臺灣博碩士論文加值系統

目前對於各式各樣的可攜式電子產品諸如行動電話及筆記型電腦之電源供應，鋰或鋰離子二次電池已是主流的選擇。然而，隨著可攜式產品的重量及體積的趨向輕薄短小，微型化也是新一代電池不得不發展的趨勢。開發更小、更輕、更高能量密度的電池乃成為業界及學術界共同追求的目標。薄膜電池(或稱為全固態微型電池)的概念乃應運而生。此外，厚度為微米級之薄膜電池可與微機電元件搭配，亦可作為記憶體之備用電源。
本研究選擇具高發展潛力的LiFePO4/C作為薄膜電池正極材料，藉由施予基座偏壓輔助磁控濺鍍沉積LiFePO4/C薄膜，進而調控離子轟擊能量以達到臨場改質(in-situ modification)，並搭配真空退火處理，成功地開發出高電容量及高放電電壓之正極薄膜材料，並有效大幅度提升其薄膜導電性。研究中發現，添加鈦底層可有效的促進LiFePO4/C結晶性，經過退火處理後，LiFePO4/C薄膜與鈦底層原子會有互擴散的現象，且添加鈦底層後會有較好的循環壽命與薄膜附著性，但電容量不如未加鈦底層薄膜。

Secondary lithium batteries have been the primary power supply components for various portable electronic devices, such as cell phones and notebook computers. However, as the weight and volume of the portable devices continuously decrease, the search for smaller, lighter, and higher power density power sources has never stopped. In order to meet these requirements, the concept of Thin Film Batteries (TFB), or all solid state micro-batteries, has therefore been of great interest. With only a few micron meters of thickness or less, thin film batteries are compatible with micron electro-mechanical devices, and can be the back-up power for SRAM, as well.
This research uses LiFePO4/C as cathode material of thin film batteries. Through substrate bias assist sputtering LiFePO4/C thin film, then control the energy of ion bombard to achieve in-situ modification. Moreover, it also uses vacuum annealing treatment to develop high capacity and high discharge voltage cathode materials, and increases electric conductivity of thin film effectively. The result shows that adding the titanium under layer can increase the crystalline of LiFePO4/C, and after anneal treatment, the LiFePO4/C thin film and titanium under layer have diffusion reciprocal, and adding the titanium under layer can have better cycle life and adhesion，but capacity lower then non-adding titanium under layer thin film.

致謝………………………………………………………………………I
中文摘要………………………………………………………………..III
英文摘要………………………………………………………………..IV
總目錄…………………………………………………………………...V
圖目錄……………………………………………………………….......X
表目錄………………………………………………………………....XV
第一章 緒論及研究動機………………………………………………1
1.1薄膜電池概論…….………………………………….........………..1
1.2研究動機…………………………………………………………….4.
第二章理論基礎與文獻回顧…………………………………………...6
2.1鋰離子電池簡介…………………………………………………….6
2.1.1電池的演進歷史…………………………………………………..6
2.1.2鋰離子電池的工作原理………………………………………….11
2.1.3固態薄膜電池……………………………………………………..12
2.1.4 陰極電極材料及電解質簡介……………………………………15
2.2 磷酸鋰鐵介紹……………………………………………………...19
2.2.1磷酸鋰鐵發展由來………………………………………………..19
2.2.2 磷酸鋰鐵結構介紹………………………………………………21
2.3磷酸鋰鐵製作方法…………………………………………………23
2.3.1固態反應法……………………………………………………….23
2.3.2機械化學活化法………………………………………………….24
2.3.3水熱法…………………………………………………………….25
2.3.4液相共沉澱法…………………………………………………….26
2.3.5微波加熱法……………………………………………………….27
2.3.6溶膠凝膠法……………………………………………………….27
2.4磷酸鋰鐵存在之問題與改善………………………………………28
2.4.1磷酸鋰鐵電容量損失…………………………………………….28
2.4.2包覆碳及添加碳製成複合材料………………………………….30
