轻希土硫氰酸盐与2,3,11,12,-四苯基-1,4,7,10,13,16-六氧-2,11-十八环二烯配合物的合成及XPS研究

SYNTHESIS AND XPS SATELLITE PHENOMENA OF COMPLEXES OF THE LIGHT RARE EARTH ISOTHIOCYANATE NATE WITH2,3,11,12-TETRAPHENYL-1,4,7,10,13,16-HEXAOXA-2,11-CYCLOOCTADECADIENE

合成了六种轻希土硫氰酸盐与标题不饱和冠醚的新固体配合物,进行了元素分析,摩尔电导率、DTA、UV、IR和XPS等表征。对Ln(NCS)_3·L和Ln(NCS)_3的XPS研究中,得到它们组成原子芯能级电子(Ln3d_(5/2),Ols,Nls,S2p)的结合能信息;观察到除Y3d_(5/2)外Ln3d_(5/2)(Ln=La、Ce、Pr、Nd、和Sm)的伴峰结构,Ln3d_(5/2)结合能与原子序数呈线性关系,并推断类似化合物Pm3d_(5/2)结合能在1035eV附近.

Six new complexes of the titled unsaturated crown ether (L) with the light rare earth (Ⅲ) isothiocyanate have been synthesized in the mixed solvent. These complexes were characterized by elemental analyses, molar conductance, UV, IR and DTA. The core-electron (Ln 3d5/2, Ols, Nlsand S2p) of the new complexes and Ln(NCS)3(Ln = La, Ce, Pr, Nd, Sm and Y) has been studied by X-ray photoelectron spectra. Except for Y, the satellite phenomena have been observed for Ln3d5/2 signals in rare earth isothiocyanate and its complexes. The binding energies (BE) of the Ln3rf5/2 peaks increase with an increase in the atomic number of the rare earth element. The relationship between the BE of Ln3d5/2 peaks for the complexes I-V and Ln(NCS)3 and their atomic number is an inclined line. We are to infer from the inclined line that the BE of Pm 3d5/2 Pcak will be about 1035eV.