石墨烯—锡基复合材料的制备及其电化学储锂性能研究
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摘要
石墨由于性能稳定、循环寿命长被认为是优秀的负极材料之一，但它安全性不佳、理论比容量较低且高倍率储锂性能较差。锡基材料由于具有安全性高、质量及体积比容量高、毒性较低等优点被认为是很有前景的石墨替代材料，但锡基材料在充放电过程中巨大的体积变化造成容量迅速衰减，限制了其应用。本文通过加入石墨烯制备SnS-石墨烯复合材料，提高锡基材料的低倍率循环性能，并对其进行水热处理制备SnO2-石墨烯基复合材料，提高材料循环性能和倍率性能。进一步制备Sn-石墨烯基复合材料，提高材料的充放电性能和首次库伦效率，并探讨其可能的作用机制。
采用修饰的Hummers法制备了氧化石墨烯，并通过还原处理制得石墨烯。所制备的石墨烯具有良好的多孔结构，使其成为制备石墨烯-锡基复合材料的优良模板。采用溶剂热法制备出SnS纳米颗粒及SnS纳米棒，具有一维纳米棒结构的SnS纳米棒相对SnS纳米颗粒具有更好的储锂性能。联合沉淀-溶剂热法制备出SnS纳米棒-石墨烯及SnS颗粒-石墨烯纳米复合物，并比较了石墨烯含量对SnS颗粒-石墨烯储锂性能的影响。实验结果表明在较低的充放电倍率下，石墨烯含量为15%的SnS颗粒-石墨烯具有较高的比容量和循环性能，该复合材料的储锂性能优于单纯的SnS电极和单纯的石墨烯电极。分别利用氮气吸脱附技术、电化学交流阻抗及透射电镜对制备的SnS颗粒-石墨烯纳米复合物的储锂机制进行研究。并利用SnS和SnS-GNS与电解质溶液的作用机制以及电子的转移机制示意图解释了其增强SnS储锂性能的作用机制。
采用更加简单、经济的均匀沉淀法制备了SnS-热处理石墨烯复合材料，研究其储锂性能，制备出电化学储锂性能较好的SnS-热处理石墨烯前躯体。以高倍率储锂性能较好的SnS-热处理石墨烯为前躯体，制备了SnO2-石墨烯，该复合材料在500mA g-1电流下充放电循环100次后的可逆容量为597mAh g-1。为了抑制SnO2-石墨烯表面SnO2的体积膨胀，采用一个简单的低温水热法制备出硫包覆SnO2-石墨烯复合材料，该复合材料的储锂性能优于单纯的SnO2电极、单纯的石墨烯电极和SnO2-石墨烯复合材料。在500mA g-1电流下充放电循环200次后该复合材料的可逆容量为815mAh g-1。倍率性能测试表明其具有优异的大电流性能，在4000mA g-1电流下可逆容量仍有580mAh g-1。分别利用循环伏安测试和电化学交流阻技术对低温水热法制备的硫包覆SnO2-石墨烯复合材料的储锂机制进行研究，并利用石墨烯和S对锡基复合材料作用机制示意图解释了其增强的电化学储锂性能的机制。
为了进一步提高石墨烯-锡基复合材料的首次库伦效率，采用低温沉淀法制备了Sn-石墨烯复合材料，研究了其储锂性能，该复合材料在500mA g-1电流下充放电循环的首次库伦效率为70.3%，较石墨烯-锡的硫化物及氧化物复合材料均有所提高，60次充放电循环后的可逆容量为430mAh g-1。采用电泳沉积制备了三维Sn-石墨烯复合材料，进一步提高了Sn-石墨烯基材料的可逆容量，该复合材料在500mA g-1电流下充放电循环60次后，仍有520mAh g-1的比容量。为了进一步提高材料的循环性能，采用一个简单的低温共沉淀法制备了Sn-Co-石墨烯，该复合材料在500mA g-1电流下充放电循环60次后仍有560mAh g-1的比容量，并且具有优良的倍率性能。最后，利用循环伏安分析并提出了Sn-石墨烯提高石墨烯-锡基复合材料首次充放电库伦效率的可能作用机制，并利用密度泛函理论计算对Sn-石墨烯增强Sn电化学储锂性能可能的机理进行了分析。
Graphite has been considered as one of the excellent anode materials because of its high stability and long service life. However, it suffers from safety issues, low theoretical capacity and poor high rate lithium storage performance. Tin-based materials have been considered as promising substitutes for graphite owing to their good safety, high weight capacity and volume capacity, and low toxicity. Nevertheless, the application of tin-based materials has been limited due to the fast capacity fading, which arises from the large volume variation during the charge-discharge cycling. In this work, graphene has been utilized to prepare SnS-graphene composite material, with enhanced low rate lithium storage capability. The as-prepared SnS-graphene is treated hydrothermally to fabricate SnO2-graphene. And SnO2-graphene composites further enhance the cyclic performance and rate capability of tin-based materials. To increase the coulombic efficiency of tin-based materials, Sn-graphene composite material has been prepared, and the enhanced lithium storage mechanisms have been discussed.
