以不同原料制备锂离子电池复合正极材料LiFePO_4/C的研究
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摘要
橄榄石结构LiFePO_4具有原料丰富、无毒、热稳定性强、循环性能好、理论容量高(170mAh·g~(-1))等优点,能很好的符合信息社会对新型能源的需求和环保的需要,是新一代商品化锂离子电池正极材料中的有力竞争者。但其固有的晶体结构和元素组成,造成材料振实密度低、导电性能差、电化学活性低。这些性能亟待改善。
本文系统研究了不同铁源和碳源对合成LiFePO_4/C材料性能的影响;探索新原料新工艺合成LiFePO_4/C,以突破国外制备工艺的专利垄断;选取具有代表性的离子,研究了Li位和Fe位掺杂对LiFePO_4材料的晶体结构和电化学性能的影响;对LiFePO_4/C电极进行表面碳包覆改性进一步提高了电极的倍率性能;采用CV和EIS研究了LiFePO_4/C电极在较高温度下的电化学行为,为进一步开辟提高材料电化学性能的途径提供理论参考。
以Fe_2O_3为铁源,详细考察了合成温度对LiFePO_4/C材料晶体性能、碳含量、振实密度和电化学性能的影响。较FeC_2O_4·2H_2O,采用Fe_2O_3合成了振实密度更高电化学性能优良的LiFePO_4/C材料。研究了不同球磨分散介质对LiFePO_4/C的充放电容量和振实密度的影响。较乙醇和水,采用丙酮作为球磨分散介质制备了充放电容量和平台以及循环和倍率性能更优、振实密度更高的LiFePO_4/C材料。
首次提出以Fe_2O_3和NH_4H_2PO_4为原料一步固相法制备Fe_2P_2O_7的工艺。以Fe_2P_2O_7和Li_2CO_3为原料制备的LiFePO_4保持了较好的颗粒形貌和均匀的粒度分布。在不额外加入还原剂的情况下实现了Fe~(3+)→Fe~(2+):Fe_2O_3→Fe_2P_2O_7→LiFePO_4。以丙酮代替乙醇作球磨分散介质合成了性能优良的LiFePO_4/C材料。
以还原铁粉、LiFePO_4和葡萄糖为原料,经球磨机械活化后高温下制备了LiFePO_4/C正极材料。700℃是合成LiFePO_4的最佳温度。具有纳米级一次粒径的软团聚LiFePO_4/C粉末材料表现出了较好的电化学性能。
大部分有机碳前驱体的无氧热解碳呈蓬松状态,在LiFePO_4/C材料颗粒间形成有效的导电连接。采用均苯四甲酸酐、柠檬酸和蔗糖可制备电化学性能优良的LiFePO_4/C材料。单独以石墨或乙炔黑对LiFePO_4进行包覆/掺杂对提高材料的电化学性能有限。
研究了LiFePO_4的Li位和Fe位掺杂对材料电化学性能的影响。一定浓度的Mg~(2+)和Ca~(2+)的Li位掺杂均可以不同程度改善LiFePO_4/C的倍率性能。Co~(2+)、Ni~(2+)和Mn~(2+)的Fe位掺杂对LiFePO_4/C电化学性能的影响取决于掺杂浓度。首次发现了正磷酸盐中Co~(3+)/Co~(2+)和Ni~(3+)/Ni~(2+)电对在较低电位下的电化学活性。LiFe_(0.94)Co_(0.06)PO_4/C和LiFe_(0.94)Ni_(0.06)PO_4/C电极的CV曲线在4.0V左右出现了Co~(3+)/Co~(2+)和Ni~(3+)/Ni~(2+)电对的氧化还原峰。
提出了碳包覆修饰LiFePO_4/C电极以提高其电化学性能:大幅度提高了电极充放电容量和倍率性能;分别降低和提高了Fe~(3+) /Fe~(2+)电对氧化和还原电位;减小了电极过程电荷转移阻抗。
分别采用CV和EIS研究了LiFePO_4/C在较高温度下的电化学性能。结果均表明:提高LiFePO_4/C电极的工作温度,可以增加电极的Li~+扩散系数,增大电极的可逆性,有利于活性材料充放电容量的发挥,提高电极的深度充放能力。
With the merits of abundant raw materials, non-toxicity, good thermal stability, excellent charge/discharge cycle ability and high theoretical capacity (170mAh·g~(-1)), olivine-structured LiFePO_4 can meet the needs of both demand of new energy-consuming information society and environmental protection. LiFePO_4 has become one of the most promising contenders among the new generation of commercial cathode materials. Its intrinsic crystal structure and elemental composition, however, result in properties of low tap density, poor electronic conductivity and electrochemical inertness, which urgently needed to be improved.
