Commercial Silk-Based Electronic Yarns Fabricated Using Microwave

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Commercial silk-based electronic yarns fabricated using microwave irradiation Deokgyu Na, Junsik Choi, Jaehee Lee, Jun Woo Jeon, and Byung Hoon Kim ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.9b08873 • Publication Date (Web): 09 Jul 2019 Downloaded from pubs.acs.org on July 17, 2019

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ACS Applied Materials & Interfaces

Commercial silk-based electronic yarns fabricated using microwave irradiation AUTHOR NAMES Deokgyu Na,†,§ Junsik Choi,†,§ Jaehee Lee,† Jun Woo Jeon,†,‡,* and Byung Hoon Kim†,‡,* AUTHOR ADDRESSES †

Department of Physics, Incheon National University, Incheon 22012, Republic of Korea

‡

Research Institute of Basic Science, Incheon National University, Incheon 22012, Republic of

Korea KEYWORDS silk, pyroprotein, microwave, electrical conductivity, electronic yarn

ABSTRACT

Electronic textiles (e-textiles) are being developed because of their potential applications in wearable and flexible electronics. However, complex procedures and chemical agents are required to synthesize carbon-based e-textiles. Pyroprotein-based e-textiles, obtained by the pyrolysis of silk proteins, consume large amounts of time and energy due to the high temperature process (from

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800 °C to 2800 °C). In this study, we report a novel method of fabricating pyroprotein-based electronic yarns (e-yarns) using microwave irradiation. Microwaves were applied to pyroprotein treated at 650 °C to remove numerous heteroatoms in a short time without the high temperature process and chemical agents. The structural modulation was confirmed by Raman spectroscopy and x-ray photoelectron spectroscopy. We found that a reduction in heteroatoms and enlargement of the carbon region. The temperature-dependent resistance was well explained by the fluctuation induced tunneling model, which also showed structural modification. The electrical conductivity of the fabricated e-yarns was comparable to that of pyroprotein-based e-textiles heat-treated at 1000 °C (order of 102 S/cm), and showed electrical stability under bending.

TEXT 1. Introduction Due to the growing interest in wearable and flexible electronics, electronic textiles (e-textiles) are increasingly considered important materials in the electronic and textile industries.1-4 e-textiles are basically defined as electrically conducting textiles. Because of their unique properties, such as light weight, flexibility, and good electrical conductivity, e-textiles are expected to be employed in various applications.5-14 To provide electrical conductivity in textiles, e-textiles have been synthesized by wet-spinning with carbon-based materials,15-17 and coating the textiles with metal particles18-20 and conductive polymers21-23 have also been reported. In particular, graphene oxide (GO)-coated e-textiles have been fabricated using commercial textiles such as nylon, cotton, polyester, and silk.24,25 However, it is difficult to directly apply carbon nanotubes and graphene in


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the current textile industry. Moreover, to fabricate e-textiles by coating the guest materials requires complex procedures and chemical agents. Silk, a protein-based natural biopolymer produced by silkworms and spiders has superior mechanical property, biocompatibility, and biological functionality.26-28 In addition, a thermal transition phenomenon of silk proteins has been reported. The -sheet structures of silk proteins can be thermally transformed into a sp2-hybridized carbon hexagonal structure by simple heat treatment.29,30 By exploiting these properties, pyroprotein-based e-textiles obtained from commercial silks were recently reported. The pyroprotein-based e-textiles show high electrical conductivity, thermal durability, and bending stability.31 However, it takes a long time and requires a lot of energy to fabricate the pyroprotein-based e-textiles, due to the high temperature procedure. One way to effectively remove heteroatoms in carbon structures is to use microwaves without heating. It is known that GO can be reduced by detaching the oxygen functional groups using microwave irradiation, resulting in improved electrical properties.32-34 Accordingly, we expected that pyroprotein could be transformed into microwave-induced graphitic structures in a short time, with improved electrical conductivity. In addition, the fabrication time of pyroprotein-based etextiles can be also reduced using microwave irradiation. Here, we report a novel way to fabricate pyroprotein-based electronic yarns (e-yarns) using microwave irradiation instead of high temperature processes. We found the pyroprotein exhibited a specific resistance to reacting with microwaves, and e-yarns could be fabricated within 10 seconds. The electrical conductivity of the e-yarns in this study was highly stable even during bending, and was similar to that of pyroprotein-based e-textiles heat-treated at 1000 °C (on the order of 102 S/cm).


