臺灣博碩士論文加值系統

現今科技的能源、通訊等應用需求越來越大，鋰離子電池逐漸受到關注，為了能同時兼具高電容量與高工作電壓兩項優點，利用Li1.12Mn0.56Ni0.16Co0.08 O2富鋰正極材料的高電容量特性與LiNi0.5Mn1.5O4 5V正極材料的高工作電壓的特性進行改質，為本實驗重點。本論文以LiNi0.5Mn1.5O4高電壓5V正極材料作為基礎以富鋰正極材料進行包覆與混摻兩種方法進行改質，得到富鋰改質高電壓正極材料，其製程分為3大部分，分別為包覆性、混摻性、混摻性改良。首先將富鋰正極材料包覆在高電壓5V正極材料重量配比為LR:LNMO(2:8、3:7、4:6)以化學共沉澱法的方式進行合成，最後與LiOH混摻進行不同3個燒結條件，得到9組包覆性富鋰改質高電壓正極材料。另一部分為LR(未球磨)富鋰與LNMO高電壓正極材料重量配比LR:LNMO(1:9、3:7、4:6)進行混摻，得到3組混摻性富鋰改質高電壓正極材料。LR(球磨後)富鋰與LNMO高電壓正極材料重量配比LR:LNMO(2:8、3:7、4:6)進行混摻，得到3組混摻性改良富鋰改質高電壓正極材料。所得粉末正極材料分別利用場發射電子顯微鏡(FE-SEM)檢測粉末表面形貌，X光繞射光譜儀(XRD)了解材料晶體結構，雷射繞射粒徑分佈分析儀(SLS)進行粉末顆粒粒徑分佈，將粉末材料製作成極板並組成測試鈕扣型電池，以鈕扣型電池電性測試系統與設備來觀察C-rate電性與循環壽命。研究結果得知在LR(球磨後)正極材料混摻LNMO正極材料重量配比(LR:LNMO)3:7，在2.5-4.8V電壓範圍0.1C/0.1C充放電速率下，表現出最佳的放電電容量211.9 mAh/g，首次不可逆電容量4 mAh/g，比原始LNMO正極材料26 mAh/g來得低。

Nowadays, the demand for the application of energy and communications is increasing, and lithium-ion batteries are receiving more and more attention. In order to have both the advantages of high capacitance and high operating voltage, the high-capacitance characteristics of lithium-rich cathode material Li1.12Mn0.56Ni0.16Co0.08O2and the high operating voltage characteristics of cathode materials LiNi0.5Mn1.5O4 5Vare upgraded, which is the focus of this experiment. In this paper, LiNi0.5Mn1.5O4 high voltage 5V cathode material was used as the basis to upgrade the lithium-rich cathode materials by coating and blending, thus generating the lithium-rich modified high voltage cathode materials. The process was divided into 3 parts: improved coating, blending, and blending. Firstly, the lithium-rich cathode materials are coated by high-voltage 5V cathode material in a weight ratio of LR:LNMO (2:8, 3:7, 4:6)and are synthesized by chemical co-precipitation. Then, it is mixed with LiOH under three different sintering conditions, and finally nine groups of coated lithium-rich modified high-voltage cathode materials are obtained. The other part is that LR (non-ball-milled) lithium-rich and LNMO high-voltage cathode materials are mixed with a weight ratio of LR:LNMO (1:9, 3:7, 4:6), and 3 sets of mixed lithium-rich modified high voltage cathode materials are obtained. LR (ball-milled) lithium-rich and LNMO high-voltage cathode materials with a weight ratio of LR: LNMO (2:8, 3:7, 4:6) are mixed, and three groups of improved lithium-rich modified high-voltage cathode materials are obtained. The resulting powder cathode material was measured by field emission electron microscopy (FE-SEM) to determine the surface morphology of the powder, X-ray diffraction spectroscopy (XRD) was used to figure out the crystal structure of the material, and the laser diffraction particle size distribution analyzer (SLS) was used to measure the powder particle size distribution. The powder material is made into electrode slabs and then constitutes test button batteries, and the C-rate electrical property and cycle life are observed with the button battery electrical test system and equipment. The research finding showed that the best discharge capacity of 211.9 mAh/g appeared when the mixture modified weight ratio was (LR:LNMO) 3:7, the irreversible capacity loss in the first cycle decreases 4 mAh/g was lower than that of the original LNMO cathode material of 26 mAh/g.

