Glycine-derived nitrogen-doped ordered mesoporous carbons with a bimodal mesopore size distribution for supercapacitors and oxygen reduction
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摘要: 掺氮多孔炭材料在电化学能量储存和转化方面具有良好的应用前景。可控的氮原子掺杂与孔结构设计对提高其性能起着重要作用。本工作利用无溶剂纳米铸造法，以甘氨酸（Gly）为单一前驱体、以SBA-15为硬模板，制备了掺氮有序介孔炭材料（N-OMCs）。甘氨酸在SBA-15孔道内的限域热解对提高碳产率、氮掺杂量以及构筑双介孔结构非常重要。N-OMCs具有高比表面积（923~1374 m2·g−1）、大孔隙体积（1.32~2.21 cm3·g−1）、双介孔分布（4.8和6.2~20 nm）和高氮含量（3.66%~12.23%）。通过改变Gly/SBA-15的质量比和温度，可以调节材料的结构有序性、粒径、孔隙率和氮掺量。N-OMCs作为电极材料在超级电容器中具有较高性能。最佳样品在0.5 A·g−1时具有298 F·g−1的比电容、高倍率性能（在30 A·g−1时保留70%）与良好的循环稳定性。同时，N-OMCs在电催化氧还原反应（ORR）中也表现出良好性能。最佳样品的起始电位和半波电位分别为0.92和0.83 V，极限电流密度为5.06 mA·cm−2。本工作还讨论了N-OMCs的理化性质与其性能的关系。Abstract: Nitrogen-doped carbon materials are promising for electrochemical energy storage and conversion. Dopant control and pore engineering play important roles in improving their performance. We have synthesized nitrogen-doped ordered mesoporous carbons (N-OMCs) with a bimodal mesopore size distribution using a solvent-free nanocasting method. The simplest amino acid (glycine, Gly) was used as the only carbon precursor and ordered mesoporous silica SBA-15 as the hard template. The confined pyrolysis of Gly in SBA-15 leads to efficient carbonization, nitrogen doping and an interesting structure. The N-OMCs have high surface areas (923–1374 m2·g−1), large pore volumes (1.32–2.21 cm3·g−1), a bimodal distribution of mesopore sizes (4.8 and 6.2–20 nm) and high nitrogen contents (3.66%–12.23%). The effects of the Gly/SBA-15 mass ratio (1–3) and carbonization temperature (700–1000 °C) on the physicochemical properties of the N-OMCs were studied. When used as electrode materials the N-OMCs have a high performance in supercapacitors. A typical sample has a large specific capacitance of 298 F·g−1, a good rate capability (70% retention at 30 A·g−1) and high stability. The different capacitances and rate capabilities of the N-OMCs are discussed by correlating them with their physicochemical properties. A balance of surface area, degree of graphitization, nitrogen doping, and an open mesoporous structure is essential to achieve the best performance. The N-OMCs also have a good performance in the electrocatalytic oxygen reduction reaction. A typical sample has a high onset of 0.92 V, a high half-wave potential of 0.83 V and a large limiting current density of 5.06 mA·cm−2.
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Key words:
- Mesoporous carbon /
- Nanocasting /
- Nitrogen doping /
- Glycine /
- Supercapacitor /
- Oxygen reduction
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Figure 1. Schematic illustration of the synthesis process of the N-OMCs: (a) the molecular structure of Gly and structure model of SBA-15, (b) Gly in the mesopores loaded by melting infiltration and the molecular models of Gly cohesive forces and silica-Gly adhesive forces, (c) polymerized Gly binding with the silica surface, (d) carbon nanowires with pore voids inside the silica mesopores after carbonization and (e) structure model of the final N-OMCs after the silica removal.
Figure 2. Small-angle XRD patterns of (a) the SBA-15 template and the N-OMCs obtained with different Gly/SBA-15 mass ratios at 800 °C, and (b) the N-OMCs with a fixed Gly/SBA-15 mass ratio of 2.5 at different temperatures, respectively.
Figure 3. (a) Wide-angle XRD patterns and (b) Raman spectra of the N-OMCs obtained at different temperatures with a fixed Gly/SBA-15 mass ratio of 2.5.
