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(MCM-41)-La_2O_3纳米复合材料的制备、表征及光学性质
引用本文:赵紫军,翟庆洲,邹明强.(MCM-41)-La_2O_3纳米复合材料的制备、表征及光学性质[J].无机化学学报,2010,26(10):1776-1783.
作者姓名:赵紫军  翟庆洲  邹明强
作者单位:1. 长春理工大学纳米技术研究中心,长春,130022
2. 中国检验检疫科学研究院,北京,100123
摘    要:借助水热法,以正硅酸乙酯为硅源,十六烷基三甲基溴化铵为模板剂,在碱性条件下制备了纳米MCM-41分子筛。通过固相热扩散法将La2O3组装到MCM-41介孔孔道中,制备出含La2O3不同浓度的(MCM-41)-La2O3主-客体纳米复合材料。采用化学分析、粉末XRD、FTIR、77K低温N2吸附-解吸附、固体扩散漫反射吸收光谱、拉曼光谱、扫描电镜和发光光谱对主-客体复合材料进行表征。粉末XRD结果表明,La2O3组装到MCM-41分子筛的孔道后并未破坏分子筛骨架,在所制备的(MCM-41)-La2O3主-客体纳米复合材料中MCM-41骨架结构仍然具有较高的有序性,并且,随着植入客体材料浓度的增加复合材料的有序度有所降低。红外光谱表明所制备的纳米复合材料主体分子筛骨架完好;低温氮气吸附-解吸附技术表明La2O3已经部分地占据了MCM-41分子筛孔道,导致分子筛的比表面积和孔体积都有所降低;固体扩散漫反射吸收光谱表明吸收光谱的吸收峰发生了蓝移现象,并表现出量子限域效应,说明La2O3已经组装到了MCM-41分子筛的孔道中;拉曼光谱表明所制备的复合材料没有出现新的特征峰,表明La2O3已经组装到了MCM-41分子筛的孔道中;扫描电镜表明(MCM-41)-La2O3样品的外观非常规整,主要呈现的是球状结构,La2O3含量为10%时,(MCM-41)-La2O3的平均粒径为(114±10)nm。发光光谱研究结果表明,所制备的复合材料(MCM-41)-La2O3样品在396nm处具有较好的发光性质,因而具有作为发光材料潜在应用前景。

关 键 词:纳米复合材料    纳米MCM-41分子筛    La2O3    固相热扩散法    发光

Preparation, Characterization and Optical Properties of (MCM-41)-La2O3 Nanocomposite Material
ZHAO Zi-Jun,ZHAI Qing-Zhou and ZOU Ming-Qiang.Preparation, Characterization and Optical Properties of (MCM-41)-La2O3 Nanocomposite Material[J].Chinese Journal of Inorganic Chemistry,2010,26(10):1776-1783.
Authors:ZHAO Zi-Jun  ZHAI Qing-Zhou and ZOU Ming-Qiang
Affiliation:Research Center for Nanotechnology, Changchun University of Science and Technology, Changchun 130022,Research Center for Nanotechnology, Changchun University of Science and Technology, Changchun 130022 and Chinese Academy of Inspection and Quarantine, Beijing 100023
Abstract:Nanoscale MCM-41 molecular sieve was prepared in alkaline medium by hydrothermal method using cetyltrimethylammonium bromide as template, tetraethoxysilane as silica resource. La2O3 was incorporated into the mesoporous channels of the MCM-41 molecular sieve by solid phase thermal diffusion method. The (MCM-41)-La2O3 nanocomposite materials with different concentrations were prepared. By means of chemical analysis, powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), low temperature nitrogen adsorption-desorption technique at 77 K, solid state diffuse reflection absorption spectroscopy, Ramam spectroscopy, scanning electronic microscopy (SEM) and luminescence spectra, the host-guest nanocomposites materials were characterized. Powder XRD results showed that after La2O3 was encapsulated into the channels of the molecular sieve, the frameworks of the prepared materials were not destroyed. The framework structures of the MCM-41 still had high ordered property in the prepared (MCM-41)-La2O3 host-guest nanocomposite materials. As the increase in the concentration of the embedded guest material, the degree of order of the composite materials decreased. Infrared spectra showed that the host molecular sieve frameworks of the prepared nanocomposite materials were intact. The low-temperature nitrogen adsorption -desorption technique indicated that the La2O3 has been partially occupied the pores of the MCM-41 molecular sieve, which resulted in the decrese in surface area and pore volume of the molecular sieve. The solid state diffuse reflection absorption spectra showed that for the absorption peaks of absorption spectra blue shift phenomena took place and the quantum confinement effect exhibited. It indicated that La2O3 has been encapsulated in the pores of the MCM-41 molecular sieve. Raman spectra showed that for the prepared composite materials no new characteristic peak appeared, showing La2O3 has been encapsulated into the channels of the MCM-41 molecular sieve. SEM showed that the appearance of the (MCM-41)-La2O3 sample was very orderly and the mainly presented form was globular structure. When the content of La2O3 was 10%, the average particle diameter of the (MCM-41)-La2O3 was (114±10) nm. The research results of luminous spectra showed that the (MCM-41)-La2O3 sample prepared has good luminous properties at 396 nm. Thus, the (MCM-41)-La2O3 have the potential foreground as luminous material.
Keywords:nanocomposite material  nanoscale MCM-41 molecular sieve  lanthanum oxide  solid phase thermal diffusion method  luminescence
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