Graphene oxide was synthesized by a modified Hummers' method, and graphene was obtained by reduction of graphene oxide. The as-prepared graphene is an excellent template for the preparation of graphene-tin based composite material owing to its open porous structure. SnS nanopartices and SnS nanorods were synthesized via a solvothermal method. SnS nanorods exhibited superior lithium storage properties to SnS nanoparticles. The SnS nanorods-graphene and SnS nanoparticles-graphene were prepared by a precipitation method followed by the solvothermal treatment. The effect of graphene content on lithium storage capability of SnS nanoparticles-graphene was also discussed. The results showed that the SnS nanoparticles-graphene with15wt.%graphene exhibited superior capacity and cycling performance at low rate. The composite material also showed superior lithium storage capability compared with bare SnS and pure graphene. The lithium storage mechanism of the as-prepared SnS nanoparticles-graphene was investigated through Brunauer-Emmett-Teller analysis, electrochemical impedance spectroscopy measurements and TEM analysis. Mechanism for interaction between SnS and electrolytes, SnS-GNS and electrolytes and mechanism of electron transfer within SnS and SnS-GNS were also proposed to explain the enhanced lithium storage capability of SnS-GNS.
SnS-graphene composite material was prepared via a facile and economic homogeneous precipitation method. The lithium storage properties of the composites were also investigated. SnO2-graphene composites were prepared with the optimized SnS-graphene precursors. The as-prepared composites exhibited a reversible capacity of597mAh g-1after100cycles at a current density of500mA g-1. To further inhibit the expansion of SnO2on the surface of the composites, a facile low temperature hydrothermal method was developed to fabricate sulfur coated SnO2-graphene composites. The composite electrode exhibited superior lithium storage properties compared to bare SnO2, bare graphene, and SnO2-graphene. The reversible capacity of the composite material was815mAh g-1after200cycles at500mA g-1. Rate capability tests indicated that the composites exhibited excellent high current properties, and the reversible capacity was as high as580mAh g-1even at4000mA g-1. The lithium storage mechanism of sulfur coated SnO2-graphene was investigated by cyclic voltammetry and electrochemical impedance spectroscopy, and mechanism about the effect of graphene and sulfur on SnO2-based composite materials was also proposed.
To further increase the coulombic efficiency of graphene-tin based composites, a low temperature precipitation method was devoted to preparing Sn-graphene composite material. The lithium storage performance was also investigated. The composites exhibited an initial coulombic efficiency of70.3%at500mA g-1, which was higher than that of graphene-tin sulfide and tin oxide. After60cycles, the reversible capacity was430mAh g-1. The three dimensional porous Sn-graphene composites were prepared through electrophoretic deposition method to improve the reversible capacity of Sn-graphene-based composites, and a reversible capacity of520mAh g-1was obtained after60cycles at500mA g-1. To further improve the reversible capacity of tin-graphene composites, a facile low temperature co-precipitation method was developed to fabricate Sn-Co-graphene composites. The Sn-Co-graphene composite material exhibited a reversible capacity of560mAh g-1after60cycles at500mA g-1and a good rate capability. Finally, the possible mechanism of higher coulombic efficiency of Sn-graphene compared with other graphene-tin-based materials was proposed. And the mechanism of the enhanced lithium storage performance of Sn-graphene compared with Sn was investigated by density functional theory.
