锂离子电池安全型电解质的制备及性能研究
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摘要
安全性问题是二次锂离子电池进一步发展的重要制约因素，而安全隐患的根源在于电解质。发展更安全的锂离子电池电解质比提高电池的功率及能量密度具有更为迫切的需求。本论文首先研究了两种不同结构的二硫化铌电极在液态有机电解质及常规凝胶态聚合物电解质的脱嵌锂性能，并将较优结构的电极材料应用于钠离子电池的电极材料；接着分别探索了新型凝胶聚合物电解质、抗热收缩的聚合物膜及匹配的不燃不爆离子液体、固体电解质等锂离子电池安全型电解质。
2H结构的二硫化铌脱嵌锂离子的性能较差，为了提高2H-NbS_2电化学性能，采用固相法分别合成了2H-Li_(0.7)NbS_2（点阵群：P6_3/mmc）和3R-NbS_2（点阵群：R3m）并研究了其脱嵌锂行为，结果表明2H-Li_(0.7)NbS_2和3R-NbS_2可以有效利用Nb(IV)/Nb(III)电对进行可逆的充放电反应。在普通液态电解质中2H-LixNbS_2在0.05C倍率时室温放电容量为169.5mAh g~(-1)，而3R LixNbS_2为169.0mAh g~(-1)。1C/1C倍率电流循环200圈后，2H-LixNbS_2容量衰减为9%，3R-LixNbS_2衰减率为14%。因此，2H和3R结构的NbS_2都是很好的脱嵌锂材料，尤其是2H结构显示了优异的电化学性能。接着，探索了两种结构的电极在聚（偏氟乙烯六氟丙烯）（P(VdF HFP)）凝胶聚合物电解质中的电化学行为。虽然在PVdF HFP聚合物电解质中的小倍率充放电时具有与液态电解质相似的循环稳定性，但倍率性能较差，尤其在10C时容量还不能达到液态电解质的一半。
将性能较好的2H-NbS_2结构应用于钠离子电池。参照2H-Li_(0.7)NbS_2的经验，采用固相法合成了Na0.5NbS_2（点阵群：P63/mmc）。在钠离子电池中，2H-Na_xNbS_2电极使用液态有机溶剂电解质的室温放电容量为143.6mAh g~(-1)，而在凝胶态PVdF HFP基聚合物电解质的放电容量略低，为141.2mAh g~(-1)，在x=0.5处出现明显的Na/空位重排现象。采用量化计算分析了重排后NaxNbS_2可能的结构及相对应的电化学性能。虽然层状NaMS_2体系允许钠离子全部嵌入，层内Na~+-Na~+之间的排斥力明显强于Li~+Li~+，导致整个钠离子层的滑移及钠离子的重新排列，这个过程反映在电压曲线上。
分别使用添加纳米Al_2O_3的共混聚合物PEO-P(VdF-HFP)及共聚物P(MMA-VAc)-co-PEGDA作为聚合物的基体，使用支撑体支撑后，制备得到凝胶聚合物电解质（GPE）。采用机械拉伸、热重分析、扫描电镜、循环伏安、电化学交流阻抗和充放电测试等对制备得到的聚合物膜及对应GPE进行性能分析。添加纳米颗粒后，两种凝胶聚合物电解质的室温锂离子电导率均可以达到3.8×10~(-3)S cm~(-1)，共混物PEO-P(VdF-HFP)的机械强度为14.3MPa，而共聚物P(MMA-VAc)-co-PEGDA为16.2MPa。采用相同结构Li/GPE/LiCoO_2的扣式电池在相同测试条件下，共混物循环50圈后容量保持率为87.2%；而共聚物循环100圈后能够保持初始容量的90.9%。制备得到的新型凝胶聚合物电解质具有较好的循环及倍率性能。
研究了抗热收缩的纳米颗粒/聚合物隔膜，同时结合离子液体PYR_(14)TFSI及锂盐LiTFSI形成新型凝胶聚合物电解质。结果显示，添加SiO_2纳米颗粒的效果优于纳米Al_2O_3。SiO_2/P(MMA-AN-VAc)+LiTFSI+PYR_(14)TFSI/VC为基体的GPE在室温下锂离子电导率为1.2×10~(-3)S cm~(-1)，氧化分解电压为5.3V (vs. Li/Li~-)。装成结构为Li/GPE/LiFePO_4的扣式电池后，0.1C倍率放电初始容量为143.4mAh g~(-1)，循环50圈后的容量保持率为99.6%。
采用高温固相法合成了Li_(3-x)Nb_(1-x)WxO_4（0≤x≤0.1）、Li_(2.9)Nb_(0.9)Mo_(0.1O4)、Li_(6+y)Zr_(2-x)0M_xO_7（M=Y、In、Zn、Ti）等系列固体电解质。空位型锂离子固体电解质Li_(2.9)Nb_(0.9)W_(0.1O4)在300℃时锂离子电导率为3.1×10~(-4)S cm~(-1)，比掺杂前的母体Li_3NbO_4的锂离子电导率（300℃，1.4×10~(-6)S cm~(-1)）提高了两个数量级。循环伏安扫描表明在0.05-5V时掺杂的W(VI)或者Mo(VI)不会被还原，可以稳定存在于扫描电压范围内。而在间隙型固体电解质Li_(6+x)Zr_(2-x)M_xO_7中，x=0.15Li很容易通过固相化学反应制备得到；室温下Li_(6+x)Zr_(1.5)Ti_(0.5)O_7结构中存在x≈0.17Li。Li_(6.15)Zr_(1.85)Y_(0.15)O_7的锂离子电导率比母体Li_6Zr_2O_7固体电解质提高了两个数量级，因此间隙位锂离子可以有效提高锂离子电导率。
Safety problem has become a major issue that inhibits the further development oflithium ion battery. Among all components in lithium ion battery, electrolyte should beresponsible for this unsafe behavior. Developing a safer electrolyte is more urgent thanimproving the power density and energy density in lithium ion battery. Firstly, two differentstructures of niobium disulfide were used as the host for lithium ion intercalation in theorganic liquid electrolyte and normal gel polymer electrolyte, respectively. The structure withbetter performance was chosen for sodium ion intercalation. Then we investigated the newsafe electrolytes of gel polymer electrolyte (GPE), anti thermal shrinkagable separatorcombined with ionic liquid to form GPE, and solid electrolyte for lithium ion battery.
