摘要
凝胶聚合物锂离子电池是在液体锂离子电池的基础上发展起来的新一代可充电锂离子电池,它不仅具有液态锂离子电池的高电压、高能量密度、长循环寿命等特点,而且改善了液态锂离子电池可能出现的漏液、爆炸等问题,电池的外形设计组装也灵活方便,广泛应用于电动汽车、移动通讯等领域,因此,对凝胶聚合物电解质膜的需求也日益增加,凝胶聚合物电解质膜的研究也得到了众多研究者的关注。尽管目前工业上凝胶聚合物电解质已经开始应用于锂离子电池,但仍存在一些尚需进一步解决的技术问题,主要有:(1)目前凝胶聚合物电解质的室温离子电导率可达10-3S/cm数量级,已经能基本满足应用的要求,但相比液态电解液的电导率(10-2S/cm),凝胶聚合物电解质的电导率仍然偏低,使得由其组装而成得锂离子电池的大电流充放电和低温性能都大大的降低;(2)纯凝胶聚合物电解质膜由于吸收了大量液体电解质而溶胀,使得膜机械强度较差。而提高聚合物电解质电导率的方法通常会降低其机械性能;(3)多孔凝胶聚合物电解质由于存在大量孔隙,容易导致漏液而降低电池的使用性能以及安全问题。
凝胶聚合物电解质要解决的核心问题是协调离子电导率和机械性能之间的关系。不同类型的凝胶聚合物电解质(纯凝胶和多孔凝胶)存在的问题也不同。本文针对纯凝胶聚合物电解质现存的问题展开了研究,设计了含氟型和杂化型两种聚合物电解质体系,对它们的结构和性能进行了较详细的研究;同时,针对多孔凝胶存在的问题,分别对孔壁和孔中心进行了修饰,设计了有机材料修饰孔壁、无机材料修饰孔壁、有机珠子修饰孔中心、无机珠子修饰孔中心等结构,较为详尽的研究了膜的结构、形貌和性能。另外,对离子在凝胶聚合物电解质的传输机理进行了初步的研究。具体如下:
1.含氟凝胶聚合物电解质
为了获得较高的离子电导率和较高的机械强度,用紫外光固化的方法,在交联的PEO网络中引入亲电解液2-丙烯酰胺-2-甲基丙磺酸锂(AMPS-Li)链段以及疏电解液的甲基丙烯酸2,2,2-三氟乙酯(TFEMA)链段。AMPS-Li的引入能够帮助聚合物膜吸收电解液,提高离子电导率;同时,由于TFEMA中的C-F键的键能高,TFEMA链段的引入能够提供良好的化学稳定性和热稳定性。
研究结果表明,当AMPS含量为35wt%,聚合物电解质膜的室温离子电导率为1.76×10-3S/cm,达到锂离子电池应用的要求;聚合物膜引入TFEMA,提高了凝胶聚合物电解质膜的强度和电化学稳定窗口,对吸液量和离子电导率没有明显降低。
2.氧化镧杂化凝胶型聚合物电解质
由于稀土元素的原子结构具有较多的4s、5d和6s空轨道,且这些轨道的能级差很小,稀土化合物(硬酸)易与锂盐中的阴离子(硬碱)通过静电吸引力形成稳定的络合物,减少离子载流体中阴离子数目,降低锂离子电池的极化程度。为进一步提高稀土化合物(氧化镧)的酸性,将氧化镧与磺酸根通过化学键连接起来,制备了“类超强酸”的结构;同时,为了解决氧化镧在聚合物基体中易聚集的问题,将其通过化学键“悬挂”到聚合物网络上。离子电导率和拉曼光谱分析表明,阴离子的含量随着氧化镧的增加而减少。对材料的微结构研究发现这种通过化学键“悬挂”到聚合物网络的氧化镧粒子易均匀的分散在聚合物膜中。
3. PVdF无纺布接枝PMMA凝胶聚合物电解质
聚偏氟乙烯(PVdF)的介电常数较高,有利于锂盐的解离,又具有机械性能好、电化学性能稳定等优点,但其也存在结晶度高、吸液量低、与锂金属的界面稳定性差等缺点;聚甲基丙烯酸甲酯(PMMA)由于MMA单元中有一羰基侧基,和碳酸酯类增塑剂中的氧原子有很强的相互作用,能够吸收大量的液体电解质溶液,并与电极有很好的相容性。静电纺丝能够制备具有微孔结构的多孔聚合物纤维无纺布材料,具有高的比表面积和孔隙率,较一般的多孔膜而言,更有利于离子的传输。综合所述的材料和结构上的优点,通过将PVdF无纺布进行预辐照,并将有机物MMA修饰到PVdF纤维的表面,形成两相多孔结构。这种特殊的结构既能赋予聚合物膜以高的离子电导率,并能维持尺寸稳定性。
4.氟硅橡胶多孔膜聚合物电解质
在目前所知的聚合物材料中,氟硅橡胶的回弹性是最好的,因而能够改善锂离子电池在充放电过程中产生的体积膨胀-缩小而带来的电池内阻的变化;同时具有优异的化学稳定性和热稳定性;另外氟硅橡胶分子链上含三氟甲基侧基,有利于锂盐的离解。因此氟硅橡胶是聚合物电解质膜的一种较为理想的候选。但是氟硅橡胶与电解液的亲合能力弱,不利于电解液的吸收和保持。为了获得满意的电化学性能,将其为基料,制备了多孔膜,并运用沉淀法在孔壁上修饰了亲电解液的无机颗粒层。研究了制膜工艺对膜形貌的影响、锂盐的种类对电池性能的影响等。
5.“孔/珠”复合电解质膜
多孔膜中由于大量孔的存在,使得在装配电池过程中,聚合物膜容易被电极材料刺穿而短路,并且在充放电过程中,多孔膜不能有效的抑制锂枝晶的生长,降低了电池的安全性和能量密度。在本章中运用简单的倒相法在孔中间引入可凝胶珠子,减小膜的孔径,增大孔的曲率,提高膜的刺穿强度。由于珠子可以被凝胶化,所以这种特殊的“孔/珠”结构既提高了电池的安全性,又不降低离子电导率。为制备高性能凝胶聚合物电解质膜提供了有效的方法。
