鋰金屬電池中鋰枝晶的生成會致使電池之循環壽命減少並產生短路燃燒的危險性，因此，鋰金屬沉積與生長機制與是一迫切且具有表徵性的研究。其中，鋰金屬與電解液之間的反應形成的固態介面層(solid electrolyte interface, SEI)扮演了相當重要的角色。為此，本研究中開發了人工固態複合介面層以抑制鋰枝晶生長並提升電池效率。本研究中將分成四個部分，分別為(1)人工固態複合介面層之技術開發及無負極電池的表徵測試、(2)高空氣穩定度之新型態雙摻雜石榴石固態電解質開發、(3)溫度對-PVDF纖維在無負極電池的電化學表徵、(4) 人工固態複合介面層 -PVDF/5%LLZO/1%LiTFSI之研發與其電化學效能。於第一部分選用高電化學穩定性之石榴石固態材料Li7La2.75Ca0.25Zr1.75Nb0.25O12以及高機械強度與黏附性的β-PVDF並添加少量鋰鹽LiClO4提升鋰離子傳輸速率，透過電紡織的技術塗佈在電極上形成石榴石/高分子人工固態複合介面層Li7La2.75Ca0.25Zr1.75Nb0.25O12@LiClO4。此固態複合介面層不僅讓鋰金屬的沉積更為均勻減少沉積缺陷的產生，更能夠抑制枝晶的生長提升電池整體的循環壽命。此人工石榴石/高分子人工固態複合介面層塗佈在銅箔上與三元系NMC陰極材料組成Cu/NMC無負極電池，於30圈充放電後仍有58.66%的電容量以及高達97.6%的平均庫倫效率，與一般Cu/NMC的無負極電池在相同圈數的電容量35.6%提升23%電容量，改善電池長效循環壽命。由於一般的石榴石材料長時間暴露於空氣下會結晶生成Li2CO3和LiOH 等離子的不良導體並覆蓋於石榴石材料外層，致使整體導離度下降，第二部分中我們利用溶膠-凝膠法藉由摻雜Ga, Nb等元素於LLZO石榴石材料，得到了一具有高導離度且具良好的空氣穩定性的立方相Li5.6La2.9Ga0.26Zr1.87Nb0.05O12 ((Ga, Nb)-LLZO)。該材料雖經長時間暴露在大氣下，於拉曼光譜的分析中仍未於表面生成Li2CO3和LiOH。第三部分討論-PVDF 於無負極電池在不同溫度下(25 oC - 60 oC) 的電化學效能。-PVDF具備良好的楊氏係數49.46 MPa以及好的伸縮率，此可以有效的阻隔碳酸酯類的電解液與活性鋰的反應並抑制枝晶的成長，但由於-PVDF於室溫下的導離度並不具有好，於室溫下並沒辦無法讓鋰金屬能夠進行穩定的沉積，會造成效率降低。但若於高溫60 oC進行活化後，可進一步改善循環穩定性，於Cu/NMC的系統中進行30圈充放電後可維持50%以上的電容量與97.04%的平均庫倫效率。最後一部分我們將-PVDF加入5%高空氣穩定性之(Ga, Nb)-LLZO以及1%高導離度鋰鹽LiTFSI形成人工固態複合介面層-PVDF/5%LLZO/1%LiTFSI，同樣在無負極電池Cu/NMC的體系下進行電化學測試，以定電流0.2 mA/cm2經過30圈充放電後可以得到63.08%的電容量以及97.77%的平均庫效率。-PVDF 抑制鋰枝晶的成長並讓鋰金屬生長平整、(Ga, Nb)-LLZO提供額外鋰離子通道以提升薄膜導離度、LiTFSI與電解液反應並於銅箔表面形成LiF良好的SEI，進一步提升循環穩定性，其電容量保持率於第30圈可提升至64.99%，平均庫倫效率則是提升至98.33%。再來嘗試在-PVDF/5%LLZO/1%LiTFSI在60 oC進行5圈的充放電活化後，更可在30圈充放電後得到極好的平均庫倫效率99.85%。本研究藉由電紡織的技術塗佈製作人工固態複合介面膜有效的增進電池的穩定性與效率，期許本研究可以對無負極的研發有進一步的推進。

The formation of Li dendrite induces notorious safety issues and poor cycle life of lithium metal batteries. The complex interface between Li metal and electrolyte plays an important role to regulating Li deposition and enhance the cycle life of a battery. Design artificial protective composite films lead to homogenous Li plating and suppressed dendritic growth. This thesis consists (1) Li7La2.75Ca0.25Zr1.75Nb0.25O12@LiClO4 composite film derived solid electrolyte interphase for anode-free lithium metal battery. (2) a new dual doped air stabile cubic garnet electrolyte (3) temperature effect on -PVDF fiber and suppression of dendritic growth and (4) improving Li deposition by incorporation of (Ga, Nb)-LLZO, LiTFSI Salt to the -PVDF fiber.
