石墨烯改性锂硫电池正极材料的制备及其电化学性能研究
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摘要
锂硫电池具有理论比容量高、成本低、环境友好等优点，被公认为最有前景的下一代二次电池之一。硫正极材料作为锂硫电池的重要组成部分，直接决定了锂硫电池的性能。本论文通过对锂硫电池正极材料的结构设计、改性和制备一体化研究，得到了电化学性能较好的正极材料，为锂硫电池的应用研究提供了重要参考。
采用超声辅助化学沉积法和真空抽滤法制备了石墨烯-硫(RGO-S)正极材料，研究了硫含量对RGO-S正极材料电化学性能影响。采用SEM、TEM、XRD、比表面积分析仪、电池测试仪和电化学工作站等对正极材料微观形貌、晶型结构、比表面积、导电率与电化学性能进行了表征和分析，探讨了电极结构与电化学性能之间的关系。研究结果表明，所制备的RGO-S正极材料具有石墨烯包覆硫的结构、较高的比表面积和导电率。当硫含量为26%时，0.1C倍率下，首次放电比容量可达1250mAh·g-1sulfur，50次充放电循环后仍保持598mAh·g-1sulfur。RGO包覆硫缩短了电子的传输路径、提高了硫的反应活性和化学反应动力学速率；并且通过RGO的包覆和吸附作用限制了循环过程中间产物多硫化锂的扩散和迁移，减缓了穿梭效应，使得电极材料具有较高的比容量、较好的循环性能和倍率性能。
利用经酸化处理的碳纤维(FCNFs)对RGO-S正极材料进行改性。采用化学沉积法制备了一维管壳状FCNFs-S材料，并以之为前驱体制备了具有同轴包覆结构的RGO-S-FCNFs正极材料，通过对FCNFs增强改性前后正极材料微观形貌、晶型结构、导电率与电化学性能的表征和分析，探讨了FCNFs对RGO-S正极材料的增强改性机制。研究结果表明，硫含量为33%时，1C倍率下，首次放电比容量可达745mAh·g-1sulfur，1500次充放电循环后保持273mAh·g-1sulfur，具有极好的高倍率长循环稳定性。RGO和FCNFs的共同作用能够有效提高RGO-S正极材料的电导率；RGO-S-FCNFs的同轴包覆能够使得硫及其循环过程中间产物多硫化锂被包夹在石墨烯和FCNFs之间，抑制了硫的团聚，阻止了大颗粒硫的生成，降低了电极材料的内部应力和电荷转移电阻，缓解了体积和穿梭效应，从而高了RGO-S正极材料的比容量、循环性能和倍率性能。
采用水热法和热处理法制备了具有高硫含量和单位面积负载量的三维结构FCNFs改性石墨烯-硫(3D-CGOS)正极材料。通过对FCNFs增强改性前后正极材料的微观形貌、晶型结构、导电率与电化学性能的表征和分析，探讨了FCNFs对3D-GOS正极材料的增强改性机制。研究结果表明，在硫含量为80%，单位面积硫负载量为11.9mg·cm-2时，FCNFs增强改性后3D-GOS正极复合材料2C倍率下的可逆放电比容量从0.5mAh·cm-2cathode提高到3.1mAh·cm-2cathode。FCNFs增强改性提高了3D-GOS材料导电性能，缩短了电子的传输路径、提高了硫的反应活性和化学反应动力学速率；并通过吸附作用将循环过程中间产物多硫化锂限制在三维结构内部，减缓穿梭效应；FCNFs改性提高了三维石墨烯的机械性能，缓解了循环过程中的体积效应，降低了电极材料的内应力，进而改善电极材料的比容量、循环性能和倍率性能。
Lithium-sulfur(Li-S) batteries are widely considered as one of the most promising next generation of secondary batteries, due to its various advantages, such as high theoretical specific capacity, low cost, environmental friendliness. As an important part of Li-S batteries, the sulfur-based cathode materials play the crucial role on the performance of the battery. In this paper, sulfur-based cathode materials with good electrochemical performance were obtained by the structure design, modification, synthesis of cathode materials. It will provide an important reference for the practical application of Li-S batteries.
The reduced graphene oxide-sulfur(RGO-S) cathode composites were synthesized using ultrasonic-assisted chemical co-deposition and vacuum filtration methods. The effect of the sulfur content on the electrochemical properties of RGO-S cathode materials was studied. Morphology, crystal structure, specific surface area, electric conductivity and electrochemical performance of the cathode materials were characterized and analyzed by scanning electron microscope(SEM), transmission electron microscope(TEM), X-ray diffraction(XRD), battery testing system and electrochemical work station, in order to study the relationship between the structure and electrochemical properties of the cathode. As a result, the as-prepared RGO-S cathode materials show a core-shell structure by graphene wrapping over sulfur particles, as well as high specific surface area and conductivity. When the sulfur content was26wt%, the RGO-S cathode could deliver a high initial capacity of1250mAh·g-1sulfur, and a reversible capacity of598mAh·g-1sulfur after50charge-discharge cycles at0.1C. The RGO wraping over the sulfur could shorten the transmission path of both electron and ion, leading the enhancement of the reaction activity and the rate of chemical reaction kinetics. And also, it could trap the diffused intermediates and remit the shuttle effect. As a result, the electrode materials showed a high specific capacity, good cycle performance and rate properties.