2.4.3摻雜金屬粉體及有機金屬鹽…………………………………….31
2.5溫度對於鋰離子擴散之影響………………………………………32
2.6 磷酸鋰鐵之熱穩定性……………………………………………..33
2.7磷酸鋰鐵薄膜製作…………………………………………………33
第三章 實驗方法與步驟………………………………………………45
3.1實驗藥品與耗材……………………………………………………45
3.2儀器與設備………………………………………………………….46
3.3靶材製備…………………………………………………………….47
3.4實驗流程…………………………………………………………….47
3.5薄膜製備……………………………………………………………49
3.5.1射頻磁控濺鍍法製備掺碳磷酸鋰鐵…………………………….49
3.5.2 Ti底層輔助薄膜成長…………………………………………….50
3.5.3 基座偏壓輔助濺鍍製程………………………………………...50
3.5.4不同溫度退火熱處理…………………………………………….51
3.6材料鑑定與分析……………………………………………………51
3.6.1低掠角X光繞射儀（Glazing Angle X-Ray Diffractometer）…...51
3.6.2掃描式電子顯微鏡( Scanning Electron Microscope ) …………..52
3.6.3輝光放電分光儀(Glow Discharge Spectrometer ) ………………53
3.6.4薄膜電性量測…………………………………………………….54
3.6.5薄膜重量量測…………………………………………………….55
3.7薄膜電化學特性分析………………………………………………56
3.7.1半電池元件製作………………………………………………….56
3.7.2紐扣型電池組裝………………………………………………….56
3.7.3電池充放電性能測試…………………………………………….57
3.7.4循環伏安測試…………………………………………………….58
3.7.5循環壽命………………………………………………………….59
3.7.6退火溫度與Ti底層擴散對薄膜之影響……………………...…..59
第四章 結果與討論……………………………………………….…..70
4.1低掠角XRD分析材料結構………………………………………70
4.1.1 不同退火壓力之效應…………………………………………..70
4.1.2 Ｔi底層效應...………………………………………………….71
4.1.3 基座偏壓之效應………………………………………………..72
4.1.4不同退火溫度…………………………………………………...74
4.2薄膜表面型態觀察………………………………………………..75
4.2.1時效現象………………………………………………………...75
4.2.2退火熱處理效應………………………………………………...76
4.2.3 基座偏壓之效應………………………………………………..77
4.2.4鈦底層效應……………………………………………………...79
4.2.5不同退火溫度…………………………………………………...80
4.3輝光放電分光儀分析……………………………………………..82
4.4薄膜組成成分之鑑定……………………………………………..84
4.5薄膜電性…………………………………………………………..85
4.6磷酸鋰鐵電池電化學特性分析…………………………………..87
4.6.1充放電特性………………………………………………………87
4.6.2循環伏安測試……………………………………………………89
4.6.3放電循環壽命特性比較…………………………………………90
第五章結論…………………………………………………………..130
第六章未來研究方向………………………………………………..133
參考文獻……………………………………………………………..134
作者簡介……………………………………………………………..141

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【47】Versatile Synthesis of Carbon-Rich LiFePO4 Enhancing Its Electrochemical Properties, Elvira M. Bauer, Electrochemical and Solid-State Letters, 7 (4) A85-A87 (2004)
【48】Characterization of LiFePO4 as the cathode material for rechargeable lithium batteries ,Takahashi M , TOBISHIMA S , J Power Sources , 2001 , 97-98 : 508 -511.
【49】 The source of first cycle capacity loss in LiFePO4 ,Andersson A S , Thomas J O. J Power Sources , 2001 , 97-98 : 498 -502.
【50】Electroactivity of natural and synthetic triphylite ,Ravet N , Chouinard Y, Magnanjf , J Power Sources , 2001 ,97-98 : 503 -507.
【51】Improved electrochemical performance of a LiFePO4-based composite cathode ,Prosini P P , ZANE D , PASQUAL I M，Electrochimica Acta , 2001 , 46 : 3517 -3523
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【54】Lithium extraction / insertion in LiFePO4 an X-ray diffraction and Mossbauer spectroscopy study ,Andersson A S , Kalska B , Solid State Ionics ,2000 ,130 (1 - 2) :41 - 52.
