PAMPSLi基电纺纤维聚合物电解质的制备与性能研究
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摘要
聚合物电解质是决定聚合物锂离子电池性能的关键材料，不仅要求其具有良好的电化学性能，还要有良好的热稳定性和尺寸稳定性。本论文针对单离子传输聚合物电解质电导率低，纤维基聚合物电解质尺寸稳定性差以及PVDF基聚合物电解质电解液泄漏等问题，以2-丙烯酰胺-2-甲基丙磺酸(AMPS)为主要单体，利用磺酸基团的离子交换反应和碳碳双键的聚合反应，采用共混、共聚和与有机-无机杂化颗粒复合等方法开展聚合物电解质的制备、改性和结构与性能的相关性研究，以实现聚合物电解质物理和电化学性能的优化。
通过将非挥发性增塑剂聚醚接枝聚硅氧烷(PSi-PE)引入到PAMPSLi基全固态单离子传输聚合物电解质体系中，缩短了体系聚合物链段运动松弛时间，进而提高了锂离子的迁移能力。电导率测试结果表明，随着PSi-PE添加量的增加电导率先增大后减小，当PSi-PE的添加量为35%时，室温离子电导率达到最大(6.9×10~(-8)S/cm)，比未添加PSi-PE的体系增加了大约20倍。
为进一步提高单离子聚合物电解质的离子电导率，制备了以有机溶剂(EC/DMC，质量比为1:1)为增塑剂的PAMPSLi纤维基单离子传输聚合物电解质。利用混合增塑剂提高锂离子的解离和迁移能力，同时借助电纺膜的超大比表面积特性增加聚合物锂盐和增塑剂的作用面积，进而提高单离子导体的离子电导率。用于电纺的PAMPSLi采用先聚合后离子交换的方法合成，热重分析表明，PAMPSLi在304℃之前不分解。通过改变纺丝液混合溶剂组成制得不同比表面积的PAMPSLi基电纺纤维膜。红外光谱测试表明，该纤维膜在增塑剂中能够发生有效解离。室温离子电导率可达2.12×10~(-5)S/cm。此外，此类聚合物电解质具有优良的尺寸稳定性和电化学稳定性。
针对聚甲基丙烯酸甲酯(PMMA)对碳酸酯类电解液亲和性好，当电解液含量较高时无法得到形态稳定的聚合物电解质薄膜这一问题，采用AMPS和MMA共聚的方法制备了P(MMA-co-AMPSLi)纤维基聚合物电解质。通过引入耐溶剂性较好的AMPSLi单元来调整聚合物对溶剂的亲和性。实验结果表明：随着AMPSLi单元含量的增加，P(MMA-co-AMPSLi)的可纺性和耐溶剂性增强，共聚物纤维膜在电解液中的溶胀程度也随之减小，孔结构保持能力得到改善，电纺膜的吸液率增大。同时P(MMA-co-AMPSLi)电纺膜的介电常数也随着AMPSLi单元含量的增加而增大。单体投料比为MMA:AMPS=2:8的P(MMA-co-AMPSLi)纤维基聚合物电解质室温电导率达到4.12×10~(-3)S/cm，电化学窗口达到5.0V。P(MMA-co-AMPSLi)的合成成功克服了PMMA凝胶聚合物电解质对制备条件的苛刻要求，同时有效提高了聚合物电解质的性能。
针对聚偏氟乙烯(PVDF)基纤维聚合物电解质存在的形状稳定性差问题，采用PAMPSLi和PVDF共混纺丝制备了一组新型复合纤维聚合物电解质。复合纤维体系无相分离结构出现，PAMPSLi和PVDF之间的相互作用提高了体系的相容性并且抑制了PVDF分子链的定向排列，降低了纤维的结晶度，同时聚合物电解质体系的尺寸稳定性也得到了显著提高。复合纤维膜的平均纤维直径远小于纯PVDF膜。当共混比例为PVDF:PAMPSLi=5:1时，所得纤维膜直径较细，平均直径可达145nm，并且吸液率、离子电导率、尺寸稳定性和电化学稳定性等性能较好。采用PAMPSLi与PVDF共混纺丝是提高PVDF纤维聚合物电解质性能的有效方法。
针对PVDF的高结晶度限制了离子电导率的提高并且容易引起电解液漏泄的问题，采用原子转移自由基聚合法合成了有机-无机杂化纳米颗粒PMMA-g-TiO_2，将其与PVDF混合纺丝制得了PVDF/PMMA-g-TiO_2复合纤维聚合物电解质。PMMA-g-TiO_2中接枝聚合物分子量相对较低且分布均匀，有利于电解液的快速渗透。杂化纳米颗粒的引入降低了PVDF的结晶度，同时由于PMMA具有较强的电解液亲和性，复合电纺膜对电解液的吸收率明显增大。PVDF/PMMA-g-TiO_2复合纤维聚合物电解质的电解液保持能力显著增强，室温离子电导率达到2.95×10~(-3)S/cm，电化学窗口为5.3V。
Polymer electrolytes as key materials for lithium ionic batteries are required topossess not only a good electrochemical performance, but also excellent thermalstability and dimensional stability. Aiming at the problems, such as the low ionicconductivity of single-ion conducting polymer electrolytes, the poor dimensionalstability of fiber-based polymer electrolytes and the leakage of electrolyte solutionfor PVDF-based gel polymer electrolytes,2-acrylamido-2-methylpropane-sulfonicacid (AMPS) was chosen as a main monomer for the modification of polymerelectrolytes utilizing ion-exchange processes and polymerization reaction. Themethods like blending, copolymerization and complex with organic-inorganichybrid particles were adopted to optimize the physical and electrochemicalproperties of polymer electrolytes. The preparation, modification, and therelationships between structures and properties were investigated.
