Li7La3Zr2O12與多壁奈米碳管填料於聚偏氟乙烯-六氟丙烯共聚物/聚碳酸亞丙酯之複合型固態電解質應用研究

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許志維(Zu-Wei Hsu) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

Li7La3Zr2O12與多壁奈米碳管填料於聚偏氟乙烯-六氟丙烯共聚物/聚碳酸亞丙酯之複合型固態電解質應用研究
(Applications of Li7La3Zr2O12 and Multi-walled Carbon Nanotubes Fillers in Poly (vinylidene fluoride)-hexafluoropropene/ Poly (propylene carbonate) Composite Electrolyte Solid-State Lithium Batteries)

★ 固相反應法製備固態電解質Li7La3Zr2O12應用於鋰離子電池

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至系統瀏覽論文 (2027-9-1以後開放)

摘要(中)

本研究內容中主要以聚偏氟乙烯-六氟丙烯共聚物(Poly (vinylidene fluoride)-hexafluoropropylene，PVDF-HFP)為高分子主體，並利用聚碳酸亞丙酯(Poly (propylene carbonate)，PPC)進行混摻，雙層式高分子層間再配合添加微量的離子液體，並加入參雜不同金屬之Li7La3Zr2O12 (LLZO)以及多壁奈米碳管(MWCNTs)形成複合型類固態電解質，探討高分子中加入奈米填料對於材料以及電化學性質的影響。本研究中製備的複合型固態電解質，除了能有效抑制系統結晶程度，進而提供鋰離子有更多之運動空間，也能結合PVDF-HFP與PPC高分子的優點來提升其電化學表現。由實驗結果得知高分子主體PVDF-HFP摻入適量的PPC交聯後，並搭配應用在NMC-811正極系統時，於室溫25 °C下有優異的電化學表現：低速比放電容量(191.40 mAh/g @ 25 mA/g)、高速比放電容量(100.56 mAh/g @ 300 mA/g)、高離子導通率(5.74×10-4 S/cm)；接續下來之研究實驗得到高分子固態電解質中添加不同含量之多壁奈米碳管(MWCNTs)，對於整體固態電解質電性表現上確實也有明顯提升，由結果可得知當1 wt.% MWCNTs添加有最佳電性表現：低速比電容量(198.18 mAh/g @ 25 mA/g)高速比電容量(110.90 mAh/g @ 300 mA/g)、高離子導通率(7.39×10-4 S/cm)。另一部分之研究實驗得到高分子固態電解質中添加不同參雜條件之LLZO粉末，對於整體固態電解質電性表現上確實有明顯提升，藉由此複合性固態電解質討論於一次燒結條件下(900 ℃，10小時)之不同過量添加碳酸鋰添加量之LLZO參雜Ga(LLZGO)的差異，可發現當10 wt.% 過量鋰添加有最佳電性表現：低速比電容量(209.62 mAh/g @ 25 mA/g)、高速比電容量(119.81 mAh/g @ 300 mA/g)、高離子導通率(7.02×10-4 S/cm)；最後一部分之研究實驗一樣藉由此複合性固態電解質中加入LLZO共參雜0.25Ga與不同參雜量的Ce，可發現LLZO共參雜0.25Ga與不同參雜量的Ce當有最佳電性表現：低速比電容量 (208.10 mAh/g @ 25 mA/g)、高速比電容量(144.15 mAh/g @ 300 mA/g)、高離子導通率(1.38×10-3 S/cm)。本研究中不同填充物添加之固態電解質於電性上有明顯提升，進階證實了PVDF-HFP混摻PPC之改質並添加適量LLZO以及MWCNTs有助於固態電解質於未來之應用。

摘要(英)

In this research, PVDF-HFP was used as the main polymer, and PPC was mixed to tune the properties of the solid electrolyte. MWCNT, Li6.25La3Zr2Ga0.25O12 (LLZGO) or Li6.25La3Zr1.7Ga0.25Ce0.2O12 (LLZGCO) were added as the inorganic filler to form a composite solid-state electrolyte. We want to study effects of nanofillers on electrochemical properties.The composite solid electrolyte prepared in this study can not only effectively suppress the crystallinity of the system, thereby providing more movement space for lithium ions, but also take advantage of the two polymers to improve the chemical potential window and the lithium ion conductivity.
In the first part of experiment, it was found that adding different contents of multi-walled carbon nanotubes (MWCNTs) into the polymer solid electrolyte significantly improve the electrical performance of the overall solid electrolyte. It can be seen from the results that the best electrochemical performance is obtained when 1wt.% MWCNT is added:specific capacity of 198.18 mAh/g @ 25mA/g, and ionic conductivity of 7.39×10-4 S/cm. The experimental results are better than pure PVDF-HFP/PPC solid polymer electrolyte.
In the second part of experiment, LLZGO powder were added as the inorganic filler. It was found that LLZGO powder with the different doping condition has improved the electrical performance of the overall solid electrolyte. It can be found that when 10wt.% excess lithium was added, ,the cell shows the best electrochemical performance : specific capacity of 209.62 mAh/g @ 25mA/g & 119.81 mAh/g @ 300 mA/g ,and ionic conductivity of 7.02×10-4 S/cm. The experimental results are better than pure PVDF-HFP/PPC solid polymer electrolyte.
In the final part of the research, LLZGCO powder were added as the inorganic filler. It was found that LLZO powder with the different doping condition has improved the electrical performance of the overall solid electrolyte. It can be found that when 10wt.% excess lithium is added ,it has the best electrochemical performance : specific capacity of 208.10 mAh/g @ 25mA/g & 144.15 mAh/g @ 300 mA/g ,and ionic conductivity of 1.38×10-3 S/cm. The experimental results are better than pure PVDF-HFP/PPC solid polymer electrolyte.
In this study, the electrical properties of the solid electrolytes are significantly improved due to inorganic fillers. It is further confirmed that the modification of PVDF-HFP mixed with PPC and the addition of appropriate amounts of MWCNT, LLZGCO and LLZO were helpful for the future application of solid electrolytes.

