figure S12, the AgNW/Textile became highly electrically conductive compared to the non-conductive textile and showed a significant increase in electrical conductivity with increasing AgNW area density. This can be attributed to the high inherent electrical conductivity and large aspect ratio of AgNW, which 9 ACS Paragon Plus Environment


facilitated the formation of an interconnected conductive networks. More detailed discussions on the electrical conductivity of the AgNW/Textile were provided in Supporting Information. Given the balance of cost and electrical performance, 0.3 mg/cm2 was chosen as the main AgNW area density of the AgNW/Textile for the following CPC coating treatment. It was clear that the electrical conductivity of the CPC-AgNW/Textile gradually increased with increasing CPC area density. This phenomenon indicated the formation of additional conductive pathways on the AgNW/Textile, due to the presence of CNT in CPC coating. For example, CPC-I realized an electrical conductivity of 343.5 S/m at 1 mg/cm2 CPC area density. Increasing CPC area density to 2 and 3 mg/cm2, the corresponding electrical conductivity increased to 415.7 and 476.2 S/m for CPC-II and CPC-III. With further increasing CPC area density to 4 mg/cm2, a maximum value of 528.3 S/m was achieved in CPC-IV, which was much higher than those previously reported conductive textiles.6,7 The joint action of AgNW and CNT was responsible for the excellent electrical conductivity of the CPC-AgNW/Textile, which made it great promise for EMI shielding applications. Figure 2g showed the EMI SE of the AgNW/Textile and the CPC-AgNW/Textile (0.6 mm in thickness) with various CPC area densities in the X band frequency range (8.2–12.4 GHz). The EMI SE exhibited weak frequency dependence and thus the average EMI SE was used to evaluate the EMI shielding performance. An average EMI SE of 39.6 dB was realized for the AgNW/Textile. As compared to AgNW/textile, introduction of CPC coating layer gave rise to increased EMI SE for the CPC-AgNW/Textile, showing a similar trend to the variation of electrical conductivity. For example, the average EMI SE of CPC-I was 42.4 dB and it increased to 46.3 and 49.1 dB for CPC-II and CPC-III, respectively. Remarkably, CPCIV achieved the maximum EMI SE of 51.5 dB. In other words, only 0.0007% transmission can pass through the shielding material. The achieved EMI SE was ranked one of the best results reported in the literature about EMI shielding materials with comparable thickness (Table S1).3-5,8,24-34 Typically, an EMI SE of 22.2 dB was reported for a graphite 10 ACS Paragon Plus Environment

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oxide/polypyrrole/cotton fabric with a thickness of 2.2 mm.3 The transition metal carbide/carbonitride/polystyrene composite required 1.0 mm thickness to obtain an EMI SE of 27 dB.34 For the CPC-AgNW/Textile, the superior EMI SE was mainly attributed to its high electrical conductivity, originating from the well-developed conductive AgNW and CNT networks. It is well-known that the EMI SE of shielding materials is thickness-dependent. The larger specimen thickness means more conductive networks formed to interact with incident electromagnetic microwaves, resulting in much stronger EMI shielding performance (Figure S13). Amazingly, CPC-IV achieved an ultrahigh EMI SE of 100.2 dB at 2.4 mm thickness, which was well-qualified for most of civil and military applications. To explore the underlying EMI shielding mechanism, the contribution of SER and SEA to overall EMI SE (SEtotal) was presented in Figure 2h. Regardless of the increase of CPC area density, SEA was always much higher than SER over the entire frequency range, demonstrating an absorptiondominant shielding mechanism in the CPC-AgNW/Textile. Huge interfacial area in the CPCAgNW/Textile is beneficial to effectively attenuate incident electromagnetic microwaves through multiple times of reflection, scattering and absorption that occurred inside the material. From a practical point of view, it is crucial for shielding materials to possess superior mechanical performance. Owing to introduction of the AgNW and CPC coating layer, the CPC-AgNW/Textile was endowed with enhanced mechanical properties in comparison to pure textile, as presented in Figure 2i and Figure S14. For instance, the tensile stress and Young’s modulus of CPC-IV were 9.4 MPa and 1.2 MPa, respectively, which increased by 38% and 361% than those of pure textile. Note that all CPC-AgNW/Textiles exhibited excellent stretchability as evidenced by having elongation at break larger than 210%. Therefore, our CPC-AgNW/Textile featuring superhydrophobicity, outstanding EMI and superior mechanical performance would be of great use in all-weather, outdoors applications, such as wearable electronics, photovoltaics, or skin of robots, to ensure safety and durability. 11 ACS Paragon Plus Environment


