Effect of KOH addition on electrochemical properties of coal-based active carbon foams
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摘要: 以强黏性炼焦煤为原料，经常压自发泡法制得的煤基泡沫炭（NCF）为碳基底，KOH为活化剂，采用机械混合、水溶液浸渍、乙醇浸渍三种不同的方式制备煤基活性泡沫炭（HPCs），并将其用作双电层电容器的电极材料，研究了KOH添加方式对其微观结构和电化学性能的影响。结果表明，KOH分散度和附着性对煤基活性泡沫炭孔隙结构的生成、晶体结构、表面化学性质以及电化学性能有显著影响。煤基泡沫炭本身具有三维连通泡孔结构，有利于活化剂（KOH）深入材料的泡孔内部并为其提供大量附着位点，增大活化剂与碳基体的接触面积进而发生高效的活化。KOH水溶液的流动性较好，可以使K+更有效地穿插在NCF的泡孔结构中，在活化过程中作用于缺陷部位，在碳基体内部基质上产生更多的微孔以及介孔结构，有效地放大了活化效果。KOH水溶液浸渍泡沫炭材料制得的ACF-W样品拥有最高的比表面积（3098.35 m2/g）、总孔体积（1.68 cm3/g）、介孔体积比（59.13%），将其用作电极材料表现出优异的比电容（310 F/g）以及循环稳定性。Abstract: Using strong-caking coking coal as raw material, coal-based carbon foam (NCF) was prepared by constant pressing and self-foaming method and used as carbon base to produce coal-based active carbon foamed (HPCs) together with KOH activator, which was used as electrode material for double-layer capacitor. The effects of KOH added by mechanical mixing, aqueous solution impregnation and ethanol solution impregnation methods on microstructure and electrochemical properties of the prepared materials were studied. The results show that formation of pore structure, crystal structure, surface chemistry and electrochemical performance of HPCs are significantly affected by KOH dispersion and adhesion. The NCF itself has a three-dimensional connected bubble pore structure, which is conducive to the activator (KOH) penetrating into the bubble pore and providing a large number of attachment sites, thus increasing the contact area between the activator and the carbon matrix and resulting in efficient activation. The good fluidity of KOH solution can make K+ more effectively interspersed in the bubble structure of NCF, act on the defect site during activation, and generate more micropores and mesoporous structures on the internal matrix of carbon matrix, effectively amplifying the activation effect. ACF-W obtained by KOH aqueous impregnation has the highest specific surface area (3098.35 m2/g), total pore volume (1.68 cm3/g), mesoporous volume ratio (59.13%). It shows excellent specific capacitance (310 F/g) and cycle stability when used as electrode material.
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Key words:
- carbon foam /
- KOH addition method /
- double layer capacitor /
- electrochemical performance
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图 2 电极的组装和三电极体系中电化学性能测试示意图
Figure 2 Schematic diagram of electrode assembly and electrochemical performance test in three-electrode system
图 3 （a）RC、（b）NCF、（c）RC-W、（d）ACF-M、（e）ACF-W和（f）ACF-E的SEM照片
Figure 3 SEM images of (a) RC, (b) NCF, (c) RC-W, (d) ACF-M, (e) ACF-W and (f) ACF-E
图 4 不同样品的N2吸附-脱附等温线（a）和t-plot 法孔径分布（b）