2H NbS_2is a potential electrode material for Li~+intercalation but its performance ispoor. In order to improve its electrochemical performance,2H Li_(0.7)NbS_2(space group:P63/mmc) and3R NbS_2(s.g: R3m) were synthesized and characterized as electrode materialsfor a lithium ion battery. Both2H Li_(0.7)NbS_2and3R NbS_2showed reversiblecharge/discharge reactions based on the Nb(IV)/Nb(III) redox couple. The dischargecapacities were169.5mAh g~(-1) for2H LixNbS_2and169.0mAh g~(-1) for3R LixNbS_2at0.05Crate and room temperature. After200cycles at1C/1C rate,9%of capacity fade wasobserved for2H LixNbS_2and14%for3R LixNbS_2. It is proven that NbS_2is a goodLi~+intercalation host regardless of its space group, especially the2H structure exhibitsexcellent electrochemical characterization. Then, two structures of NbS_2were used aselectrodes in the poly(vinylidene fluoride hexafluoropropylene)(PVdF HFP) based gelpolymer electrolyte (GPE). The cyclic capacity of GPE was almost the same with organicliquid electrolyte in small charge/discharge current, but the rate performance was poor in GPE:the capacity is less half at10C rate compared with that of the liquid electrolyte.
The better performance of2H NbS_2structure was chose as an intercalated host for aNa ion battery. Based on the experience of2H Li_(0.7)NbS_2, the Na0.5NbS_2(space group:P6_3/mmc), was synthesized instead of2H NbS_2, by a conventional solid state reaction. The2H NaxNbS_2electrode shows a specific capacity of143.6mAh g~(-1) in organic liquidelectrolyte and141.2mAh g~(-1) in PVdF HFP based GPE, and the voltage profile occurs asignature of Na/vacancy ordering at x=0.5. First principles calculation was applied to revealpossible structures of NaxNbS_2and describe the corresponding electrochemical properties.Although layered NaMS_2systems allow full sodium intercalation, the stronger Na~+Na~+intralayer interaction compared to Li~+Li~+interaction induces layer gliding and Na ion ordering which can be reflected in the voltage profile.
Adding nano Al_2O_3in blending polymer PEO P(VdF HFP) and copolymerP(MMA VAc) co PEGDA to form polymer matrix, the gel polymer electrolytes (GPEs)were developed after coating the polymer matrix to mechanical support. The performances ofthe polymer membranes and the corresponding GPEs are characterized with mechanical test,thermogravimetric analyzer, scanning electron microscopy, cyclic voltammetry,electrochemical impedance spectroscopy, and charge/discharge test. With doping~(-1)0wt.%nano Al_2O_3, the ionic conductivity of both GPEs was3.8×10~(-3)S cm~(-1), but the mechanicalstrength was a little different,14.3MPa for blending polymer PEO P(VdF HFP); while16.2MPa for P(MMA VAc) co PEGDA. With the same structure of coin cell, Li/GPE/LiCoO_2,the capacity retention is87.2%for PEO P(VdF HFP) after50cycles; andP(MMA VAc) co PEGDA based GPE can keep90.9%of initial capacity after100cycles.
