锂离子和锂聚合物电池用LiFePO_4-C阴极材料的合成及其电化学性能研究
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摘要
最近,具有层状的橄榄石结构的锂过渡金属磷酸盐,LiMPO4 (M=Fe、Mn、Ni、Co),因为其高的理论比容量(170 mAh g-1),已经吸引了广泛的注意力。LiMPO4中M3+/M2+氧化还原对的电位如下所述:LiFePO_4的电位是3.5 V,LiMnPO4的电位是4.1 V,LiNiPO4的电位是5.2-5.4 V,LiCoPO_4的电位是4.8 V。在这些磷酸盐当中,LiFePO_4的出色的稳定性,低廉的价格和对环境的高度亲和性,是最吸引人的。
我们采用水热法合成了LiFePO_4,随后对其进行了高效能球磨和热处理。为了加强LiFePO_4的电子电导率,我们加入了不同的碳导电添加剂:纳米级别的乙炔黑(acetylene black, AB)和多壁纳米碳管(multi-walled carbon nanotubes, MWCNTs)。通过X射线衍射仪、扫描电镜、透射电镜、高分辨透射电镜,我们调查了LiFePO_4-C的结构和形貌特性。组装电化学电池时,我们使用了不同的电解质:液体电解质(liquid electrolyte, LE)和固体聚合物电解质(solid polymer electrolyte, SPE)。通过循环伏安法和充放电实验,我们分析了Li/LE/LiFePO_4、Li/LE/LiFePO_4-C、Li/SPE/LiFePO_4、Li/SPE/LiFePO_4-C电池的电化学性能。实验结果证实了具有5 wt% MWCNTs的Li/LE/LiFePO_4-MWCNTs电池有最好的电化学性能,在0.25 C速率放电时,室温放电容量达到了142 mAh g-1。同时实验结果也表明了具有5 wt% MWCNTs的Li/SPE/LiFePO_4-MWCNTs电池有最好的电化学性能,在0.25 C速率放电时,室温放电容量达到了115 mAh g-1。
In this study, LiFePO_4 and LiFePO_4-C composite were synthesized by a hydrothermal method followed by ball-milling and heat treating. Different carbon conductive additives including nano-sized acetylene black (AB) and multi-walled carbon nanotubes (MWCNTs) were used to enhance the electronic conductivity of LiFePO_4. In the meantime, different electrolytes including liquid electrolyte (LE) and solid polymer electrolyte (SPE) were used. The physical performance of LiFePO_4 and LiFePO_4-C composite was analysed by electronic conductivity, BET, SEM, TEM HR-TEM and XRD. The electrochemical performance of Li/LE/LiFePO_4, Li/LE/LiFePO_4-AB, Li/LE/LiFePO_4-MWCNTs, Li/SPE/LiFePO_4 and Li/SPE/LiFePO_4-MWCNTs batteries was analysed by AC impedance, CV and charge/discharge tests.
LiFePO_4 was synthesized by a hydrothermal method at different temperatures. LiFePO_4 synthesized at 170℃and subsequent 500℃can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma and the average particle size of 200 nm. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4 powders. The discharge capacity of 167 mAh g-1 (98% of the theoretical capacity) at discharge rate of 0.1 C is the largest compared to other samples. CV results demonstrate that the reversibility and reactivity of lithium extraction/insertion reactions at the electrode/electrolyte interface in LiFePO_4 synthesized at 170℃and subsequent 500℃are the best. The charge/discharge tests at different C rates indicate that the battery may operate at relatively high rates, confirming the improved kinetics of LiFePO_4 cathode materials.
LiFePO_4-AB composite was synthesized by a hydrothermal method followed by ball-milling and heat treating. The tests demonstrate that the electronic conductivities are 5.86×10-9 S cm-1 for LiFePO_4, 8.00×10-5 S cm-1 for LiFePO_4-AB with 5 wt%, 7.85×10-4 S cm-1 for LiFePO_4-AB with 10 wt% and 2.71×10-2 S cm-1 for LiFePO_4-AB with 15 wt%. SEM and TEM observations indicate that LiFePO_4 is mixed well with AB and make the elctronic conductivity of LiFePO_4-AB composite improve. XRD results demonstrate that LiFePO_4-AB composite can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4-AB powders. There is no evidence for amorphous carbon. It is demonstrated that the added nano-sized AB does not change crystal structure of LiFePO_4. The charge/discharge tests demonstrate that the discharge capacities of Li/LE/LiFePO_4-AB batteries with 5 wt%, 10 wt% and 15 wt% AB hardly change upon cycling and cycling performance of Li/LE/LiFePO_4-AB battery with 10 wt% is the best and its discharge capacity is 123 mAh g-1.
