混合鹼/鹼土金屬硼酸鹽與鈦矽酸鹽的合成及結構與性質研究;Synthesis, Structures and Properties of mixed Alkali-Alkaline Earth Borates and a Titanium Silicate

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题名:	混合鹼/鹼土金屬硼酸鹽與鈦矽酸鹽的合成及結構與性質研究;Synthesis, Structures and Properties of mixed Alkali-Alkaline Earth Borates and a Titanium Silicate
作者:	蔡承恩;Tsai, Cheng-En
贡献者:	化學學系
关键词:	助熔劑長晶法;單晶;硼酸鹽;鈦矽酸鹽;Flux growth method;Single crystal;Borate;Titanium silicate
日期:	2018-01-17
上传时间:	2018-04-13 10:49:19 (UTC+8)
出版者:	國立中央大學
摘要:	本論文以高溫溶液反應法以及助熔劑長晶法合成兩個系列之化合物，第一系列為硼酸鹽 K2BaB10O17∙3.5H2O (A1)、K2.8Ba1.2B10O17Cl1.2 (A2)、K5Ba2B20O34Cl (A3)、(Ba3F)B10O17F (A4)；第二系列為鹼金屬鈦矽酸鹽Cs17(Ti4O7F)[(Ti10O17)(Si2O7)4] (B1)。兩系列皆利用單晶X光繞射方法鑑定出化合物的晶體結構，並以粉末 X 光繞射儀鑑定化合物純度，再以分散式 X 光光譜儀、熱重/示差掃描熱分析以及固態核磁共振等方法進行鑑定。 A 系列化合物皆為雙層結構，結構中都具有雙六圓環的硼氧單元並有相似之基礎結構單元。結構中 A1、A2、A3 都具有鉀鋇原子混合於同一位置之特性，依據分散式 X 光光譜儀證實其元素莫爾比以及結構中氯元素的存在，層中可發現陰陽離子的種類與數量影響著雙層中內層的連接與排列模式，且雙層的結構型貌皆呈現平整或波浪狀。而化合物 A4 則是具有 [BO3F] 單元且 B-F 鍵於結構中屬於懸浮鍵，使得雙層結構呈現鋸齒狀。化合物 B1 為三維骨架結構，結構中的鈦原子全是以五配位的模式且幾乎為具有懸浮鍵之單元，其中包含一個全新的 [Ti10O33] 啞鈴狀單元，此單元利用四個 Q1 形式的 [Si2O7] 單元相互連接並形成籠狀結構，使得籠狀結構內部的銫離子出現獨特的四配位平面四邊形。結構中的氟原子則是以鈦元素之間的橋梁存在於 [Ti2O7F] 單元中。 ;Two series of borates and titanium silicate were synthesized by the high temperature solution reaction, flux growth method and solid-state reaction. Series A denotes borate, K2BaB10O17∙3.5H2O (A1), K2.8Ba1.2B10O17Cl1.2 (A2), K5Ba2B20O34Cl (A3), (Ba3F)B10O17F (A4), Series B denotes titanium silicate Cs17(Ti4O7F)[(Ti10O17)(Si2O7)4] (B1). The stuctures of all compounds were determined by single-crystal X-ray diffraction and confirmed by the good agreement between calculated and observed powder X-ray diffraction patterm. The properties of each compound were further characterized by EDS, IR, TGA/DSC and solid-state NMR. The structures of all series A compounds are double-layered structure and have the similar fundamental building units contained double hexagonal rings. A1, A2, A3 are mixed alkali and alkaline-earth borate which potassium and barium atoms have the same occupancy. The shapes of double-layered structure are smooth or wavy determined by types of inner layer atoms. In A4, the shape of double-layered structure is serrated which contains [BO3F] tetragonal units with B-F dangling bondings. B1 have 3-D framework structure containing new titanium oxide cluster [Ti10O33] with dumbbell shape. Part of cesium ions which locate in the center of the cage build by two [Ti10O33] clusters and four Q1-Si [Si2O7] units have unique square planar geometry in four-coordinate position. All of the titanium atoms connect with five oxygen or fluorine atoms to form square pyramid units and almost have dangling bondings. Fluorine atoms connect with two titanium atoms as bridges to form [Ti2O7F] units.
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