Twistable and Stretchable Sandwich Structured. Fiber for Wearable Sensors and Supercapacitors

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1 Supporting Information Twistable and Stretchable Sandwich Structured Fiber for Wearable Sensors and Supercapacitors Changsoon Choi 1, Jae Myeong Lee 1, Shi Hyeong Kim 1, Jiangtao Di 2, Ray H. Baughman 3* and Seon Jeong Kim 1* 1. C. Choi, J. M. Lee, S. H. Kim, Prof. S. J. Kim Center for Self-powered Actuation, Department of Biomedical Engineering, Hanyang University, Seoul 04763, Korea 2. Prof. J. Di Suzhou Institute of Nano-Tech and Nano-Bionics,Chinese Academy of Sciences, Suzhou, Jiangsu , China. 3. Prof. R. H. Baughman The Alan G. MacDiarmid NanoTech Institute, University of Texas at Dallas, Richardson, TX, 75083, USA. These authors equally contributed to this work. *To whom correspondence should be addressed. Keywords: Strain Sensor, Elastomeric Supercapacitor, Buckled Nanotubes, Sandwich Fiber

2 Experimental Section Sandwich Fiber Preparation: Dielectric core fiber with a rectangular cross-section was obtained by cutting commercially available Ecoflex 0030 film into narrow ribbons. This core fiber was stretched about 300%, and about 120 layers of CNT sheets, drawn from a CNT forest, were deposited as electrodes on opposite fiber sides (so that the CNT alignment direction was parallel to the fiber direction). Ethanol was repeatedly dropped on the CNT surface for evaporation-based densification of the deposited sheets. The microbuckled CNT structure was formed on the fiber surface during fiber relaxation from the fabrication strain. For sensing and electrochemical performance measurements, the CNT electrodes of the sandwich fiber electrode were electrically connected to 180 µm diameter Cu wire by using silver paste. Finally, the silver paste and Cu wire were coated with silicone paste (Wacker) for insulation. MnO 2 and PEDOT Pseudocapacitive Coating: The electrochemical deposition of MnO 2 on the pristine CNT surfaces of the sandwich fiber was performed by using a potentiostatic method. Approximately 1.3 V (vs. Ag/AgCl as the reference electrode and Pt mesh as the counter electrode in the three-electrode system) was applied by using an electrochemical analyzer (CHI 627b system; CH instruments, Austin, TX). The electrolyte contained 0.02 M MnSO 4 5H 2 O and 0.2 M Na 2 SO 4 (all chemical products were purchased from Sigma-Aldrich). The vapor-phase polymerization (VPP) method was utilized to polymerize EDOT that was dropped around the CNT surfaces of the sandwich fibers. A 20 wt% solution of iron(iii) p-toluenesulfonate hexahydrate (Fe(III)PTS) in butanol (containing 1.6 volume % of pyridine) was diluted to 8 wt% of oxidant and used as the oxidizing agent for the polymerization. The diluted catalyst solution was dropped on the CNT electrodes of the

3 sandwich fibers and dried at 60 C for approximately 30 minutes. These catalyst-containing CNT electrodes were then exposed to EDOT vapor at 60 C for 1 hour in a VPP chamber. Characterization: The morphology of the CNT electrode surfaces of the sandwich fiber were determined by scanning electron microscopy (SEM-S4700 microscope, Hitachi). All capacitance measurements for the capacitive strain sensor were obtained using an E4980A LCR meter (HP E4980A precision LCR meter, Agilent technology). A home-built machine equipped with a motor (K6G3C, GGM) and a reducer (K6RG6NC-D, GGM) was used to insert twist into the sandwich fibers. Electrochemical Performance Characterization and Specific Capacitance Calculation: The PVA LiCl gel electrolyte was prepared by using 4.5 g PVA (M w 146, ,000) and 6 g LiCl in 30 ml deionized water. The solution was heated at 90 C until it became transparent (all chemical products were purchased from Sigma-Aldrich and used without further processing). The fabrication of both symmetric and asymmetric sandwich fiber supercapacitors were completed by coating the entire device with 15 wt% PVA LiCl gel electrolyte. All static electrochemical measurements for solid-state fiber supercapacitors utilized the two-electrode configuration and were obtained using an electrochemical analyzer (CHI 627b system; CH instruments, Austin, TX). CV curves during dynamic deformation were measured at 10 mv s 1 as the fiber supercapacitor was stretched and released at 4% s 1 strain rate, and twisted and untwisted at 35 rad m 1 s 1. The capacitance of a single electrode was calculated from the CV curves. From C = I/(dV/dt), where I is average current, the specific areal capacitance (C sp ) was calculated using: C sp (F/cm 2 ) = 2C/A surface, where A surface is the surface area of one side of a sandwich fiber. The total length of the sandwich was used

