助熔劑法合成鹼土金屬硼酸鹽及其結構研究;Flux Syntheses and Characterization of Alkaline Earth Metal Borates

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题名:	助熔劑法合成鹼土金屬硼酸鹽及其結構研究;Flux Syntheses and Characterization of Alkaline Earth Metal Borates
作者:	呂歡軒;Lu, Huan-Xuan
贡献者:	化學學系
关键词:	化學;熔鹽法合成;新穎結構;鉍化合物;硼酸鹽;結構鑑定
日期:	2022-07-26
上传时间:	2022-10-04 10:58:54 (UTC+8)
出版者:	國立中央大學
摘要:	本論文利用助熔劑法和密閉系統下熔鹽法分別成功合成出兩個新穎鹼土金屬硼酸鹽氧化物 Sr11Bi2B20O44 (A)，Ba4B11O19(OH)3 (B)兩化合物皆由單晶 X 光繞射方法，鑑定出化合物的晶體結構，再以粉末繞射分析比對確定樣品純度，並利用 EDS 元素分析儀和固態核磁共振儀確定化合物 A 元素組成以及其配位環境。化合物 A 為透明片狀晶體，空間群屬於 R-3c 為中心對稱，晶胞參數為 a = b = 9.501(1)Å , c = 67.899(9) Å , α=β= 90°,γ= 120° , 化合物 Sr11Bi2B20O44具有極長的 c 軸且為二維雙層狀(Double-layer)結構，雙層內和雙層彼此間有 Sr2+ 陽離子穩定結構，每層由無限的共角 BO4 四面體和 BO3 三角形組成而以 Bi3+ 陽離子連接而形成此雙層結構。化合物 B 空間群為 P21/n 中心對稱，晶胞參數為 a = 6.639(1)Å ，b = 30.497(6)Å , c = 8.756(6) Å ,β= 90.768°, 化合物 B 晶體結構可將其分為為 FBB 1 2Δ3 □：<Δ2□>-<Δ2□> 和 FBB 2 2Δ4□：<Δ2□>-<3□>Δ，FBB 1 形成之含九圓環的中心硼酸鹽片且與 FBB 2 所形成的單鏈以共角方式連接，Ba 陽離子坐落在 FBB1 與 FBB2 所形成之環狀通道穩定結構，而論文中也將比較化合物 B 與相似化合物 [Ba3Pb(H2O)][B11O19(OH)3] 晶體結構之間的差異。;Two new compounds, Sr11Bi2B20O44 (A) and Ba4B11O19(OH)3 (B), were synthesized by flux growth methods in an open air platinum crucible and in a sealed gold ampoule,respectively. Both compounds were structurally determined by single-crystal X-ray diffraction, The purity of each prouduct was confirmed by powder X-ray diffraction. Compound A was further characterized by EDS and solid-state NMR spectroscopy. Compound A crystallizes as a transparent lamellar plate in the space group R-3c with a = 9.501(1), b = 9.501(1), c = 67.899(9) Å , V = 5308.20(13) Å 3, and Z = 2. The structure consists of six double layers and each layer is built from B3O9 units which were connected with six BO3 triangles by sharing corners. The BO3 triangles are connected with each other via one BO4 tetrahedron and the other BO3 triangles are connected to an adjacent layer via Bi3+ cations to form a double layer. The Sr3+ cations are located in both the intralayer and interlayer regions. The space group of compound B is P21/n with a = 6.639(1) Å , b = 30.497(6) Å , c = 8.756(6) Å , andβ = 90.768°. The crystal structure of compound B consists of the fundamental building block 1 (FBB 1) 2Δ3□: <Δ2□>-<Δ2□> and the FBB 2 2Δ4□: <Δ2□>-<3□>Δ. The central borate sheet contains nine-membered rings formed by FBB 1 which are connected with chains of FBB 2 by sharing corners. The Ba2+ cations are situated in the cyclic channel formed by FBB1 and FBB2. The structure of compound B is compared with that of [Ba3Pb(H2O)][B11O19(OH)3].
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