KOH添加方式对煤基活性泡沫炭电化学性能的影响

周慧敏; 杨暖暖; 符海朝; 王美君; 申岩峰; 刘冬; 王建成; 常丽萍

doi:10.1016/S1872-5813(23)60372-X

KOH添加方式对煤基活性泡沫炭电化学性能的影响

doi: 10.1016/S1872-5813(23)60372-X

周慧敏^{1, 2,},
杨暖暖^{1, 2,},
符海朝^{1, 2,},
王美君^{1, 2,},
申岩峰^{1, 2,},
刘冬^{1, 2, 3,},
王建成^{1, 2,},
常丽萍^{1, 2, ,}

1.
太原理工大学省部共建煤基能源清洁高效利用国家重点实验室, 山西太原 030024
2.
太原理工大学化学工程与技术学院, 山西太原 030024
3.
山西省丹源碳素股份有限公司, 山西晋中 030900

基金项目: 晋中市科技重点研发计划（Y201002）资助

详细信息

作者简介:
周慧敏（1998−），女，山西大同人，硕士研究生。E-mail：2024745429@qq.com

通讯作者:
E-mail：lpchang@tyut.edu.cn

中图分类号: TQ536
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- 文章访问数: 103
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- PDF下载量: 20
- 被引次数: 0
出版历程
- 收稿日期: 2023-03-04
- 修回日期: 2023-04-21
- 录用日期: 2023-05-05
- 网络出版日期: 2023-06-14

Effect of KOH addition method on electrochemical properties of coal-based active carbon foams

ZHOU Huimin^{1, 2
,},
YANG Nuannuan^{1, 2
,},
FU Haichao^{1, 2
,},
WANG Meijun^{1, 2
,},
SHEN Yanfeng^{1, 2
,},
LIU Dong^{1, 2, 3
,},
WANG Jiancheng^{1, 2
,},
CHANG Liping^{1, 2
, ,}

1.
State Key Laboratory of Clean and Efficient Coal Utilization, Taiyuan University of Technology, Taiyuan 030024, China
2.
College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024, China
3.
Shanxi Danyuan Carbon Holdings Co., Ltd., Jinzhong 030900, China

Funds: The project was supported by Jinzhong Key Research and Development Plan of Science and Technology (Y201002)

摘要

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⁺更有效的穿插在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。
- 煤基泡沫炭 /
- KOH添加方式 /
- 双电层电容器 /
- 电化学性能
Abstract: Using strong viscous 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 the coal-based active carbon foamed (HPCs) together with KOH activator, which would be used as electrode material for double-layer capacitor. The effects of KOH added by mechanical mixing, aqueous solution impregnation and ethanol solution impregnation on the microstructure and electrochemical properties of prepared materials were studied. The results show that the formation of pore structure, crystal structure, surface chemistry and electrochemical performance of coal-based active carbon foam are significantly affected by KOH dispersion and adhesion. The coal-based carbon foam itself has a three-dimensional connected bubble pore structure, which is conducive to the activator (KOH) to penetrate into the material's bubble pore and provide a large number of attachment sites for it, thus increasing the contact area between the activator and the carbon matrix and resulting in efficient activation. The fluidity of KOH aqueous solution is good, which can make K⁺ more effectively interspersed in the bubble structure of NCF, act on the defect site during the activation process, 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 method has the highest specific surface area (3098.35 m²/g), total pore volume (1.68 cm³/g), mesoporous volume ratio (59.13%), and shows excellent specific capacitance (310 F/g) and cycle stability when used as electrode material.
- carbon foam /
- KOH addition method /
- double layer capacitor /
- electrochemical performance

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图 1 原料煤膨胀度和流动度曲线

Figure 1 Dilatation and fluidity curves of raw coal

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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

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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

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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

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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

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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)

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图 7 （a）样品的Raman谱图（b）ACF-E的分峰拟

Figure 7 (a) Raman patterns of samples (b) The split-peak fitting diagram of ACF-E

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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

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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 curves at a current density of 1 A/g

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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

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图 11 （a）比电容（C_g）与电流密度的关系；（b）HPCs的BET比表面积分布、孔径分布与比电容（C_g）的关系

Figure 11 (a) Dependence of specific capacitance (C_g) on various current densities; (b) Relationship between BET specific surface area distribution, pore size distribution and specific capacitance (C_g) of HPCs

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图 12 HPCs的Nyquist图

Figure 12 Nyquist plots of HPCs

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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 (C_g) on various current densities; (d) Nyquist plots

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图 14 （a）ACF-W//ACF-W的Ragone图；（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; (b) Cycling stability and corresponding coulombic efficiency of ACF-W//ACF-W at 5 A/g

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表 1 原料煤的煤质分析

Table 1 Proximate and ultimate analyses of coal

Proximate analysis w/%				Ultimate analysis w_daf/%					G
M_ad	A_d	V_daf	FC_daf	C	H	N	O*	S	G
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	S_BET/ (m²·g⁻¹)	S_mic/ (m²·g⁻¹)	v_total/ (cm³·g⁻¹)	v_mic/ (cm³·g⁻¹)	v_mes/ (cm³·g⁻¹)	v_mes/v_total	d_ave/ nm	Yield/%
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	S_{BET(0.5−1 nm)}/ (m²·g⁻¹)	S_{BET(1−2 nm)}/ (m²·g⁻¹)	S_{BET(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乙醇溶液的粘度对比

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	A_γ	2θ₀₀₂/°	2θ₁₀₀/°	A₀₀₂	d₀₀₂/nm	L_a/nm	L_c/nm	f_a	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 /(at.%)
Sample	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 the X-ray photoelectron C 1s and O 1sspectra

Sample	The relative content of different types of oxygen on the surface /%			The relative content of different types of carbon on the surface /%
Sample	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（C_g）对比

Table 8 Specific capacitance (C_g) comparison of different carbon materials under the three-electrode configuration

Precursor	S_BET/ (m²·g⁻¹)	Current density/ (A·g⁻¹)	C_g/ (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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