銣鎢氧化物已被發現其氧含量的變化會影響其物性，以及超導臨界溫度會隨銣氧含量變化而有所不同。為了能更進一步的確定銣鎢氧化物其超導臨界溫度的改變的來源。藉著穿透式電子顯微鏡，觀察在銣鎢氧化物Rb0.23WOy之超導抗磁單晶樣品其細微結構上的變化，與其超導臨界溫度的關西。不同氧含量的單晶樣品，在面(100)上並沒有明顯的變化，而在(001)的面上並沒有足夠大的區塊可以觀察，藉由改變單晶樣品的燒結溫度、降溫速率、及不同的試片製作方法，來觀測其區塊上面積的大小是否有所增長。

Rubidium tungsten bronze, had been observed that physical property and superconductivity critical temperature were depend on oxygen contents of rubidium tungsten bronze . To confirm the source that rubidium tungsten oxide superconductive of change of critical temperature .We could observe the variation on nanostructure of different oxygen content of crystalline sample by using transmission electron microscope. The surface,(100), didn’t have any obviously change even though oxygen content of crystalline sample is different .The surface,(001),there is not enough large block that can be observed ,by changing the sintering temperature of the single crystal sample, cooling speed, and different preparation method for samples, to observe the changing on the surface of samples.

目錄
第一章 緒論	1
(一) 鎢化物回顧	1
(二) 銣鎢氧化物	2
(三) 銣鎢氧化物的研究方向	3
第二章 實驗儀器與原理	6
2.1電子天平	6
2.2 壓模機	6
2.3高溫爐	6
2.3.1	預燒樣品的高溫爐	6
2.3.2	燒結樣品的高溫爐	7
2.4 X-ray繞射系統	7
2.4.1	實驗室XRD	7
2.4.2	XRD接收器	7
2.5磁性量測系統	9
2.5.1	操作原理	9
2.5.2	磁性量測儀器介紹	9
2.6圖像軟體	11
2.6.1	結構建構軟體(Diamond)	11
2.6.2	圖像分析軟體(DigitalMicrograph)	11
2.6.3	圖像模擬軟體(JEMS)	11
2.7 SEM觀測系統	12
2.7.1	儀器簡述:	12
2.7.2	構造簡述	12
2.7.3	功用簡述	13
2.8 TEM觀測系統	14
2.8.1	儀器簡介	14
2.8.2	原理簡述	14
2.8.3	組件介紹	14
2.8.4	功能簡述	15
2.8.5	補充敘述:	16
2.9 TEM樣品製備系統	17
2.9.1	研磨機	17
2.9.2	加熱平台	17
2.9.3	離子蝕薄機	17
第三章 樣品製備步驟與方法	19
3.1 單晶樣品製備步驟與方法	19
3.2 TEM樣品製備步驟與方法	23
第四章實驗數據分析與討論	25
4.1多晶樣品RbxWOy之結構分析	25
4.2單晶樣品Rb0.23WOy之數據分析	27
4.3單晶Rb0.23WOy之磁性數據分析	29
4.4單晶Rb0.23WO3.0的X-RAY繞射分析	31
4.5單晶Rb0.23WOy的質量分析	32
4.6單晶Rb0.23WOy的SEM觀測	32
4.7單晶Rb0.23WOy之TEM試片製作	33
4.8單晶Rb0.23WOy之TEM樣品數據分析	34
第五章結論	37
References	81

