磷酸铁锂正极材料表面结构的构架及其电化学性能研究
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摘要
随着能源危机和环境危机的出现,锂离子动力电池成为当前研究的热点。磷酸铁锂因其具有较高的理论容量、循环性能优良、安全性高、成本低廉和环境友好等诸多优点而备受关注。本文以廉价化学试剂为主要原料,采用原位固相合成法和二步法成功制备了LiFePO4/C正极材料、金属氧化物修饰LiFePO4/C正极材料、金属氧化物和碳共包覆LiFePO4正极材料和共生化合物修饰LiFePO4/C正极材料,采用XRD、Raman、SEM、TEM、EDS和XPS等技术手段对正极材料的结构与组成进行了分析和表征；采用充放电测试、循环伏安(CV)和交流阻抗(EIS)等方法对正极材料的电化学性能进行了分析和研究。其研究结果总结如下：
1.铁源、碳源和煅烧方法对LiFePO4/C正极材料的影响。分别以草酸亚铁和氧化铁为铁源,葡萄糖、蔗糖、柠檬酸、聚乙二醇4000、可溶性淀粉和己二酸为碳源,以碳酸锂为锂源、磷酸二氢铵为磷源采用原位固相法合成了LiFePO4/C正极材料。(1)不同碳源对正极材料的颗粒大小、形貌及碳结构有一定的影响,其中以葡萄糖和蔗糖为碳源合成的正极材料的颗粒大小均匀、分散性良好,且碳的石墨化程度较高。(2)对比两种铁源发现,以草酸亚铁为铁源,葡萄糖为碳源合成的正极材料粒度较小,分散性好,颗粒形貌较规则,且具有相对较好的充放电性能。(3)随着煅烧温度的升高和时间的延长,正极材料的结晶度逐渐提高,颗粒大小逐渐均匀,分散性逐渐变好,当温度升高至800℃以上时正极材料的粒径随温度变化较大,同时有杂相Fe2P生成。
2.金属氧化物修饰LiFePO4/C正极材料。以草酸亚铁(或三氧化二铁)、碳酸锂、磷酸二氢铵、葡萄糖、碳酸锌、钨酸铵和钼酸铵为原料,采用原位合成法成功合成了ZnO修饰LiFePO4/C正极材料,并首次合成了WO2和MoO2修饰LiFePO4/C正极材料及MoO2修饰LiFePO4正极材料。在合成过程中,各金属氧化物前驱体及碳源的分解在LiFePO4正极材料的颗粒之间及表面构架了以金属氧化物和碳为混合体的导电介质,从而达到提高正极材料电化学性能的目的。研究发现：(1)由于ZnO的电子电导率相对较低,ZnO的添加对提高正极材料的电化学性能的贡献很小。(2)电子导电率高的WO2和MoO2的添加能明显改善正极材料的电化学性能,当导电金属氧化物W02和M002含量为5wt%时,正极材料在0.1C倍率下具有最大的首次放电比容量,分别为120.1mAh/g和142.6mAh/g,此时正极材料的表观锂离子扩散系数最大,电荷转移阻抗最小。但由于导电金属氧化物结晶度较低、表面部分被氧化及其在电解液中的部分溶解导致正极材料在不同倍率下的循环性能较差。(3)在对不含碳的MoO2修饰LiFePO4正极材料研究时发现,仅仅依靠Mo02的添加也可以提高正极材料的电化学性能,MoO2含量为5wt%时,正极材料在0.1C倍率下的首次放电比容量已提高至76.6mAh/g,与未添加Mo02的样品相比,放电比容量提高了59.8mAh/go
3.金属氧化物和碳共包覆LiFePO4正极材料。以草酸亚铁、碳酸锂、磷酸二氢铵、葡萄糖及硝酸锌、钨酸铵、钼酸铵、碳酸铵和柠檬酸为原料,采用二步法成功合成了ZnO与碳共包覆LiFePO4正极材料,并首次合成了WO2和MoO2与碳共包覆LiFePO4正极材料。由于LiFePO4/C正极材料中的少量碳不能在LiFePO4颗粒表面形成完整的包覆层,因此金属氧化物对LiFePO4颗粒表面裸露部分的修复将提高包覆层的完整性和连续性,从而改善正极材料的电化学性能。研究发现：(1)适量的ZnO包覆提高了正极材料的充放电比容量和锂离子扩散系数,降低了电荷转移阻抗,同时具有较好的循环性能。(2)电子电导率更高的WO2和Mo02的包覆相对于ZnO包覆来讲,能更好的提高正极材料的电化学性能,其充放电比容量和表观锂离子扩散系数更高,同时也具有较好的循环性能,其中WO2与碳共包覆LiFePO4正极材料在0.1、0.2、0.5和1.0C倍率下110次循环后的放电比容量分别为153.7、144.5、137.5和121mAh/g;MoO2与碳共包覆LiFePO4正极材料在0.1、0.2、0.5和1.0C倍率下110次循环后的放电比容量分别为157、136.16、131.3和119.1mAh/g,说明导电金属氧化物对提高正极材料的电化学性能具有良好的促进作用。
4.共生化合物修饰LiFePO4/C正极材料。以草酸亚铁、碳酸锂、磷酸二氢铵、葡萄糖和钨酸铵为原料,采用原位固相法合成了共生化合物(Li3PO4、Li4P2O7和Fe2P2O7)修饰LiFePO4/C正极材料和FeWO4修饰LiFePO4/C正极材料。研究发现：(1) FeWO4的添加对正极材料电化学性能的提高没有贡献。(2)由于Li3PO4离子电导率较低,其对提高正极材料电化学性能的贡献较小。(3)作为快离子导体的Li4P2O7的添加能较好的提高正极材料的充放电性能,但其循环性能较差。(4)首次研究了共生化合物Fe2P2O7对正极材料的影响,相比之下,Fe2P2O7的添加不仅可以更好的提高正极材料的充放电比容量,而且具有较好的循环性能,这可能是由于Fe2P2O7具有良好离子导电性或电子导电性而实现的。(5)当正极材料的Fe2P2O7含量为5wt%时,在0.1C倍率下具有最高的首次放电比容量146.7mAh/g,110次循环后仍保持130mAh/g以上,同时具有最高的表观锂离子扩散系数。
