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研究生:王上瑜
研究生(外文):Shang-YuWang
論文名稱:新穎薄膜晶種成長技術於大尺寸釔鋇銅氧超導晶體之研究
論文名稱(外文):Growth of Large Single Grain Y-Ba-Cu-O Bulk Superconductors with Novel Thin Film Seed Technique
指導教授:陳引幹陳引幹引用關係
指導教授(外文):In-Gann Chen
學位類別:碩士
校院名稱:國立成功大學
系所名稱:材料科學及工程學系碩博士班
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2012
畢業學年度:100
語文別:中文
論文頁數:115
中文關鍵詞:釔鋇銅氧大尺寸超導體薄膜晶種多重晶種法
外文關鍵詞:YBCOlarge superconductor bulkthin film seedmulti-seeds
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薄膜磊晶晶種相對於塊體單晶粒晶種有較少的缺陷,且有晶面方位可控性,可提升晶體成長品質,且達多顆晶種同時成長製程之可能性,使晶體成長面積擴展數倍。

本文探討單顆、多顆薄膜晶種於釔鋇銅氧單晶粒成長製程,包含操作溫度範圍、異質成核溫度及降溫速率掌控、晶種擺放方位及間距影響、多顆薄膜晶種晶體成長應用等。藉由比較不同降溫速率之長晶形貌,繪製連續冷卻晶體形貌變態圖,以期可做為工程量產製程設計參考。

YBCO超導體以(001)方位垂直樣品表面之性能為最佳,但薄膜晶種接種製程會產生非理想(103)晶面孕核或45°晶面旋轉,同時於非晶種處同質成核次晶粒。本研究特設計6℃/h、4℃/h兩段式降溫控制,以YBCO包晶溫度(1010℃)做為控制轉折點,成功成長出直徑大於25mm單晶粒塊材。

於多顆晶種成長晶體之研究,本團隊研究指出當兩顆晶種方位為(100)/(100)時,兩個晶粒界面會有明顯第二相堆積及微裂縫,產生弱接點效應造成塊材整體的擄獲磁場能力下降;當晶種間的方位為(110)/(110)時,成長出的晶粒界面無明顯第二相堆積,但當晶種間的距離大於10mm時,擄獲磁場分布圖仍呈現為雙峰,顯示仍存在弱接點效應。隨著晶種距離接近且小於5mm時,充磁後擄獲磁場分布圖形狀接近單峰,成功去除雙顆晶種法製程產生之弱接點現象。而本研究觀察偏光顯微鏡中的雙晶形貌,發現該製程之雙面接合成功與否與晶格方位誤差(misorientation)有關,並將該技術應用於四顆晶種晶體成長。
Epitaxial thin film seed has higher crystalline than bulk seed and it can improve the quality of crystal growth. The crystal orientation can also controlled by thin film seed., and it will use in multi-seed technique. By multi-seeding, the crystal growth area can extended several times.

The single crystal growth with NdBCO thin film seeds is discussed in this study including multi-seed technique. The factor likes operation temperature window, the cooling rate during nucleation, the seed setting distance, and the seed setting orientation should be concerned and optimized. The crystal growth morphology is concluded into the “continues cooling morphology transformation diagram” for the mass production dependence.

It is suggested that the (001) single grain perpendicular to the bulks surface, shows the best performance. The (103) orientation, (001) 45° in plane, undesirable grain boundary, and random orientated subgrains are needed to be eliminated. We got the large single crystal YBCO bulks larger than 25mm successfully, with the special two step cooling fabrication. First use 6℃/h cooling, and then change the rate into 4℃/h at the YBCO peritectic temperature 1010℃.