【55】Synthesis and characterization of LiFePO4 cathode material dispersed with nano-structured carbon, S.T. Yang，Electrochimica Acta 51 (2005) 166–171
【56】Structural and Electrochemical Properties of Multihollow LiFePO4 for Lithium Battery Cathodes ,Junbiao Lu, Journal of The Electrochemical Society, 152 (7) A1441-A1444 m (2005)
【57】A Novel Concept for the Synthesis of an Improved LiFePO4 Lithium Battery Cathode ,F. Croce, Electrochemical and Solid-State Letters, 5 (3) A47-A50 (2002)
【58】Comparison between different LiFePO4 synthesis routes and their influence on its physico-chemical properties ,Sylvain Franger , Journal of Power Sources 119–121 (2003) 252–257
【59】Effect of Surface Carbon Structure on the Electrochemical
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【60】Electrochemical Performance of Sol-Gel Synthesized LiFePO4 in Lithium Batteries ,Yaoqin Hu,，Journal of The Electrochemical Society, 151 (8) A1279-A1285 (2004)
【61】Surface Chemistry of Carbon-Treated LiFePO4 Particles for Li-Ion Battery Cathodes Studied by PES ,Marie Herstedt, Electrochemical and Solid-State Letters, 6 (9) A202-A206 (2003)
【62】Electrochemical performance of nanocrystalline LiMPO4 thin-films prepared by electrostatic spray deposition ,Jun Ma, Qi-Zong Qin，Journal of Power Sources 148 (2005) 66–71
【63】Stability and electrochemical behavior of lithium iron phosphates ,Yang S F , Song Y N , Elect rochem. Commun. , 2002 , 4 (3) : 239～244
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【68】Optimized LiFePO4 for lithium battery cathodes ,Yamada A , Chung S C , J . Elect rochem. Soc. , 2001 , 148 (3) : A224～A229
【69】Synthesis of LiFePO4 by co-precipitation and microwave heating ,Park K S , Son J T , Elect rochem. Commun. , 2003 , 5 (10) : 839～842
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【73】Improved electrochemical performance of a LiFePO4 based composite cathode ,Prosini P P，ZANED，Electrochemical Acta，2001，46:3 517- 3 523
【74】A new synthetic route to prepare LiFePO4 with enhanced electrochemical performence ,Prosini P P，CAREWSKA M，2001 International Joint ESC meeting
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【76】Reducing carbon in LiFePO4/ C composite electrodes to maximize specific energy , volumetric energy , and tap density ,Zhaohui C , Dahn J R， J Electrochem Soc , 2002 , 149 (9) : A1 184 - A1 189.
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【80】An unexpected conductor ,Thuckeray M.，Nature Mater , 2002 , 2 : 81 - 82.
【81】Electronically conductive phosphor-olivines as lithium storage electrodes , Chung S Y,Blocking J T , Nature Mater , 2002 , 2 : 123 - 128.
【82】Preparation of LiFePO4 Thin Films by Pulsed Laser Deposition and Their Electrochemical Properties, Yasutoshi Iriyama, Electrochemical and Solid-State Letters, 7 (10) A340-A342 (2004)
【83】Reaction behavior of LiFePO4 as a cathode material for rechargeable lithium batteries ,Takahashi M , Tobishima S , Solid State Ionics , 2002 ,148 (3 - 4) :283 - 289.
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【85】Porous, carbon-decorated LiFePO4 prepared by sol–gel method based on citric acid ,Miran Gabersceka, Solid State Ionics 176 (2005) 1801 – 1805
【86】Electrochemical Deposition and Modification of LiFePO4 for the Preparation of Cathode with Enhanced Battery Performance ,Ali Eftekhari , J.Electrochem. Soc. A1816-A1819 (2004)
【87】Emulsion drying synthesis of olivine LiFePO4/C composite and its electrochemical properties as lithium intercalation material ,Seung-Taek Myung. Electrochimica Acta 49 (2004) 4213–4222
【88】A novel concept for the synthesis of an improved LiFePO4 lithium battery cathode ,F. Croce, Electrochemical and Solid-State Letters, 5 (3) A47-A50 (2002)
【89】Improved electrochemical performance of a LiFePO4 based composite cathode ,Prosini P P，ZANED，Electrochemical Acta，2001，46:3 517- 3 523
【90】A new synthetic route to prepare LiFePO4 with enhanced electrochemical performence ,Prosini P P，CAREWSKA M，2001 International Joint ESC meeting
【91】Approaching theoretical capacity of LiFePO4 at room temperature at high rates ,Huang H , Yin S C , Electrochem and Solid State Lett , 2001 ,4 (10) :A170 - A172.
【92】An unexpected conductor ,Thuckeray M.，Nature Mater , 2002 , 2 : 81 - 82.
【93】Electronically conductive phosphor-olivines as lithium storage electrodes ,Chung S Y,Blocking J T , Nature Mater , 2002 , 2 : 123 - 128.
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【95】Electrochemical Deposition and Modification of LiFePO4 for the Preparation of Cathode with Enhanced Battery Performance ,Ali Eftekhari , J.Electrochem. Soc. A1816-A1819 (2004)
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