The lithium ion power battery has become the research hotspot in recent years with the emergency of energy crisis and environmental crisis. LiFePO4has received much attention as a promising storage compound for cathodes in lithium-ion batteries due to it has high specific capacity, good cycle performance, safety, low costs and environmental friendliness. In this paper, the LiFePO4/C, metallic oxide modified LiFePO4/C, metallic oxide and carbon co-coated LiFePO4and symbiotic compounds modified LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method and two step method with the cheap chemistry reagents as raw materials. The phase composition and structure of cathode materials were characterized and analyzed by XRD、Raman、 SEM、 TEM, EDS and XPS. The electrochemical performances of cathode materials were tested and studied by charge-discharge technology, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The main results are as follows:
1. The effects of carbon source, iron source and calcination method on the electrochemical performances of LiFePO4/C cathode materials. The LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4and Fe2O3as iron source, glucose, sucrose, citric acid, polyethylene glycol4000, starch and hexanedioic acid as carbon source, Li2CO3as lithium source and NH4H2PO4as phosphorous source, respectively.(1) There were the obvious effects of carbon sources on carbon structure, particle size and shape of LiFePO4/C cathode materials, the samples synthesized with glucose and sucrose as carbon sources had uniform particle size, well dispersibility and higher graphitization degree of carbon.(2) The cathode materials synthesized with Fe2C2C2O4as iron source and glucose as carbon sources had smaller particle size, well dispersibility and regular shape.(3) With calcination temperature increasing and time prolonging, the crystallinity of LiFePO4increased, particles size become gradually uniform and dispersion become gradually good. When calcination temperature was increased over800℃, the increasing of particles size was significant with the temperature change, and the new phase of Fe2P generated.