A new GPE system was developed by using anti thermal shrinkagablenanoparticles/polymer incorporating with lithium salt LiTFSI in ionic liquid PYR_(14)TFSI. Itseems that nanoparticle of SiO_2exibites better performance than nano Al_2O_3. Roomtemperature lithium ionic conductivity of SiO_2/P(MMA AN VAc)+LiTFSI+PYR_(14)TFSI/VC based GPE is1.2×103S cm1with an oxidative decomposition potential of5.3V (vs. Li/Li~+). The battery Li/GPE/LiFePO4shows high initial discharge capacity of143.4mAh g~(-1) at0.1C rate, and keeps99.6%capacity after50cycles.
Serial of solid electrolytes, Li3xNb1xWxO4(0≤x≤0.1), Li_(2.9)Nb_(0.9)Mo_(0.1O4)andLi6+yZr2xMxO7(M=Y, In, Zn, Ti) were synthesized by conventional solid state reaction. Thestructure and performance of newly developed solid electrolyte were characterized by powderX ray diffraction, scanning electron spectroscopy, energy dispersive X ray, electrochemicalimpedance spectroscopy, cyclic voltammetry and charge discharge test. The ionicconductivity of Li_(2.9)Nb_(0.9)W_(0.1O4)with vacancy structural solid electrolyte is3.1×10~(-4)S cm~(-1)at300℃, which is two orders of magnitude enhancement compared with the parent Li_3NbO_4(1.4×10~(-6)S cm~(-1)at300℃). Cyclic voltammetry measurement indicates that doping tungsten(VI) or molybdenum (VI) can be stable in the voltage scanning range of0.05V and4.5V.Insertion of x=0.15Li in the form of interstitial structure Li_(6+x)Zr_(2-x)M_xO_7can be obtained bysimple solid state synthesis. Electrochemical insertion into Li_(6+x)Zr_(1.5)Ti_(0.5)O_7of excess Li is atleast x≈0.17at room temperature. The ionic conductivity of Li_(6.15)Zr_(1.85)Y_(0.15)O_7is almost twoorders of magnitude higher than the parent Li_6Zr_2O_7, thus, interstitial site of lithium ion canimprove the ionic conductivity effectively.
2H结构的二硫化铌脱嵌锂离子的性能较差，为了提高2H-NbS_2电化学性能，采用固相法分别合成了2H-Li_(0.7)NbS_2（点阵群：P6_3/mmc）和3R-NbS_2（点阵群：R3m）并研究了其脱嵌锂行为，结果表明2H-Li_(0.7)NbS_2和3R-NbS_2可以有效利用Nb(IV)/Nb(III)电对进行可逆的充放电反应。在普通液态电解质中2H-LixNbS_2在0.05C倍率时室温放电容量为169.5mAh g~(-1)，而3R LixNbS_2为169.0mAh g~(-1)。1C/1C倍率电流循环200圈后，2H-LixNbS_2容量衰减为9%，3R-LixNbS_2衰减率为14%。因此，2H和3R结构的NbS_2都是很好的脱嵌锂材料，尤其是2H结构显示了优异的电化学性能。接着，探索了两种结构的电极在聚（偏氟乙烯六氟丙烯）（P(VdF HFP)）凝胶聚合物电解质中的电化学行为。虽然在PVdF HFP聚合物电解质中的小倍率充放电时具有与液态电解质相似的循环稳定性，但倍率性能较差，尤其在10C时容量还不能达到液态电解质的一半。
将性能较好的2H-NbS_2结构应用于钠离子电池。参照2H-Li_(0.7)NbS_2的经验，采用固相法合成了Na0.5NbS_2（点阵群：P63/mmc）。在钠离子电池中，2H-Na_xNbS_2电极使用液态有机溶剂电解质的室温放电容量为143.6mAh g~(-1)，而在凝胶态PVdF HFP基聚合物电解质的放电容量略低，为141.2mAh g~(-1)，在x=0.5处出现明显的Na/空位重排现象。采用量化计算分析了重排后NaxNbS_2可能的结构及相对应的电化学性能。虽然层状NaMS_2体系允许钠离子全部嵌入，层内Na~+-Na~+之间的排斥力明显强于Li~+Li~+，导致整个钠离子层的滑移及钠离子的重新排列，这个过程反映在电压曲线上。
分别使用添加纳米Al_2O_3的共混聚合物PEO-P(VdF-HFP)及共聚物P(MMA-VAc)-co-PEGDA作为聚合物的基体，使用支撑体支撑后，制备得到凝胶聚合物电解质（GPE）。采用机械拉伸、热重分析、扫描电镜、循环伏安、电化学交流阻抗和充放电测试等对制备得到的聚合物膜及对应GPE进行性能分析。添加纳米颗粒后，两种凝胶聚合物电解质的室温锂离子电导率均可以达到3.8×10~(-3)S cm~(-1)，共混物PEO-P(VdF-HFP)的机械强度为14.3MPa，而共聚物P(MMA-VAc)-co-PEGDA为16.2MPa。采用相同结构Li/GPE/LiCoO_2的扣式电池在相同测试条件下，共混物循环50圈后容量保持率为87.2%；而共聚物循环100圈后能够保持初始容量的90.9%。制备得到的新型凝胶聚合物电解质具有较好的循环及倍率性能。