Figure 4 N2 adsorption/desorption isotherms of different samples (a) and PSD from t-plot method (b) of different samples
图 5 不同样品的比表面积和比率（a）以及孔隙体积及比值（b）
Figure 5 Specific surface area distribution and ratio analysis (a) and pore volume distribution and ratio analysis (b) of different samples
图 6 样品的XRD谱图（a）和ACF-E的分峰拟合（b）
Figure 6 XRD patterns of samples (a) and the split-peak fitting diagram of ACF-E (b)
图 7 （a）样品的Raman谱图和（b）ACF-E的分峰拟合图
Figure 7 (a) Raman patterns of samples and (b) split-peak fitting diagram of ACF-E
图 8 （a）样品的XPS全谱；（b）ACF-M、ACF-W、ACF-E的C 1s XPS分峰拟合谱图；（c）RC-W的C 1s XPS分峰拟合谱图；（d）ACF-M、ACF-W、ACF-E的O 1s XPS分峰拟合谱图；（e）RC-W的O 1s XPS分峰拟合谱图；（f）FT-IR谱图
Figure 8 (a) XPS survey spectra of samples; (b) Deconvolution C 1s XPS spectra of ACF-M, ACF-W, ACF-E; (c) Deconvolution C 1s XPS spectra of RC-W; (d) Deconvolution O 1s XPS spectra of ACF-M, ACF-W, ACF-E; (e) Deconvolution O 1s XPS spectra of RC-W; (f) FT-IR spectra
图 9 三电极体系下HPCs电极的电化学性能（（a）10 mV/s扫描速率下的CV曲线；（b）1 A/g电流密度下的GCD曲线）
Figure 9 Electrochemical performances of HPCs as supercapacitor electrode in the three-electrode configuration ((a) CV curves at a scan rate of 10 mV/s; (b) GCD at current density of 1 A/g)
图 10 三电极体系下HPCs电极的电化学性能（（a）−（d）在5−100 mV/s扫描速率下的CV曲线；（e）−（h）在0.5−50 A/g电流密度下的GCD曲线）
Figure 10 Electrochemical performances of HPC as supercapacitor electrode in the three-electrode configuration ((a)−(d) CV curves at the scan rates of 5−100 mV/s; (e)−(h) GCD curves at different current densities of 0.5−50 A/g)
图 11 （a）比电容（Cg）与电流密度的关系和（b）HPCs的BET比表面积分布、孔径分布与比电容（Cg）的关系
Figure 11 (a) Dependence of specific capacitance (Cg) on various current densities and (b) Relationship between BET specific surface area distribution, pore size distribution and specific capacitance (Cg) of HPCs
图 13 两电极体系下ACF-W作为超级电容器电极的电化学性能（（a）在5−500 mV/s扫描速率下的CV曲线；（b）在0.5−50 A/g电流密度下的GCD曲线；（c）比电容与电流密度的关系；（d）Nyquist图）
Figure 13 Electrochemical performances of ACF-Ws as supercapacitor electrode in the two-electrode configuration ((a) CV curves at the scan rates of 5−500 mV/s; (b) GCD curves at different current densities of 0.5−50 A/g; (c) Dependence of specific capacitance (Cg) on various current densities; (d) Nyquist plots)
图 14 （a）ACF-W//ACF-W的Ragone图和（b）ACF-W//ACF-W在5 A/g的循环稳定性及库伦效率
Figure 14 (a) Ragone plots of ACF-W//ACF-W and (b) Cycling stability and corresponding coulombic efficiency of ACF-W//ACF-W at 5 A/g
表 1 原料煤的煤质分析
Table 1 Proximate and ultimate analyses of coal
Proximate analysis w/% Ultimate analysis wdaf/% G Mad Ad Vdaf FCdaf C H N O* S 0.63 10.52 29.18 70.82 77.85 4.48 1.36 15.17 1.14 95 Note: ad is air-dried basis; d is dry basis; daf is dried and ash-free basis; G is caking index;
*: by difference.