 
圖表目錄
表一各種鎢氧化物之結構與超導臨界溫度	39
圖1-1(a) TTB NaxWO3超導臨界溫度對Na濃度之關係圖	40
圖1-1(b) NaxWO3不同Na濃度之光電子發射圖	40
圖1-2 RbXWO3超導臨界溫度對Rb濃度之關係圖	41
圖1-3(a) RbXWO3不同Rb濃度的電阻率對溫度之關係圖	42
圖1-3(b) 圖(a)中的TB對Rb濃度x之關係圖	42
圖1-4 RbXWOy在x=0.19,0.23,0.27之超導臨界溫度對氧含量的關係圖，以交叉符號表示在2 K以上沒發現超導現象	43
圖1-5 左邊小圖為Brusetti所得結果，而右圖為我們變動氧含量所得的結果	44
圖2-1 XRD燈絲構造	45
圖2-2 XRD的基本架設	45
圖2-3 TEM剖面構造圖	46
圖4-1 Rb0.33WO3之結構(a)角落共享的八面體WO6圍成六角晶相結構	47
圖4-1 Rb0.33WO3之結構(b) 稍微傾斜c軸之六角晶相結構	47
圖4-2 Rb0.27WO3的X-RAY繞射圖	48
圖4-3 Rb0.19WOy不同氧含量之一般解析度x-ray繞射圖	49
圖4-4 Rb0.23WOy不同氧含量之一般解析度x-ray繞射圖	50
圖4-5 Rb0.27WOy不同氧含量之一般解析度x-ray繞射圖	51
圖4-6 Rb0.19WOy之晶格常數a和c對氧含量之關係	52
圖4-7 Rb0.23WOy之晶格常數a和c對氧含量之關係圖	53
圖4-8 Rb0.27WOy之晶格常數a和c對氧含量之關係圖	54
圖4-9(a) 不同晶向卻熔在一塊的Rb0.23WO3.00單晶樣品	55
圖4-9(b) 燒結後具有較佳方向性的Rb0.23WO3.00單晶樣品	55
圖4-10 量測磁性VSM的樣品座	56
圖4-11 Rb0.23WO3.00單晶樣品經過在氧中退火後之磁化率對溫度	56
圖4-12 Rb0.23WO3.00單晶樣品在圖二十二中第十一次與第十九次退火之磁化率對溫度變化圖	57
圖4-13 Rb0.23WO2.90單晶樣品之磁化率對溫度變化圖	58
圖4-14 Rb0.23WO3.02單晶樣品之磁化率對溫度變化圖	58
圖4-15 Rb0.23WO3.00單晶樣品晶格常數c與(0 0 2)繞射峰半高寬對退火次數關係圖，圖中0~11與16~19之退火條件為通氧氣1 atm下400oc持12小時，12~15為抽真空下400oc持溫12小時	59
圖4-16 單晶樣品的質量變化率對退火次數的變化圖，退火方式為通氧氣1 atm下400oc持溫24小時	60
圖4-17為單晶樣品(粉末狀)在SEM的觀測圖	61
圖4-18單晶樣品(顆粒狀)在SEM的觀測圖	61
圖4-19(a)單晶樣品片狀小單晶在SEM的觀測圖	62
圖4-19(b)單晶樣品片狀小單晶在SEM的觀測圖	62
圖4-20 單晶樣品磨碎成粉將其與丙酮或酒精混合的HR-image	63
圖4-21 單晶樣品磨碎成粉末與樹酯結合的HR-image	63
圖4-22 真空箱中單晶樣品磨碎成粉與丙酮或酒精混合HR-image	64
圖4-23 真空箱中單晶樣品磨碎成粉末與樹酯結合的HR-image	64
圖4-25 diamond軟體所建構的Rb0.33WO3的立體結構圖(001)俯視圖	65
圖4-26 Rb0.23WO3.00單晶樣品直接置入TEM觀測	66
圖4-27 Rb0.23WO3.00單晶樣品傾斜面(100)的HR-image	66
圖4-28 diamond軟體所建構去除氧原子的Rb0.33WO3的立體結構圖(100)俯視圖	67
圖4-29 Rb0.23WO3.00單晶樣品經過tiltholder傾斜後得單晶(100)的圖	67
圖4-30 JEMS軟體所模擬出來的繞射圖型	68
圖4-31 Rb0.23WO3.00單晶樣品經過傾斜些角度後得單晶(100)的繞射圖	68
圖4-32 超導抗磁單晶樣品Rb0.23WO2.9	69
圖4-33 超導抗磁單晶樣品Rb0.23WO3.02	69
圖4-34 無超導抗磁單晶樣品Rb0.23WO2.97	70
圖4-35 放大後發現似六角型的區域	70
圖4-36 圖片為燒結溫度1000度的HR-image Rb0.23WO3.00	71
圖4-37 圖片為燒結溫度1050度的HR-image Rb0.23WO3.00	71
圖4-38 圖片為燒結溫度1100度的HR-image Rb0.23WO3.00	72
圖4-39 圖片為燒結溫度1150度的HR-image Rb0.23WO3.00	72
圖4-40圖片為燒結溫度1200度的HR-image Rb0.23WO3.00	73
圖4-41圖片為燒結溫度1210度的HR-image Rb0.23WO3.00	73
圖4-42 圖片為燒結溫度1220度的HR-image Rb0.23WO3.00	74
圖4-43 圖片為燒結溫度1230度的HR-image Rb0.23WO3.00	74
圖4-44 圖片為燒結溫度1240度的HR-image Rb0.23WO3.00	75
圖4-45 圖片為燒結溫度1250度的HR-image Rb0.23WO3.00	75
圖4-46 圖片為燒結溫度1260度的HR-image Rb0.23WO3.00	76
圖4-47 圖片為燒結溫度1270度的HR-image Rb0.23WO3.00	76
圖4-48 圖片為燒結溫度1280度的HR-image Rb0.23WO3.00	77
圖4-49 圖片為燒結溫度1290度的HR-image Rb0.23WO3.00	77
圖4-50 圖片為燒結溫度1300度的HR-image Rb0.23WO3.00	78
圖4-51 圖片為降溫速率0.1oc/hr的HR-image Rb0.23WO3.00	78
圖4-52圖片為降溫速率1oc/hr的HR-image Rb0.23WO3.00	79
圖4-53 圖片為降溫速率10oc/hr的HR-image Rb0.23WO3.00	79
圖 4-54 (a) Conventional axial HRTEM image of a thin crystal of KxWO3 oriented along [0 0 1] showing the cation sites clearly resolved. ReO3 and HTB regions of the crystal are indicated and the K insertion tunnel sites are marked with arrows. (b) Phase of the specimen exit wavefunction restored from afocal series of images including (a) with all cation and anion sites clearly resolved.	80

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