de Jesús Morales Ramírez Angel, Murillo Antonieta García, de Jesús Carrillo Romo Felipe, Hernández Margarita García, Palmerin Joel Moreno, Guerrero Rosario Ruiz
Instituto Politécnico Nacional, CIITEC IPN, Cerrada de Cecati S/N. Col. Santa Catarina, Azcapotzalco Mexico D.F. C.P. 02250, Mexico; E-Mails:
Int J Mol Sci. 2011;12(9):6240-54. doi: 10.3390/ijms12096240. Epub 2011 Sep 23.
Nanocrystalline Eu(3+), Tb(3+) co-doped Lu(2)O(3) powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O(2) atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu(2)O(3) nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu(3+) dopant (5 mol%), Tb(3+) codoped Lu(2)O(3) exhibited a typical red emission at 611 nm (D(°)→(7)F(2)), furthermore, the effect of Tb(3+) molar content (0.01, 0.015 and 0.02% mol) on the Eu(3+) radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb(3+) content.
采用溶胶 - 凝胶法,以硝酸镥、硝酸铕和硝酸铽为前驱体,乙醇为溶剂,制备了最大尺寸为25.5 nm的纳米晶Eu(3 +)、Tb(3 +)共掺杂Lu(2)O(3)粉末。利用差示热分析(DTA)和红外光谱(IR)研究干凝胶退火过程中的化学变化。在100℃蒸发溶胶后,将形成的凝胶在富氧气氛下于300至900℃退火30分钟,并用X射线衍射(XRD)对所得产物进行分析,以表征微观结构行为并确认晶体结构。结果表明,Lu(2)O(3)纳米粉末在400℃开始结晶,且微晶尺寸随退火温度升高而增大。对在700℃和900℃退火的样品进行了透射电子显微镜(TEM)研究,以分析微晶的微观结构和尺寸。最后,关于闪烁性能,Eu(3 +)掺杂剂(5 mol%)、Tb(3 +)共掺杂的Lu(2)O(3)在611 nm处呈现典型的红色发射(D(°)→(7)F(2)),此外,分析了Tb(3 +)摩尔含量(0.01、0.015和0.02% mol)对Eu(3 +)辐射发光的影响,发现发射强度越高,Tb(3 +)含量越低。