In the paper, the impacts of different iron sources and carbon precursors on the properties of LiFePO_4/C material were studied systematically: the tap density of LiFePO_4/C was enhanced with improved technological conditions; new raw materials and new techniques were explored for synthesis of LiFePO_4/C in order to bypass the monopoly of foreign patents; doping effects of representative ions on both Li and Fe sites on the crystal structure and electrochemical properties of LiFePO_4 were investigated; the rate performance of LiFePO_4/C electrode was further improved by coating the electrode surface with carbon; CV and EIS were used to investigate the electrochemical behavior of LiFePO_4/C electrode at higher working temperatures, which provided a theoretical reference for opening up a method to further improve material's electrochemical performance.
Using Fe_2O_3 as the iron source, the influences of synthesis temperature on the crystal property, carbon content, tap density and electrochemical performance of LiFePO_4/C were investigated in detail. LiFePO_4/C material of high tap density and excellent electrochemical performance was prepared when using Fe_2O_3, compared to FeC_2O_4·2H_2O as an iron source. The effects of different ball-milling dispersive media on charge/discharge capacity and tap density of LiFePO_4/C were studied. Compared to ethanol and water, using acetone as dispersive medium, LiFePO_4/C cathode material of better charge/discharge capacity and plateau, better cycling and rate performance and higher tap density was synthesized.
In the paper, one-step solid state reaction was for the first time put forward to prepare Fe_2P_2O_7 using Fe_2O_3 and NH_4H_2PO_4 as raw materials. Fe_2P_2O_7 and Li_2CO_3 were employed to synthesize LiFePO_4 which exhibited good particle morphology and even size distribution. Fe~(3+)→Fe~(2+) was realized with no extra addition of reducing agent: Fe_2O_3→Fe_2P_2O_7→LiFePO_4. LiFePO_4/C of good property was synthesized by using acetone instead of ethanol as dispersive medium.
Reduced iron, LiH_2PO_4 and glucose were mechanically activated by ball-milling and LiFePO_4/C cathode material was prepared at high temperature. 700℃was the optimum synthesis temperature. With nano-sized primary articles, LiFePO_4/C powder material showed a good electrochemical performance.
Most carbon from oxygen free pyrolysis of organic precursors exhibited a fluey morphology and formed an effective conducting connection between LiFePO_4/C particles. LiFePO_4/C of good electrochemical properties could be prepared using pyromellitic anhydride, citric acid and sucrose as carbon precursor respectively. Little improvement in electrochemical performance could be obtained by modifying LiFePO_4 with using only graphite or acetylene black.
The doping effects of Li and Fe site on the electrochemical properties of LiFePO_4 were investigated. Electrochemical performance of LiFePO_4 could be enhanced to different extent by Mg~(2+) and Ca~(2+) doping on Li site with a certain concentration. The influences of Fe site doping by Co~(2+), Ni~(2+) and Mn~(2+) depended on doping concentration. The electrochemical activity at lower potential of Co~(3+)/Co~(2+) and Ni~(3+)/Ni~(2+) redox couples in orthophosphate was for the first time discovered in the paper. 4V redox peaks for Co~(3+)/Co~(2+) and Ni~(3+)/Ni~(2+) were revealed on the CV curves for LiFe_(0.94)Co_(0.06)PO_4/C and LiFe_(0.94)Ni_(0.06)PO_4/C electrode.
Electrochemical properties of LiFePO_4/C electrode were improved by carbon coating modification: discharge capacity and rate ability weregreatly enhanced; oxidation and reduction voltages for Fe~(3+) /Fe~(2+) couple were decreased and increased respectively; charge transfer impedance was greatly reduced.