關鍵字(中)

★ 複合型固態電解質
★ 多壁奈米碳管
★ 聚偏氟乙烯-六氟丙烯共聚物
★ 聚碳酸亞丙酯

關鍵字(英)

★ Li7La3Zr2O12

論文目次

摘要 i
Astract iii
目錄 6
圖目錄 9
表目錄 13
第一章緒論 14
1-1 前言： 14
1-2 研究動機： 16
第二章文獻回顧 19
2-1 無機陶瓷固態電解質Li7La3Zr2O12(LLZO)介紹： 19
2-2 Garnet結構-Li7La3Zr2O12： 22
2-3 Li7La3Zr2O12電解質的製備： 27
2-4 Li7La3Zr2O12中的鋰離子傳遞機制： 29
2-5 Li7La3Zr2O12之優化-元素摻雜： 31
2-6 高分子固態電解質： 41
2-7 複合型固態電解質： 52
2-8 碳材應用於複合式電解質應用： 56
第三章實驗方法 62
3-1 實驗藥品 62
3-2 實驗設備 63
3-3 實驗步驟 64
3-3-1 Li7La3Zr2O12與不同金屬摻雜之Li7La3Zr2O12製備 64
3-3-2 高分子固態電解質層製備 64
3-3-3 複合型固態電解質層製備 65
3-3-4 複合電極製備 66
3-3-5 離子液體配置 66
3-3-6 鈕扣電池組裝 67
3-4 材料分析與鑑定 68
3-4-1 粉末X光繞射儀 (Powder X-ray diffraction, PXRD)： 68
3-4-2 冷場發射掃描式電子顯微鏡(The field-emission scanning electron microscope, FE-SEM)： 68
3-4-3 能量散射X射線譜（Energy-dispersive X-ray spectroscopy，EDS）： 68
3-4-4 熱重分析 (Thermogravimetric analysis, TGA)： 68
3-4-5 感應耦合電漿放射光譜儀(ICP-OES)： 68
3-4-6 拉伸測試(Tensile testing)： 69
3-4-7動態光散射粒徑分析儀(Dynamic Light Scattering, DLS)： 69
3-5 電化學性質分析與鑑定： 70
3-5-1 計時電位法 (Chronopotentimetry) 70
3-5-2 交流阻抗 (Electrochemical impedance spectroscopy)： 70
3-5-3 循環壽命測試 (The Cycling performance)： 70
第四章結果與討論 71
4-1添加不同含量的多壁奈米碳管(MWCNTs)對於電池性能之影響應用於LiNi0.8Co0.1Mn0.1O2對於電池性能之影響： 72
4-1-1 LiNi0.8Co0.1Mn0.1O2分析與鑑定： 72
4-1-2 SEM表面形貌分析： 74
4-1-3 EDS元素分佈分析： 77
4-1-4 TGA熱穩定性分析： 79
4-1-5拉伸測試： 82
4-1-6定電流充放電分析： 86
4-1-7交流阻抗分析： 93
4-1-8交流阻抗分析： 96
4-2複合式固態電解質PVDF-HFP/PPC內含不同額外鋰添加LLZGO應用對於電池性能之影響： 98
4-2-1 氧化物陶瓷LLZGO粉末之合成分析與鑑定： 98
4-2-2 ICP-OES定量分析： 102
4-2-3 SEM表面形貌分析： 104
4-2-4 EDS元素分佈分析： 106
4-2-5定電流充放電分析： 110
4-2-6交流阻抗分析： 117
4-2-7 循環壽命分析： 120
4-3 0.25Ga與不同Ce參雜量之共參雜LLZO對於電池性能之影響： 122
4-3-1氧化物陶瓷LLZGCO粉末之合成分析與鑑定： 123
4-3-2 ICP-OES定量分析： 126
4-3-3 SEM表面形貌分析： 128
4-3-4 EDS元素分佈分析： 131
4-3-5定電流充放電分析： 142
4-3-6交流阻抗分析： 151
4-3-7循環壽命分析： 154
第五章結論與未來展望 157
第六章附錄 159

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指導教授

李岱洲張仍奎(Tai-Chou Lee Jeng-Kuei Chang)

審核日期

2022-9-14

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