活性碳/硬碳非对称超级电容器的研究
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摘要
化学电源作为一种将化学能转换为电能的高效能量转换装置越来越受到关注和重视。超级电容器是介于常规电容器和二次电池之间的一种新型储能装置,它具有较常规电容器更大的容量和能量以及比二次电池更高的功率密度,且能够进行快速充放电,拥有极长的使用寿命和较宽的工作温度范围。超级电容器的使用十分广泛,比如在航空航天军事方面、移动通信技术、电子消费产品、燃料电池、电动汽车和城市交通以及太阳能和风能中都有重要而广阔的应用前景,其中有的应用领域还是无法代替的。将超级电容器和二次电池组合形成的混合动力电源系统,能够很好地满足高功率输出的需要,在电动汽车瞬间启动、加速和制动方面发挥很大作用。研究开发新的超级电容器电极材料具有很重要的现实意义。
石墨(MCMB)和硬碳(hard carbon)作为商业锂离子蓄电池中最常用的负极材料,它们都具有高导电性,电化学性能优良,其中,硬碳具有独特的卡片层状结构,理论比容量比石墨高,可以考虑作为超级电容器电极材料,与活性碳(activated carbon)材料装配成非对称电容器。本论文第一部分主要是考察了MCMB电极的嵌锂性能和高比表面活性碳电极的电化学性能,第二部分则分别以高嵌锂容量的硬碳和活性碳电极作为超级电容器的负极和正极,考察了硬碳负极的嵌锂性能,并对初步研究了AC/HC非对称超级电容器的电化学性能。通过电化学实验研究得到以下结论：
1、对MCMB电极进行循环伏安测试表明,电极表面的SEI膜基本上是在首次CV过程中形成,形成SEI膜的电压范围主要在0.75-0.2 V,而锂离子嵌入石墨层间的电压范围是0.2-0.01 V。但MCMB电极大倍率放电时衰减严重,高倍率性能不太理想。活性碳电极在有机电解液1.3 mol/L LiPF6/EC+DMC(质量比为1：3)中的电化学性能测试表明,活性碳电极在工作电压范围内稳定性良好,表现出很好的功率特性和电容特性。
2、本文中的硬碳材料层间距较大,嵌锂比容量较高,硬碳纽扣电池嵌锂实验和循环伏安测试表明,25 mA/g电流密度时放电比容量为284.7 mAh/g,它具有较好地快速脱嵌锂性能,可进行大倍率性能实验,可以运用于非对称超级电容器中；在循环伏安扫描过程中发生了锂离子的嵌入脱出反应,基本在首次CV过程中形成SEI膜,形成SEI膜的电压范围主要在1.0-0.5 V,锂离子嵌入硬碳层间的电压范围是0.5-0 V。
3、通过恒流充放电测试、循环伏安和交流阻抗测试手段研究了活性碳/硬碳非对称超级电容器的电化学性能。结果显示,当正负极质量比为1：1时,非对称电容器的比容量值达到最佳,在25 mA/g电流密度时,单极比电容为80.1 F/g,100 mA/g时电容值为78.9 F/g,容量保持率为98.5%。以25 mA/g电流密度的循环性能测试表明,非对称电容器的交流阻抗值小于活性碳双层电容器,且充放电效率都在98%左右,1000次循环后,比容量保持率为70.4%,此非对称超级电容器的电化学性能还有待提高。
As a high efficient energy conversion device (convert chemical energy into electric energy), chemical power sources received much attention. Among those devices, supercapacitors are a kind of intermediate systems between conventional capacitors and rechargeable batteries which have many advantages over conventional capacitors,such as possessing higher capacities and energy, higher specific power compared to batteries, and fast charge-discharge speed, extremely long cycle life and wide operating temperature range. Supercapacitors are widely used in many areas such as military aerospace, mobile telecommunication and information technology, consumer electronics, fuel cells, electric vehicles and urban transports, solar and wind energy. Some of the aeras are often irreplaceable. When the supercapacitors combined with rechargeable batteries formed the hybrid power system, which can meet the high power out-put need, and play an significant role in electric vehicles in condition of instantly starting, acceletating and braking. Consequently, it is significant to do research and development on a new kinds of electrode materials of supercapacitors.