LiFePO_4-MWCNTs composite was synthesized by a hydrothermal method followed by ball-milling and heat treating. The tests demonstrate that the electronic conductivities are 5.86×10-9 S cm-1 for LiFePO_4, 1.08×10-1 S cm-1 for LiFePO_4-MWCNTs with 5 wt%. SEM observations show that the MWCNTs intertwine with LiFePO_4 particles together to form a three-dimensional network. The dispersed MWCNTs provide pathways for electron transference and make the elctronic conductivity of LiFePO_4-MWCNTs composite obviously improve. XRD results demonstrate that LiFePO_4-MWCNT composite can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4-MWCNTs powders. There is no evidence for amorphous carbon. It is demonstrated that the added nano-sized MWCNTs do not change crystal structure of LiFePO_4. The charge/discharge tests demonstrate that the discharge capacities of Li/LE/LiFePO_4-MWCNTs batteries with 2.5 wt%, 5 wt% and 10 wt% MWCNTs hardly change upon cycling and cycling performance of Li/LE/LiFePO_4-MWCNTs battery with 5 wt% is the best and its discharge capacity is 142 mAh g-1. In the meantime, it is demonstrated that the cycling performance of Li/LE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/LE/LiFePO_4-AB battery with 5 wt% AB.
The lithium-ion diffusion coefficient of LiFePO_4-MWCNTs composite with 5 wt% MWCNTs is improved from 2.41×10-15 cm2 s-1 for pure LiFePO_4 to 1.50×10-14 cm2 s-1 for LiFePO_4-MWCNTs composite with 5 wt% MWCNTs. It is demonstrated that the resistance of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs does not change upon cycling and is 280 ?. CV results demonstrate that the redox peak profile of Li/SPE LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is more symmetric and spiculate than that of Li/SPE/LiFePO_4, demonstrating that the reversibility and reactivity of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs are enhanced due to improvement of electronic conductivity and the reduced diffusion length resulting from a decrease in the crystallite size by MWCNTs. The initial charge/discharge curves of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at a discharge rate of 0.25 C demonstrate that Li/SPE/LiFePO_4 -MWCNTs battery with 5 wt.% MWCNTs exhibits the highest specific capacity with a charge capacity of 122 mAh g-1 and a discharge capacity of 115 mAh g-1. The rate capability of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at various C rates ranging from 0.1C to 3C rate (1C=170 mA g-1) at room temperature demonstrate that the discharge rate capability of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/SPE/LiFePO_4. The cycling performance of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at various C rates ranging from 0.1C to 3C rate (1C=170 mA g-1) at room temperature demonstrates that the high-rate discharge performance of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/SPE/LiFePO_4.
我们采用水热法合成了LiFePO_4,随后对其进行了高效能球磨和热处理。为了加强LiFePO_4的电子电导率,我们加入了不同的碳导电添加剂:纳米级别的乙炔黑(acetylene black, AB)和多壁纳米碳管(multi-walled carbon nanotubes, MWCNTs)。通过X射线衍射仪、扫描电镜、透射电镜、高分辨透射电镜,我们调查了LiFePO_4-C的结构和形貌特性。组装电化学电池时,我们使用了不同的电解质:液体电解质(liquid electrolyte, LE)和固体聚合物电解质(solid polymer electrolyte, SPE)。通过循环伏安法和充放电实验,我们分析了Li/LE/LiFePO_4、Li/LE/LiFePO_4-C、Li/SPE/LiFePO_4、Li/SPE/LiFePO_4-C电池的电化学性能。实验结果证实了具有5 wt% MWCNTs的Li/LE/LiFePO_4-MWCNTs电池有最好的电化学性能,在0.25 C速率放电时,室温放电容量达到了142 mAh g-1。同时实验结果也表明了具有5 wt% MWCNTs的Li/SPE/LiFePO_4-MWCNTs电池有最好的电化学性能,在0.25 C速率放电时,室温放电容量达到了115 mAh g-1。
In this study, LiFePO_4 and LiFePO_4-C composite were synthesized by a hydrothermal method followed by ball-milling and heat treating. Different carbon conductive additives including nano-sized acetylene black (AB) and multi-walled carbon nanotubes (MWCNTs) were used to enhance the electronic conductivity of LiFePO_4. In the meantime, different electrolytes including liquid electrolyte (LE) and solid polymer electrolyte (SPE) were used. The physical performance of LiFePO_4 and LiFePO_4-C composite was analysed by electronic conductivity, BET, SEM, TEM HR-TEM and XRD. The electrochemical performance of Li/LE/LiFePO_4, Li/LE/LiFePO_4-AB, Li/LE/LiFePO_4-MWCNTs, Li/SPE/LiFePO_4 and Li/SPE/LiFePO_4-MWCNTs batteries was analysed by AC impedance, CV and charge/discharge tests.
