University of Lyon1, Institut Lumière Matière, UMR5306 CNRS, Bâtiment Kastler, 10 rue Ada Byron, 69622 Villeurbanne, France.
Dalton Trans. 2013 Sep 21;42(35):12633-43. doi: 10.1039/c3dt50605c.
A series of anhydrous cerium(III) trifluoroacetate complexes with neutral O-donor ligands, namely Ce2(OAc)(TFA)5(DMF)3 (1), Ce(TFA)3(L)x [x = 2, L = THF (2), DMF (3), DMSO (4); x = 1, L = diglyme (5)] and Ce2(TFA)6(DMSO)x(DMF)y [x = 6, y = 0 (6); x = 4, y = 2 (7)] (where OAc = acetate, TFA = trifluoroacetate, THF = tetrahydrofuran, DMF = dimethylformamide, DMSO = dimethylsulphoxide, and diglyme = MeO(C2H4O)2Me] were synthesized and completely characterized by elemental analysis, FT-IR spectroscopy and TG-DTA-MS studies. A partially hydrated complex [Ce(TFA)3(diglyme)(H2O)] (8) was obtained by slow evaporation of the THF solution of anhydrous 5 in the air. The single crystal X-ray diffraction analysis of 1, 3, 4, and 6–8 showed the versatile bonding mode of the TFA ligand (terminal, chelating and bridging). These complexes, on decomposition in 1-octadecene in inert atmosphere, gave CeF3 nanoparticles of 8–11 nm size. The complex 5 proved to be the best precursor in the series because of the ability of the diglyme ligand to act as capping reagent during decomposition to render the CeF3 particles monodisperse in organic solvents. The obtained CeF3 nanoparticles were characterized by FT-IR, EDX analysis and TEM studies and their luminescence and scintillation responses under UV and X-ray excitation were studied and compared with that of CeF3 single crystal.
一系列无水铈(III)三氟乙酸盐配合物与中性 O-供体配体,即 Ce2(OAc)(TFA)5(DMF)3 (1)、Ce(TFA)3(L)x [x = 2, L = THF (2)、DMF (3)、DMSO (4);x = 1, L = 二甘醇 (5)] 和 Ce2(TFA)6(DMSO)x(DMF)y [x = 6, y = 0 (6);x = 4, y = 2 (7)](其中 OAc = 醋酸盐,TFA = 三氟乙酸盐,THF = 四氢呋喃,DMF = 二甲基甲酰胺,DMSO = 二甲亚砜,和 二甘醇 = MeO(C2H4O)2Me] 通过元素分析、FT-IR 光谱和 TG-DTA-MS 研究合成并完全表征。通过在空气中缓慢蒸发无水 5 的 THF 溶液获得部分水合配合物 [Ce(TFA)3(diglyme)(H2O)] (8)。1、3、4 和 6-8 的单晶 X 射线衍射分析表明 TFA 配体具有多种键合模式(末端、螯合和桥接)。这些配合物在惰性气氛下在 1-十八烯中分解,得到 8-11nm 尺寸的 CeF3 纳米粒子。该配合物 5 是该系列中最好的前体,因为二甘醇配体在分解过程中能够作为封端试剂,使 CeF3 颗粒在有机溶剂中呈单分散状态。所得 CeF3 纳米粒子通过 FT-IR、EDX 分析和 TEM 研究进行了表征,并研究了它们在紫外和 X 射线激发下的发光和闪烁响应,并与 CeF3 单晶进行了比较。