The nonvolatile and chemically inert plasticizer poly(siloxane-g-ethyleneoxide)(PSi-PE) was introduced into a PAMPSLi-based all-solid-state single-ionconducting polymer electrolyte. The addition of PSi-PE shortened the relaxationtime of the polymer chain segments and improved the mobility of the segments,which was beneficial to the migration of lithium ions. The test results of theconductivity showed that the conductivity first increased and then decreased withthe increase of PSi-PE. When35mass%PSi-PE was added, the ionic conductivity atroom temperature got the maximum value (6.9×10~(-8)S/cm), which was about20times larger than that of the membrane without PSi-PE.
To further enhance the ionic conductivity, the method adopting an organicsolvent(EC/DMC,1:1, mass ratio) as a plasticizer to promote both the ionicdissociation of the polymeric lithium salt and the ionic migration was considered.Meanwhile, the large specific surface area of the electrospinning membrane wasused to improve the contact area between the polymeric lithium salt and theplasticizer, further to enhance the ionic conductivity of the single-ion conductor.PAMPSLi used for the electrospinning procedure was synthesized by free-radicalpolymerization of2-acrylamido-2-methyl propanesulfonic acid, followed byion-exchange of H~+with Li~+. TG analysis showed that its decomposition did notoccur until304℃. PAMPSLi electrospun membranes with different specific surfaceareas were fabricated by varying the solvent composition of polymer solutions.FTIR tests showed PAMPSLi dissociated effectively in the plasticizer. Theroom-temperature ionic conductivity was up to2.12×10-5S/cm. In addition, this kind of polymer electrolytes had excellent dimensional stability and electrochemicalstability.
To solve the problem that it was difficult to obtain PMMA-based polymerelectroytes with good dimensional stability under high content of electrolyte,P(MMA-co-AMPSLi) fiber-based polymer electrolytes were prepared through thecopolymerization of AMPS and MMA. The introduction of AMPSLi units whichhave better solvent resistance can adjust the solvent affinity ofP(MMA-co-AMPSLi). The test results manifested that the spinnability ofP(MMA-co-AMPSLi) was improved with the increase of the content of AMPSLiunits. Meanwhile, the solvent resistance of P(MMA-co-AMPSLi) was improved,and the degree of swelling of the fibers in the electrolyte solution decreased. Theholding ability of pore structure and the uptake of electrolyte solution wereenhanced. The dielectric constants of P(MMA-co-AMPSLi) electrospun membranesalso increased with the increase of the AMPSLi unit content. When the feed ratio ofMMA:AMPS was2:8, the ionic conductivity of the resultant fibrous polymerelectrolyte at room temperature was4.12×10~(-3)S/cm, and the electrochemicalwindow was up to5.0V. The synthesis of P(MMA-co-AMPSLi) successfullyovercame the requirements of the preparation conditions for PMMA gel polymerelectrolyte, and improved effectively the performance of the polymer electrolyte.
