超级电容器用低阶煤基活性炭的制备及电化学性能研究
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摘要
超级电容器是一种介于传统电容器与电池之间的新型储能元件，具有广阔的应用前景和巨大的经济价值。活性炭是制造超级电容器电极的首选材料，其结构及性质对超级电容器的性能起着关键性作用。本文以低阶煤为原料，采用低温N_2吸附法、XRD、SEM、FTIR及XPS等方法，系统考察了KOH活化法制备超级电容器用低阶煤基活性炭的制备工艺、低阶煤种类及煤炭有机显微组分等对活性炭孔结构和性能的影响；探索了微波加热活化法（微波法）及中低温（＜600℃）活化条件下制备超级电容器用活性炭的工艺及方法；深入研究了活性炭的孔结构、微观结构及表面化学性质对其电极材料电化学性能的影响规律及KOH活化法制备低阶煤基活性炭的活化机理。
研究表明，以低阶煤为原料可制备出孔结构及表面化学性质可调的超级电容器用活性炭。原料煤原生孔隙丰富、挥发分高有利于促进活性炭中孔结构的发育；煤中无机矿物成分不仅会削弱活化反应剧烈程度，而且会降低活性炭的质量及性能。以褐煤为原料，KOH为活化剂，可制备出比表面积为665～3885m~2/g，总孔容为0.356～2.211cm~3/g，中孔率为18.8～74.9%的煤基活性炭。改变碱炭比及活化温度等工艺参数，可以有效调控活性炭的孔结构和表面化学性质。煤炭显微组分对活性炭孔结构、表面化学性质及电化学性能有一定影响。惰质组所制活性炭的比表面积最大，中孔率及氧含量最高，其电极材料在KOH和有机电解液体系中的电化学性能最优，其次为镜质组与壳质组所制活性炭。
对活性炭电极材料电化学性能的研究发现，在KOH电解液体系中，微孔对电极材料比电容的贡献稍大于中孔，当活性炭的BET比表面积超过2500m2/g后，表面化学性质对提高电极材料的比电容比孔结构更为重要；在有机电解液体系中，中孔对比电容的贡献远大于微孔，活性炭的孔结构是影响电极材料比电容的主要因素，表面含氧官能团对提高电极材料的比电容基本没有促进作用。针对两种电解液体系对活性炭电极材料孔结构和表面化学性质的要求不同，制备出在KOH及有机电解液体系中比电容分别高达420F/g和197F/g的低阶煤基活性炭，并形成了按不同电解液体系设计、制备超级电容器用煤基活性炭的思路。
将微波法用于低阶煤基活性炭的制备，实现了活性炭的高效活化。以褐煤为原料，KOH为活化剂，采用微波法可制备出比表面积为2097m~2/g，总孔容为1.193cm~3/g，中孔率为53.6%的超级电容器用煤基活性炭。改变碱炭比及微波加热时间可以对活性炭的孔结构进行调控。
探索出中低温活化条件制备超级电容器用活性炭的新方法。该方法所制活性炭具有中等比表面积，丰富的表面官能团，高的成型密度等特点，在KOH电解液体系中具有优异的电化学性能，其质量比电容最高可达369F/g，面积比电容可达23.1μF/cm~2，体积比电容可达215F/cm~3。通过微波法对该活性炭进行二次活化处理，可大幅度提高其在有机电解液体系中的电化学性能。
提出KOH活化法制备低阶煤基活性炭的分段活化机理：脱水阶段（＜200℃），主要是活化料中水分脱除；预活化阶段（200～400℃），主要是在原料煤表面引入活性组分；中低温活化阶段（400～600℃），主要是活性炭微孔的形成与发展；高温活化阶段（600℃以上），主要是活性炭微孔的扩展。
Supercapacitor is a new energy storage device which between conventional capacitor and battery, it has wide application prospect and huge economic value. Activated carbon is the first choice electrode materials for supercapacitor, its structure and properties play a key role to supercapacitor performance. In this paper, activated carbons for supercapacitor were prepared from low-rank coal by KOH chemical activation. The effects of the preparation technological, low-rank coal types and organic maceral components on the pore structure and performance of activated carbon were systematically investigated by nitrogen adsorption at77K, XRD, SEM, FTIR and XPS. Preparation technology and method of activated carbon for supercapacitor prepared by microwave heating and moderate temperature (<600℃) activation condition were discussed. The influence of pore structure, microstructure and surface chemical properties of activated carbon to the electrochemical performance of electrode materials were also studied. Finally, activation mechanism of preparation low-rank coal based activated carbon by KOH chemical activation was investigated.