Figure 2. SEM images of the CPC-AgNW/Textiles with CPC area densities of (a) 1 mg/cm2, (b) 2 mg/cm2, (c) 3 mg/cm2, (d) 4 mg/cm2. (e) The CA and electrical conductivity of pure textile, the AgNW/Textile and the CPC-AgNW/Textiles (CPC-I, CPC-II, CPC-III, and CPCIV). (f) The self-cleaning process of dust on the surface of CPC-IV. (g) The EMI SE of the AgNW/Textile and the CPC-AgNW/Textiles. (h) SER and SEA of the AgNW/Textile and the CPC-AgNW/Textiles. (i) Typical stress−strain curves of pure textile, the AgNW/Textile and the CPC-AgNW/Textiles. Whether the CPC-AgNW/Textiles can remain robust and have little change of the performance under mechanical deformations is vitally important to realize life-term protection of all-weather outdoor equipment. Figure 3a showed CA of CPC-IV as a function of tensile strain. The CPC-IV maintained a CA more than 157° even with the strain up to 30%. To understand the superhydrophobic behavior of CPC-IV under stretching, SEM was employed to observe its hierarchical structure change at 30% strain. It is worth noting that CPC-IV at 30% strain (Figure S15a) exhibited a similar surface morphology as its original form (Figure 1h), indicating the robustness of CPC coating layer to stretching deformation. Furthermore, CPC-IV was evaluated by a cyclic stretching-releasing measurement (Figure 3b). Its CA 12 ACS Paragon Plus Environment

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remained constant at 156.3° even after 5000 stretching-releasing cycles (30% terminal strain). The excellent stable superhydrophobicity should be attributed to the well-retained surface roughness. As shown in Figure 3b, surface morphology of CPC-IV stayed intact after 5000 stretching-releasing cycles. In addition, complex kneading deformation, involving a collective action of bending, creasing and folding was performed on PU-AgNWs/Textile to further validate the robustness of its surface features. Similarly, both the superhydrophobic property and surface morphology were well-preserved after 5000 kneading cycles (Figure 3c and Figure S15b). Next, EMI shielding was evaluated under physical deformation, i.e. stretching and kneading (Figure 3d). It was nice to see that CPC-IV maintained a high EMI SE value of 44.8 dB at 30% strain. Even after 5000 stretching-releasing cycles, the EMI SE was still as high as 42.6 dB, showing 83% retention compared to the original EMI SE. Similarly, CPC-IV also maintained 89% of the original EMI SE after 5000 kneading-releasing cycles. This deformation-independent of EMI shielding performance was mainly due to that conductive networks stayed well-preserved over the entire mechanical deformation, which hich was reflected by the reliable electrical conductivity (Figure S16). The stability mechanism behind this interesting phenomenon can arise from the unique distribution of AgNW and CPC layers on the textile, with mainly existing on fiber yarns, instead of filling whole cavities of fiber yarns (Figure 1g-i). When the tensile strain was applied to the textile, it was stretched through yarn-yarn sliding in the weaving structure due to readily available inter-yarn interactions within the elastic region. Therefore, the AgNW and CPC layers showed excellent stability, thus guaranteeing the durability of the EMI SE and superhydrophobicity for the CPCAgNW/Textile even after 5000 cycles of stretching.35



Figure 3. (a) CA of CPC-IV at different tensile strains. The inset showed the digital image of water droplets on CPC-IV at 30% strain. (b) CA of CPC-IV after various stretching–releasing cycles at 30% terminal strain. The inset showed SEM image for the surface morphology of CPC-IV after 5000 stretching-releasing cycles. (c) CA of CPC-IV after various kneadingreleasing cycles. The left inset showed the kneading state of CPC-IV specimen and the right inset showed the digital image for water droplets on CPC-IV surface after 5000 kneadingreleasing cycles. (d) EMI SE of CPC-IV before and after 5000 stretching-releasing and kneading-releasing cycles as well as the EMI SE under 30% strain. To further study the reliability of multifunctional coatings on CPC-AgNW/Textile, a variety of verification tests including ultrasonic treatments, mechanical peeling, exposure to different pH values and chemical solvents were performed. Figure 4a showed the change of CA and weight retention of CPC-IV as a function of ultrasonic time. Notably, CPC-IV did not show any notable weight loss and change of CA. After ultrasonication for 60 min, the water remained clear and transparent, suggesting no substance was released from textile surface. It was clear that AgNW and CPC coatings firmly adhered to the textile surface and were acting very robust. Next, 3M Scotch tape was applied to the textile surface and then peeled to see if 14 ACS Paragon Plus Environment

