高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (7): 1610.

• 研究论文 • 上一篇    下一篇

溶胶-凝胶法载银SiO2杂化材料的红外光谱和热分析

杨靖,侯海云   

  1. 西安工程大学环境与化学工程学院, 西安 710048
  • 收稿日期:2010-07-15 修回日期:2010-10-19 出版日期:2011-07-10 发布日期:2011-06-02
  • 通讯作者: 杨靖 E-mail:hao2560@163.com
  • 基金资助:

    陕西省教育厅自然科学专项基金(批准号:   09JK466)和西安工程大学博士科研启动基金(批准号:   BS1006)资助.

FTIR and Thermal Αnalysis  of Silver-doped Hybrid Silica Material by Sol-gel Method

YANG Jing*, HOU Hai-Yun   

  1. School of Environmental & Chemistry Engineering, Xi'an Polytechnic University, Xi'an 710048, China
  • Received:2010-07-15 Revised:2010-10-19 Online:2011-07-10 Published:2011-06-02
  • Contact: Jing Yang E-mail:hao2560@163.com
  • Supported by:

    陕西省教育厅自然科学专项基金(批准号:   09JK466)和西安工程大学博士科研启动基金(批准号:   BS1006)资助.

摘要: 采用溶胶-凝胶法,在甲基化改性SiO2溶胶中掺杂硝酸银,制备Ag/MTES-SiO2杂化材料。通过XRD、红外光谱和TG-DTG分析,考察Ag/MTES-SiO2杂化材料的热稳定性,利用Coast-Redfern积分法和Achar微分法相结合的方法,求算Ag/MTES-SiO2杂化材料在热分解过程中各阶段的活化能和指前因子。结果表明:Ag/MTES-SiO2杂化材料经120℃以上焙烧后,样品中即出现了纳米金属Ag粒子,这些金属Ag为AgNO3还原所得。随着焙烧温度的升高,Ag粒子的衍射峰强度和SiO2颗粒结晶的趋势增加。当焙烧温度达到600 ℃时,Si-CH3基团完全消失,当焙烧温度增至750℃时,残余C-H基团完全无机化。金属银的摻杂并未对样品中-CH3基的热稳定性产生明显影响。在N2气氛中,Ag/MTES-SiO2杂化材料中-CH3的无机化历程经历了4个阶段,各阶段具有不同的热分解动力学机理函数,其活化能分别为71.92、125.78、235.73和417.37 kJ?mol?1,指前因子分别为1.18×109、7.14×1010、8.35×1013和1.16×1020 s?1。

关键词: 载银, 杂化材料, 红外光谱;热稳定性;热分析动力学

Abstract: Ag/MTES-SiO2 hybrid material was prepared by sol-gel method, in which AgNO3 was added into methyl-modified silica sol. According to XRD, FTIR spectra and TG-DTG analysis, the thermal stability of Ag/MTES-SiO2 hybrid material was discussed. The activation energies and frequency factors were figured out by using Coast-Redfern intergral method and Αchar differential method. The results show that, metallic nano-silver peaks can be clearly found in the silica materials calcined above 120°C. The metallic silver results from the reduction of AgNO3. The Si?CH3 vibrational bands disappear completely when the calcination temperature is increased to 600 ℃, which mineralized when the calcination temperature is further increased to 750 ℃. The introduction of Ag nanoparticles nearly has no influence on the thermal stability of -CH3 groups. As the calcining temperature is increased, the diffraction peaks of metallic silver in intensity and the tendency of silica particles to form crystals increase. The metallic silver results from the reduction of AgNO3. There are four steps in the thermal decomposition of Ag/MTES-SiO2 materials in N2 atmosphere, with different mechanism functions. The activation energies are 71.92、125.78、235.73 and 417.37 kJ?mol?1, and the frequency factors are 1.18×109、7.14×1010、8.35×1013 and 1.16×1020 s?1 for the four steps, respectively.

Key words: Silver loaded, Hybrid material, Infrared spectra;Thermal stability;Thermal analysis kinetics

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