The results showed that activated carbon with adjustable pore structure and surface chemical properties for supercapacitor can be prepared from low-rank coal. Abundant primitive pores and high volatile of raw coal were advantageous to develop mesopore, and the mineral not only weakened the activation reaction intensity, but also degraded the quality and performance of activated carbon. Activated carbons were prepared from lignite with KOH as activation agent, which specific surface area was665～3885m2/g, total pore volume was0.356～2.211cm3/g and the ratio of mesopore was18.8～74.9%. The pore structure and surface chemical properties of activated carbon can be tailored effectively by changing technological conditions, such as the weight ratio of KOH to coal, activation temperature and so on. Moreover, the pore structure, surface chemical properties and electrochemical performance of activated carbon were affected by maceral components. Activated carbon prepared from inertinite of low-rank coal had the largest specific surface area, highest ratio of mesopore and oxygen content, therefore its electrode materials had the most excellent electrochemical performance in KOH and (C2H5)4NBF4/PC electrolyte, secondly were activated carbons prepared from vitrinite and exinite.
Based on investigating the electrochemical performance of activated carbon electrode materials, it was found that the contribution of micropore to the specific capacitance was slightly more important than mesopore in KOH electrolyte, when the specific surface area of activated carbon exceeded2500m2/g, surface chemical properties was more important than pore structure to improve the specific capacitance of electrode materials. In (C2H5)4NBF4/PC electrolyte, the contribution of mesopore to the specific capacitance was remarkable more important than micropore, the pore structure was crucial factor to affect the specific capacitance of activated carbon electrode materials, the surface oxygen-containing functional groups of activated carbon had no effect to improve the specific capacitance. In view of KOH and (C2Hs)4NBF4/PC electrolyte had different requirements to pore structure and surface chemical properties of activated carbon electrode materials, activated carbons were prepared from low-rank coal, which specific capacitance reached420F/g and197F/g, respectively. The opinion about designing and preparing coal based activated carbons for supercapacitor according to different electrolyte was also pointed out
The efficient activation of low-rank coal based activated carbon was realized by microwave heating. Activated carbon for supercapacitor was prepared from lignite by microwave heating with KOH as activation agent, which specific surface area was2097m2/g, total pore volume was1.193cm3/g and the ratio of mesopore was53.6%. The pore structure of activated carbon can be tailored effectively by changing the weight ratio of KOH to coal and microwave heating time.
A new method of preparation activated carbon for supercapacitor under moderate temperature activation condition was explored. The activated carbon prepared under moderate temperature activation condition exhibited moderate specific surface area, abundant surface functional groups and high pressing density, and it had excellent electrochemical performance in KOH electrolyte. Furthermore, the gravimetric specific capacitance, surface specific capacitance and volumetric specific capacitance of the as-prepared activated carbon can reach369F/g,23.1μF/cm2and215F/cm3, respectively. The electrochemical performance in (C2Hs)4NBF4/PC electrolyte can be improved remarkably after reactivated by microwave heating.
Segmented activation mechanism of preparation low-rank coal based activated carbon by KOH chemical activation was propounded, such as dehydration (<200℃) pre-activation (200～400℃), moderate temperature activation (400～600℃) and high temperature activation (>600℃). The main function of each stage are shown as following, dehydration was to removal moisture from activation materials, pre-activation was to induce active components on the raw coal surface, moderate temperature activation was to form and develop micropores, and high temperature activation was to widen micropores of activated carbon.
研究表明，以低阶煤为原料可制备出孔结构及表面化学性质可调的超级电容器用活性炭。原料煤原生孔隙丰富、挥发分高有利于促进活性炭中孔结构的发育；煤中无机矿物成分不仅会削弱活化反应剧烈程度，而且会降低活性炭的质量及性能。以褐煤为原料，KOH为活化剂，可制备出比表面积为665～3885m~2/g，总孔容为0.356～2.211cm~3/g，中孔率为18.8～74.9%的煤基活性炭。改变碱炭比及活化温度等工艺参数，可以有效调控活性炭的孔结构和表面化学性质。煤炭显微组分对活性炭孔结构、表面化学性质及电化学性能有一定影响。惰质组所制活性炭的比表面积最大，中孔率及氧含量最高，其电极材料在KOH和有机电解液体系中的电化学性能最优，其次为镜质组与壳质组所制活性炭。
对活性炭电极材料电化学性能的研究发现，在KOH电解液体系中，微孔对电极材料比电容的贡献稍大于中孔，当活性炭的BET比表面积超过2500m2/g后，表面化学性质对提高电极材料的比电容比孔结构更为重要；在有机电解液体系中，中孔对比电容的贡献远大于微孔，活性炭的孔结构是影响电极材料比电容的主要因素，表面含氧官能团对提高电极材料的比电容基本没有促进作用。针对两种电解液体系对活性炭电极材料孔结构和表面化学性质的要求不同，制备出在KOH及有机电解液体系中比电容分别高达420F/g和197F/g的低阶煤基活性炭，并形成了按不同电解液体系设计、制备超级电容器用煤基活性炭的思路。
将微波法用于低阶煤基活性炭的制备，实现了活性炭的高效活化。以褐煤为原料，KOH为活化剂，采用微波法可制备出比表面积为2097m~2/g，总孔容为1.193cm~3/g，中孔率为53.6%的超级电容器用煤基活性炭。改变碱炭比及微波加热时间可以对活性炭的孔结构进行调控。
探索出中低温活化条件制备超级电容器用活性炭的新方法。该方法所制活性炭具有中等比表面积，丰富的表面官能团，高的成型密度等特点，在KOH电解液体系中具有优异的电化学性能，其质量比电容最高可达369F/g，面积比电容可达23.1μF/cm~2，体积比电容可达215F/cm~3。通过微波法对该活性炭进行二次活化处理，可大幅度提高其在有机电解液体系中的电化学性能。
提出KOH活化法制备低阶煤基活性炭的分段活化机理：脱水阶段（＜200℃），主要是活化料中水分脱除；预活化阶段（200～400℃），主要是在原料煤表面引入活性组分；中低温活化阶段（400～600℃），主要是活性炭微孔的形成与发展；高温活化阶段（600℃以上），主要是活性炭微孔的扩展。
