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1 Copyright WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, Germany, Supporting Information for Adv. Energy Mater., DOI: /aenm Screen-Printable Thin Film Supercapacitor Device Utilizing Graphene/Polyaniline Inks Yanfei Xu,* Matthias Georg Schwab, Andrew James Strudwick, Ingolf Hennig, Xinliang Feng, Zhongshuai Wu, and Klaus Müllen*
2 Supporting Information for Adv. Energy Mater., DOI: /aenm Screen-Printable Thin Film Supercapacitor Device Utilizing Graphene/Polyaniline Inks Yanfei Xu 1 *, Matthias Georg Schwab 1, Andrew James Strudwick 1, Ingolf Hennig 2, Xinliang Feng 3, Zhongshuai Wu 3, and Klaus Müllen 3 * Materials: Nano graphene platelet (NGP, N002-PDR ) was purchased from Angstron Materials Inc., the NGP thickness is ~1-10 nm, electrical conductivity is around S/cm, when measured in form of a compressed pellet. Polyaniline (CAS Number , Aldrich) was purchased from Sigma-Aldrich. The polyaniline (emeraldine base, undoped) average molecular weight is ~5,000, electrical conductivity is ~10-9 S/cm. PTFE (60% in water) was purchased from DuPont Company. The carbon fabric (34BA) was purchased from SGL Carbon SE. The flexible carbon substrate (H2315 IX 11) is purchased from Freudenberg. Instruments and measurements: Ball milling experiments have been carried out using a Dispermat Vma-Getzmann, GMBH, D Reichshof ball miller. The milling ball material is ZrO 2 68%/ SiO 2 32% (SAZ- Zirkonmischoxid ER 120 S, bead diameter mm). The printing experiments have been carried out using a fully automated Screen Printer (Alraun Technik, AT 701 M), with Sefar sreen mesh (32-100W PW). Viscosity is measured by HAAKE analytical instruments, using a 60 mm Ø, 0.5 o cone and plate. The XPS analyses were carried out with a Phi Versa Probe 5000 spectrometer using monochromatic Al Kα radiation (49 W). Raman spectra taken with an NT-MDT NTEGRA Raman spectrometer (grating with 600 lines/mm used) with an Argon Ion laser operating at a wavelength of 514 nm. A 20X optical objective was used to focus the Laser spot which was filtered to 10% of its maximum power using a neutral density filter (leading to ~1 mw power on the sample surface). The exposure time used was 100 s. 1 1
3 Scanning electron microscope (SEM) measurements are carried out with a Zeiss Ultra 55 (FE- SEM), operated at 5 kv. Nitrogen adsorption and desorption isotherm measurements are carried out at 77 K with a Quantachrom Autosorb 6B analyzer. Electrochemical Measurements: In a three-electrode system, the cell is equipped with NGP/PANI carbon fabric as the working electrode, a platinum plate as the counter electrode and a SCE as a reference electrode, 1 M H 2 SO 4 is used as the aqueous electrolyte. The NGP/PANI electrode diameter is 2 cm, and electrochemical measurements are carried out on an EG&G potentiostat/galvanostat Model 2273 instrument. The NGP/PANI weights of the electrode materials is the difference weight between the substrate weight before printing and the substrate weight after printing. In a symmetric two-electrode system, the NGP/PANI electrodes (diameter 2 cm) on the carbon fabric substrate are assembled in a stainless steel supercapacitor cell with titanium electrodes. For the flexible supercapacitor, two the NGP/PANI 1:1.5 thin film electrodes (2.3 cm X 2.6 cm) on a flexible carbon substrates are used as the active electrodes, and the carbon substrate is used as the current collector. A separator paper is placed between the two electrodes. The device is thermally encapsulated within a laminated pouch. All electrochemical measurements are carried out using 1 M H 2 SO 4 as the electrolyte. The electrochemical impedance spectroscopy, cyclic voltammetry, and galvanostatic chargedischarge were measured on an electrochemical workstation IM6eX Zahner Elektrik at room temperature. 2 2
4 Figure S1. (A) NGP powder XRD pattern. (B, C) SEM image of the bulk NGP materials. (D) TEM images of NGP, indicating the curved NGP material can be dispersed at the state of 3 3
5 exfoliated, crumpled graphene sheets in ethanol. (E, F) XPS spectrum of the surface of NGP sample. Figure S2. The viscosity vs. shear rate curves for NGP/PANI based inks: (1) NGP, (2) NGP/PANI 1:0.5, (3) NGP /PANI 1:1, (4) NGP/PANI 1:1.5, (5) NGP /PANI 1:2, (6) PANI. Figure S3. (A) The NGP/PANI 1:1.5 patterns screen-printed on the hard carbon fabric substrate, (B) The NGP/PANI 1:1.5 pattern screen-printed on soft carbon substrate, (C) The NGP/PANI 1:1.5 thin film active electrode for the supercapacitor. Figure S4. Raman spectrum of NGP and NGP/PANI thin films. A 20X optical objective was used to focus the laser spot which was filtered to 10% of its maximum power using a neutral 4 4
6 density filter (leading to ~1 mw power on the sample surface). The exposure time used was 100 s. Figure S5. (A, B) SEM surface images of the NGP/PANI 1:0.5. (C, D) SEM images of the graphene/pani 1:1 and (E, F) NGP/PANI 1:2. Figure S5A, S5C, S5E show low-magnification SEM images. Figure S5B, S5D, S5F show high-magnification SEM images, the morphology of NGP/PANI sheets. Figure S6. CV results of the NGP and NGP/PANI thin film electrodes at different scan rates, in 1.0 M aqueous H 2 SO 4 electrolyte, three-electrode system. (A) NGP, (B) NGP/PANI 1:0.5, (C) NGP/PANI 1:1, (D) NGP/PANI 1:2. 5 5
7 Figure S7. CV results of the NGP and NGP/PANI thin film electrodes at different scan rates, in 1.0 M aqueous H 2 SO 4 electrolyte, two-electrode system. (A) NGP, (B) NGP/PANI 1:0.5, (C) NGP/PANI 1:1, (D) NGP/PANI 1:2. Figure S8. (A) Specific capacitance as a function of scan rate in two-electrode system, with 1M H 2 SO 4 aqueous electrolyte. (B) Galvanostatic charge-discharge curves of NGP/PANI 1:1.5 electrodes. 6 6
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