The electrochemical properties of LiFePO_4/C at higher temperatures were examined with CV and EIS. Results indicated diffusion coefficient for Li~+ and irreversibility for LiFePO_4 electrode were raised by increasing working temperature. Higher temperature could benefit exertion of charge/discharge capacity and raise the depth of charge and discharge.
本文系统研究了不同铁源和碳源对合成LiFePO_4/C材料性能的影响;探索新原料新工艺合成LiFePO_4/C,以突破国外制备工艺的专利垄断;选取具有代表性的离子,研究了Li位和Fe位掺杂对LiFePO_4材料的晶体结构和电化学性能的影响;对LiFePO_4/C电极进行表面碳包覆改性进一步提高了电极的倍率性能;采用CV和EIS研究了LiFePO_4/C电极在较高温度下的电化学行为,为进一步开辟提高材料电化学性能的途径提供理论参考。
以Fe_2O_3为铁源,详细考察了合成温度对LiFePO_4/C材料晶体性能、碳含量、振实密度和电化学性能的影响。较FeC_2O_4·2H_2O,采用Fe_2O_3合成了振实密度更高电化学性能优良的LiFePO_4/C材料。研究了不同球磨分散介质对LiFePO_4/C的充放电容量和振实密度的影响。较乙醇和水,采用丙酮作为球磨分散介质制备了充放电容量和平台以及循环和倍率性能更优、振实密度更高的LiFePO_4/C材料。
首次提出以Fe_2O_3和NH_4H_2PO_4为原料一步固相法制备Fe_2P_2O_7的工艺。以Fe_2P_2O_7和Li_2CO_3为原料制备的LiFePO_4保持了较好的颗粒形貌和均匀的粒度分布。在不额外加入还原剂的情况下实现了Fe~(3+)→Fe~(2+):Fe_2O_3→Fe_2P_2O_7→LiFePO_4。以丙酮代替乙醇作球磨分散介质合成了性能优良的LiFePO_4/C材料。
以还原铁粉、LiFePO_4和葡萄糖为原料,经球磨机械活化后高温下制备了LiFePO_4/C正极材料。700℃是合成LiFePO_4的最佳温度。具有纳米级一次粒径的软团聚LiFePO_4/C粉末材料表现出了较好的电化学性能。
大部分有机碳前驱体的无氧热解碳呈蓬松状态,在LiFePO_4/C材料颗粒间形成有效的导电连接。采用均苯四甲酸酐、柠檬酸和蔗糖可制备电化学性能优良的LiFePO_4/C材料。单独以石墨或乙炔黑对LiFePO_4进行包覆/掺杂对提高材料的电化学性能有限。
研究了LiFePO_4的Li位和Fe位掺杂对材料电化学性能的影响。一定浓度的Mg~(2+)和Ca~(2+)的Li位掺杂均可以不同程度改善LiFePO_4/C的倍率性能。Co~(2+)、Ni~(2+)和Mn~(2+)的Fe位掺杂对LiFePO_4/C电化学性能的影响取决于掺杂浓度。首次发现了正磷酸盐中Co~(3+)/Co~(2+)和Ni~(3+)/Ni~(2+)电对在较低电位下的电化学活性。LiFe_(0.94)Co_(0.06)PO_4/C和LiFe_(0.94)Ni_(0.06)PO_4/C电极的CV曲线在4.0V左右出现了Co~(3+)/Co~(2+)和Ni~(3+)/Ni~(2+)电对的氧化还原峰。
提出了碳包覆修饰LiFePO_4/C电极以提高其电化学性能:大幅度提高了电极充放电容量和倍率性能;分别降低和提高了Fe~(3+) /Fe~(2+)电对氧化和还原电位;减小了电极过程电荷转移阻抗。
分别采用CV和EIS研究了LiFePO_4/C在较高温度下的电化学性能。结果均表明:提高LiFePO_4/C电极的工作温度,可以增加电极的Li~+扩散系数,增大电极的可逆性,有利于活性材料充放电容量的发挥,提高电极的深度充放能力。
With the merits of abundant raw materials, non-toxicity, good thermal stability, excellent charge/discharge cycle ability and high theoretical capacity (170mAh·g~(-1)), olivine-structured LiFePO_4 can meet the needs of both demand of new energy-consuming information society and environmental protection. LiFePO_4 has become one of the most promising contenders among the new generation of commercial cathode materials. Its intrinsic crystal structure and elemental composition, however, result in properties of low tap density, poor electronic conductivity and electrochemical inertness, which urgently needed to be improved.