采用修饰的Hummers法制备了氧化石墨烯，并通过还原处理制得石墨烯。所制备的石墨烯具有良好的多孔结构，使其成为制备石墨烯-锡基复合材料的优良模板。采用溶剂热法制备出SnS纳米颗粒及SnS纳米棒，具有一维纳米棒结构的SnS纳米棒相对SnS纳米颗粒具有更好的储锂性能。联合沉淀-溶剂热法制备出SnS纳米棒-石墨烯及SnS颗粒-石墨烯纳米复合物，并比较了石墨烯含量对SnS颗粒-石墨烯储锂性能的影响。实验结果表明在较低的充放电倍率下，石墨烯含量为15%的SnS颗粒-石墨烯具有较高的比容量和循环性能，该复合材料的储锂性能优于单纯的SnS电极和单纯的石墨烯电极。分别利用氮气吸脱附技术、电化学交流阻抗及透射电镜对制备的SnS颗粒-石墨烯纳米复合物的储锂机制进行研究。并利用SnS和SnS-GNS与电解质溶液的作用机制以及电子的转移机制示意图解释了其增强SnS储锂性能的作用机制。
采用更加简单、经济的均匀沉淀法制备了SnS-热处理石墨烯复合材料，研究其储锂性能，制备出电化学储锂性能较好的SnS-热处理石墨烯前躯体。以高倍率储锂性能较好的SnS-热处理石墨烯为前躯体，制备了SnO2-石墨烯，该复合材料在500mA g-1电流下充放电循环100次后的可逆容量为597mAh g-1。为了抑制SnO2-石墨烯表面SnO2的体积膨胀，采用一个简单的低温水热法制备出硫包覆SnO2-石墨烯复合材料，该复合材料的储锂性能优于单纯的SnO2电极、单纯的石墨烯电极和SnO2-石墨烯复合材料。在500mA g-1电流下充放电循环200次后该复合材料的可逆容量为815mAh g-1。倍率性能测试表明其具有优异的大电流性能，在4000mA g-1电流下可逆容量仍有580mAh g-1。分别利用循环伏安测试和电化学交流阻技术对低温水热法制备的硫包覆SnO2-石墨烯复合材料的储锂机制进行研究，并利用石墨烯和S对锡基复合材料作用机制示意图解释了其增强的电化学储锂性能的机制。
为了进一步提高石墨烯-锡基复合材料的首次库伦效率，采用低温沉淀法制备了Sn-石墨烯复合材料，研究了其储锂性能，该复合材料在500mA g-1电流下充放电循环的首次库伦效率为70.3%，较石墨烯-锡的硫化物及氧化物复合材料均有所提高，60次充放电循环后的可逆容量为430mAh g-1。采用电泳沉积制备了三维Sn-石墨烯复合材料，进一步提高了Sn-石墨烯基材料的可逆容量，该复合材料在500mA g-1电流下充放电循环60次后，仍有520mAh g-1的比容量。为了进一步提高材料的循环性能，采用一个简单的低温共沉淀法制备了Sn-Co-石墨烯，该复合材料在500mA g-1电流下充放电循环60次后仍有560mAh g-1的比容量，并且具有优良的倍率性能。最后，利用循环伏安分析并提出了Sn-石墨烯提高石墨烯-锡基复合材料首次充放电库伦效率的可能作用机制，并利用密度泛函理论计算对Sn-石墨烯增强Sn电化学储锂性能可能的机理进行了分析。
Graphite has been considered as one of the excellent anode materials because of its high stability and long service life. However, it suffers from safety issues, low theoretical capacity and poor high rate lithium storage performance. Tin-based materials have been considered as promising substitutes for graphite owing to their good safety, high weight capacity and volume capacity, and low toxicity. Nevertheless, the application of tin-based materials has been limited due to the fast capacity fading, which arises from the large volume variation during the charge-discharge cycling. In this work, graphene has been utilized to prepare SnS-graphene composite material, with enhanced low rate lithium storage capability. The as-prepared SnS-graphene is treated hydrothermally to fabricate SnO2-graphene. And SnO2-graphene composites further enhance the cyclic performance and rate capability of tin-based materials. To increase the coulombic efficiency of tin-based materials, Sn-graphene composite material has been prepared, and the enhanced lithium storage mechanisms have been discussed.
