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Synthesis and Characterization of Mesoporous Europium (Ⅲ) Silicate Molecular Sieves

Synthesis and Characterization of Mesoporous Europium (Ⅲ) Silicate Molecular Sieves
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摘要 The luminescent nanosized Eu-MCM (1:10) was synthesized by means of sol-gel-assisted self-assembly under basic conditions at room temperature. The results of ^29Si-MAS NMR show that the peaks are Q^4, Q^3, Q^2[ (SiO)4-mSi - (OH)m(m=0, 1, 2), at -δ111, -δ103, -δ90], and q^3, q^2, q^1, q^0[(SiO)4-nSi-(O-Eu)n(n=1, 2, 3, 4), at - δ83, - δ72, - δ55, - δ47]. The result proves Eu^3+ doped Si - O framework. The HRTEM image shows that the regular uniform nanoparticles with a diameter of 15 nm possess large pore with Ф8 nm, which is consistent with the result of N2 adsorption. The patterns of selected-area electron diffraction, XRD, and pore-size distribution plot of Eu-MCM ( 1 : 10) show that the sample of Eu-MCM ( 1 : 10) possesses the both of crystal and amorphous phases. The FT IR results indicate that the peaks near 970 cm^-1 are assigned to the deformation vibration of silanol group. The as-product was calcined at 800 ℃ and the mesoporous material possesses enormous specific areas and large pores, which shows that the mesoporous material is ultrastable. The luminescent nanosized Eu-MCM (1:10) was synthesized by means of sol-gel-assisted self-assembly under basic conditions at room temperature. The results of ^29Si-MAS NMR show that the peaks are Q^4, Q^3, Q^2[ (SiO)4-mSi - (OH)m(m=0, 1, 2), at -δ111, -δ103, -δ90], and q^3, q^2, q^1, q^0[(SiO)4-nSi-(O-Eu)n(n=1, 2, 3, 4), at - δ83, - δ72, - δ55, - δ47]. The result proves Eu^3+ doped Si - O framework. The HRTEM image shows that the regular uniform nanoparticles with a diameter of 15 nm possess large pore with Ф8 nm, which is consistent with the result of N2 adsorption. The patterns of selected-area electron diffraction, XRD, and pore-size distribution plot of Eu-MCM ( 1 : 10) show that the sample of Eu-MCM ( 1 : 10) possesses the both of crystal and amorphous phases. The FT IR results indicate that the peaks near 970 cm^-1 are assigned to the deformation vibration of silanol group. The as-product was calcined at 800 ℃ and the mesoporous material possesses enormous specific areas and large pores, which shows that the mesoporous material is ultrastable.
作者 尹伟
机构地区 Department ofChemistry
出处 《Journal of Rare Earths》 SCIE EI CAS CSCD 2005年第4期411-415,共5页 稀土学报(英文版)
基金 Project supported by Appropriative Research Fund for Professor and Doctor , Guangdong Institute of Education (ARF0406)
关键词 Eu-MCM LUMINESCENCE HRTEM FT IR ^29Si-MAS NMR rare earths Eu-MCM luminescence HRTEM FT IR ^29Si-MAS NMR rare earths
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