Supercapacitor is a new energy storage device which between conventional capacitor and battery, it has wide application prospect and huge economic value. Activated carbon is the first choice electrode materials for supercapacitor, its structure and properties play a key role to supercapacitor performance. In this paper, activated carbons for supercapacitor were prepared from low-rank coal by KOH chemical activation. The effects of the preparation technological, low-rank coal types and organic maceral components on the pore structure and performance of activated carbon were systematically investigated by nitrogen adsorption at77K, XRD, SEM, FTIR and XPS. Preparation technology and method of activated carbon for supercapacitor prepared by microwave heating and moderate temperature (<600℃) activation condition were discussed. The influence of pore structure, microstructure and surface chemical properties of activated carbon to the electrochemical performance of electrode materials were also studied. Finally, activation mechanism of preparation low-rank coal based activated carbon by KOH chemical activation was investigated.
The results showed that activated carbon with adjustable pore structure and surface chemical properties for supercapacitor can be prepared from low-rank coal. Abundant primitive pores and high volatile of raw coal were advantageous to develop mesopore, and the mineral not only weakened the activation reaction intensity, but also degraded the quality and performance of activated carbon. Activated carbons were prepared from lignite with KOH as activation agent, which specific surface area was665～3885m2/g, total pore volume was0.356～2.211cm3/g and the ratio of mesopore was18.8～74.9%. The pore structure and surface chemical properties of activated carbon can be tailored effectively by changing technological conditions, such as the weight ratio of KOH to coal, activation temperature and so on. Moreover, the pore structure, surface chemical properties and electrochemical performance of activated carbon were affected by maceral components. Activated carbon prepared from inertinite of low-rank coal had the largest specific surface area, highest ratio of mesopore and oxygen content, therefore its electrode materials had the most excellent electrochemical performance in KOH and (C2H5)4NBF4/PC electrolyte, secondly were activated carbons prepared from vitrinite and exinite.
Based on investigating the electrochemical performance of activated carbon electrode materials, it was found that the contribution of micropore to the specific capacitance was slightly more important than mesopore in KOH electrolyte, when the specific surface area of activated carbon exceeded2500m2/g, surface chemical properties was more important than pore structure to improve the specific capacitance of electrode materials. In (C2H5)4NBF4/PC electrolyte, the contribution of mesopore to the specific capacitance was remarkable more important than micropore, the pore structure was crucial factor to affect the specific capacitance of activated carbon electrode materials, the surface oxygen-containing functional groups of activated carbon had no effect to improve the specific capacitance. In view of KOH and (C2Hs)4NBF4/PC electrolyte had different requirements to pore structure and surface chemical properties of activated carbon electrode materials, activated carbons were prepared from low-rank coal, which specific capacitance reached420F/g and197F/g, respectively. The opinion about designing and preparing coal based activated carbons for supercapacitor according to different electrolyte was also pointed out
The efficient activation of low-rank coal based activated carbon was realized by microwave heating. Activated carbon for supercapacitor was prepared from lignite by microwave heating with KOH as activation agent, which specific surface area was2097m2/g, total pore volume was1.193cm3/g and the ratio of mesopore was53.6%. The pore structure of activated carbon can be tailored effectively by changing the weight ratio of KOH to coal and microwave heating time.
A new method of preparation activated carbon for supercapacitor under moderate temperature activation condition was explored. The activated carbon prepared under moderate temperature activation condition exhibited moderate specific surface area, abundant surface functional groups and high pressing density, and it had excellent electrochemical performance in KOH electrolyte. Furthermore, the gravimetric specific capacitance, surface specific capacitance and volumetric specific capacitance of the as-prepared activated carbon can reach369F/g,23.1μF/cm2and215F/cm3, respectively. The electrochemical performance in (C2Hs)4NBF4/PC electrolyte can be improved remarkably after reactivated by microwave heating.
Segmented activation mechanism of preparation low-rank coal based activated carbon by KOH chemical activation was propounded, such as dehydration (<200℃) pre-activation (200～400℃), moderate temperature activation (400～600℃) and high temperature activation (>600℃). The main function of each stage are shown as following, dehydration was to removal moisture from activation materials, pre-activation was to induce active components on the raw coal surface, moderate temperature activation was to form and develop micropores, and high temperature activation was to widen micropores of activated carbon.
引文
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