臺灣博碩士論文加值系統

氧化鎢（WO3）是一種多功能無機金屬氧化物半導體材料，該材料具有良好的物理及化學性質，如氣敏、光催化、光致變色、電致變色等性能，在氣敏傳感器、光催化劑、電致變色智能窗和光電化學設備等領域都具有良好的應用前景。現今為止，多種物理及化學合成方法被用於氧化鎢的製備，如物理氣相沉積法、化學氣相沉積法、熱蒸發法、溶膠凝膠法、水熱法等。其中，水熱法具有操作簡單，反應條件易控制，可獲得多種特殊形貌的產物等優勢。而目前，水熱法製備氧化鎢粉體的常見形貌有：奈米顆粒、奈米棒、奈米線、奈米片等結構。本研究使用鎢酸鈉（Na2WO4·2H2O）作為原料，利用水熱合成法製備氧化鎢(WO3)粉體，在製程中加入多種表面活性劑，分別為十六烷基三甲基溴化銨（CTAB）、十二烷基硫酸鈉（SDS）、草酸。為了觀察表面活性劑對顆粒形狀、尺寸和相形成的影響，以XRD，SEM、Raman、FTIR和XPS等儀器來分析粉末之結晶型態、微觀結構、相變性質及特性。由SEM觀察粉體表面形貌發現本實驗所製備之氧化鎢粉體表面從無添加任何表面活性劑的片狀結構，到加入草酸時轉變為球狀結構，而顆粒大小從200 nm轉變為100 nm，厚度也由150 nm轉變至50 nm。實驗結果顯示，本實驗所製備之氧化鎢利用水熱合成法200℃加熱24小時後，經由X-ray繞射分析結果得到氧化鎢的相為monoclinic結構，與文獻結果一致。

Tungsten Oxide (WO3) is a multifunctional inorganic metal oxide semiconductor material with good physical and chemical properties such as gas sensing, photocatalysis, photochromism, electrochromism, etc. in gas sensors and photocatalysts. The fields of electrochromic smart windows and photoelectrochemical devices have good application prospects. Nowadays, various physical and chemical synthesis methods have been used for the preparation of tungsten oxide, such as physical vapor deposition, chemical vapor deposition, thermal evaporation, sol-gel, hydrothermal, and the like. Among them, the hydrothermal method has the advantages of simple operation, easy control of reaction conditions, and various products with special morphologies. At present, the common forms of preparation of tungsten oxide powder by hydrothermal method include: nano particles, nano rods, nanowires, nanosheets and the like. In this study, sodium tungstate (Na2WO4·2H2O) was used as a raw material to prepare tungsten oxide (WO3) powder by hydrothermal synthesis. Various surfactants were added in the process, which were cetyltrimethylammonium bromide ( CTAB), sodium dodecyl sulfate (SDS), oxalic acid. In order to observe the effect of surfactant on particle shape, size and phase formation, the crystal form, microstructure, phase transition properties and properties of the powder were analyzed by XRD, SEM, Raman, FTIR and XPS. The surface morphology of the powder was observed by SEM. It was found that the surface of the tungsten oxide powder prepared in this experiment changed from a sheet structure without any surfactant to a spherical structure when oxalic acid was added, and the particle size changed from 200 nm to 100. In nm, the thickness also changes from 150 nm to 50 nm. The experimental results show that the tungsten oxide prepared in this experiment is heated by hydrothermal synthesis at 200 ° C for 24 hours, and the phase of tungsten oxide is obtained as a monoclinic structure by X-ray diffraction analysis, which is consistent with the literature results.

致謝I
摘要II
目錄III
圖目錄VI
第一章緒論1
第二章文獻回顧與理論說明2
2.1氧化鎢2
2.1.1氧化鎢之晶體結構[15,16,17] 2
2.1.2氧化鎢之光催化性質5
2.1.3氧化鎢之氣體感測性質[29-31]6
2.2表面活性劑8
2.2.1表面活性劑之基本介紹8
2.2.2表面活性劑之分類[35]9
2.3製備氧化鎢的方式12
2.3.1溶膠凝膠法12
2.3.2水熱合成法12
2.3.3電沉積法13
2.3.4模板法14
2.4水熱合成法14
2.4.1水熱合成法之原理[43][44]14
2.4.2水熱合成法之分類15
2.4.3水熱合成法之機制16
2.4.4水熱合成法之優點[49]18
第三章實驗方法與步驟19
3.1實驗藥品器材19
3.2實驗設備21
3.3實驗流程圖22
3.4實驗步驟23
3.4.1溶液調配23
3.4.2均勻攪拌23
3.4.3水熱反應23
3.4.4清洗乾燥23
3.4.5檢測分析24
3.4.6實驗參數24
3.5儀器介紹.25
3.5.1場發射掃描式電子顯微鏡分析(FE-SEM)25
3.5.2晶體繞射分析(XRD)27
3.5.3拉曼光譜分析儀(Raman28
3.5.4化學分析電子光譜儀(ESCA)30
第四章結果與討論31
4.1 SEM分析31
4.1.1利用鎢酸鈉製備氧化鎢結構之影響31
4.1.2添加不同濃度CTAB對氧化鎢結構之影響32
4.1.3添加不同濃度SDS對氧化鎢結構之影響34
4.1.4添加不同濃度草酸對氧化鎢結構之影響36
4.2 XRD分析39
4.2.1添加不同濃度CTAB對氧化鎢之結構解析39
4.2.2添加不同濃度SDS對氧化鎢之結構解析40
4.2.3添加不同濃度草酸對氧化鎢之結構解析41
4.2拉曼光譜分析42
4.3XPS分析46
第五章結論52
第六章參考文獻53

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