氟化磷酸铟的合成与表征(英文)  

Synthesis and characterization of fluorinated indium phosphate

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作  者:李兴亮[1,2] 苏哲[2] 李首建[2] 

机构地区:[1]中国工程物理研究院核物理与化学研究所,绵阳621900 [2]四川大学化学学院,成都610064

出  处:《中国科学院研究生院学报》2009年第3期310-318,共9页Journal of the Graduate School of the Chinese Academy of Sciences

基  金:supported by National Natural Science Foundation of China(20571053)

摘  要:以尿素与氯化胆碱的低共熔点液体同时兼做溶剂和模板传递剂,在离子热体系下合成了InF2[PO3(OH)]2(NH4)3.采用同样的低共熔点液体在水热条件下不能得到相同的产物.产物晶体参数如下:C2/c(No.15)空间群,a=13.799(3)°A,b=5.091(2)°A,c=16.094(3)°A,β=112.942(16)°,V=1041.2(5)A°3andZ=4;R1=0.0582,wR2=0.1589.在产物结构中,In八面体与P四面体形成四员环,顶角相连形成链状结构.客体铵分子填充于链与链间的空穴中,通过氢键与骨架中的F原子,POH和P O基团作用,链与链间靠范德华力吸引进而形成层状结构.产物进一步通过粉末XR,EDX,IR,XPS和TG/DTA进行表征.A. fluorinated indiumphosphate, InF2 [ PO3 ( OH)]2 ( NH4 )3, has been prepared under ionothermal condition using deep-eutectic solvents of choline chloride and urea as solvent and templatedelivery agents. The same material can not be observed with the presence of the same deep-eutectie mixture under normal hydrothermal process. The compound crystallized in the monoclinic system, space group C2/c (No. 15)with cell parameters a = 13.799(3)A^°, b = 5.091(2)A^°, c = 16.094(3)A^°,β= 112. 942(16) °, V = 1041.2 (5) A^°^3 and Z = 4 ; the final residual faetors were R1 = 0.0582 and wR2 = 0.1589. The strueture is built from an infinite chain composed of interconnected 4-member ring with formula of InF2 [PO3 (OH)]2^3- . The guest ammonium are hydrogen bonded to the F atoms loeated in two outmost vertexes of indium octahedral and terminal P=OH and P=O groups in the chain respectively. The integrated framework is formed by van der Waals forces holding the chains together as extensive H bond array exists in the compound. The further characterizations of the compound have been performed by X-ray powder diffraction, EDX, IR, XPS and TG/DTA analyses.

关 键 词:低共熔点液体 离子热合成 氟化磷酸铟 

分 类 号:TQ031.2[化学工程]

 

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