Pd/SiO_2有机-无机薄膜的制备及其在N_2气氛中的热稳定性  

Preparation and thermal stability in N_2 atmosphere of Pd/SiO_2 organic-inorganic films

作　　者：杨靖[1] 许好 李保松[1] 霍翔[1] 李悦[1] 

机构地区：[1]西安工程大学环境与化学工程学院,西安710048

出　　处：《膜科学与技术》2015年第1期9-13,19,共6页Membrane Science and Technology

基　　金：国家自然科学基金(21103132);陕西省自然科学基金(2011JQ2016);陕西省教育厅自然科学专项基金(12JK0591);西安工程大学博士科研启动基金(BS1006)资助

摘　　要：采用溶胶-凝胶法,在甲基化改性SiO2溶胶中掺杂PdCl2,制备Pd/SiO2有机-无机薄膜.通过XRD、红外光谱、TG-DTG分析、接触角以及SEM测试,考察该样品在N2气氛中的热稳定性.结果表明,Pd/SiO2膜材料经200℃以上温度焙烧后,样品中即出现了少量纳米金属Pd粒子,这些金属Pd为PdCl2还原所得.随着焙烧温度的升高,金属Pd粒子的衍射峰强度增加,膜材料中的Si-CH3吸收峰和Si-OH吸收峰减弱.样品中的Si-CH3吸收峰在750℃时完全消失.金属Pd的掺杂对SiO2膜材料的化学结构基本没影响.保持Pd/SiO2有机-无机薄膜及分离膜疏水性的最适宜焙烧温度为350℃.Pd/SiO2 organic-inorganic films were prepared by sol-gel method, in which PdCl2 was added into methyl-modified silica sol. According to XRD, FTIR spectra, TG-DTG analysis, contact angle and SEM measurement, the thermal stability of Pd/SiO2 samples in N2 atmosphere was discussed. The results show that, metallic palladium peaks can be found in the Pd/SiOz materials calcined at 200 ℃. The metallic palladium results from the reduction of PdCl2. With the increase of calcination temperature, the diffraction peaks intensity of metallic palladium increase, the Si-CH3 and Si-OH bands in Pd/SiO2 samples are found to be decreased in absorption intensity. As the calcining temperature reaches 750 ℃, the Si-CH3 band completely disappears. The introduction of metallic palladium has little influence on the chemical structure of the methyl-modified silica materials. In order to preserve the hydrophobicity of Pd/SiO2 films and membranes, the optimal calcination temperature should be 350℃.

关 键 词：Pd/SiO2薄膜 溶胶-凝胶法 疏水性 热稳定性 

分 类 号：O484.1[理学—固体物理]