The RGO-S cathode materials were modified by functional carbon nanofibers (FCNFs). Firstly, FCNFs-S composites were synthesized with a uniform sulfur layer on the outside of FCNFs using chemical deposition method. And it was used as the precursor in the preparation of RGO-S-FCNFs multilayered coaxial cathode composites. In order to study the modification mechanism of the FCNFs for RGO-S cathode materials, micro-morphology, crystal structure, conductivity and electrochemical performance of RGO-S materials before and after the modification were studied. As a result, the cathode with33%sulfur could deliver an initial specific capacitance of745mAh·g-1sulfur, and maintained273mAh·g-1sulfur after1500charge-discharge cycles at a rate of1C, showing excellently long cycle stability at high rate. The conductivity of RGO-S cathode materials were improved by synergistic effect of RGO and FCNFs. Because of the coaxial-coated structure, sulfur and intermediates during charge-discharge process could be trapped between graphene and FCNFs, the reunion and growth of big sulfur particles was suppressed, the volume change was accommodated, the shuttle effect, the internal stress of the cathode materials and the resistance of charge-transfer was decreased. As a result, the specific capacity, cycle performance and rate capability could be further improved.
FCNFs modified three-dimensional graphene-sulfur cathode materials with large sulfur content and areal mass loading were prepared by hydrothermal method and thermal treatment. In order to investigate the modification mechanism of the FCNFs for3D-CGOS cathode materials, micro-morphology, crystal structure, conductivity and electrochemical performance of RGO-S materials before and after the FCNFs modification were studied. The results showed that the reversible discharge-specific capacity of the3D-CGOS composites were increased from0.5mAh·cm-2cathode to3.1mAh·cm-2cathode at2C, when the sulfur content was80%and the areal mass loading of sulfur was11.9mg cm-2. The modification of FCNFs can be enhanced and the conductivity of3D-GOS materials was improved. Both of the electron and ion transportation length were shorted, the reaction activity and the rate of chemical reaction kinetics were accelerated, as well as the shuttle effect was slowed. Meanwhile, the mechanical property of3D graphene can be enhanced, which is benefit for the accommodation of volume changes during the charge-discharge process. As a result, the specific capacity, cycle performance and rate capability were significantly improved.
采用超声辅助化学沉积法和真空抽滤法制备了石墨烯-硫(RGO-S)正极材料，研究了硫含量对RGO-S正极材料电化学性能影响。采用SEM、TEM、XRD、比表面积分析仪、电池测试仪和电化学工作站等对正极材料微观形貌、晶型结构、比表面积、导电率与电化学性能进行了表征和分析，探讨了电极结构与电化学性能之间的关系。研究结果表明，所制备的RGO-S正极材料具有石墨烯包覆硫的结构、较高的比表面积和导电率。当硫含量为26%时，0.1C倍率下，首次放电比容量可达1250mAh·g-1sulfur，50次充放电循环后仍保持598mAh·g-1sulfur。RGO包覆硫缩短了电子的传输路径、提高了硫的反应活性和化学反应动力学速率；并且通过RGO的包覆和吸附作用限制了循环过程中间产物多硫化锂的扩散和迁移，减缓了穿梭效应，使得电极材料具有较高的比容量、较好的循环性能和倍率性能。
利用经酸化处理的碳纤维(FCNFs)对RGO-S正极材料进行改性。采用化学沉积法制备了一维管壳状FCNFs-S材料，并以之为前驱体制备了具有同轴包覆结构的RGO-S-FCNFs正极材料，通过对FCNFs增强改性前后正极材料微观形貌、晶型结构、导电率与电化学性能的表征和分析，探讨了FCNFs对RGO-S正极材料的增强改性机制。研究结果表明，硫含量为33%时，1C倍率下，首次放电比容量可达745mAh·g-1sulfur，1500次充放电循环后保持273mAh·g-1sulfur，具有极好的高倍率长循环稳定性。RGO和FCNFs的共同作用能够有效提高RGO-S正极材料的电导率；RGO-S-FCNFs的同轴包覆能够使得硫及其循环过程中间产物多硫化锂被包夹在石墨烯和FCNFs之间，抑制了硫的团聚，阻止了大颗粒硫的生成，降低了电极材料的内部应力和电荷转移电阻，缓解了体积和穿梭效应，从而高了RGO-S正极材料的比容量、循环性能和倍率性能。
采用水热法和热处理法制备了具有高硫含量和单位面积负载量的三维结构FCNFs改性石墨烯-硫(3D-CGOS)正极材料。通过对FCNFs增强改性前后正极材料的微观形貌、晶型结构、导电率与电化学性能的表征和分析，探讨了FCNFs对3D-GOS正极材料的增强改性机制。研究结果表明，在硫含量为80%，单位面积硫负载量为11.9mg·cm-2时，FCNFs增强改性后3D-GOS正极复合材料2C倍率下的可逆放电比容量从0.5mAh·cm-2cathode提高到3.1mAh·cm-2cathode。FCNFs增强改性提高了3D-GOS材料导电性能，缩短了电子的传输路径、提高了硫的反应活性和化学反应动力学速率；并通过吸附作用将循环过程中间产物多硫化锂限制在三维结构内部，减缓穿梭效应；FCNFs改性提高了三维石墨烯的机械性能，缓解了循环过程中的体积效应，降低了电极材料的内应力，进而改善电极材料的比容量、循环性能和倍率性能。
Lithium-sulfur(Li-S) batteries are widely considered as one of the most promising next generation of secondary batteries, due to its various advantages, such as high theoretical specific capacity, low cost, environmental friendliness. As an important part of Li-S batteries, the sulfur-based cathode materials play the crucial role on the performance of the battery. In this paper, sulfur-based cathode materials with good electrochemical performance were obtained by the structure design, modification, synthesis of cathode materials. It will provide an important reference for the practical application of Li-S batteries.
