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1 Supporting Information N,P-co-doped Meso-/microporous Carbon Derived from Biomass Materials via a Dual-activation Strategy as High-performance Electrodes for Deionization Capacitors Dong Xu,, Ying Tong,, Tingting Yan, Liyi Shi, and Dengsong Zhang*, School of Materials Science and Engineering, Jiangsu University, No. 301 Xuefu Road, Zhenjiang , P. R. China Research Center of Nano Science and Technology, Shanghai University, No. 99 Shangda Road, BaoShan District, Shanghai , P. R. China *To whom correspondence should be addressed: Fax: ; Tel: ; dszhang@shu.edu.cn. S1
2 Characterization The morphology of fabricated materials were studied by using scanning electron microscopy (SEM, JEOL JSM-700F) and transmission electron microscopy (TEM, JEOL JEM-200CX). The graphitization degree of the sample was examined by X-Ray diffraction (XRD) and Raman (JY H800UV). The N and P elements on the surface of MMC was tested by X-ray photoelectron spectroscopy (XPS, Perkin-Elmer PHI 5000C). The elemental mapping and energy dispersive X-ray spectroscopy (EDX) was examined by an Inca Energy 200 TEM system from Oxford Instruments.. The thermogravimetry (TG) was tested on PE Paris 1 TGA instrument under the atmosphere of N 2 and heated at 800 o C with a heating rate of 10 o C min -1. The N 2 adsorption-desorption tests were carried out on an Autosorb-IQ2, Quantachrome Corporation at 77 K. The pore size distributions were obtained using nonlocal density functional theory (NLDFT). The surface wettability of the electrodes was conducted on a drop shape analysis system (Krüss, DSA100). S2
3 Figure S1 TG curves of the Pomelo Peel under the atmosphere of N 2 with a heating rate of 10 o C min -1 from 25 o C to 800 o C. The pyrolysis process of pomelo peel was presented in Figure S1. The process could be divided into three stages. Stage Ⅰwas attributed to the removing of water in the biomass materials. StageⅡ could be correlated to the decomposition of lignose and cellulose, which could create a lot of volatile components. Stage Ⅲ was related to the decomposition of the remaining materials. S3
4 Figure S2 TEM images of (a, b) K-C, (c, d) P-C and (e, f) D-C. S4
5 Figure S3 (a) C 1s, (b) N 1s and (c) P 2p XPS spectra of MMC. The XPS spectra of O, N and P can be seen from the Figure S3. The doped amount of N and P is 0.7% and 0.12%, respectively. The C 1s spectrum can be divided into four peaks at 284.5, 285.6, 286.3, and ev, corresponding to C-C, C-N, C-O, and C=C, respectively (Figure S3a). 1 Similarly, the N 1s spectrum can be divided into two kinds of nitrogen functional groups, one is pyridinic nitrogen (N-6), the other is pyrrolic nitrogen (N-5) (Figure S3b). 2-3 N-6 atom is in a six-membered ring which is located at the edge of the graphitic carbon layer by replacing a carbon atom, and N-5 is a nitrogen atom in a five-membered ring, respectively, indicating that there are two forms of nitrogen atoms in the sample. Meanwhile, the main peak of the high-resolution P2p peak spectrum at eV (Figure S3c) corresponds to P-C binding. 4 S5
6 Figure S4 (a) XRD patterns and (b) Raman spectra of MMC. The XRD patterns of MMC (Figure S4a) indicate that the obtained materials are graphite-like. 5 As shown in the Raman spectra (Figure S4b), the I D /I G of MMC is 1.06, suggesting the MMC has more defects. 6-7 It can be concluded that the MMC has much defective structures due to the hierarchically porous structure. S6
7 Figure S5 Current transient curves and charge efficiency for the electrodes in a mg L -1 NaCl solution at 1.4 V. S7
8 Figure S6 CV curves of (a) MMC, (b) K-C, (c) P-C, and (d) D-C electrodes at a scan rate of 1-30 mv s -1. All the curves were obtained in a 0.5 M NaCl aqueous solution. S8
9 Figure S7 CV curves of the two electrodes at 10 mv s -1. All the curves were obtained in a 0.5 M NaCl aqueous solution. The change of the prepare process of MMC-4h is that the sample was heated at 800 o C for 4 h during the second activation process. The specific capacitances of MMC-2h and MMC-4h are 66.9 F g -1 and 51.4 F g -1. S9