4 for the linear capacitance calculation. For a given constant scan rate ν and initial discharge voltage (V i ), the energy was calculated using E= 1 3,600ν 0 IVdV V i.

5 Figure S1. Schematic illustration showing the fabrication process used to obtain the sandwich fiber sensors. (i) An Ecoflex silicone rubber core fiber was stretched about 300%; (ii) CNT aerogel sheets, drawn from a multiwalled carbon nanotube forest, were wrapped on opposite sides of the fiber; and (iii) the fiber was relaxed from the fabrication strain to form microbuckled electrodes. Figure S2. Photo image showing PU mask removing process using tweezer (scale bar = 3 mm).

6 Figure S3. Fiber-direction linear resistance of an electrode of a non-stretched sandwich fiber as a function of a) the number of CNT layers in the electrode (N) and b) N -1. Figure S4. Scanning electron microscopy (SEM) image showing the surface of a 200% stretched sandwich fiber with partially unbuckled CNT wrinkles (scale bar: 25 µm).

7 Figure S5. Surface SEM image of sandwich fiber after deformation cycles (200 times for each 200% stretching, 1700 rad m -1 twisting, and 150 o bending). Figure S6. Capacitance change versus applied tensile strain for a sandwich fiber sensor. The slope of the curve indicates sensitivity.

8 Figure S7. Dynamic capacitance change in response to various pressures applied perpendicular to the electrodes of a sandwich fiber sensor. Figure S8. a) Photographs of twisted sandwich fiber sensors having bias angles of 0, 37, and 57, which were obtained by inserting twists of 0, 850, and 1700 rad m 1, respectively. b) The measured ratio of the maximum thickness of a twisted sandwich sensor (d) to the interelectrode separation for the non-twisted sensor (d 0 ) as a function or the bias angle of the twisted sandwich fiber sensor. Here and elsewhere, fiber twist was inserted while the sandwich fiber was held at fixed length.

9 Figure S9. Converted tensile strain versus length-normalized twist angle for sandwich fiber. The slope was calculated by experimentally measuring the fiber thickness decrease per tensile strain ( d/ε = mm/%) and per twist insertion ( d/length normalized twist angle = mm/rad m -1 ). Figure S10. a) CV curves (scan rate from 10 to 100 mv s -1 ) and b) galvano-static charge/discharge curves (current density from 0.03 to 0.33 ma cm -2 ) for PEDOT/CNT anode sandwich fiber measured in 0.1 M Na 2 SO 4 solution using three electrode system (Ag/AgCl, and Pt mesh were used as reference, and counter electrodes, respectively).

10 Figure S11. a) CV curves (scan rate from 10 to 100 mv s-1) and b) linear, and areal specific capacitances as a function of scan rate for asymmetric, solid-state sandwich fiber supercapacitor, coated with 15 wt% PVA LiCl gel electrolyte. Figure S12. Surface SEM images for MnO2 coated (a) pristine, (b) twisted (1700 rad m 1), (c) stretched (200%) cathode side, and PEDOT coated (d) pristine, (e) twisted (1700 rad m 1 ), (f) stretched (200%) anode side for sandwich fiber (all scale bar is 10 µm).

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