In the paper, the impacts of different iron sources and carbon precursors on the properties of LiFePO_4/C material were studied systematically: the tap density of LiFePO_4/C was enhanced with improved technological conditions; new raw materials and new techniques were explored for synthesis of LiFePO_4/C in order to bypass the monopoly of foreign patents; doping effects of representative ions on both Li and Fe sites on the crystal structure and electrochemical properties of LiFePO_4 were investigated; the rate performance of LiFePO_4/C electrode was further improved by coating the electrode surface with carbon; CV and EIS were used to investigate the electrochemical behavior of LiFePO_4/C electrode at higher working temperatures, which provided a theoretical reference for opening up a method to further improve material's electrochemical performance.
Using Fe_2O_3 as the iron source, the influences of synthesis temperature on the crystal property, carbon content, tap density and electrochemical performance of LiFePO_4/C were investigated in detail. LiFePO_4/C material of high tap density and excellent electrochemical performance was prepared when using Fe_2O_3, compared to FeC_2O_4·2H_2O as an iron source. The effects of different ball-milling dispersive media on charge/discharge capacity and tap density of LiFePO_4/C were studied. Compared to ethanol and water, using acetone as dispersive medium, LiFePO_4/C cathode material of better charge/discharge capacity and plateau, better cycling and rate performance and higher tap density was synthesized.
In the paper, one-step solid state reaction was for the first time put forward to prepare Fe_2P_2O_7 using Fe_2O_3 and NH_4H_2PO_4 as raw materials. Fe_2P_2O_7 and Li_2CO_3 were employed to synthesize LiFePO_4 which exhibited good particle morphology and even size distribution. Fe~(3+)→Fe~(2+) was realized with no extra addition of reducing agent: Fe_2O_3→Fe_2P_2O_7→LiFePO_4. LiFePO_4/C of good property was synthesized by using acetone instead of ethanol as dispersive medium.
Reduced iron, LiH_2PO_4 and glucose were mechanically activated by ball-milling and LiFePO_4/C cathode material was prepared at high temperature. 700℃was the optimum synthesis temperature. With nano-sized primary articles, LiFePO_4/C powder material showed a good electrochemical performance.
Most carbon from oxygen free pyrolysis of organic precursors exhibited a fluey morphology and formed an effective conducting connection between LiFePO_4/C particles. LiFePO_4/C of good electrochemical properties could be prepared using pyromellitic anhydride, citric acid and sucrose as carbon precursor respectively. Little improvement in electrochemical performance could be obtained by modifying LiFePO_4 with using only graphite or acetylene black.
The doping effects of Li and Fe site on the electrochemical properties of LiFePO_4 were investigated. Electrochemical performance of LiFePO_4 could be enhanced to different extent by Mg~(2+) and Ca~(2+) doping on Li site with a certain concentration. The influences of Fe site doping by Co~(2+), Ni~(2+) and Mn~(2+) depended on doping concentration. The electrochemical activity at lower potential of Co~(3+)/Co~(2+) and Ni~(3+)/Ni~(2+) redox couples in orthophosphate was for the first time discovered in the paper. 4V redox peaks for Co~(3+)/Co~(2+) and Ni~(3+)/Ni~(2+) were revealed on the CV curves for LiFe_(0.94)Co_(0.06)PO_4/C and LiFe_(0.94)Ni_(0.06)PO_4/C electrode.
Electrochemical properties of LiFePO_4/C electrode were improved by carbon coating modification: discharge capacity and rate ability weregreatly enhanced; oxidation and reduction voltages for Fe~(3+) /Fe~(2+) couple were decreased and increased respectively; charge transfer impedance was greatly reduced.
The electrochemical properties of LiFePO_4/C at higher temperatures were examined with CV and EIS. Results indicated diffusion coefficient for Li~+ and irreversibility for LiFePO_4 electrode were raised by increasing working temperature. Higher temperature could benefit exertion of charge/discharge capacity and raise the depth of charge and discharge.
引文
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