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coating might come with tape and fall off (Figure 4b). The coating was intact as evidenced from unchanging CA, which remained at 155.2° invariably, even after 100 peeling tests. In what follows, the chemical resistance of CPC-IV was tested by immersing the specimens into acid/alkali solutions and various organic solvents (e.g. ethanol, ethyl acetate, acetone, dimethyl formamide). The coating was immune to different pH solutions (pH = 2, 4, 6, 8, 10, 12) and organic solvents and stayed very stable over extensive exposure time of 10 h, which was indicated by a constant CA before and after treatment (Figure 4c and 4d). Apart from the durable superhydrophobicity, the CPC-AgNW/Textile can also maintain superior EMI shielding performance when exposed to the above-mentioned tested factors, as shown in Figure 4e. Overall, the highly reliable superhydrophobic feature and EMI SE of CPCAgNW/Textile made it very promising as durable EMI shielding material in all-weather outdoor applications against extreme environmental conditions.



Figure 4. (a) CA and weigh retention changes of CPC-IV with ultrasonic time. The insets showed the digital photographs of the sample in the bottles with water before and after ultrasonic treatment for 60 min. (b) CA change of the CPC-IV as a function of peeling cycles. The left inset showed the digital photograph for the peeling test by 3M scotch tape. The right inset showed the water droplets on CPC-IV after 100 peeling cycles. (c) Variation of CA at different pH solutions for 10 h. The inset showed the corresponding digital photograph for the water droplets on CPC-IV. (d) CA of CPC-IV before and after immersing in different organic solvents (ethanol, ethyl acetate, acetone, and dimethyl formamide) for 10 h. (e) EMI SE changes of CPC-IV before and after ultrasonic treatment for 60 min, peeling for 100 cycles, and immersing in strong acidic or alkali solution and organic solvents for 10 h, respectively. To determine the role of each coating component in the durable superhydrophobic EMIST, a series of control experiments were carried out, as presented in Table 1. In 16 ACS Paragon Plus Environment

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comparison to CPC-IV, CC-AgNW/Textile without PTFE had a lower CA of 154.5° but a higher SA of 7.4°. PC-AgNW/Textile without CNT showed an even lower CA of 145.1° and an average EMI SE of 40.3 dB. In the absence of Capstone ST-110, CP-AgNW/Textile became hydrophilic with a CA of 0°, and showed poor EMI shielding durability. Lacking of AgNWs, CPC/Textile suffered from a poor EMI SE of 13.8 dB, though it remained superhydrophobic with a CA of 161.2°. Getting rid of CPC coating results in AgNW/Textile being very hydrophilic with a CA of 0°, despite its EMI shielding is relatively high (39.6 dB). These results indicated that superhydrophobicity should be attributed to both the low surface energy of Capston ST-110 and the nanoscale roughness imparted by the combination of CNT and PTFE on the microscale textile. Moreover, addition of PTFE rendered the coating with low adhesion. Capston ST-110 also functioned as a binder to hold AgNWs, CNT and PTEF together in the coating layers, and archor them tightly on the textile surface, hence improving the durability, as shown in Figure 5. AgNWs and CNTs worked together to construct efficient conductive networks to benefit EMI shielding. In a word, superoleophobicity, superior EMI SE as well as excellent durability were derived from a synergistic combination of AgNWs, CNT, PTFE and Capston ST-110.

