雷射加熱提拉生長法生長不同配比鈮酸鋰晶纖與性質之量測

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研究生：	陳智勇 Chi-Yung Chen
論文名稱：	雷射加熱提拉生長法生長不同配比鈮酸鋰晶纖與性質之量測 Growth and Properties of Different Compositions of LiNbO3 Single Crystal Fiber by LHPG method
指導教授：	陳志臣 Jyh-Chen Chen
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 機械工程學系 Department of Mechanical Engineering
畢業學年度：	95
語文別：	中文
論文頁數：	105
中文關鍵詞：	化學計量配比鈮酸鋰、鈮酸鋰
外文關鍵詞：	stoichiometric lithium niobate, LN, lithium niobate
相關次數：	點閱：7 下載：0
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本研究是使用雷射加熱基座提拉法(LHPG)生長化學劑量配比鈮酸鋰之晶纖。在化學劑量配比鈮酸鋰晶體生長的機制上，成功發現使用LHPG法生長化學劑量配比鈮酸鋰時的長晶機制，它是依循著平衡相圖的觀念，也就是說晶體所生長出來的[Li]/[Nb]的濃度配比是依照當時熔區中Li的濃度來生長的，所以晶體的Li濃度會隨著生長的長度而漸漸增加，當熔區中Li濃度達到58 mole %時才從熔區中生長出化學劑量配比鈮酸鋰，並非直接從熔區中淬火生長出化學劑量配比，這樣的結果我們可以經由化學分析電子光譜儀(ECSA)得知。對於所生長出來的晶體，我們還使用了X光粉末繞射儀、單晶繞射儀、光學顯微鏡與感應偶合電漿質譜儀等儀器來幫助我們對於晶體的研究。
由於鈮酸鋰有一個非常大的固熔區，利用研究得到的長晶機制，可以藉由控制提供的材料棒濃度來控制所生長出來的LN晶體濃度，並藉由控制晶種濃度來加快生長的速度，進而成功生長出固熔區中不同配比的鈮酸鋰。對於鈮酸鋰的性質量測，我們使用UV吸收光譜、FTIR光譜與Raman光譜等光學儀器來確定其性質，並從結果中來討論其中的物理特性。
在不同配比LN組成(Li1-xNb1+xO3，0 ≤ x ≤ 0.12)中，可以藉由不同配比LN晶體所得到的拉曼光譜來解釋光誘發o-e散射效應，可以藉由分析光譜中之峰值強度來分析其與晶體的鋰空缺情形之關係。而入射的o-wave穿透光轉換成e-wave散射光也會隨著以空缺的增加而增加，並從中研究其能量轉換與轉換效率。

In this study, SLN single crystal fibers are grown by the laser-heated pedestal growth technique. We successfully find out the growth mechanisms of SLN single crystal by utilizing LHPG method. This growth mechanism is followed the equilibrium phase diagram concept. The composition of [Li]/[Nb] of the grown crystal fibers are based upon the Li2O concentration in the melting zone during growing process. Therefore, the Li2O concentration within the crystal fiber will gradually increase with the grown length. When the Li2O concentration reaches to 58 mole%, the SLN is obtained and it is not grown from the melting zone by quenching. We can examine the growth mechanism by ECSA. Besides, we can also use the XRPD、XRD/CCD、OM and ICP-AES to help us to investigate the properties of the grown crystals.
LN has a wide solid solution phase field. Using the fore-mentioned growth mechanism, we can grow different compositions of LiNbO3 single crystal fibers by controlling the composition of the feeding rod. By controlling the seed rods, we can reduce the grow time. We followed the aforementioned growth mechanism to successfully grow different composition LN single crystal fibers. We investigate the optical properties of the crystal fibers form the equipments of UV absorption edge, IR absorption spectrum and Raman spectrum. We also discuss the physic characteristics from the measured optical properties.
In different composition LN crystals (Li1-xNb1+xO3，0 ≤ x ≤ 0.12), we can explain the light induced o-e scattering effect from Raman spectrum. By analyzing the Raman spectra, the relationship between the intensity of Raman phonons and Li vacancies can be found. The energy transformation increased due to the enhancement of o-wave scattering transfers to e-wave scattering with the vacancies of Li increased. The energy transformation and transfer efficiency can be also investigated.

中文摘要	I
Abstract	II
致謝	IV
目錄	V
表目錄	VII
圖目錄	VIII
符號說明	X
第一章 緒論................................................1
1-1 前言...................................................1
1-2 材料簡介...............................................2
1-3 相關研究...............................................4
1-3-1 鈮酸鋰晶體生長方式...................................4
1-3-2 拉曼光譜之應用.......................................8
1-4 研究動機與目的.........................................9
1-5 研究方法..............................................10
第二章 實驗設備、材料製程與研究方法.......................18
2-1雷射加熱基座提拉法 (LHPG)..............................18
2-1-1 鈮酸鋰粉末製備......................................18
2-1-2 陶瓷材料棒的製作....................................19
2-1-3 實驗設備............................................19
2-1-4 長晶過程............................................21
2-1-5 晶體後續處理及檢測..................................22
2-2 拉曼光譜實驗裝置與原理................................25
2-2-1 實驗裝置............................................25
2-2-2 實驗原理............................................26
第三章 化學劑量配比鈮酸鋰晶纖生長.........................33
3-1 長晶機制..............................................33
3-2 晶纖生長..............................................34
3-3 晶體性質檢測..........................................35
3-3-1 X光粉末繞射(XRPD)...................................35
3-3-2 單晶繞射(X-Ray/CCD).................................36
3-3-3 光學顯微鏡對陶瓷、晶纖與晶纖蝕刻後鐵電域的觀察......36
3-3-4 化學分析電子光譜 (ESCA).............................37
3-3-5 感應偶合電漿質譜儀 (ICP-AES)........................40
3-4 長晶機制之探討........................................40
3-5 本章結論..............................................42
第四章 不同配比鈮酸鋰晶纖生長.............................57
4-1 晶纖生長..............................................57
4-2 晶體性質檢測..........................................59
4-2-1 X光粉末繞射 (XRPD)..................................59
4-2-2 單晶繞射 (X-Ray/CCD)................................60
4-2-3 紫外光吸收光譜 (UV Absorption Spectra)..............60
4-2-4 傅立葉紅外光譜 (FTIR)...............................63
4-2-5 拉曼光譜 (Raman Spectra)............................64
4-3 本章結論..............................................66
第五章 光誘發o-e散射效應..................................80
5-1 何謂光誘發o-e散射現象.................................80
5-2 LN晶體之本質缺陷結構..................................81
5-3 能量轉換與轉換效率....................................82
5-4 本章結論..............................................86
第六章 總結論.............................................97
參考文獻..................................................99

                                

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