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2. Results and discussion Figure 1a shows scanning electron microscopy (SEM) and optical images of the commercial silk (CS) used in this study. The twisted morphology of the CS, consisting of thin silk bundles, was observed. Although shrinkage of CS volume occurred, this morphology was maintained even after heat treatment at 650 °C (P650) (Figure 1b). The color of P650 changed to black due to carbonization. The P650 was connected to a simple circuit with a blue LED lamp (circle in Fig. 1(c)) to visually demonstrate its electrical conducting property. However, no light was observed from the LED lamp. This indicates that the P650 is not electrically conductive (Figure 1c), due to the large number of heteroatoms in P650 compared to the pyroproteins treated at high temperatures.29,30 To remove heteroatoms from the P650 carbon structures, microwaves were applied using a microwave oven (2.45 GHz, 700 W). Since the pyroprotein can be burned out by microwave energy in the ambient condition, the samples were microwave irradiated in a vacuum tube (Figure 1d). We found that the pyroproteins exhibited electrical conductivity after glowing in the tube. Figure 1e shows the initial resistance-dependent reaction time (when they started to glow due to microwave irradiation) of pyroproteins treated at various temperatures (650, 660, 670, 680, 690, and 700 °C, 257 samples). We confirmed that the reaction time increased as the initial resistance of the pyroproteins increased. These results are closely related to the amount of π-conjugated systems in the pyroproteins. According to results reported in a previous study,34 it was known that microwaves are strongly absorbed in π-conjugated systems, and the absorbed energy can cause Joule heating in the system. High resistance in the pyroproteins means that there are relatively few π-conjugated systems compared to the pyroproteins with low resistance, due to a large number of


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oxygen functional groups. Therefore, it takes a relatively long time for the high resistance pyroproteins to react. Based on these results, e-yarns were prepared at the optimal heat treatment temperature of 650 °C to allow rapid reaction, within 10 seconds. Figure 1f provides SEM and optical images of the microwave-induced P650 (M650). The morphology of M650 was similar to that of P650 even after microwave irradiation. A blue LED lamp connected with the M650 (Figure 1g) lit up, and it was confirmed that the M650 was electrically conducting even when the M650 was bent (Figure 1h). To verify changes in the properties of the samples before and after microwave irradiation, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy were performed. Figures 2a, 2b, and 2c show the XPS C1s core-level spectra of the CS, P650, and M650, respectively. Since the CS consists of many functional groups, including amide groups and oxygen functional groups in the silk fibroin, numerous heteroatoms exist in the CS as shown in Figure 2a. However, the oxygen functional groups were significantly reduced after heat treatment at 650 °C due to the thermal energy (Figure 2b). Furthermore, after microwave irradiation of the P650, the amount of nitrogen and oxygen decreased, resulting in increases in chemical states of C-C and C=C, from 64.71 % for P650 to 75.07% for M650 (Figure 2c and Table 1). This indicates that high temperature is generated in the P650 due to Joule heating induced by microwave irradiation. As a result, the functional groups were detached from carbon structures by the thermal energy. Figure 2d shows the Raman spectra of P650 and M650. In the Raman spectra, the G peak (1584 cm-1) related to the in-plane vibration mode of sp2 graphitic structure and the D peak (1331 cm-1) corresponding to the disorder sp3 structure were characterized. We focused on the intensity ratio


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of the D and G peaks (ID/IG) to evaluate the defect states in the graphitic structures. After microwave treatment, the ID/IG value decreased from 1.49 to 1.31, indicating that defects in the carbon hexagonal structures were reduced by the microwaves. From the XPS and Raman spectra, we found that heteroatoms in the P650 were detached from the carbon structures by the microwave irradiation. Next, we analyzed the electrical conductivity () and temperature-dependent charge transport behavior of the e-yarns before and after microwave irradiation. The current-voltage (I-V) characteristics of one P650 and three M650s were measured using a conventional 4-probe method (Figure 3a). An increase in the slope in the graph means an increase in . The P650 exhibited a very low  (9.57 ⅹ 10-3 S/cm). However, it was observed that the slope of the three M650 samples (M650/1, M650/2, and M650/3) dramatically increased after the microwave irradiation. The values of  were 2.35 ⅹ 10 S/cm for M650/1, 6.25 ⅹ 10 S/cm for M650/2, and 1.29 ⅹ 102 S/cm for M650/3 (Figure 3b). Average conductivity (1.10 ⅹ 102 S/cm) of the 32 M650s was also obtained to demonstrate the stability and reproducibility of this method (Figure S2, Supporting Information). The conductivity of M650 was improved up to the 5 orders (from the order of 10-3 to 102) after microwave treatment. This phenomenon can be explained if the chemical bonds between the functional groups and carbon atoms were broken by the microwave. As a result, the graphitic structures were restored, as mentioned above. Moreover, the M650 samples were found to have performance similar to that of the pyroproteinbased e-textiles fabricated by heat treatment at 1000 °C.31 The XPS results showed that the P650 and M650 had numerous heteroatoms. They acted as a potential barrier between carbon clusters. As a result, the charge transport behavior in P650 and M650 originates from quantum tunneling, and this potential barrier is overcome when the temperature increases. Namely, the resistance