2. Metallic oxide modified LiFePO4/C cathode materials. ZnO modified LiFePO4/C, W02modified LiFePO4/C, MoO2modified LiFePO4/C and MoO2modified LiFePO4cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4(or Fe2O3), Li2CO3, NH4H2PO4, ZnCO3,(NH4)10W12O41·xH2O,(NH4)6Mo7O24-4H2O and glucose as raw materials. In the synthesis process, the conducting medium composed by metal oxide and carbon on the LiFePO4particles surface and in gap of particles would improve the electrochemical performances of cathode materials, which were formed by the decomposition of metal oxide precursors and carbon sources.(1) The existence of ZnO could improve the charge-discharge specific capacity of cathode materials, but the improvement was very low because of lower electronic conductivity of ZnO.(2) The adding of WO2and MoO2with high electronic conductivity could obvious improve electrochemical performances of cathode materials. The cathode materials with5wt%conductive metal oxides exhibited the best electrochemical performance; they had the maximum value of initial discharge specific capacity of120.1mAh/g and142.6mAh/g at0.1C at room temperature, respectively, the maximum apparent lithium ion diffusion coefficient and the minimum charge transfer resistance. However, because of WO2and MoO2lower crystallinity, partially oxidized of surface and partially dissolved by electrolyte, the cycle performance of cathode materials is poor at different charge-discharge rate.(3) MoO2modified LiFePO4cathode materials without carbon had better charge-discharge performance, when the MoO2content is5wt%, the sample had higher initial discharge specific capacity of76.6mAh/g at0.1C at room temperature, compared with the sample without MoO2, the discharge specific capacity rose59.8mAh/g.
3. Metallic oxide and carbon co-coated LiFePO4cathode materials. ZnO and carbon co-coated LiFePO4, WO2and carbon co-coated LiFePO4and MoO2and carbon co-coated LiFePO4cathode materials were synthesized by two step method. In LiFePO4/C, the small amounts of carbon can not form a full coating layer on the surface of LiFePO4, but the adding of metal oxides could repair the bare surface of LiFePO4particles, make the coating layer more full and continuous and improve electrochemical performances of cathode materials.(1) The right amount of ZnO coating could improve charge-discharge specific capacity and apparent lithium ion diffusion coefficient, and decrease charge transfer resistance, and the sample with3wt%ZnO has better cycle performance in different charge-discharge rate.(2) Relative to ZnO coating, the WO2and MoO2coating could improve electrochemical performances even more, including higher charge-discharge specific capacity, higher apparent lithium ion diffusion coefficient and lower charge transfer resistance and good cycle performance. The discharge specific capacity of WO2and carbon co-coated LiFePO4cathode materials are153.7,144.5,137.5and121mAh/g at0.1,0.2,0.5and1.0C after110-cycle, respectively, The discharge specific capacity of MoO2and carbon co-coated LiFePO4cathode materials are157,136.16,131.3and119.1mAh/g at0.1,0.2,0.5and1.0C after110-cycle, respectively. It indicated the positive effects of conductive metallic oxide on electrochemical performances of cathode materials.
4. Symbiotic compounds modified LiFePO4/C cathode materials. Symbiotic compounds (Li3PO4, Li4P2O7and Fe2P2O7) modified LiFePO4/C and FeWO4modified LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4, Li2CO3, NH4H2PO4,(NH4)10W12O41·xH2O and glucose as raw materials.(1) The FeWO4adding did not contribute to the improved electrochemical performances of cathode materials.(2) The symbiotic compound of Li3PO4adding can improve the charge-discharge performance of LiFePO4cathode materials, but the improvements were very little because of lower lithium ionic conductivity of Li3PO4.(3) The existence of Li4P2O7as fast ionic conductor can improve electrochemical performances of cathode materials, but the cycling performance was very bad.(4) Compared with the adding of Li4P2O7, the existence of Fe2P2O7can not only improve the charge-discharge performance, but also maintain good cycling performance, it could be because of higher lithium ionic conductivity or electronic conductivity of Fe2P2O7.(5) When the Fe2P2O7content is5wt%, the sample had the highest discharge specific capacity of146.7mAh/g at0.1C at room temperature, the discharge specific capacity still reached130mAh/g after110charge-discharge cycle, and the sample had the highest apparent lithium ion diffusion coefficient.