In the first part Lithium ion-conducting composite film comprising of cubic garnet (Li7La2.75Ca0.25Zr1.75Nb0.25O12) (LLCZN), polyvinylidene fluoride (PVDF) and lithium perchlorate (LiClO4) salt have prepared via electrospinning techniques. The composite film induces inorganic rich (LiF and LiCl) solid electrolyte interphase during the galvanostatic charge/discharge process. In the (Cu@LLCZN/PVDF‖NMC) full cell configuration demonstrate improved capacity retention of 58.66% and an average coulombic efficiency of 97.6% after 30th cycles at a current density of 0.2 mA cm-2. In contrast, the bare Cu‖NMC cell capacity retention was 3.56% in 1M LiPF6 ethylene carbonate (EC) diethyl carbonate (DEC) (1:1 v/v ratio) electrolyte. The second portion was about the new air-stable dual doped (Ga, Nb)-LLZO cubic garnet with a composition of Li5.6La2.9Ga0.26Zr1.87Nb0.05O12 which was prepared via enhanced sol-gel method. Because of doping at the Li, and Zr sites and inherited synergy of Ga and Nb exhibits unique characteristics towards air stability.
In the third part, a conformal coating was achieved with the widely known PVDF polymer material on the copper (Cu) current collector via an electrospinning technique. A highly polar -PVDF fiber was obtained which exhibited good Li plating/stripping. In the temperature effect study on the -PVDF fiber conducted electrochemical cycling at different temperatures (25 oC - 60 oC) provides superior cyclability. The reaction of carbonated solvent electrolytes with the active lithium was blocked effectively. Therefore, -PVDF fiber imparting a stable SEI composition during plating/stripping at 60 oC, which retains more than 50% with an average coulombic efficiency (CE) of 97.04% at 30th cycle at a current density of 0.2 mA cm-2. The basic benefit of this -PVDF fiber is its flexibility with having about 49.46 MPa modulus. The insulating nature of the polymer leads to surface Li growth. Initiated smooth Lithium nucleation at 60 oC benefited to enhance battery cycle life in an ambient temperature. Once Li grow on the surface next Li follows the redeposited nucleation site. This scenario leads some smooth Li depositions therefore, 99.04% CE was obtained with a retention capacity of 50% at the 30th cycle by activation cycles at high temperature and operated the electrochemical charge/discharge cycle at an ambient temperature.
In the last section, the air-stable (Ga, Nb)-LLZO was incorporated as an active filler into the -PVDF fiber. The (Cu@5%LLZO -PVDF fiber‖NMC) full cell configuration demonstrates capacity retention and average Coulombic efficiency of 63.08%, 98.23% at 30th cycle and 58.84%, 98.32% at 35th cycle respectively used 1M LiPF6 EC/DEC (1:1 v/v ratio) electrolyte at a current density of 0.2 mA cm-2. Li‖Cu@-PVDF 5%LLZO composite fiber half-cell exhibits negligible polarization compared to Li‖Cu cell (bare Cu). This is due to obtained additional channels through the garnet nanoparticles embedded within the fiber. Therefore, facile uniform plating/stripping of lithium and stable cycling performance was recorded at 60 oC. LiTFSI salt-based fiber demonstrates improved capacity retention of 64.99% and average coulombic efficiency of 98.33% at a current density of 0.2 mA cm-2. After 5 activation cycle at elevated temperature (60 oC), the Cu@-PVDF 5%LLZO-1%LiTFSI fiber‖NMC full cell charge/discharge test operated at 25 oC retained more than 50% of its initial capacity at 30th cycle with 99.85% average Coulombic efficiency.

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