Lithium ion battery based on gel-type polymer electrolyte (GPE) is the new generation of rechargeable system developed from liquid lithium ion battery. It possesses high energy density, long cycle life, negligible leakage, light weight and flexible shape. The polymer electrolyte lithium battery is attractive power source applied in electric vehicle, cellular phones and others. The main technical problems of polymer electrolytes include: first, although the ionic conductivity can reach the magnitude of 10-3S/cm, which can satisfy the practical request, it is still lower than that of liquid electrolyte (10-2S/cm). The low ionic conductivity will limit the discharge rate and low-temperature performance of the battery system. Second, swelling of the pure gel-type polymer membranes due to absorbing a lot of liquid electrolytes leads to the poor mechanical property of GPE. In general, the methods of enhancing the ionic conductivity are unfavorable for the mechanical strength. Third, porous GPE often faces potential safety issues arising from liquid leakage. The core problem of GPE is how to coordinate ionic conductivity and mechanical properties. The existing problems of different types of GPEs (non-porous or porous gels) are also different. In order to solve these problems, we have designed and prepared fluorine-containing polymer electrolytes and hybrid polymer electrolytes. In addition, A modification of the pore wall and pore center in multi-pore membranes have been also conducted. The more details about membrane structure, morphology and performance have been studied, and the ion transfer mechanism in GPE has also been investigated. They are summarized as follows:
1. Fluorine containing gel polymer electrolytes
Novel gel network polymer electrolytes containing fluorine and sulfonic acid lithium are prepared by the UV polymerization of poly(ethylene glycol) dimethylacrylate (PEGDMA)/ 2-acrylamido-2-methyl propanesulfonic acid (AMPS)/trifluoroethyl methacrylate (TFEM). They are activated by uptaking the solutions of 1.0 M LiPF6/EC/DMC to prepare gel network polymer electrolytes. The characteristics of the polymer networks including gel fractions, thermal stability, liquid electrolyte uptake and electrochemical properties have been studied. When the weight ratio of PEGDMA/AMPS/TFEM is 60/35/5, the network polymer electrolytes show the highest liquid electrolyte uptake (144%) and ionic conductivity (about the order of 10?3 S/cm) at room temperature (25℃). The network polymer electrolytes are electrochemically stable up to 5.0 V versus Li+/Li. The performances of the network polymer electrolytes suggest that they are suitable for application in high performance lithium ion batteries.