Figure 4. Low-magnification SEM images of (a) the SBA-15 template and the N-OMCs obtained at 800 °C with a Gly/SBA-15 mass ratio of (b) 1, (c) 1.5, (d) 2, (e) 2.5 and (f) 3, respectively.
Figure 5. HRSEM images of (a) the SBA-15 template and the N-OMCs obtained at 800 °C with a Gly/SBA-15 mass ratio of (b) 1, (c) 1.5, (d) 2, (e) 2.5 and (f) 3, respectively.
Figure 6. TEM characterization of several N-OMCs obtained at 800 °C with different Gly/SBA-15 mass ratios: (a) TEM image of N-OMC-Gly-1.5-800; (b) TEM, (c, g) DF-STEM, (d) HRTEM and (h-j) the elemental maps of N-OMC-Gly-2.5-800; and (e) TEM and (f) HRTEM images of N-OMC-Gly-3-800.
Figure 7. N2 adsorption-desorption isotherms and the corresponding pore size distribution curves of (a, b) the N-OMCs obtained with different Gly/SBA-15 mass ratios at 800 °C and (c, d) at different temperatures with a Gly/SBA-15 mass ratio of 2.5, respectively.
Figure 8. (a) XPS survey spectrum, and (b) high-resolution N 1s, (c) C 1s and (d) O 1s XPS spectra of various N-OMCs.
Figure 9. (a) CV and (b) GCD curves, (c) capacitance at different current densities, (d) the Nyquist plots, and (e) capacitance retention for cyclic test and the inset CV curves before and after cycling of the N-OMCs obtained at different temperatures with a Gly/SBA-15 mass ratio of 2.5.
Figure 10. (a) Capacitance at different current densities and (b) the Nyquist plots of the N-OMCs obtained at 800 °C with different Gly/SBA-15 mass ratios.
Figure 11. (a) CV curves of N-OMC-Gly-2.5-1000 in N2- and O2-saturated 0.1 mol L−1 KOH solution, (b) LSV curves of the samples obtained at 700–1000 °C with a Gly/SBA-15 mass ratio of 2.5, and (c) LSV curves at different rotation speeds and the corresponding (d) K-L plots of N-OMC-Gly-2.5-1000.
Table 1. Summary of textural properties of the template SBA-15 and the N-OMCs obtained with different Gly/SBA-15 mass ratios and temperatures.
Samples SBET (m2·g−1) Smicro (m2·g−1) Vtotal (cm3·g−1) Vmicro (cm3·g−1) Pore size (nm) SBA-15 535 54 1.09 0.018 9.4 N-OMC-Gly-1-800 1374 18 2.00 0.004 4.3, 6.2-20 N-OMC-Gly-1.5-800 1306 86 2.21 0.034 4.7, 6.2-20 N-OMC-Gly-2-800 1203 104 2.03 0.043 4.8, 6.2-20 N-OMC-Gly-2.5-800 1030 132 1.60 0.056 4.8, 6.2-20 N-OMC-Gly-3-800 923 182 1.32 0.078 4.8, 6.2-20 N-OMC-Gly-2.5-700 954 149 1.42 0.065 4.8, 6.2-20 N-OMC-Gly-2.5-900 1166 106 1.88 0.045 5.5, 6.2-20 N-OMC-Gly-2.5-1000 1060 123 1.76 0.053 5.0, 6.2-20 
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Table 2. Summary of the chemical compositions from elemental analysis and the supercapacitor performances of the N-OMCs obtained with different Gly/SBA-15 mass ratios and temperatures.
Samples C (%) N (%) N/C ratio Capacitance (F·g−1 at 0.5 A·g−1) Rate capability at 30 A·g−1 N-OMC-Gly-1-800 79.66 5.83 0.063 227 73% N-OMC-Gly-1.5-800 80.98 6.84 0.072 249 71% N-OMC-Gly-2-800 77.26 8.32 0.092 248 65% N-OMC-Gly-2.5-800 81.24 9.08 0.096 298 70% N-OMC-Gly-3-800 79.26 9.20 0.100 95 70% N-OMC-Gly-2.5-700 71.92 12.23 0.150 209 47% N-OMC-Gly-2.5-900 83.88 4.68 0.048 184 73% N-OMC-Gly-2.5-1000 80.88 3.66 0.039 185 75%
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