In the multi-seeding fabrication, it is indicated that the second phase agglomeration is observed, with the seed (100)/(100) facet textured growing. Weak ling effect is displayed, limited the superconductive current flowing in these samples. Some precious study reports that the (110)/(110) facet textured growing can avoid this condition. In this study, the (110)/(110) facet textured growing samples with the seed distance larger than 10mm shows the multiple peaks in the trapped magnetic field profile distribution, implied the weak linkage still exits. With the seed distance is 5mm, a symmetry cone shape trap field distribution with the maximum value 2201Gauss. We assumed that the orientation alignment between two textured grains plays an important rule, and can be supported in the twin structure observed in the OM images. This technique can also be used in the four seeds growth texture grains samples in different kind of YBCO pellets.
目錄

摘要 I
Abstract II
誌謝 IV
目錄 VI
表目錄 IX
圖目錄 X
第一章 緒論 1
1-1 前言 1
1-2 銅氧化物超導塊材的研究與應用 1
1-3 研究目的 2
第二章 理論基礎與文獻回顧 3
2-1 超導體的發展歷程與基礎理論 3
2-1.1 超導體的發展歷程 3
2-1.2 超導體特性[4] 5
2-1.3 超導體的分類[4] 7
2-1.4 BCS 理論[4] 8
2-1.5 弱接點效應(Weak-Link effect) [4] 9
2-1.6 Bean Model[4] 10
2-2 Y-Ba-Cu-O高溫超導體 12
2-2.1 晶體結構 12
2-2.2 RE-Ba-Cu-O系統相圖 13
2-3 Y-Ba-Cu-O超導材料晶體製程 14
2-3.1 熔融製程(Melt Texture Growth) 14
2-3.2 熔融製程基本原理 16
2-3.3 Y123晶體成長模式[5,25] 17
2-3.4 Push-trap effect 19
2-3.5 充氧退火製程及雙晶結構生成 19
2-4 大面積單晶粒Y-Ba-Cu-O熔融製程影響因素 20
2-4.1 頂端接種技術:晶種的影響 20
2-4.2 製程溫度曲線的影響 23
2-4.3 抑制次晶粒的生成 25
2-4.4 多重晶種成長技術 26
2-4.5 鑽洞技術 27
第三章 實驗方法及步驟 49
3-1 實驗材料 49
3-2 實驗流程 49
3-2.1 Y123、Y211起始粉末製作 49
3-2.2 頂端接種熔融製程(TSMG:Top seed melt-texture growth) 50
3-2.3 建立薄膜晶種新長晶曲線 50
3-2.4 多重晶種法 50
3-2.5 充氧退火(Oxygen annealing) 51
3-3 性質分析 51
3-3.1 臨界電流密度的測量 51
3-3.2 晶面方向性之鑑定 51
3-3.3 微結構觀察 52
3-3.4 超導塊材擄磁力量測(Trap field mapping) 52
3-4 儀器設備 53
第四章 實驗結果與討論 57
4-1 薄膜晶種晶體成長曲線開發 57
4-1.1 超導塊體晶種與薄膜晶種之比較 57
4-1.2 成核降溫速率對薄膜晶體成長影響 59
4-1.3 兩階段式降溫之轉折點Tn對晶體形貌成長影響 60
4-1.4 兩階段式成核降溫速率控制對晶體形貌成長影響 61
4-2 薄膜晶種晶體成長機制討論及最佳化曲線繪製 70
4-2.1 非晶種成核之次晶粒形成機制探討 70
4-2.2 晶種可能異質成核方位分類概述 70
4-2.3 晶種異質成核晶面討論及其超導性質影響 72
4-2.4 連續冷卻晶面形貌圖製作及最佳參數探討 72
4-3 探討多重薄膜晶種成長技術 79
4-3.1 探討晶種晶粒間的方向性 79
4-3.2 雙晶種距離、超導塊材上下層性質比較 80
4-3.3 晶界分析與晶粒偶合性 82
4-3.4 雙晶種法總結 85
4-4 大尺寸超導塊材成長技術綜合應用 95
4-4.1 多重晶種(4 seeds)成長超大尺寸超導塊材 95
4-4.2 多重晶種(4 seeds)性質分析 95
4-4.3 利用多重晶種成長中心鑽洞的超導大塊材 96
第五章 結論 107
參考文獻 109
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