2. Lanthanum oxide hybrid gel polymer electrolytes
As the atomic structure of rare earth elements with more of the 4s, 5d and 6s unoccupied orbit, and these can track the differential small, rare earth compounds (hard acid) in the lithium salt-and the anion (hard base) to form a stable complex through electrostatic attraction, to reduce mobile anion numbers in the electrolyte and suppress the polarization degree. To further enhance the acidity of rare earth compounds (lanthanum oxide), acid and lanthanum oxide root through the bond linking of the“super acid like”.In order to prevent lanthanum oxide from aggregation in the polymer matrix, its bond“hanging”to the polymer network is set up. The measurements of ionic conductivity and Raman spectrum indicate that the content of anions decreases with the increase of lanthanum oxide. By examining the microstructure of the materials it is found that lanthanum oxide particles chemically bonded by“hanging”to the polymer network are uniformly dispersed in the polymer membrane.
3. PMMA grafted PVdF non-woven fabric gel polymer electrolytes
To achieve high ionic conductivity in polymer electrolyte, dual phase poly(vinylidenefluoride) (PVdF) based fibrous polymer electrolytes membrane is prepared via pre-irradiation. The PVdF fiber serves as supporting phase providing dimensional stability. Poly(methyl methacrylate) (PMMA) as gel phase help for trapping liquid electrolyte and substitute non-conductive PVdF phase to contact with electrodes thus increasing conductive area. PVdF based fibrous membrane can be used as polymer electrolyte in lithium ion battery after it is activated by uptaking 1 M LiPF6/EC-DMC electrolyte solution. Its room-temperature ionic conductivity is enhanced greatly by introduction of PMMA phase, from 2.3×10-3 S/cm (pristine PVdF fibrous membrane) to 7.9×10-3 S/cm (DOG=111.8%). The coin cells containing the dual phase fibrous membrane demonstrate excellent rate performance. The combination PMMA phase to PVdF phase is a novel approach to achieve high ionic conductivity in polymer electrolytes.
4. Fluorosilicone rubber porous GPE
In the current knowledge of polymer materials, the elasticity of fluorosilicone rubber is the best. Thus, the electrolyte membrane based on fluorine silicone rubber is favorable for lighting the battery resistance fluctuation caused by volume expansion and contraction in the charge and discharge process. Moreover, the fluorosilicone rubber has excellent chemical stability and thermal stability. On the other hand, trifluoromethyl-side-groups on the fluorosilicone rubber molecular chains are favorable for lithium salt dissociation. Therefore, fluorosilicone rubber polymer is an ideal candidate for electrolyte membrane. But fluorosilicone rubber electrolyte and the weak capacity of affinity, not conducive to the absorption of electrolyte and maintain. In order to obtain the satisfaction of electrochemical properties of the base material of its prepared porous membrane, and use hole in the wall precipitated a loose pro-modified inorganic particles electrolyte layer. Study of the membrane morphology of the film, the type of lithium battery performance, and so on.
5.“Pore/bead”gel polymer electrolytes
A special“pore/bead”composite membrane is prepared by facile approach. The combination of bead into pore is a novel approach to achieve polymer electrolyte with excellent comprehensive properties. The bead (MCM-41) in the composite membrane is considered as the key factor to improve puncture strength and suppress thermal shrinkage, which would greatly improve the safety of lithium ion battery. The composite membrane displays highly ionic conductivity which is attributed to the porous structure both in the binder and the bead. The battery based on the composite electrolyte show satisfactory C-rate performance. Primary results showed that it is promising as polymer electrolyte for scale-up lithium ion battery. In addition, this facile approach also provides a new avenue for further improve polymer electrolyte performances.
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