研究了抗热收缩的纳米颗粒/聚合物隔膜，同时结合离子液体PYR_(14)TFSI及锂盐LiTFSI形成新型凝胶聚合物电解质。结果显示，添加SiO_2纳米颗粒的效果优于纳米Al_2O_3。SiO_2/P(MMA-AN-VAc)+LiTFSI+PYR_(14)TFSI/VC为基体的GPE在室温下锂离子电导率为1.2×10~(-3)S cm~(-1)，氧化分解电压为5.3V (vs. Li/Li~-)。装成结构为Li/GPE/LiFePO_4的扣式电池后，0.1C倍率放电初始容量为143.4mAh g~(-1)，循环50圈后的容量保持率为99.6%。
采用高温固相法合成了Li_(3-x)Nb_(1-x)WxO_4（0≤x≤0.1）、Li_(2.9)Nb_(0.9)Mo_(0.1O4)、Li_(6+y)Zr_(2-x)0M_xO_7（M=Y、In、Zn、Ti）等系列固体电解质。空位型锂离子固体电解质Li_(2.9)Nb_(0.9)W_(0.1O4)在300℃时锂离子电导率为3.1×10~(-4)S cm~(-1)，比掺杂前的母体Li_3NbO_4的锂离子电导率（300℃，1.4×10~(-6)S cm~(-1)）提高了两个数量级。循环伏安扫描表明在0.05-5V时掺杂的W(VI)或者Mo(VI)不会被还原，可以稳定存在于扫描电压范围内。而在间隙型固体电解质Li_(6+x)Zr_(2-x)M_xO_7中，x=0.15Li很容易通过固相化学反应制备得到；室温下Li_(6+x)Zr_(1.5)Ti_(0.5)O_7结构中存在x≈0.17Li。Li_(6.15)Zr_(1.85)Y_(0.15)O_7的锂离子电导率比母体Li_6Zr_2O_7固体电解质提高了两个数量级，因此间隙位锂离子可以有效提高锂离子电导率。
Safety problem has become a major issue that inhibits the further development oflithium ion battery. Among all components in lithium ion battery, electrolyte should beresponsible for this unsafe behavior. Developing a safer electrolyte is more urgent thanimproving the power density and energy density in lithium ion battery. Firstly, two differentstructures of niobium disulfide were used as the host for lithium ion intercalation in theorganic liquid electrolyte and normal gel polymer electrolyte, respectively. The structure withbetter performance was chosen for sodium ion intercalation. Then we investigated the newsafe electrolytes of gel polymer electrolyte (GPE), anti thermal shrinkagable separatorcombined with ionic liquid to form GPE, and solid electrolyte for lithium ion battery.
2H NbS_2is a potential electrode material for Li~+intercalation but its performance ispoor. In order to improve its electrochemical performance,2H Li_(0.7)NbS_2(space group:P63/mmc) and3R NbS_2(s.g: R3m) were synthesized and characterized as electrode materialsfor a lithium ion battery. Both2H Li_(0.7)NbS_2and3R NbS_2showed reversiblecharge/discharge reactions based on the Nb(IV)/Nb(III) redox couple. The dischargecapacities were169.5mAh g~(-1) for2H LixNbS_2and169.0mAh g~(-1) for3R LixNbS_2at0.05Crate and room temperature. After200cycles at1C/1C rate,9%of capacity fade wasobserved for2H LixNbS_2and14%for3R LixNbS_2. It is proven that NbS_2is a goodLi~+intercalation host regardless of its space group, especially the2H structure exhibitsexcellent electrochemical characterization. Then, two structures of NbS_2were used aselectrodes in the poly(vinylidene fluoride hexafluoropropylene)(PVdF HFP) based gelpolymer electrolyte (GPE). The cyclic capacity of GPE was almost the same with organicliquid electrolyte in small charge/discharge current, but the rate performance was poor in GPE:the capacity is less half at10C rate compared with that of the liquid electrolyte.
