Abstract
Micro- and mesoporous carbide-derived carbons (CDCs) were synthesised from TiC powder via a gas-phase reaction using HCl and Cl2 within the temperature range of 700–1,100 °C. Analysis of X-ray diffraction results show that TiC-CDCs consist mainly of graphitic crystallites. The first-order Raman spectra showed the graphite-like absorption peaks at ~1,577 cm−1 and the disorder-induced peaks at ~1,338 cm−1. The low-temperature N2 sorption experiments were performed, and specific surface areas up to 1,214 and 1,544 m2 g−1 were obtained for TiC-CDC (HCl) synthesised at T = 800 °C and TiC-CDC (Cl2) synthesised at T = 900 °C, respectively. For the TiC-CDC powders synthesised, a bimodal pore size distribution has been established with the first maximum in the region up to 1.5 nm and the second maximum from 2 to 4 nm. The energy-related properties of supercapacitors based on 1 M (C2H5)3CH3NBF4 in acetonitrile and TiC-CDC (Cl2) and TiC-CDC (HCl) as electrode materials were also investigated by cyclic voltammetry, impedance spectroscopy, galvanostatic charge/discharge and constant power methods. The specific energy, calculated at U = 3.0 V, are maximal for TiC-CDC (Cl2 800 °C) and TiC-CDC (HCl 900 °C), which are 43.1 and 31.1 W h kg−1, respectively. The specific power, calculated at cell potential U = 3.0 V, are maximal for TiC-CDC (Cl2 1,000 °C) and TiC-CDC (HCl 1,000 °C), which are 805.2 and 847.5 kW kg−1, respectively. The Ragone plots for CDCs prepared by using Cl2 or HCl are quite similar, and at high power loads, the TiC-CDC material synthesised using Cl2 at 900 °C, i.e. the material with optimal pore structure, delivers the highest power at constant energy.
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Acknowledgments
This work was supported in part by the Estonian Ministry of Education and Research (project SF0180002s08), by the Estonian Centre of Excellence in Science: High Technology Materials for Sustainable Development, by the graduate school “Functional Materials and Technologies”, receiving funding from the European Social Fund under project 1.2.0401.09-0079 in Estonia and by the Estonian Science Foundation under project no. 8172. Prof. K. Kirsimäe from the Institute of Ecology and Geography and Dr. I. Sildos from the Institute of Physics at the University of Tartu are thanked for the help with the XRD and Raman studies of carbon samples, respectively.
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Tallo, I., Thomberg, T., Kurig, H. et al. Supercapacitors based on carbide-derived carbons synthesised using HCl and Cl2 as reactants. J Solid State Electrochem 17, 19–28 (2013). https://doi.org/10.1007/s10008-012-1850-0
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DOI: https://doi.org/10.1007/s10008-012-1850-0