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表 2 不同样品的孔结构
Table 2 Pore structure parameters of different samples
Sample SBET/
(m2·g−1)Smic/
(m2·g−1)vtotal/
(cm3·g−1)vmic/
(cm3·g−1)vmes/
(cm3·g−1)vmes/vtotal dave/
nmYield/% RC 2.23 1.21 3.14 × 10−3 4.79 × 10−4 2.66 × 10−3 84.76 5.65 − NCF 1.43 0.99 1.54 × 10−3 3.56 × 10−4 1.18 × 10−3 76.87 4.31 − RC-W 1739.32 1419.21 0.85 0.61 0.24 28.43 1.96 36.23 ACF-M 3023.46 1755.84 1.59 0.75 0.84 52.56 2.11 48.26 ACF-W 3098.35 1628.27 1.68 0.68 0.99 59.13 2.16 50.50 ACF-E 2850.44 1921.94 1.44 0.81 0.63 43.74 2.02 50.75
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表 3 不同样品的孔隙结构特征
Table 3 Pore structure characteristics of different samples
Sample SBET(0.5−1 nm)/
(m2·g−1)SBET(1−2 nm)/
(m2·g−1)SBET(2−8 nm)/
(m2·g−1)v(0.5−1 nm)/
(cm3·g−1)v(1−2 nm)/
(cm3·g−1)v(2−8 nm)/
(cm3·g−1)RC-W 752.89 329.77 137.33 0.21 0.20 0.16 ACF-M 900.24 600.44 412.97 0.27 0.36 0.52 ACF-W 789.09 670.78 454.46 0.22 0.41 0.59 ACF-E 926.41 588.60 308.11 0.26 0.36 0.37
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表 4 KOH水溶液与KOH乙醇溶液的黏度对比
Table 4 Viscosity comparison between KOH aqueous solution and KOH ethanol solution
Sample KOH aqueous solution KOH ethanol solution Viscosity/(MPa·s) 0.53 1.58
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表 5 样品的微晶结构参数
Table 5 Crystal structure parameters of samples
Sample Aγ 2θ002/(°) 2θ100/(°) A002 d002/nm La/nm Lc/nm fa N RC 5036.69 25.21 43.92 11133.75 0.3531 2.02 2.55 0.6885 7.21 NCF 3957.89 25.19 43.89 10925.60 0.3535 2.23 2.81 0.7341 7.94 RC-W 443.75 25.71 43.75 1842.42 0.3464 3.58 1.49 0.8059 4.31 ACF-M 174.69 25.88 43.50 1045.83 0.3443 3.67 1.56 0.8569 4.54 ACF-W 188.38 25.39 43.03 1232.29 0.3507 3.79 1.58 0.8674 4.51 ACF-E 416.79 23.77 43.71 3702.12 0.3744 4.39 1.70 0.8988 4.55
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表 6 XPS光谱所得样品表面元素相对含量
Table 6 Related concentration of the chemical element on the surface of samples from XPS spectra
Sample Concentration of chemical element/% C O N S RC 75.02 21.48 2.74 0.76 NCF 90.60 6.48 2.16 0.77 RC-W 86.26 12.34 1.11 0.30 ACF-M 90.43 8.01 1.36 0.20 ACF-W 87.44 11.40 0.96 0.20 ACF-E 87.64 10.86 1.13 0.37
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表 7 样品的C 1s和O 1s光谱分峰拟合
Table 7 Contribution of the components in the area of C 1s and O 1s XPS spectra
Sample Relative content of different types of
oxygen on the surface
/%Relative content of different types of
carbon on the surface
/%C=O IO C−O sp2-C sp3-C C−O C=O RC 32.79 2.75 64.46 61.92 12.30 3.73 2.44 NCF 39.10 3.43 57.48 84.66 9.07 3.61 2.66 RC-W 68.03 2.41 29.56 57.59 26.61 7.57 8.23 ACF-M 80.99 − 19.01 60.41 24.03 7.02 8.53 ACF-W 74.82 − 25.18 61.27 22.92 6.87 8.93 ACF-E 77.34 − 22.66 61.85 22.54 6.91 8.70
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表 8 三电极体系中不同炭材料比容量（Cg）对比
Table 8 Specific capacitance (Cg) comparison of different carbon materials under the three-electrode configuration
Precursor SBET/
(m2·g−1)Current density/
(A·g−1)Cg/
(F·g−1)Electrolyte Ref. Bituminous coal 3098.4 0.5 310 6 mol/L KOH this work Agricultural wastes 952.0 1.0 160 6 mol/L KOH [38] Pitaya peel 1872.0 1.0 255 6 mol/L KOH [51] Lignite 2728.0 1.0 246 6 mol/L KOH [52] Bituminous coal 2784.0 0.5 293 6 mol/L KOH [17] Coal 877.0 1.0 260 6 mol/L KOH [53] Zhundong coal 1872.0 1.0 211 6 mol/L KOH [35] Taixi anthracite 984.6 1.0 199 6 mol/L KOH [22] Anthracite coal 2455.0 0.05 104 6 mol/L KOH [54] Qitaihe bituminous 2985.9 1.0 194 6 mol/L KOH [55]
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