To overcome the disadvantage of poor dimensional stability of PVDF-basedelectrospun fibrous polymer electrolytes and facilitate the assemblage of batteries, anew type of bicomponent fibrous membranes based on PVDF/PAMPSLi blendsystems with different blend ratios were fabricated via electrospinning method. Theinteraction between PAMPSLi and PVDF improved the miscibility of two polymers,suppressed the orientation of the PVDF molecular chain, and reduced thecrystallinity of PVDF. Meanwhile, the introduction of PAMPSLi improved thedimensional stability of the polymer electrolytes. The average diameters of thebicomponent fibrous membranes were far lesser than those of the pure PVDFfibrous membranes. The average fibrous diameter of the composite fibrousmembrane with the blend ratio of5:1(PVDF:PAMPSLi) was145nm, and theproperties of the corresponding polymer electrolyte, such as the uptake ofelectrolyte, ionic conductivity, dimensional stability, and electrochemical stability,reached optimal value. Incorporation of PAMPSLi has been verified to be aneffective method in improving the properties of PVDF based fibrous polymerelectrolytes.
The high crystallinity of PVDF limits the increase of ionic conductivity, andoften causes the problem of the electrolyte leakage. To solve these problems, organic-inorganic hybrid nanoparticles PMMA-g-TiO_2was synthesized throughatom transfer radical polymerization. The PVDF/PMMA-g-TiO_2composite fiberpolymer electrolytes were fabricated using electrospinning technology. Themolecular weight of the grafted polymer distributed uniformly and the averagemolecular weight was relatively low, which was beneficial to the penetration of theelectrolyte solution. The introduction of PMMA-g-TiO_2reduced the crystallinity ofPVDF, and improved the electrolyte uptake due to the excellent affinity of PMMAtoward the liquid electrolyte. The capability of electrolyte retention of fibrouspolymer electrolytes was enhanced by the incorporation of PMMA-g-TiO_2. Theionic conductivity at room temperature was up to2.95×10~(-3)S/cm, and theelectrochemical window reached5.3V.
通过将非挥发性增塑剂聚醚接枝聚硅氧烷(PSi-PE)引入到PAMPSLi基全固态单离子传输聚合物电解质体系中，缩短了体系聚合物链段运动松弛时间，进而提高了锂离子的迁移能力。电导率测试结果表明，随着PSi-PE添加量的增加电导率先增大后减小，当PSi-PE的添加量为35%时，室温离子电导率达到最大(6.9×10~(-8)S/cm)，比未添加PSi-PE的体系增加了大约20倍。
为进一步提高单离子聚合物电解质的离子电导率，制备了以有机溶剂(EC/DMC，质量比为1:1)为增塑剂的PAMPSLi纤维基单离子传输聚合物电解质。利用混合增塑剂提高锂离子的解离和迁移能力，同时借助电纺膜的超大比表面积特性增加聚合物锂盐和增塑剂的作用面积，进而提高单离子导体的离子电导率。用于电纺的PAMPSLi采用先聚合后离子交换的方法合成，热重分析表明，PAMPSLi在304℃之前不分解。通过改变纺丝液混合溶剂组成制得不同比表面积的PAMPSLi基电纺纤维膜。红外光谱测试表明，该纤维膜在增塑剂中能够发生有效解离。室温离子电导率可达2.12×10~(-5)S/cm。此外，此类聚合物电解质具有优良的尺寸稳定性和电化学稳定性。