中文摘要……………………………………………………………………………………………………………………………………………………………………i
Abstract…………………………………………………………………………………………………………………………………………………………………ii
誌謝………………………………………………………………………………………………………………………………………………………………………………iv
目錄………………………………………………………………………………………………………………………………………………………………………………v
表目錄…………………………………………………………………………………………………………………………………………………………………………vii
圖目錄…………………………………………………………………………………………………………………………………………………………………………viii
第一章 緒論………………………………………………………………………………………………………………………………………………………1
1.1 前言………………………………………………………………………………………………………………………………………………………………1
1.2 研究目的……………………………………………………………………………………………………………………………………………………1
第二章 文獻回顧………………………………………………………………………………………………………………………………………………2
2.1 鋰離子電池簡介……………………………………………………………………………………………………………………………………2
2.1.1 鋰離子電池之工作原理…………………………………………………………………………………………………………………2
2.1.2 鋰離子電池特點………………………………………………………………………………………………………………………………3
2.1.3 鋰離子電池結構組成……………………………………………………………………………………………………………………3
2.1.3.1 負極材料………………………………………………………………………………………………………………………………………………4
2.1.3.2 電解液……………………………………………………………………………………………………………………………………………………6
2.1.3.3 隔離膜……………………………………………………………………………………………………………………………………………………6
2.1.3.4 正極材料………………………………………………………………………………………………………………………………………………6
2.2 LiNixMn2-xO4 高電壓正極材料LNMO…………………………………………………………………………………10
2.2.1 LiNixMn2-xO4 高電壓正極材料之改質研究…………………………………………………………………14
2.3 LiNixCoyMn1-x-yO2富鋰層狀正極材料LR………………………………………………………………………15
2.3.1 LiNixCoyMn1-x-yO2富鋰層狀正極材料之改質研究…………………………………………………19
第三章 實驗步驟………………………………………………………………………………………………………………………………………21
3.1 實驗材料與設備……………………………………………………………………………………………………………………………21
3.1.1 實驗材料…………………………………………………………………………………………………………………………………………21
3.1.2 實驗設備………………………………………………………………………………………………………………………………………21
3.2 實驗流程…………………………………………………………………………………………………………………………………………22
3.2.1 共沉澱法製備富鋰LR正極材料包覆LNMO正極材料……………………………………………………24
3.2.1.1 合成富鋰前驅物包覆LNMO正極材料 – 共沉澱法………………………………………………………24
3.2.1.2 合成富鋰LR正極材料包覆LNMO正極材料 – 固態燒結法………………………………………24
3.2.2 製備富鋰LR正極材料混摻LNMO正極材料-混摻法……………………………………………………25
3.2.2.1 合成富鋰LR正極前驅體Mn0.56Ni0.16Co0.08(CO3)0.8 – 共沉澱法……25
3.2.2.2 合成富鋰LR正極材料Li1.12Mn0.56Ni0.16Co0.08 O2 – 固態燒結法……25
3.2.2.3 研磨富鋰LR正極材料Li1.12Mn0.56Ni0.16Co0.08O2…………………………………26
3.2.2.4 富鋰LR正極材料及高電壓正極材料混摻………………………………………………………………26
3.3 鋰離子電池正極極板製備…………………………………………………………………………………………28
3.4 鈕扣型電池組裝……………………………………………………………………………………………………………31
3.5 分析設備…………………………………………………………………………………………………………………………32
3.5.1 場發射電子顯微鏡(FE-SEM) ……………………………………………………………………………32
3.5.2 X光繞射分析儀(XRD) …………………………………………………………………………………………32
3.5.3 雷射繞射粒徑分佈分析儀……………………………………………………………………………………32
3.5.4 鈕扣型電池電性測試系統與設備………………………………………………………………………32
第四章 結果與討論………………………………………………………………………………………………………………………………35
4.1 富鋰正極材料(lithium rich cathode) (LR)之性能分析……………35
4.1.1 LR正極材料之結構與形貌分析……………………………………………………………35
4.1.2 LR正極材料之電性分析…………………………………………………………………………37
4.2 LNMO高電壓正極材料之性能分析………………………………………………………39
4.2.1 LNMO正極材料之結構與形貌分析……………………………………………………39
4.2.2 LNMO正極材料之電性分析……………………………………………………………………41
4.3 LR正極材料包覆LNMO正極材料之改質研究……………………………………43
4.3.1 以不同比例LR前驅物包覆LNMO前驅物之形貌分析……………………43
4.3.2 燒結溫度對不同比例前驅物結構與形貌之影響…………………………44
4.3.3 不同燒結條件對LR包覆LNMO之電性影響………………………………………49
4.4 LR正極材料混摻LNMO正極材料之改質研究……………………………………54
4.4.1 LR混摻LNMO正極之結構與形貌分析影響………………………………………55
4.4.2 LR混摻LNMO正極之電性影響………………………………………………………………57
4.4.3 LR(球磨後)混摻LNMO正極材料之結構與形貌分析影響…………60
4.4.4 LR(球磨後) 混摻LNMO正極材料之電性影響………………………………63
第五章 結論…………………………………………………………………67
參考文獻………………………………………………………………………………68
Extended Abstract……………………………………………………75
簡歷………………………………………………………………………………………78

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