机构地区:[1]长春理工大学材料科学与工程学院,吉林长春130022
出 处:《光谱学与光谱分析》2009年第2期300-304,共5页Spectroscopy and Spectral Analysis
基 金:教育部科学技术研究重点项目(204038);吉林省教育厅科技计划项目(2006237)资助
摘 要:在室温下,以掺Yb3+的MCM-41作为主体,"热处理"后的Tb(aspirin)3phen作为发光客体,将其进行组装,通过XRD和N2-吸附脱附和IR对组装体的结构和物理性质进行了研究。利用激发和发射光谱分析了组装体的光致发光性能和主客体关系。采用了一种新型的掺杂方法"直接焙烧法",用以避免在试样合成中掺杂离子的损失。在Yb/MCM-41和Tb(aspirin)3phen-Yb/MCM-41的XRD谱图中同时在2θ=2.6时出现了(100)晶面衍射峰,表明试样为规则有序,六方结构的MCM-41材料。Tb(aspirin)3phen进入Yb/MCM-41孔道后,无机骨架的有序性进一步增加。相对于MCM-41,Yb/MCM-41在IR谱图中波数963cm-1的谱带减弱,表明Yb3+已经进入无机骨架。另外,波数1 384 cm-1的吸收谱带也能提供组装体Tb(as-pirin)3phen-MCM-41中成键的特征信息。PL测试结果表明,Tb(aspirin)3phen在240~375 nm区间的宽激发吸收分别归属于配体aspirin羰基n→π*跃迁,苯环π→π*跃迁和phen的杂菲基团吸收。对客体Tb(aspi-rin)3phen进行热处理,能增强Tb(aspirin)3phen在MCM-41孔道中的发光效率,并且当基质MCM-41硅骨架掺杂Yb3+后,组装体的发光强度进一步增强,当Yb/Si=7.579×10-3时,发光强度最高。Assembly system with MCM-41 doped with Yb^3+ as a host, and Tb(aspirin)3phen, which had been heat treated, as an active optical guest, was synthesized at room temperature. The structure and physical properties of the composites were characterized by a combination of different techniques such as XRD, N2 adsorption-desorption and IR, while the photoluminescence properties of the composites were analyzed by PL. Excitation and emission spectra were examined to explore the PL properties of the prepared samples and the relationship between the optical guest and the inorganic host. The present paper reports a new synthesis method called "Direct-Calcination" to avoid the loss of rare earth ions in the process of synthesis. Strong reflections at 2θ = 2. 6 attributed to (100) reflection were presented in XRD patterns of both Yb/MCM-41 and Tb(aspirin)3 phen-Yb/MCM-41, which always can be observed for regular, spherical structure of MCM-41 materials, and the inorganic framework order increased after Tb(aspirin)3 phen being incorporated into the channels of Yb/MCM-41. The intensity of the band at 963 cm^-1 decreased in IR spectrum of Yb/MCM-41, relative to that in IR spectrum of MCM-41, implying that Yb^3+ had been banded with the framwork. And a sharp band at i 384 cm^-1 in IR spectrum of Tb(aspirin)3 phen-Yb/MCM-41 also gives the characteristic information about the bands in Tb(aspirin)3 phen-MCM-41. The results from the characterization of PL show that the wide excitation band over 240-375 nm of Tb(aspirin)3 phen is assigned to the carbonyl group n→π^* transition absorption, benzene ring π→π^* transition absorption of aspirin, and phenanthrene absorption of phen. The luminescence intensity of Tb(aspirin)3 phen incorporated into the channels of MCM-41 can be enhanced by heat treating in the synthesis process of Tb(aspirin)3 phen, while the intensity also can further increases by doping Yb3+ in the silicon framework of MCM-41. The luminescence intensity of the assembl
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