The reduced graphene oxide-sulfur(RGO-S) cathode composites were synthesized using ultrasonic-assisted chemical co-deposition and vacuum filtration methods. The effect of the sulfur content on the electrochemical properties of RGO-S cathode materials was studied. Morphology, crystal structure, specific surface area, electric conductivity and electrochemical performance of the cathode materials were characterized and analyzed by scanning electron microscope(SEM), transmission electron microscope(TEM), X-ray diffraction(XRD), battery testing system and electrochemical work station, in order to study the relationship between the structure and electrochemical properties of the cathode. As a result, the as-prepared RGO-S cathode materials show a core-shell structure by graphene wrapping over sulfur particles, as well as high specific surface area and conductivity. When the sulfur content was26wt%, the RGO-S cathode could deliver a high initial capacity of1250mAh·g-1sulfur, and a reversible capacity of598mAh·g-1sulfur after50charge-discharge cycles at0.1C. The RGO wraping over the sulfur could shorten the transmission path of both electron and ion, leading the enhancement of the reaction activity and the rate of chemical reaction kinetics. And also, it could trap the diffused intermediates and remit the shuttle effect. As a result, the electrode materials showed a high specific capacity, good cycle performance and rate properties.
The RGO-S cathode materials were modified by functional carbon nanofibers (FCNFs). Firstly, FCNFs-S composites were synthesized with a uniform sulfur layer on the outside of FCNFs using chemical deposition method. And it was used as the precursor in the preparation of RGO-S-FCNFs multilayered coaxial cathode composites. In order to study the modification mechanism of the FCNFs for RGO-S cathode materials, micro-morphology, crystal structure, conductivity and electrochemical performance of RGO-S materials before and after the modification were studied. As a result, the cathode with33%sulfur could deliver an initial specific capacitance of745mAh·g-1sulfur, and maintained273mAh·g-1sulfur after1500charge-discharge cycles at a rate of1C, showing excellently long cycle stability at high rate. The conductivity of RGO-S cathode materials were improved by synergistic effect of RGO and FCNFs. Because of the coaxial-coated structure, sulfur and intermediates during charge-discharge process could be trapped between graphene and FCNFs, the reunion and growth of big sulfur particles was suppressed, the volume change was accommodated, the shuttle effect, the internal stress of the cathode materials and the resistance of charge-transfer was decreased. As a result, the specific capacity, cycle performance and rate capability could be further improved.
FCNFs modified three-dimensional graphene-sulfur cathode materials with large sulfur content and areal mass loading were prepared by hydrothermal method and thermal treatment. In order to investigate the modification mechanism of the FCNFs for3D-CGOS cathode materials, micro-morphology, crystal structure, conductivity and electrochemical performance of RGO-S materials before and after the FCNFs modification were studied. The results showed that the reversible discharge-specific capacity of the3D-CGOS composites were increased from0.5mAh·cm-2cathode to3.1mAh·cm-2cathode at2C, when the sulfur content was80%and the areal mass loading of sulfur was11.9mg cm-2. The modification of FCNFs can be enhanced and the conductivity of3D-GOS materials was improved. Both of the electron and ion transportation length were shorted, the reaction activity and the rate of chemical reaction kinetics were accelerated, as well as the shuttle effect was slowed. Meanwhile, the mechanical property of3D graphene can be enhanced, which is benefit for the accommodation of volume changes during the charge-discharge process. As a result, the specific capacity, cycle performance and rate capability were significantly improved.
引文
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