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

鍾鎮鴻(Chen-hung Chung)

指導教授 ： 李光華

國立中央大學/理學院/化學系/碩士(2015年)

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。

關鍵字

水熱合成法

並列摘要

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.

並列關鍵字

Hydrothermal Synthesis

參考文獻

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