臺灣博碩士論文加值系統

本研究主要利用靜電紡絲技術製作鈮酸鈉鉀(KxNa1-xNbO3；KNN)奈米線，然而影響靜電紡絲主要三種因素，包括黏度、表面張力及庫倫力，其中吾人改變聚乙烯醇(PVA)濃度及分子量探討黏度對靜電紡絲之影響並藉由KNN電紡絲混合溶液流量控制奈米線尺寸範圍，且本實驗又利用外加電場強度的改變及不同電紡絲針孔規格改善KNN奈米線黏結問題，然而吾人進一步增加前驅物(KNN)濃度使得鈮酸鈉鉀奈米線分佈較均勻，再以不同熱處理溫度及持溫時間降低鈮酸鹽它相之析出。
首先吾人將鈮酸鈉鉀前驅液與聚乙烯醇(PVA)高分子溶液均勻混合，以靜電紡絲技術牽引出所需之電紡絲成品，接著利用熱重分析儀(TGA)觀察電紡絲高分子及有機物質熱裂解之溫度，並使用SEM、EDS及XRD觀察KNN奈米線表面形貌與確認其為鈣鈦礦結構，吾人將最適化參數所製備出KNN奈米線進行壓電力顯微鏡(PFM)分析，由量測數值顯示KNN奈米線壓電性質優於其他壓電材料，故鈮酸鈉鉀奈米線適用於開發可撓性壓電材料。

The goal of this study is to investigate the fabrication potassium sodium niobate (KxNa1-xNbO3,KNN) nanowires and nanofibers by electrospinning process (ESP) and the characterization of KNN nanowires by piezoelectric force microscopy (PFM). There are a number of key parameters involved in electrospinning process such as viscosity and surface tension of precursor solution as well as the Coulombic force during the electrospinning. The effect of molecular weight and concentration of polyvinyl alcohol (PVA) on viscosity and electrospinning performance was analyzed. The size distribution of KNN nanowires and entanglement of KNN nanofibers were adjusted by the flow rate of PVA solution, needle specifications, and applied electrical field. Furthermore, the increased concentration of KNN precursor solution achieved an even uniform size distribution of KNN nanowires, of which the precipitation of niobate salts was avoided under various post-heat treatment conditions.
The precursor solution, a mixture of KNN chemical precursors and PVA polymeric solution, was transformed into the form of KNN nanowires via ESP process. The electrospun samples were tested under thermal gravimetric analyzer (TGA) to identify its on-set temperature for thermal decomposition. Both crystalline phase and microstructure of acquired KNN nanowires and nanofibers were analyzed by SEM/EDS and XRD. The piezoelectric properties of KNN products, which were manufactured by optimized process conditions, were examined by a PFM. The electrospun KNN nanowires and nanofibers were successfully obtained with much outstanding piezoleectric quality, as compared to equivalent materials made y other methods and are qualified to be a candidate material for the development of flexible electronic devices in the near future.

摘 要 i
ABSTRACT ii
表 目 錄 xii
第一章緒論 1
1.1 壓電陶瓷材料之簡介 1
1.2 無鉛壓電陶瓷發展及介紹 4
1.3 靜電紡絲技術介紹及應用 5
1.4 軟性電子產業應用及發展 9
1.5 研究動機及方向 15
第二章理論基礎與文獻回顧 20
2.1 靜電紡絲之理論與研究 20
2.1.1 靜電紡絲之研究 20
2.1.2 臨界電位理論(Theory of Critical Value) 25
2.1.3 靜電紡絲之射流剖面 26
2.1.4 靜電紡絲之不穩定性射流 26
2.1.5 影響靜電紡絲基本參數 27
2.1.6 合成無機靜電紡絲 39
2.2 材料系統簡介 41
2.2.1 鈮酸鉀(KNbO3，KN) 41
2.2.2 鈮酸鈉(NaNbO3，NN) 45
2.2.3 鈮酸鉀鈉((Na1- xK x)NbO3，KNN) 47
2.2.4 鈮酸鋰(LiNbO3；LN) 51
2.2.5 鎢青銅結構(tungsten bronze，TB) 52
2.2.6 鈦酸鋇BaTiO3 (簡稱BT)系 53
2.2.7 鈦酸鉍鈉(Bi0.5Na0.5TiO3；BNT)系 54
2.3 壓電陶瓷的重要電氣特性 54
2.3.1 機電耦合因子(k) 54
2.3.2 介電損失因子 55
2.3.3 機械品質因子(Qm) 57
2.3.4 頻率常數(N) 58
2.3.5 壓電應變常數(d) 58
2.4 元素摻雜相關因素 61
2.4.1 置換原理 61
2.4.2 容忍因子 61
第三章 實驗步驟與方法 63
3.1 實驗藥品之物化性質 63
3.2 負極收集器製作及試片準備 64
3.2.1 試片清洗及製作 64
3.2.2 負極收集器之製作 65
3.3 利用靜電紡絲技術製作鈮酸鈉鉀(KNN)奈米線 66
3.3.1 鈮酸鈉鉀(KNN)前驅液之製備 66
3.3.2 製備聚乙烯醇(PVA)溶液 66
3.3.3 低分子量PVA溶液添加量對靜電紡絲KNN奈米線之影響 68
3.3.4 不同高分子量PVA濃度對靜電紡絲KNN奈米線之影響 70
3.3.5 熱處理條件對靜電紡絲KNN奈米線之影響 71
3.3.6 溶液流量對靜電紡絲KNN奈米線之影響 73
3.3.7 針頭規格對靜電紡絲KNN奈米線之影響 74
3.3.8 工作電壓對靜電紡絲KNN奈米線之影響 75
3.3.9 工作距離對靜電紡絲KNN奈米線之影響 75
3.3.10 鈮酸鈉鉀濃度對靜電紡絲KNN奈米線之影響 76
3.4分析儀器及設備簡介 77
3.4.1 圓錐-平板式黏度計 77
3.4.2 冷場發射掃描式電子顯微鏡(FE-SEM) 78
3.4.3 多弁貆光繞射儀(HRXRD) 79
3.4.4 高解析多弁鈺蓬y式探針顯微鏡 80
3.4.5 原子力顯微鏡之壓電響應力特性分析 81
3.4.6 熱重分析儀(TGA) 87
3.4.7 傅立葉轉換紅外光譜儀( Fourier Transform Infrared Spectroscopy；FTIR) 88
第四章結果與討論 90
4.1 低分子量PVA添加量對靜電紡絲KNN奈米線之影響 90
4.2 不同高分子量PVA濃度對靜電紡絲KNN奈米線之影響 96
4.3 不同熱處理條件靜電紡絲KNN奈米線之影響 102
4.4 溶液流量對靜電紡絲KNN奈米線之影響 112
4.5 針頭規格對於靜電紡絲製備KNN奈米線之影響 115
4.6 工作電壓對靜電紡絲KNN奈米線之影響 124
4.7 工作距離對於靜電紡絲製備KNN奈米線之影響 129
4.8 鈮酸鈉鉀濃度對靜電紡絲KNN奈米線之影響 133
4.9 鈮酸鈉鉀(KNN)奈米線之PFM特性分析 137
4.10 未來研究方向 143
第五章 結 論 147
參考文獻 150

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