水熱合成鋅釩磷酸鹽及其結構與性質研究;Hydrothermal Synthesis, Crystal Structures and Properties of Zinc Vanadium Phosphates

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题名:	水熱合成鋅釩磷酸鹽及其結構與性質研究;Hydrothermal Synthesis, Crystal Structures and Properties of Zinc Vanadium Phosphates
作者:	鍾鎮鴻;Chung,Chen-hung
贡献者:	化學學系
关键词:	水熱合成法;Hydrothermal Synthesis
日期:	2015-07-30
上传时间:	2015-09-23 10:51:03 (UTC+8)
出版者:	國立中央大學
摘要:	本論文利用中溫水熱合成法合成出兩個鋅釩磷酸鹽的化合物 Zn(VO)2(PO4)2(H2O)4 (A1)以及[(VVO)(VIVO)3Zn2(OH)(PO4)4(H2O)7]‧ H2O (A2)。以上化合物均能獲得單晶產物，利用單晶X 光繞射方法收集數據後進行結構解析，並以粉末X 光圖譜與理論圖譜做比對以確定樣品純度後，用X 光光電子能譜儀測量A2 之釩金屬價數及熱重分析儀(TGA)來分析A2 的水分子裂解現象，最後使用超導量子干涉磁量儀(SQUID)分別來量測A1 及A2 磁性現象。在反應條件中，A1 與A2 的起始物比例完全相同，而卻在不同的反應溫度及恆溫時間下可以得到兩種不同的產物，其中A1 為純V(IV) 產物，而A2 為V(IV)以及V(V)的混價化合物，推測可能跟所加入的還原劑鋅粒的反應程度有很大的關係。;Two Zinc Vanadium Phosphates, Zn(VO)2(PO4)2(H2O)4 (A1) and [(VVO)(VIVO)3Zn2(OH)(PO4)4(H2O)7]‧H2O (A2), were synthesized under mild hydrothermal conditions. Both of these two structures were determined by single-crystal X-ray diffraction. The purity of each compound was confirmed by powder X-ray diffraction. These compounds were further characterized by TGA, SQUID, XPS. The reaction agent ratio of A1 and A2 are same, but reaction temperature are different, A1 is a Vanadium(IV) compound, A2 is a mixed-valance compound, the reducing agent zinc maybe play a big role in this reactions to show this results. Magnetic Susceptibility also can proof A2 is a mixed-valance vanadium compound. A1 crystal data: Zn(VO)2(PO4)2(H2O)4, tetragonal, I4/m(No. 87), a = 6.2518(2) Å, c = 13.4642(6) Å, V = 526.25(3) Å3, Z = 2, R1 = 0.0481 and wR2 = 0.1144. A2 crystal data: [(VVO)(VIVO)3Zn2(OH)(PO4)4(H2O)7]‧H2O, monoclinic, I4/m(No. 87), a = 12.6432(6) Å, b = 12.6408(6) Å, c = 13.5881(6) Å, =108.627(2)°, V = 2057.90(17) Å3, Z = 4, R1 = 0.0202 and wR2 = 0.0570.
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