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    題名: 超臨界水熱法合成新型鈾矽酸鹽與鋇鋁硼酸鹽;Supercritical Hydrothermal Synthesis of New Compounds:Uranium Silicate and Barium Aluminum Borate
    作者: 彭淳琪;PENG, CHUN-CHI
    貢獻者: 化學學系
    關鍵詞: 超臨界水熱法;鈾矽酸鹽;鋇鋁硼酸鹽
    日期: 2017-07-21
    上傳時間: 2017-10-27 12:57:34 (UTC+8)
    出版者: 國立中央大學
    摘要: 本論文以超臨界水熱法合成兩個系列的化合物,A系列為鈾矽酸鹽化合物:Cs2[(UO2)(Si4O10)] (A1);B系列為鋇鋁硼酸鹽化合物:BaAlB4O8(OH) (B1)。藉由單晶X光繞射儀,解析出化合物的晶體結構,輔以粉末X光繞射圖比對理論圖,確定樣品純度以供後續分析。另外透過X光能量散布分析、光致放光光譜、紅外線光譜、熱重-示差掃描分析及固態核磁共振等方式進行定性及光學性質的分析。
    化合物 A1為淡黃色的針狀晶體,結構中的矽氧四面體以共角方式連接形成一維單鏈,每三條無分支的單鏈以共角形成無限延伸的多重鏈狀,其再與UO6雙四角錐連接,形成一個三維骨架結構。銫離子座落於八員環以及長方形的十二環中。依據SiO4的配位環境分類,A1 同時包含三種矽氧配位環境 Q2、Q3、Q4。
    化合物 B1 為中心對稱的透明片狀晶體,以AlO4¬¬四面體和BO3平面三角形、BO4四面體連接,形成二維層狀結構,而鋇離子分布於層與層之間。其基本建構單元由一個AlO4、一個BO4以及兩個BO3所組成,硼在此結構有兩種配位環境。經由紅外線光譜儀的測量,在3500 cm-1有一個非常強的訊號峰,進一步確認化合物B1結構中有OH基的存在。
    ;Two series of uranium silicate and barium aluminum borate were synthesized by the supercritical hydrothermal method. The crystal structures of the uranium silicate Cs2[(UO2)Si4O10] (A1) and the barium aluminum borate BaAlB4O¬8(OH) (B1) have been determined by single crystal X-ray diffraction. The purity of each compound was confirmed by the good agreement between observed powder X-ray pattern and the calculated pattern derived from the single-crystal X-ray diffraction data. These compounds were further characterized by EDS, PL, IR, TGA/DSC and solid state NMR spectroscopy.
    A1 is a cesium-containing uranium silicate. The silicate anions in the structure form multiple chains which are linked by UO6 tetragonal bipyramids to form three-dimensional framework. The multiple chain is observed for the first time and contains Q2 , Q3 and Q4 Si.
    The structure of B1 consists of the following distinct structural elements: two BO3 triangles, one BO3H group, one BO4 tetrahedron, one AlO4 tetrahedron, and one Ba atom. The borate cluster with the formula B4O8(OH) links by sharing three triangular vertices and one tetrahedral vertex with four AlO4 tetrahedra to form an aluminum borate layer in the ac plane. the Ba2+ cations between the layers. The presence of OH group in the structure was confirmed by IR spectroscopy.
    顯示於類別:[化學研究所] 博碩士論文

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