1.铁源、碳源和煅烧方法对LiFePO4/C正极材料的影响。分别以草酸亚铁和氧化铁为铁源,葡萄糖、蔗糖、柠檬酸、聚乙二醇4000、可溶性淀粉和己二酸为碳源,以碳酸锂为锂源、磷酸二氢铵为磷源采用原位固相法合成了LiFePO4/C正极材料。(1)不同碳源对正极材料的颗粒大小、形貌及碳结构有一定的影响,其中以葡萄糖和蔗糖为碳源合成的正极材料的颗粒大小均匀、分散性良好,且碳的石墨化程度较高。(2)对比两种铁源发现,以草酸亚铁为铁源,葡萄糖为碳源合成的正极材料粒度较小,分散性好,颗粒形貌较规则,且具有相对较好的充放电性能。(3)随着煅烧温度的升高和时间的延长,正极材料的结晶度逐渐提高,颗粒大小逐渐均匀,分散性逐渐变好,当温度升高至800℃以上时正极材料的粒径随温度变化较大,同时有杂相Fe2P生成。
2.金属氧化物修饰LiFePO4/C正极材料。以草酸亚铁(或三氧化二铁)、碳酸锂、磷酸二氢铵、葡萄糖、碳酸锌、钨酸铵和钼酸铵为原料,采用原位合成法成功合成了ZnO修饰LiFePO4/C正极材料,并首次合成了WO2和MoO2修饰LiFePO4/C正极材料及MoO2修饰LiFePO4正极材料。在合成过程中,各金属氧化物前驱体及碳源的分解在LiFePO4正极材料的颗粒之间及表面构架了以金属氧化物和碳为混合体的导电介质,从而达到提高正极材料电化学性能的目的。研究发现：(1)由于ZnO的电子电导率相对较低,ZnO的添加对提高正极材料的电化学性能的贡献很小。(2)电子导电率高的WO2和MoO2的添加能明显改善正极材料的电化学性能,当导电金属氧化物W02和M002含量为5wt%时,正极材料在0.1C倍率下具有最大的首次放电比容量,分别为120.1mAh/g和142.6mAh/g,此时正极材料的表观锂离子扩散系数最大,电荷转移阻抗最小。但由于导电金属氧化物结晶度较低、表面部分被氧化及其在电解液中的部分溶解导致正极材料在不同倍率下的循环性能较差。(3)在对不含碳的MoO2修饰LiFePO4正极材料研究时发现,仅仅依靠Mo02的添加也可以提高正极材料的电化学性能,MoO2含量为5wt%时,正极材料在0.1C倍率下的首次放电比容量已提高至76.6mAh/g,与未添加Mo02的样品相比,放电比容量提高了59.8mAh/go
3.金属氧化物和碳共包覆LiFePO4正极材料。以草酸亚铁、碳酸锂、磷酸二氢铵、葡萄糖及硝酸锌、钨酸铵、钼酸铵、碳酸铵和柠檬酸为原料,采用二步法成功合成了ZnO与碳共包覆LiFePO4正极材料,并首次合成了WO2和MoO2与碳共包覆LiFePO4正极材料。由于LiFePO4/C正极材料中的少量碳不能在LiFePO4颗粒表面形成完整的包覆层,因此金属氧化物对LiFePO4颗粒表面裸露部分的修复将提高包覆层的完整性和连续性,从而改善正极材料的电化学性能。研究发现：(1)适量的ZnO包覆提高了正极材料的充放电比容量和锂离子扩散系数,降低了电荷转移阻抗,同时具有较好的循环性能。(2)电子电导率更高的WO2和Mo02的包覆相对于ZnO包覆来讲,能更好的提高正极材料的电化学性能,其充放电比容量和表观锂离子扩散系数更高,同时也具有较好的循环性能,其中WO2与碳共包覆LiFePO4正极材料在0.1、0.2、0.5和1.0C倍率下110次循环后的放电比容量分别为153.7、144.5、137.5和121mAh/g;MoO2与碳共包覆LiFePO4正极材料在0.1、0.2、0.5和1.0C倍率下110次循环后的放电比容量分别为157、136.16、131.3和119.1mAh/g,说明导电金属氧化物对提高正极材料的电化学性能具有良好的促进作用。
4.共生化合物修饰LiFePO4/C正极材料。以草酸亚铁、碳酸锂、磷酸二氢铵、葡萄糖和钨酸铵为原料,采用原位固相法合成了共生化合物(Li3PO4、Li4P2O7和Fe2P2O7)修饰LiFePO4/C正极材料和FeWO4修饰LiFePO4/C正极材料。研究发现：(1) FeWO4的添加对正极材料电化学性能的提高没有贡献。(2)由于Li3PO4离子电导率较低,其对提高正极材料电化学性能的贡献较小。(3)作为快离子导体的Li4P2O7的添加能较好的提高正极材料的充放电性能,但其循环性能较差。(4)首次研究了共生化合物Fe2P2O7对正极材料的影响,相比之下,Fe2P2O7的添加不仅可以更好的提高正极材料的充放电比容量,而且具有较好的循环性能,这可能是由于Fe2P2O7具有良好离子导电性或电子导电性而实现的。(5)当正极材料的Fe2P2O7含量为5wt%时,在0.1C倍率下具有最高的首次放电比容量146.7mAh/g,110次循环后仍保持130mAh/g以上,同时具有最高的表观锂离子扩散系数。