Table 1. Influence of coating materials on surface wettability and EMI shielding performance of the coated textile. Coated textile

CA (°)

EMI SE (dB)

Durability

CPC-AgNW/Textile

160.8±1.8

51.5±1.1

Yes

CC-AgNW/Textile

154.5±2.1

51.2±1.9

Yes

PC-AgNW/Textile

145.1±1.5

40.3±0.9

Yes

CP-AgNW/Textile

0

50.7±1.6

No

CPC/Textile

161.2±1.3

13.8±2.1

Yes

AgNW/Textile

0

39.6±1.3

No



Figure 5. Schematic for the surface morphology of CPC-AgNW coating on the textile. 3. CONCLUSION We have demonstrated the development of a robustly superhydrophobic conductive textile for efficient EMI shielding by implementing AgNW networks and a superhydrophobic coating onto a commercial textile. The superhydrophobic EMIST exhibited a high CA of 160.8° and a low SA of 2.9°, along with a superior EMI SE of 51.5 dB. The EMIST also presented high resistance to physical damages, reflected by the retentive superhydrophobic feature and EMI shielding level, even after 5000 stretching-releasing cycles. Besides, the EMIST can withstand ultrasonic treatment up to 60 min, peeling test up to 100 cycles, strong acidic/alkaline solutions and different organic solvents, indicating excellent mechanical robustness and chemical durability. The unique attributes of our EMISE were ascribed to the synergistic combination of AgNWs, CNT, PTFE and Capston ST-110. This work is expected to open up the avenue for designing superhydrophobic robust EMISTs with long life-time to serve in all-weather outdoor applications.


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4. EXPERIMENTAL SECTION 4.1. Materials Commercially available tricot-weave textile, woven by 82 wt% polyester yarns and 18 wt% spandex yarns, was purchased from Fujian Lida Knitting Co., Ltd, with an area density of 190 g/m2. AgNW/isopropyl alcohol (IPA) dispersion was provided by Zhejiang Kechuang Advanced Materials Co., Ltd. The AgNW holds an average diameter of 30 nm and an average length of 15 μm. CNT aqueous dispersion (10 wt%) was purchased from Chengdu Organic Chemicals Co., Ltd. PTFE emulsion (DISP30, DuPont) was provided by Dupont China Holding Co., Ltd, with 60 wt% solid content and a median particle size of 220 nm (The size distribution of PTFE emulsion was shown in Figure S3). Capstone ST-110 aqueous dispersion (25 wt%) was provided by DuPont Inc. Rhodamine, Congo-red, IPA, and deionized water were purchased from Chengdu Kelong Chemical Reagent Factory (Chengdu, China).

4.2. Fabrication of the superhydrophobic EMIST The CPC-AgNW/Textile was fabricated through a facile drop-coating method. First, the original textile was soaked in NaOH solution (37.5 mM) at 75 oC for 60 min, and washed in deionized water for several times under ultrasonication, followed by drying in an oven at 60 °C. Then AgNW/IPA dispersion (5 mg/mL) was dropped onto the pre-strained textile (100% pre-strain) and dried at 25 °C for 120 min. Subsequently, the superhydrophobic coating (denoted as CPC) dispersion was prepared by mixing CNT dispersion (4.00 g), PTFE emulsion (0.67 g), Capstone ST-110 dispersion (1.20 g), and deionized water (24.13 g) with a vortex mixer (2500 r/min) for 30 min. The obtained CPC dispersion was then added to the released AgNW/Textile. After dried at 80 ℃ for 60 min, the CPC coated AgNW/textile was further heated at 150 °C for 5 min. At a fixed AgNW area density of 0.3 mg/cm2, a series of CPC area densities (1, 2, 3 and 4 mg/cm2) were incorporated and the corresponding CPCAgNW/textiles were labeled as CPC-I, CPC-II, CPC-III and CPC-IV, respectively. To 19 ACS Paragon Plus Environment