The better performance of2H NbS_2structure was chose as an intercalated host for aNa ion battery. Based on the experience of2H Li_(0.7)NbS_2, the Na0.5NbS_2(space group:P6_3/mmc), was synthesized instead of2H NbS_2, by a conventional solid state reaction. The2H NaxNbS_2electrode shows a specific capacity of143.6mAh g~(-1) in organic liquidelectrolyte and141.2mAh g~(-1) in PVdF HFP based GPE, and the voltage profile occurs asignature of Na/vacancy ordering at x=0.5. First principles calculation was applied to revealpossible structures of NaxNbS_2and describe the corresponding electrochemical properties.Although layered NaMS_2systems allow full sodium intercalation, the stronger Na~+Na~+intralayer interaction compared to Li~+Li~+interaction induces layer gliding and Na ion ordering which can be reflected in the voltage profile.
Adding nano Al_2O_3in blending polymer PEO P(VdF HFP) and copolymerP(MMA VAc) co PEGDA to form polymer matrix, the gel polymer electrolytes (GPEs)were developed after coating the polymer matrix to mechanical support. The performances ofthe polymer membranes and the corresponding GPEs are characterized with mechanical test,thermogravimetric analyzer, scanning electron microscopy, cyclic voltammetry,electrochemical impedance spectroscopy, and charge/discharge test. With doping~(-1)0wt.%nano Al_2O_3, the ionic conductivity of both GPEs was3.8×10~(-3)S cm~(-1), but the mechanicalstrength was a little different,14.3MPa for blending polymer PEO P(VdF HFP); while16.2MPa for P(MMA VAc) co PEGDA. With the same structure of coin cell, Li/GPE/LiCoO_2,the capacity retention is87.2%for PEO P(VdF HFP) after50cycles; andP(MMA VAc) co PEGDA based GPE can keep90.9%of initial capacity after100cycles.
A new GPE system was developed by using anti thermal shrinkagablenanoparticles/polymer incorporating with lithium salt LiTFSI in ionic liquid PYR_(14)TFSI. Itseems that nanoparticle of SiO_2exibites better performance than nano Al_2O_3. Roomtemperature lithium ionic conductivity of SiO_2/P(MMA AN VAc)+LiTFSI+PYR_(14)TFSI/VC based GPE is1.2×103S cm1with an oxidative decomposition potential of5.3V (vs. Li/Li~+). The battery Li/GPE/LiFePO4shows high initial discharge capacity of143.4mAh g~(-1) at0.1C rate, and keeps99.6%capacity after50cycles.
Serial of solid electrolytes, Li3xNb1xWxO4(0≤x≤0.1), Li_(2.9)Nb_(0.9)Mo_(0.1O4)andLi6+yZr2xMxO7(M=Y, In, Zn, Ti) were synthesized by conventional solid state reaction. Thestructure and performance of newly developed solid electrolyte were characterized by powderX ray diffraction, scanning electron spectroscopy, energy dispersive X ray, electrochemicalimpedance spectroscopy, cyclic voltammetry and charge discharge test. The ionicconductivity of Li_(2.9)Nb_(0.9)W_(0.1O4)with vacancy structural solid electrolyte is3.1×10~(-4)S cm~(-1)at300℃, which is two orders of magnitude enhancement compared with the parent Li_3NbO_4(1.4×10~(-6)S cm~(-1)at300℃). Cyclic voltammetry measurement indicates that doping tungsten(VI) or molybdenum (VI) can be stable in the voltage scanning range of0.05V and4.5V.Insertion of x=0.15Li in the form of interstitial structure Li_(6+x)Zr_(2-x)M_xO_7can be obtained bysimple solid state synthesis. Electrochemical insertion into Li_(6+x)Zr_(1.5)Ti_(0.5)O_7of excess Li is atleast x≈0.17at room temperature. The ionic conductivity of Li_(6.15)Zr_(1.85)Y_(0.15)O_7is almost twoorders of magnitude higher than the parent Li_6Zr_2O_7, thus, interstitial site of lithium ion canimprove the ionic conductivity effectively.
引文
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