The lithium ion power battery has become the research hotspot in recent years with the emergency of energy crisis and environmental crisis. LiFePO4has received much attention as a promising storage compound for cathodes in lithium-ion batteries due to it has high specific capacity, good cycle performance, safety, low costs and environmental friendliness. In this paper, the LiFePO4/C, metallic oxide modified LiFePO4/C, metallic oxide and carbon co-coated LiFePO4and symbiotic compounds modified LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method and two step method with the cheap chemistry reagents as raw materials. The phase composition and structure of cathode materials were characterized and analyzed by XRD、Raman、 SEM、 TEM, EDS and XPS. The electrochemical performances of cathode materials were tested and studied by charge-discharge technology, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The main results are as follows:
1. The effects of carbon source, iron source and calcination method on the electrochemical performances of LiFePO4/C cathode materials. The LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4and Fe2O3as iron source, glucose, sucrose, citric acid, polyethylene glycol4000, starch and hexanedioic acid as carbon source, Li2CO3as lithium source and NH4H2PO4as phosphorous source, respectively.(1) There were the obvious effects of carbon sources on carbon structure, particle size and shape of LiFePO4/C cathode materials, the samples synthesized with glucose and sucrose as carbon sources had uniform particle size, well dispersibility and higher graphitization degree of carbon.(2) The cathode materials synthesized with Fe2C2C2O4as iron source and glucose as carbon sources had smaller particle size, well dispersibility and regular shape.(3) With calcination temperature increasing and time prolonging, the crystallinity of LiFePO4increased, particles size become gradually uniform and dispersion become gradually good. When calcination temperature was increased over800℃, the increasing of particles size was significant with the temperature change, and the new phase of Fe2P generated.