Graphene oxide was synthesized by a modified Hummers' method, and graphene was obtained by reduction of graphene oxide. The as-prepared graphene is an excellent template for the preparation of graphene-tin based composite material owing to its open porous structure. SnS nanopartices and SnS nanorods were synthesized via a solvothermal method. SnS nanorods exhibited superior lithium storage properties to SnS nanoparticles. The SnS nanorods-graphene and SnS nanoparticles-graphene were prepared by a precipitation method followed by the solvothermal treatment. The effect of graphene content on lithium storage capability of SnS nanoparticles-graphene was also discussed. The results showed that the SnS nanoparticles-graphene with15wt.%graphene exhibited superior capacity and cycling performance at low rate. The composite material also showed superior lithium storage capability compared with bare SnS and pure graphene. The lithium storage mechanism of the as-prepared SnS nanoparticles-graphene was investigated through Brunauer-Emmett-Teller analysis, electrochemical impedance spectroscopy measurements and TEM analysis. Mechanism for interaction between SnS and electrolytes, SnS-GNS and electrolytes and mechanism of electron transfer within SnS and SnS-GNS were also proposed to explain the enhanced lithium storage capability of SnS-GNS.
SnS-graphene composite material was prepared via a facile and economic homogeneous precipitation method. The lithium storage properties of the composites were also investigated. SnO2-graphene composites were prepared with the optimized SnS-graphene precursors. The as-prepared composites exhibited a reversible capacity of597mAh g-1after100cycles at a current density of500mA g-1. To further inhibit the expansion of SnO2on the surface of the composites, a facile low temperature hydrothermal method was developed to fabricate sulfur coated SnO2-graphene composites. The composite electrode exhibited superior lithium storage properties compared to bare SnO2, bare graphene, and SnO2-graphene. The reversible capacity of the composite material was815mAh g-1after200cycles at500mA g-1. Rate capability tests indicated that the composites exhibited excellent high current properties, and the reversible capacity was as high as580mAh g-1even at4000mA g-1. The lithium storage mechanism of sulfur coated SnO2-graphene was investigated by cyclic voltammetry and electrochemical impedance spectroscopy, and mechanism about the effect of graphene and sulfur on SnO2-based composite materials was also proposed.
To further increase the coulombic efficiency of graphene-tin based composites, a low temperature precipitation method was devoted to preparing Sn-graphene composite material. The lithium storage performance was also investigated. The composites exhibited an initial coulombic efficiency of70.3%at500mA g-1, which was higher than that of graphene-tin sulfide and tin oxide. After60cycles, the reversible capacity was430mAh g-1. The three dimensional porous Sn-graphene composites were prepared through electrophoretic deposition method to improve the reversible capacity of Sn-graphene-based composites, and a reversible capacity of520mAh g-1was obtained after60cycles at500mA g-1. To further improve the reversible capacity of tin-graphene composites, a facile low temperature co-precipitation method was developed to fabricate Sn-Co-graphene composites. The Sn-Co-graphene composite material exhibited a reversible capacity of560mAh g-1after60cycles at500mA g-1and a good rate capability. Finally, the possible mechanism of higher coulombic efficiency of Sn-graphene compared with other graphene-tin-based materials was proposed. And the mechanism of the enhanced lithium storage performance of Sn-graphene compared with Sn was investigated by density functional theory.
引文
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