10 Figure S8 Electrosorption behavior of MMC, K-C, P-C, and D-C electrodes. S10
11 Figure S9 The plot of ph-fluctuation in the process of desalination at 1.4 V in a 500 mg L -1 NaCl aqueous solution with a flow rate of 40 ml min -1. S11
12 Table S1 The element compositions of the samples. Samples Element compositions (%) C O N P MMC The sample after the first-step calcination The sample after the second-step calcination S12
13 Table S2 Comparison of SAC of various carbon electrode materials from the literatures. Electrode material Cell voltage (V) NaCl concentration (mg L -1 ) SAC (mg g -1 ) Ref. Activated Carbon Graphene AerogelS Nitrogen-doped Porous Carbon Spheres Porous Carbon Polyhedra Graphenic Fibers Nitrogen-doped Porous Carbon D Hierarchical Carbon D Graphene Architectures MMC This work MMC This work S13
14 References (1) Qie, L.; Chen, W.; Xu, H.; Xiong, X.; Jiang, Y.; Zou, F.; Hu, X.; Xin, Y.; Zhang, Z.; Huang, Y. Synthesis of functionalized 3D hierarchical porous carbon for high-performance supercapacitors. Energy Environ. Sci. 2013, 6, (2) Lee, W.; Moon, J. Monodispersed N-Doped Carbon Nanospheres for Supercapacitor Application. ACS Appl. Mater. Interfaces 2014, 6, (3) Aijaz, A.; Fujiwara, N.; Xu, Q. From metal organic framework to nitrogen-decorated nanoporous carbons: high CO 2 uptake and efficient catalytic oxygen reduction. J. Am. Chem. Soc. 2014, 136, (4) Paraknowitsch, J. P.; Zhang, Y.; Wienert, B.; Thomas, A. Nitrogen-and phosphorus-co-doped carbons with tunable enhanced surface areas promoted by the doping additives. Chem. Commun. 2013, 49, (5) Luo, W.; Wang, B.; Heron, C. G.; Allen, M. J.; Morre, J.; Maier, C. S.; Stickle, W. F.; Ji, X. Pyrolysis of cellulose under ammonia leads to nitrogen-doped nanoporous carbon generated through methane formation. Nano Lett. 2014, 14, (6) Lv, Y.; Gan, L.; Liu, M.; Xiong, W.; Xu, Z.; Zhu, D.; Wright, D. S. A self-template synthesis of hierarchical porous carbon foams based on banana peel for supercapacitor electrodes. J. Am. Chem. Soc. 2012, 209, (7) Jänes, A.; Kurig, H.; Lust, E. Characterisation of activated nanoporous carbon for supercapacitor electrode materials. Carbon 2007, 45, (8) Chen, Z.; Song, C.; Sun, X.; Guo, H.; Zhu, G. Kinetic and Isotherm Studies on the Electrosorption of NaCl from Aqueous Solutions by Activated Carbon Electrodes. Desalination 2011, 267, (9) Yin, H.; Zhao, S.; Wan, J.; Tang, H.; Chang, L.; He, L.; Zhao, H.; Gao, Y.; Tang, Z. Three-Dimensional Graphene/Metal Oxide Nanoparticle Hybrids for High-Performance Capacitive Deionization of Saline Water. Adv. Mater. 2013, 25, (10) Liu, Y.; Chen, T.; Lu, T.; Sun, Z.; Chua, D. H. C.; Pan, L. Nitrogen-Doped Porous Carbon Spheres for Highly Efficient Capacitive Deionization. Electrochim. Acta 2015, 158, (11) Liu, Y.; Xu, X.; Wang, M.; Lu, T.; Sun, Z.; Pan, L. Metal-Organic Framework-Derived Porous Carbon Polyhedra for Highly Efficient Capacitive Deionization. Chem. Commun. 2015, 51, (12) Pugazhenthiran, N.; Sen Gupta, S.; Prabhath, A.; Manikandan, M.; Swathy, J. R.; Raman, V. K.; Pradeep, T. Cellulose Derived Graphenic Fibers for Capacitive Desalination of Brackish Water. ACS Appl. Mater. Interfaces 2015, 7, (13) Wang, Z.; Yan, T.; Fang, J.; Shi, L.; Zhang, D. Nitrogen-doped porous carbon derived from a bimetallic metal organic framework as highly efficient electrodes for flow-through deionization capacitors. J. Mater. Chem. A 2016, 4, (14) Zhao, S.; Yan, T.; Wang, H.; Zhang, J.; Shi, L.; Zhang, D. Creating 3D Hierarchical Carbon Architectures with Micro-, Meso-, and Macropores via a Simple Self-Blowing Strategy for a Flow-through Deionization Capacitor. ACS Appl. Mater. Interfaces 2016, 8, (15) Shi, W.; Li, H.; Cao, X.; Leong, Z. Y.; Zhang, J.; Chen, T.; Zhang, H.; Yang, H. Y. Ultrahigh Performance of Novel Capacitive Deionization Electrodes Based on a Three-Dimensional Graphene Architecture with Nanopores. Sci. Rep. 2016, 6, S14
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