2. Metallic oxide modified LiFePO4/C cathode materials. ZnO modified LiFePO4/C, W02modified LiFePO4/C, MoO2modified LiFePO4/C and MoO2modified LiFePO4cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4(or Fe2O3), Li2CO3, NH4H2PO4, ZnCO3,(NH4)10W12O41·xH2O,(NH4)6Mo7O24-4H2O and glucose as raw materials. In the synthesis process, the conducting medium composed by metal oxide and carbon on the LiFePO4particles surface and in gap of particles would improve the electrochemical performances of cathode materials, which were formed by the decomposition of metal oxide precursors and carbon sources.(1) The existence of ZnO could improve the charge-discharge specific capacity of cathode materials, but the improvement was very low because of lower electronic conductivity of ZnO.(2) The adding of WO2and MoO2with high electronic conductivity could obvious improve electrochemical performances of cathode materials. The cathode materials with5wt%conductive metal oxides exhibited the best electrochemical performance; they had the maximum value of initial discharge specific capacity of120.1mAh/g and142.6mAh/g at0.1C at room temperature, respectively, the maximum apparent lithium ion diffusion coefficient and the minimum charge transfer resistance. However, because of WO2and MoO2lower crystallinity, partially oxidized of surface and partially dissolved by electrolyte, the cycle performance of cathode materials is poor at different charge-discharge rate.(3) MoO2modified LiFePO4cathode materials without carbon had better charge-discharge performance, when the MoO2content is5wt%, the sample had higher initial discharge specific capacity of76.6mAh/g at0.1C at room temperature, compared with the sample without MoO2, the discharge specific capacity rose59.8mAh/g.
3. Metallic oxide and carbon co-coated LiFePO4cathode materials. ZnO and carbon co-coated LiFePO4, WO2and carbon co-coated LiFePO4and MoO2and carbon co-coated LiFePO4cathode materials were synthesized by two step method. In LiFePO4/C, the small amounts of carbon can not form a full coating layer on the surface of LiFePO4, but the adding of metal oxides could repair the bare surface of LiFePO4particles, make the coating layer more full and continuous and improve electrochemical performances of cathode materials.(1) The right amount of ZnO coating could improve charge-discharge specific capacity and apparent lithium ion diffusion coefficient, and decrease charge transfer resistance, and the sample with3wt%ZnO has better cycle performance in different charge-discharge rate.(2) Relative to ZnO coating, the WO2and MoO2coating could improve electrochemical performances even more, including higher charge-discharge specific capacity, higher apparent lithium ion diffusion coefficient and lower charge transfer resistance and good cycle performance. The discharge specific capacity of WO2and carbon co-coated LiFePO4cathode materials are153.7,144.5,137.5and121mAh/g at0.1,0.2,0.5and1.0C after110-cycle, respectively, The discharge specific capacity of MoO2and carbon co-coated LiFePO4cathode materials are157,136.16,131.3and119.1mAh/g at0.1,0.2,0.5and1.0C after110-cycle, respectively. It indicated the positive effects of conductive metallic oxide on electrochemical performances of cathode materials.
4. Symbiotic compounds modified LiFePO4/C cathode materials. Symbiotic compounds (Li3PO4, Li4P2O7and Fe2P2O7) modified LiFePO4/C and FeWO4modified LiFePO4/C cathode materials were synthesized by in-situ solid phase synthetic method with Fe2C2O4, Li2CO3, NH4H2PO4,(NH4)10W12O41·xH2O and glucose as raw materials.(1) The FeWO4adding did not contribute to the improved electrochemical performances of cathode materials.(2) The symbiotic compound of Li3PO4adding can improve the charge-discharge performance of LiFePO4cathode materials, but the improvements were very little because of lower lithium ionic conductivity of Li3PO4.(3) The existence of Li4P2O7as fast ionic conductor can improve electrochemical performances of cathode materials, but the cycling performance was very bad.(4) Compared with the adding of Li4P2O7, the existence of Fe2P2O7can not only improve the charge-discharge performance, but also maintain good cycling performance, it could be because of higher lithium ionic conductivity or electronic conductivity of Fe2P2O7.(5) When the Fe2P2O7content is5wt%, the sample had the highest discharge specific capacity of146.7mAh/g at0.1C at room temperature, the discharge specific capacity still reached130mAh/g after110charge-discharge cycle, and the sample had the highest apparent lithium ion diffusion coefficient.
引文
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