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decreases as the temperature increases. This behavior can be described by the fluctuation induced tunneling (FIT) model as follows,35 R(T)=R0 exp (

T1 ) T+T0

where R is the resistance and T is the temperature. T0 means the temperature above which the thermally activated conduction over the barrier begins to occur, and T1 is the energy required for an electron to cross the insulating gap between conductive clusters. Figures 3c and 3d show the temperature-dependent resistance (circles) of P650 and M650 fitted by the FIT model (red lines) from 100 K to 300 K, respectively. As expected, the P650 and M650 exhibited a decrease in resistance with increasing temperature, and the resistance in both samples were well fitted to the FIT model. It was also observed that the temperature factors T0 and T1 decreased from 337.46 K to 208.17 K and from 10185.21 K to 350.16 K, respectively. This can be interpreted to indicate that the potential barriers caused by the heteroatoms in the carbon structures were considerably reduced after the microwave irradiation. This is well consistent with the results from XPS and Raman spectroscopy. To use M650 in e-yarns, the electrical characteristics of the M650 have to be stable under bending. Accordingly, variation in conductance was investigated using a homemade bending device. Figure 4a indicates the bending position-dependent conductance of M650. The insets in Figure 4a are optical images of the bent M650 corresponding to each bending state (each bending degree was described in Figure S3, Supporting Information). The positions from 1 to 5 indicate the increase in bending degree (blue area) and positions 5 to 9 represent the return to position 1 (yellow area). We confirmed that the conductance did not change for bending degrees less than 4.9 %.


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The bending cycle-dependent conductance of M650 was also evaluated by repeatedly bending between position 1 and position 5 as shown in Figure 4b. During 650 cycles, the change in conductance was maintained within 3.7 %. From the bending test with the M650, we determined that the e-textile fabricated by microwave irradiation was stable and durable with respect to bending degree and cycles.

3. Conclusion In conclusion, we produced pyroprotein-based e-yarns using microwave irradiation in place of high temperature processes. Although the initial P650 sample exhibited poor electrical conductivity due to the existence of numerous heteroatoms between carbon structures, the electrical performance of the e-yarns was improved by microwave irradiation. After microwave treatment, the electrical conductivity of the e-yarns increased on the 5 orders (from the order of 10-3 to 102), to a level similar to that of pyroprotein-based e-textiles heat-treated at 1000 °C. Moreover, the e-yarns produced by microwave irradiation were flexible and stable even under bending. In this study, we introduced a simple way to fabricate e-yarns using microwave irradiation without high temperature processing.

4. Experimental Section Preparation of P650 and M650 produced by commercial silks. The P650 was prepared from pyrolysis of commercial silks using the same procedure reported by the previous study. 29,30 Heat treatment of the commercial silks was performed by a tube furnace (Daeheung Science). The commercial silks were placed in an alumina boat and put into the tube furnace. It was heat-treated to 150 °C in a nitrogen atmosphere and maintained the temperature (150 °C) for 1 h to remove


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absorbed water molecules. Then, the temperature was increased until 350 °C as a rate of 2.0 °C min-1. After isothermal treatment at 350 °C for 3 h, it was heated to 650 °C as a rate of 2.0 °C min1

and maintained at 650 °C for 1 h (P650). To apply the microwave onto the P650, we used the

microwave oven (Samsung) with the power of 700 W and the frequency of 2.45 GHz. Before microwave irradiation, P650 was put into the vacuum tube and then it was evacuated down to 103