LiFePO_4 was synthesized by a hydrothermal method at different temperatures. LiFePO_4 synthesized at 170℃and subsequent 500℃can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma and the average particle size of 200 nm. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4 powders. The discharge capacity of 167 mAh g-1 (98% of the theoretical capacity) at discharge rate of 0.1 C is the largest compared to other samples. CV results demonstrate that the reversibility and reactivity of lithium extraction/insertion reactions at the electrode/electrolyte interface in LiFePO_4 synthesized at 170℃and subsequent 500℃are the best. The charge/discharge tests at different C rates indicate that the battery may operate at relatively high rates, confirming the improved kinetics of LiFePO_4 cathode materials.
LiFePO_4-AB composite was synthesized by a hydrothermal method followed by ball-milling and heat treating. The tests demonstrate that the electronic conductivities are 5.86×10-9 S cm-1 for LiFePO_4, 8.00×10-5 S cm-1 for LiFePO_4-AB with 5 wt%, 7.85×10-4 S cm-1 for LiFePO_4-AB with 10 wt% and 2.71×10-2 S cm-1 for LiFePO_4-AB with 15 wt%. SEM and TEM observations indicate that LiFePO_4 is mixed well with AB and make the elctronic conductivity of LiFePO_4-AB composite improve. XRD results demonstrate that LiFePO_4-AB composite can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4-AB powders. There is no evidence for amorphous carbon. It is demonstrated that the added nano-sized AB does not change crystal structure of LiFePO_4. The charge/discharge tests demonstrate that the discharge capacities of Li/LE/LiFePO_4-AB batteries with 5 wt%, 10 wt% and 15 wt% AB hardly change upon cycling and cycling performance of Li/LE/LiFePO_4-AB battery with 10 wt% is the best and its discharge capacity is 123 mAh g-1.
LiFePO_4-MWCNTs composite was synthesized by a hydrothermal method followed by ball-milling and heat treating. The tests demonstrate that the electronic conductivities are 5.86×10-9 S cm-1 for LiFePO_4, 1.08×10-1 S cm-1 for LiFePO_4-MWCNTs with 5 wt%. SEM observations show that the MWCNTs intertwine with LiFePO_4 particles together to form a three-dimensional network. The dispersed MWCNTs provide pathways for electron transference and make the elctronic conductivity of LiFePO_4-MWCNTs composite obviously improve. XRD results demonstrate that LiFePO_4-MWCNT composite can be indexed to a single-phase material having an orthorhombic olivine-type structure with a space group of Pnma. No impurity such as Fe2O3, Li_3Fe_2(PO_4)_3 and Li3PO4 is found in the LiFePO_4-MWCNTs powders. There is no evidence for amorphous carbon. It is demonstrated that the added nano-sized MWCNTs do not change crystal structure of LiFePO_4. The charge/discharge tests demonstrate that the discharge capacities of Li/LE/LiFePO_4-MWCNTs batteries with 2.5 wt%, 5 wt% and 10 wt% MWCNTs hardly change upon cycling and cycling performance of Li/LE/LiFePO_4-MWCNTs battery with 5 wt% is the best and its discharge capacity is 142 mAh g-1. In the meantime, it is demonstrated that the cycling performance of Li/LE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/LE/LiFePO_4-AB battery with 5 wt% AB.
The lithium-ion diffusion coefficient of LiFePO_4-MWCNTs composite with 5 wt% MWCNTs is improved from 2.41×10-15 cm2 s-1 for pure LiFePO_4 to 1.50×10-14 cm2 s-1 for LiFePO_4-MWCNTs composite with 5 wt% MWCNTs. It is demonstrated that the resistance of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs does not change upon cycling and is 280 ?. CV results demonstrate that the redox peak profile of Li/SPE LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is more symmetric and spiculate than that of Li/SPE/LiFePO_4, demonstrating that the reversibility and reactivity of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs are enhanced due to improvement of electronic conductivity and the reduced diffusion length resulting from a decrease in the crystallite size by MWCNTs. The initial charge/discharge curves of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at a discharge rate of 0.25 C demonstrate that Li/SPE/LiFePO_4 -MWCNTs battery with 5 wt.% MWCNTs exhibits the highest specific capacity with a charge capacity of 122 mAh g-1 and a discharge capacity of 115 mAh g-1. The rate capability of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at various C rates ranging from 0.1C to 3C rate (1C=170 mA g-1) at room temperature demonstrate that the discharge rate capability of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/SPE/LiFePO_4. The cycling performance of Li/SPE/LiFePO_4-MWCNTs batteries with different MWCNTs contents at various C rates ranging from 0.1C to 3C rate (1C=170 mA g-1) at room temperature demonstrates that the high-rate discharge performance of Li/SPE/LiFePO_4-MWCNTs battery with 5 wt% MWCNTs is better than that of Li/SPE/LiFePO_4.
引文
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