illustrate the role of each ingredient in the formation of superhydrophobic coating, three kinds of compound dispersion with CNT@Capstone ST-110/deionized water (2.00 [email protected] g/12.40 g), CNT@PTFE/deionized water (2.00 [email protected] g/12.66 g), and PTFE@Capstone ST110/deionized water (0.34 [email protected] g/14.06 g) were used to prepare the coated AgNW/Textiles with an area density of 2.0 mg/cm2, which were denoted as CC-AgNW/Textiles, CPAgNW/Textiles and PC-AgNW/Textiles, respectively. Additionally, the 4.0 mg/cm2 CPC/Textile without AgNWs coating was prepared by dropping the CPC dispersion on the pure textile for comparison. 4.3. Characterization CA measurements were carried out on a Drop Shape Analysis System DSA25 (Kruess, Germany) at ambient temperature using liquid droplets of 4 μL in volume. SA was measured with a water droplet of 8 μL dropping on the substrate with a tilt angle. Both CA and SA were determined by average value from five different points on each specimen. The surface morphologies of the CPC/AgNW/Textiles were observed by a field emission scanning electron microscope (SEM) (Inspect-F, FEI, USA) at an accelerating voltage of 5 kV. Atomic force microscopy (AFM) images were performed on a Bruker Dimension Icon scanning probe microscope. The particle size distribution of PTFE emulsion was measured by a dynamic light scattering particle size analysis (DLS; Zetasizer Nano ZS90, UK). The zeta potential of CPC dispersion was determined on a dynamic light scattering particle size analysis (DLS; Zetasizer Nano ZS90, UK). EMI shielding performance was measured by an Agilent N5247A vector network analyzer, which was combined with a coaxial test cell (APC-7 connector), (Schematic of measurement setup was shown in our previous work36). The specimens with 10 mm diameter was used to fit the coaxial specimen holder. The APC-7 connector is a precision coaxial connector that can be used on laboratory microwave test equipment from frequencies up to 18 GHz. The recorded scattering parameters (S11 and S21) were applied to calculate the EMI SE (SEtotal), SER, and SEA in the frequency range of 8.2–12.4 GHz (The detailed 20 ACS Paragon Plus Environment

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calculations were shown in Supporting Information). The electrical conductivity was measured using a four-point probe (RTS-8, Guangzhou Four-Point Probe Technology Co., Ltd, China). Tensile test was performed on an Instron universal test instrument (Model 5576, Instron Instruments, USA), with crosshead speed of 10 mm/min and the gauge length of 15 mm. More than five specimens were tested for calculating the average value and standard deviation. The real-time resistance of the specimens under mechanical deformation (stretching-releasing and kneading-releasing) was recorded with a FLUKE-15B+ digital multimeter. Both ends of the specimens was covered with silver paste and connected with copper tapes to make good contact of the specimens with the electrodes. The adhesion of the AgNW and CPC coatings to textile substrates was evaluated by peeling test with 3M scotch tape and ultrasonic treatment for 60 min (ultrasonic cleaner SB-5200DT, 300 W). To examine the chemical durability, the CPC/AgNW/Textile was exposed to various harsh liquid chemicals including acidic/alkaline solutions and organic solvents (ethanol, ethyl acetate, acetone, dimethyl formamide) for 10 h, respectively. ASSOCIATED CONTENT Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI: (1) The calculation of EMI shielding effectiveness (SEtotal), microwave reflection (SER) and microwave absorption (SEA) from scattering parameters; (2) The stability of CPC dispersion; (3) SEM and TEM images of AgNWs; (4) SEM image of the CC/Textile; (5) The size distribution of PTFE emulsion; (6) SEM image of PTFE particles; (7) The fracture surface morphology of the pure textile; (8) Sliding angle (SA) of CPC-IV; (9) SEM images of pure Textile, AgNW/Textile and CPC-AgNW/Textile; (10) Atomic force microscope images of the pure textile and the CPC-AgNW/Textile; (11) The digital photograph of the CPC21 ACS Paragon Plus Environment


AgNW/Textile underwater service; (12) SEM images of the CPC-AgNW/Textile with CPC area densities; (13) The electrical conductivity of AgNW/Textile with different AgNW area density; (14) Comparison of EMI SE of different materials reported in literature; (15) The effect of thicknesses on EMI SE of CPC-IV; (17) Mechanical properties of the AgNWs/Textile and CPC-AgNW/Textile; (13) SEM image of CPC-IV at 30% strain and after 5000 kneading cycles; (18) The electrical conductivity of CPC-IV before and after undergoing deformation (PDF) AUTHOR INFORMATION Corresponding Authors *(Y.D.X) E-mail: [email protected]. *(L.Z.M.) E-mail: [email protected].

ACKNOWLEDGEMENT The authors gratefully acknowledge the financial support from the National Key R&D Program of China (Grant Nos. 2018YFB0704200), the National Natural Science Foundation of China (Grant Nos. 21704070, 51673134, and 51721091), the Science and Technology Department of Sichuan Province (Grant No. 2017GZ0412 and 2018RZ0041) and the Fundamental Research Funds for the central Universities (2017SCU04A03, sklpme2017306, 2012017yjsy102).

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