Torr using a rotary pump. The M650 was obtained from microwave irradiation to P650. Measurement of electrical properties. The charge transport property of the P650 and M650

was measured by a conventional 4-probe method with a model 6221 current source (Keithley) and a model 2182 nanovoltmeter (Keithley). To confirm the temperature-dependent resistance, the samples were loaded in a closed cycle refrigerator cryostat (Seongwoo Instruments) which was evacuated by a turbo pump (10-6 Torr). The temperature was controlled at 10 K intervals from 300 K to 100 K using a model 335 temperature controller (Lake Shore Cryotronics). The variations in conductance as a function of bending positions and cycles were investigated by a homemade two probe bending device with a model 4200-SCS Semiconductor Characterization System (Keithley). The bending device is described in the Supporting Information (Figure S6) in detail. Materials characterization. SEM images were taken by a model CX-200TM (COXEM). XPS was characterized with PHI 5000 Versaprobe II (ULVAC-PHI) using a monochromatic Al-Kα xray source at 25 W. Raman spectroscopy was performed with a model LabRAM Hr800 (HORIBA Jobin Yvon) under excitation of 633 nm laser.


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FIGURES

Figure 1. Fabrication of microwave-induced e-yarns. SEM and optical images of (a) CS and (b) P650. (c) Optical image of unlighted LED lamp (red circle) connected with P650. (d) Schematic illustration of experimental procedure. (e) The initial resistance-dependent reaction time of the pyroproteins during microwave irradiation. (f) SEM and optical images of M650. The lighted blue LED lamp connected with (g) straight M650 and (h) bent M650.


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Figure 2. Characterization of the pyroproteins before and after microwave irradiation. XPS C1s core-level spectra of (a) CS, (b) P650, and (c) M650. (d) Raman spectra of P650 (black line) and M650 (red line).


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Figure 3. Charge transport properties of the e-yarns. (a) I-V characteristics of P650 (black line) and three different M650s (M650/1, M650/2, and M650/3). (b) Electrical conductivity of P650 and three M650s. Temperature-dependent electrical properties of (c) P650 and (d) M650 fitted with FIT model (red lines).


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Figure 4. Electrical stability of the e-yarns under bending. Variation in the electrical conductance of M650 as a function of (a) bending degrees and (b) bending cycles. The inset images show each bending state.

TABLE Table 1. Peak areas obtained from XPS C1s core-level spectra of CS, P650, and M650. Peak area (%) C-C & C=C

C-N

C-O

C=O

C(O)O

CS

56.53

14.83

12.61

13.76

2.27

P650

64.71

14.33

11.46

7.35

2.15

M650

75.07

9.53

7.6

5.87

1.93


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ASSOCIATED CONTENT Supporting Information. Supporting Information: Additional results such as the cross-section SEM images of the fibers, average electrical conductivity of the M650s, information of bending experiment, and optical image of stitched M650s. (PDF) Supporting Information for Review: Marked version of revised manuscript. (PDF) AUTHOR INFORMATION Corresponding Author *E-mail: [email protected] (J.W.J.) *E-mail: [email protected] (B.H.K.) Author Contributions §D.N. and J.C. contributed equally. Funding Sources National Research Foundation of Korea funded by the Ministry of Education (NRF2017R1A6A1A06015181) Incheon National University Research Grant (2018-0161)


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Notes The authors declare no competing financial interest.

ACKNOWLEDGMENT This work was supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education (NRF-2017R1A6A1A06015181) and the Incheon National University Research Grant in 2018-0161.

ABBREVIATIONS e-textiles, electronic textiles; e-yarns, electronic yarns; CS, commercial silk; P650, pyroprotein heat-treated at 650 °C; M650, microwave-induced P650.

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(33) Jiang, W.-S.; Yang, C.; Chen, G.-X.; Yan, X.-Q.; Chen, S.-N.; Su, B.-W.; Liu, Z.-B.; Tian, J.-G. Preparation of High-Quality Graphene using Triggered Microwave Reduction under an Air Atmosphere. J. Mater. Chem. C 2018, 6, 1829-1835. (34) Han, H. J.; Chen, Y. N.; Wang, Z. J. Effect of Microwave Irradiation on Reduction of Graphene Oxide Films. RSC Adv. 2015, 5, 92940-92946. (35) Sheng, P. Fluctuation-Induced Tunneling Conduction in Disordered Materials. Phys. Rev. B 1980, 21, 2180-2195.

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Commercial Silk-Based Electronic Yarns Fabricated Using Microwave

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