Graphite (MCMB) and hard carbon with good electrochemical performance and high conductivity are most uaually used as negative electrode materials in lithium-ion battery. Especially hard carbon has a "card" layered structure and its theoretical lithium insertion capacity higher than graphite. We consider using hard carbon and activated carbon as anode and cathode respecitively for a new type of asymmetric supercapacitor. In this dissertation, MCMB material and activated carbon have been researched in the former section. The second part will focus on the hybrid capacitor. The conclusions can be drawn as follows by doing a series of experiments:
1. The CV results of graphite(MCMB) in a three-electrode using 1.3 mol/L LiPF6/EC+DMC show:the SEI formation potential range in the first cathodic process was 0.75-0.2 V, and the de-intercalation potential range was 0.2-0.01 V. The SEI film was formed mostly in the first cycle. However, the high rate performance of the MCMB electrode was not so satisfactory. The electrochemical tests of activated carbon electrode indicated its good power and capacitance characteristics. And the electrode was very stable during the whole process.
2. The layer spacing of hard carbon in this paper was relatively large and its corresponding lithium intercalated capacity was high. The lithium intercalation experiments and CV tests of hard carbon using 1.3 mol/L LiPF6/EC+ DMC demonstrate:the SEI formation potential range in the first cathodic process was 1.0-0.5 V, and the de-intercalation potential range was 0.5-0 V. In addition, the SEI film was formed mostly in the first cycle. And the discharge capacity of hard carbon was 284.7 mAh/g at the current density of 25 mA/g. Morever, hard carbon can intercalate lithium at a fast speed, which made it suitable to work at high rate. So it can be used as electrode for supercapacitors.
3. The AC/HC asymmetric capacitor was characterized by galvanostatic charge/discharge, cyclic voltammetry and EIS tests. The results indicate:The specific capacity of the hybrid capacitor can reach to the best value when the mass ratio of cathode to anode was 1:1. And the EIS value was lower than AC symmetric capacitor. Besides, the unipolar specific capacity was 80.1 F/g and 78.9 F/g when the current density was 25 mA/g and 100 mA/g, respectively, retained 98.5%. Finally, the cycle performance tests for the hybrid supercapacitor showed:afer 1000 cycles, the specific capacitance retained 70.4%, while the charge/discharge efficiency was 98%, and the electrochemical performance of the hybrid capacitor needs to be improved.
石墨(MCMB)和硬碳(hard carbon)作为商业锂离子蓄电池中最常用的负极材料,它们都具有高导电性,电化学性能优良,其中,硬碳具有独特的卡片层状结构,理论比容量比石墨高,可以考虑作为超级电容器电极材料,与活性碳(activated carbon)材料装配成非对称电容器。本论文第一部分主要是考察了MCMB电极的嵌锂性能和高比表面活性碳电极的电化学性能,第二部分则分别以高嵌锂容量的硬碳和活性碳电极作为超级电容器的负极和正极,考察了硬碳负极的嵌锂性能,并对初步研究了AC/HC非对称超级电容器的电化学性能。通过电化学实验研究得到以下结论：
1、对MCMB电极进行循环伏安测试表明,电极表面的SEI膜基本上是在首次CV过程中形成,形成SEI膜的电压范围主要在0.75-0.2 V,而锂离子嵌入石墨层间的电压范围是0.2-0.01 V。但MCMB电极大倍率放电时衰减严重,高倍率性能不太理想。活性碳电极在有机电解液1.3 mol/L LiPF6/EC+DMC(质量比为1：3)中的电化学性能测试表明,活性碳电极在工作电压范围内稳定性良好,表现出很好的功率特性和电容特性。
2、本文中的硬碳材料层间距较大,嵌锂比容量较高,硬碳纽扣电池嵌锂实验和循环伏安测试表明,25 mA/g电流密度时放电比容量为284.7 mAh/g,它具有较好地快速脱嵌锂性能,可进行大倍率性能实验,可以运用于非对称超级电容器中；在循环伏安扫描过程中发生了锂离子的嵌入脱出反应,基本在首次CV过程中形成SEI膜,形成SEI膜的电压范围主要在1.0-0.5 V,锂离子嵌入硬碳层间的电压范围是0.5-0 V。
3、通过恒流充放电测试、循环伏安和交流阻抗测试手段研究了活性碳/硬碳非对称超级电容器的电化学性能。结果显示,当正负极质量比为1：1时,非对称电容器的比容量值达到最佳,在25 mA/g电流密度时,单极比电容为80.1 F/g,100 mA/g时电容值为78.9 F/g,容量保持率为98.5%。以25 mA/g电流密度的循环性能测试表明,非对称电容器的交流阻抗值小于活性碳双层电容器,且充放电效率都在98%左右,1000次循环后,比容量保持率为70.4%,此非对称超级电容器的电化学性能还有待提高。