针对聚甲基丙烯酸甲酯(PMMA)对碳酸酯类电解液亲和性好，当电解液含量较高时无法得到形态稳定的聚合物电解质薄膜这一问题，采用AMPS和MMA共聚的方法制备了P(MMA-co-AMPSLi)纤维基聚合物电解质。通过引入耐溶剂性较好的AMPSLi单元来调整聚合物对溶剂的亲和性。实验结果表明：随着AMPSLi单元含量的增加，P(MMA-co-AMPSLi)的可纺性和耐溶剂性增强，共聚物纤维膜在电解液中的溶胀程度也随之减小，孔结构保持能力得到改善，电纺膜的吸液率增大。同时P(MMA-co-AMPSLi)电纺膜的介电常数也随着AMPSLi单元含量的增加而增大。单体投料比为MMA:AMPS=2:8的P(MMA-co-AMPSLi)纤维基聚合物电解质室温电导率达到4.12×10~(-3)S/cm，电化学窗口达到5.0V。P(MMA-co-AMPSLi)的合成成功克服了PMMA凝胶聚合物电解质对制备条件的苛刻要求，同时有效提高了聚合物电解质的性能。
针对聚偏氟乙烯(PVDF)基纤维聚合物电解质存在的形状稳定性差问题，采用PAMPSLi和PVDF共混纺丝制备了一组新型复合纤维聚合物电解质。复合纤维体系无相分离结构出现，PAMPSLi和PVDF之间的相互作用提高了体系的相容性并且抑制了PVDF分子链的定向排列，降低了纤维的结晶度，同时聚合物电解质体系的尺寸稳定性也得到了显著提高。复合纤维膜的平均纤维直径远小于纯PVDF膜。当共混比例为PVDF:PAMPSLi=5:1时，所得纤维膜直径较细，平均直径可达145nm，并且吸液率、离子电导率、尺寸稳定性和电化学稳定性等性能较好。采用PAMPSLi与PVDF共混纺丝是提高PVDF纤维聚合物电解质性能的有效方法。
针对PVDF的高结晶度限制了离子电导率的提高并且容易引起电解液漏泄的问题，采用原子转移自由基聚合法合成了有机-无机杂化纳米颗粒PMMA-g-TiO_2，将其与PVDF混合纺丝制得了PVDF/PMMA-g-TiO_2复合纤维聚合物电解质。PMMA-g-TiO_2中接枝聚合物分子量相对较低且分布均匀，有利于电解液的快速渗透。杂化纳米颗粒的引入降低了PVDF的结晶度，同时由于PMMA具有较强的电解液亲和性，复合电纺膜对电解液的吸收率明显增大。PVDF/PMMA-g-TiO_2复合纤维聚合物电解质的电解液保持能力显著增强，室温离子电导率达到2.95×10~(-3)S/cm，电化学窗口为5.3V。
Polymer electrolytes as key materials for lithium ionic batteries are required topossess not only a good electrochemical performance, but also excellent thermalstability and dimensional stability. Aiming at the problems, such as the low ionicconductivity of single-ion conducting polymer electrolytes, the poor dimensionalstability of fiber-based polymer electrolytes and the leakage of electrolyte solutionfor PVDF-based gel polymer electrolytes,2-acrylamido-2-methylpropane-sulfonicacid (AMPS) was chosen as a main monomer for the modification of polymerelectrolytes utilizing ion-exchange processes and polymerization reaction. Themethods like blending, copolymerization and complex with organic-inorganichybrid particles were adopted to optimize the physical and electrochemicalproperties of polymer electrolytes. The preparation, modification, and therelationships between structures and properties were investigated.
The nonvolatile and chemically inert plasticizer poly(siloxane-g-ethyleneoxide)(PSi-PE) was introduced into a PAMPSLi-based all-solid-state single-ionconducting polymer electrolyte. The addition of PSi-PE shortened the relaxationtime of the polymer chain segments and improved the mobility of the segments,which was beneficial to the migration of lithium ions. The test results of theconductivity showed that the conductivity first increased and then decreased withthe increase of PSi-PE. When35mass%PSi-PE was added, the ionic conductivity atroom temperature got the maximum value (6.9×10~(-8)S/cm), which was about20times larger than that of the membrane without PSi-PE.
