低温固相反应合成苯乙酸稀土配合物及铕(Ⅲ)、铽(Ⅲ)的发光性能  

Synthesis of Phenylacetic Acid Rare Earth Complexes at Low Temperature Solid State Reaction and Luminescence Property of Eu^(3+),Tb^(3+) Complexes

作　　者：李文先[1] 张瑞平[1] 郭磊[1] 夏海庭[1] 陈丽娟[1] 赵永亮[1] 

机构地区：[1]内蒙古大学化学化工学院,内蒙古呼和浩特010021

出　　处：《发光学报》2007年第2期207-213,共7页Chinese Journal of Luminescence

基　　金：国家自然科学基金(20461002);内蒙古大学"513"二层次人才基金(ND205150);内蒙古教育厅科研基金(NJ06047)资助项目

摘　　要：采用低温固相反应合成了4种苯乙酸稀土配合物:RE(L)3.nH2O(n=0.5～1.5;RE=La,Nd,Eu,Tb;L=C6H5CH2COO-),经元素分析、稀土络合滴定、摩尔电导及热重分析确定了配合物的组成,测定了配体及配合物的IR谱、1HNMR及配体的磷光光谱和铕、铽配合物荧光激发和发射光谱。根据磷光发射光谱数据计算了配体的三重态平均能级值。铕(Ⅲ)、铽(Ⅲ)配合物的荧光光谱和配体的磷光光谱表明,配体仅对铽(Ⅲ)的荧光具有一定的敏化作用。对镧配合物进行了扫描电镜形貌分析,发现苯乙酸镧为球状空穴结构,粒径在十几微米到几十微米。The most characteristic of solid state reaction at low temperature is that reaction is in progress at room temperature or near room temperature. Compare with liquid state reaction, solid state reaction is high selection and high yield. Because solid state reaction don＇t need solvent, and this is environtly friendly, so it is a green synthesis method. A lot of people are interested in it recently. We have synthesized four solid complexes of rare earth with phenylacetic acid （L） by method of solid state reaction at low temperature. Elemental analysis, rare earth coordination titration, Molar conductivity studies suggest that the composition of the complexes is RE （ L ） 3 · nH2O （ n = 0. 5 - 1.5 ;RE = La, Nd, Eu, Tb L = C6H5CH2COO^-）. TGA curve of La^3＋ complex began to lose weight at 65.41 -86.03℃ and weight loss was 1. 835%,which was good accordance with the theoretical data 1. 628% when complex had 0.5 water molecular. The temperature of losing water was lower, so water is induced to be crystal water. At 345.78 - 376.52 ℃ there is a great lose weight which was caused by the decomposition of La^3＋ complex. The IR spectra of sodium salt of the ligand show bands at 1 571 cm^-1（s） and 1 386 cm^-1（s） ,assigned to carboxyl group＇s antisymmerty stretch vibration vas （COO^-） and symmetry stretch vibration vs （COO^-）. In addition, the band at 3 026,1 491,706 cm^-1 are individaully assigned to phenyl＇s vC-H ,vC-C ,δC-H vibration. The IR spectra of complexes shows bands at nearby 1 546 - 1 553 cm^-1（s） assigned to vas（COO^- ） with a shift of 18 -25 cm^-1 to the lower frequency region ,which compared with sodium salt of ligand; The band at nearby 1 393 - 1 403 cm^-1 （s） is assigned to vs （ COO^- ） with a shift of 7 - 17 cm^-1 to the higher frequency region, which still compared with sodium salt of ligand. These results indicate that the carboxyl group is bonded to the metal ions through two oxygen atoms as a symmetrical chelating bidentate group. The ^1H NMR of

关 键 词：稀土配合物 苯乙酸 低温固相反应 发光 形貌分析 

分 类 号：O614.33[理学—无机化学] O482.31[理学—化学]