As a high efficient energy conversion device (convert chemical energy into electric energy), chemical power sources received much attention. Among those devices, supercapacitors are a kind of intermediate systems between conventional capacitors and rechargeable batteries which have many advantages over conventional capacitors,such as possessing higher capacities and energy, higher specific power compared to batteries, and fast charge-discharge speed, extremely long cycle life and wide operating temperature range. Supercapacitors are widely used in many areas such as military aerospace, mobile telecommunication and information technology, consumer electronics, fuel cells, electric vehicles and urban transports, solar and wind energy. Some of the aeras are often irreplaceable. When the supercapacitors combined with rechargeable batteries formed the hybrid power system, which can meet the high power out-put need, and play an significant role in electric vehicles in condition of instantly starting, acceletating and braking. Consequently, it is significant to do research and development on a new kinds of electrode materials of supercapacitors.
Graphite (MCMB) and hard carbon with good electrochemical performance and high conductivity are most uaually used as negative electrode materials in lithium-ion battery. Especially hard carbon has a "card" layered structure and its theoretical lithium insertion capacity higher than graphite. We consider using hard carbon and activated carbon as anode and cathode respecitively for a new type of asymmetric supercapacitor. In this dissertation, MCMB material and activated carbon have been researched in the former section. The second part will focus on the hybrid capacitor. The conclusions can be drawn as follows by doing a series of experiments:
1. The CV results of graphite(MCMB) in a three-electrode using 1.3 mol/L LiPF6/EC+DMC show:the SEI formation potential range in the first cathodic process was 0.75-0.2 V, and the de-intercalation potential range was 0.2-0.01 V. The SEI film was formed mostly in the first cycle. However, the high rate performance of the MCMB electrode was not so satisfactory. The electrochemical tests of activated carbon electrode indicated its good power and capacitance characteristics. And the electrode was very stable during the whole process.
2. The layer spacing of hard carbon in this paper was relatively large and its corresponding lithium intercalated capacity was high. The lithium intercalation experiments and CV tests of hard carbon using 1.3 mol/L LiPF6/EC+ DMC demonstrate:the SEI formation potential range in the first cathodic process was 1.0-0.5 V, and the de-intercalation potential range was 0.5-0 V. In addition, the SEI film was formed mostly in the first cycle. And the discharge capacity of hard carbon was 284.7 mAh/g at the current density of 25 mA/g. Morever, hard carbon can intercalate lithium at a fast speed, which made it suitable to work at high rate. So it can be used as electrode for supercapacitors.
3. The AC/HC asymmetric capacitor was characterized by galvanostatic charge/discharge, cyclic voltammetry and EIS tests. The results indicate:The specific capacity of the hybrid capacitor can reach to the best value when the mass ratio of cathode to anode was 1:1. And the EIS value was lower than AC symmetric capacitor. Besides, the unipolar specific capacity was 80.1 F/g and 78.9 F/g when the current density was 25 mA/g and 100 mA/g, respectively, retained 98.5%. Finally, the cycle performance tests for the hybrid supercapacitor showed:afer 1000 cycles, the specific capacitance retained 70.4%, while the charge/discharge efficiency was 98%, and the electrochemical performance of the hybrid capacitor needs to be improved.
引文
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