To further enhance the ionic conductivity, the method adopting an organicsolvent(EC/DMC,1:1, mass ratio) as a plasticizer to promote both the ionicdissociation of the polymeric lithium salt and the ionic migration was considered.Meanwhile, the large specific surface area of the electrospinning membrane wasused to improve the contact area between the polymeric lithium salt and theplasticizer, further to enhance the ionic conductivity of the single-ion conductor.PAMPSLi used for the electrospinning procedure was synthesized by free-radicalpolymerization of2-acrylamido-2-methyl propanesulfonic acid, followed byion-exchange of H~+with Li~+. TG analysis showed that its decomposition did notoccur until304℃. PAMPSLi electrospun membranes with different specific surfaceareas were fabricated by varying the solvent composition of polymer solutions.FTIR tests showed PAMPSLi dissociated effectively in the plasticizer. Theroom-temperature ionic conductivity was up to2.12×10-5S/cm. In addition, this kind of polymer electrolytes had excellent dimensional stability and electrochemicalstability.
To solve the problem that it was difficult to obtain PMMA-based polymerelectroytes with good dimensional stability under high content of electrolyte,P(MMA-co-AMPSLi) fiber-based polymer electrolytes were prepared through thecopolymerization of AMPS and MMA. The introduction of AMPSLi units whichhave better solvent resistance can adjust the solvent affinity ofP(MMA-co-AMPSLi). The test results manifested that the spinnability ofP(MMA-co-AMPSLi) was improved with the increase of the content of AMPSLiunits. Meanwhile, the solvent resistance of P(MMA-co-AMPSLi) was improved,and the degree of swelling of the fibers in the electrolyte solution decreased. Theholding ability of pore structure and the uptake of electrolyte solution wereenhanced. The dielectric constants of P(MMA-co-AMPSLi) electrospun membranesalso increased with the increase of the AMPSLi unit content. When the feed ratio ofMMA:AMPS was2:8, the ionic conductivity of the resultant fibrous polymerelectrolyte at room temperature was4.12×10~(-3)S/cm, and the electrochemicalwindow was up to5.0V. The synthesis of P(MMA-co-AMPSLi) successfullyovercame the requirements of the preparation conditions for PMMA gel polymerelectrolyte, and improved effectively the performance of the polymer electrolyte.
To overcome the disadvantage of poor dimensional stability of PVDF-basedelectrospun fibrous polymer electrolytes and facilitate the assemblage of batteries, anew type of bicomponent fibrous membranes based on PVDF/PAMPSLi blendsystems with different blend ratios were fabricated via electrospinning method. Theinteraction between PAMPSLi and PVDF improved the miscibility of two polymers,suppressed the orientation of the PVDF molecular chain, and reduced thecrystallinity of PVDF. Meanwhile, the introduction of PAMPSLi improved thedimensional stability of the polymer electrolytes. The average diameters of thebicomponent fibrous membranes were far lesser than those of the pure PVDFfibrous membranes. The average fibrous diameter of the composite fibrousmembrane with the blend ratio of5:1(PVDF:PAMPSLi) was145nm, and theproperties of the corresponding polymer electrolyte, such as the uptake ofelectrolyte, ionic conductivity, dimensional stability, and electrochemical stability,reached optimal value. Incorporation of PAMPSLi has been verified to be aneffective method in improving the properties of PVDF based fibrous polymerelectrolytes.
The high crystallinity of PVDF limits the increase of ionic conductivity, andoften causes the problem of the electrolyte leakage. To solve these problems, organic-inorganic hybrid nanoparticles PMMA-g-TiO_2was synthesized throughatom transfer radical polymerization. The PVDF/PMMA-g-TiO_2composite fiberpolymer electrolytes were fabricated using electrospinning technology. Themolecular weight of the grafted polymer distributed uniformly and the averagemolecular weight was relatively low, which was beneficial to the penetration of theelectrolyte solution. The introduction of PMMA-g-TiO_2reduced the crystallinity ofPVDF, and improved the electrolyte uptake due to the excellent affinity of PMMAtoward the liquid electrolyte. The capability of electrolyte retention of fibrouspolymer electrolytes was enhanced by the incorporation of PMMA-g-TiO_2. Theionic conductivity at room temperature was up to2.95×10~(-3)S/cm, and theelectrochemical window reached5.3V.
引文
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