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Preparation and Thermal Stability in N2 Atmosphere of Pd/SiO2 Organic-inorganic Films

Authors： YANG Jing，XU Hao，LI Baosong，HUO Xiang，LI Yue

Units： School of Environmental&Chemistry Engineering, Xi’an Polytechnic University, Xi’an 710048)

KeyWords： Pd/SiO2 films；sol-gel method；hydrophobicity；thermal stability

ClassificationCode：O484

year,volume(issue):pagination： 2015,35(1):9-13

Abstract：

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/SiO2 materials calcined at 200℃. The metallic palladium results from the reduction of PdCl2. With the increase of calcination temperature, the diffraction peaks of metallic palladium in intensity increase, the SiCH3 and Si－OH bands in Pd/SiO2 samples are found to be decreased in absorption intensity. As the calcining temperature reaches 750 C, the SiCH3 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 C.

Funds：

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）和西安工程大学博士科研启动基金（BS1006）资助

AuthorIntro：

杨靖（1976-），女，湖北武汉人，博士，副教授，硕士生导师，从事膜分离技术的研究. < jingy76@163.com>

Reference：

[1] Nijmeijer A. Hydrogen Selective Silica Membranes for use in Membrane Steam Reforming[D]. University of Twente, F.A. van Vugst, Enschede, 1999.12.
[2] Lu G Q, da Costa J C D, Duke M, et al. Inorganic membranes for hydrogen production and purification: A critical review and perspective [J]. Journal of Colloid and Interface Science, 2007, 314: 589-603.
[3] Huang T C, Wei M C, Chen H I. Preparation of hydrogen-permselective palladium-silver alloy composite membranes by electroless co-deposition[J]. Separation and Purification Technology, 2003, 32(1-3): 239-245.
[4] Bosko M L, Miller J B, Lombardo E A, et al. Surface characterization of Pd-Ag composite membranes after annealing at various temperatures[J]. Journal of Membrane Science, 2011, 369(1-2): 267-276.
[5] Okazaki J, Ikeda T, Tanaka D A P, et al. An investigation of thermal stability of thin palladium-silver alloy membranes for high temperature hydrogen separation[J]. Journal of Membrane Science, 2011, 366(1-2): 212-219.
[6] Kanezashi M, Yada K, Yoshioka T, et al. Organic–inorganic hybrid silica membranes with controlled silica network size: Preparation and gas permeation characteristics[J]. Journal of Membrane Science, 2010, 348(1-2): 310-318.
[7] Levy R A , Ramos E S , Krasnoperov L N , et al. Microporous SiO2/Vycor membranes for gas separation[J]. Journal of Materials Research, 1996,11(12): 3164-3173.
[8] De Vos R M, Maier W F, Verweij H. Hydrophobic silica membranes for gas separation[J]. Journal of Membrane Science, 1999,158 (1-2): 277-288.
[9] Williams M, Pineda-Vargas C A, Khataibe E V, et al. Surface functionalization of porous ZrO2-TiO2 membranes using γ-aminopropyltriethoxysilane in palladium electroless deposition[J]. Applied Surface Science, 2008,254(10):3211-3219.
[10] Gestel T V, Sebold D, Hauler F, et al. Potentialities of microporous membranes for H2/CO2 separation in future fossil fuel power plants: Evaluation of SiO2, ZrO2, Y2O3-ZrO2 and TiO2-ZrO2 sol–gelmembranes[J]. Journal Of Membrane Science, 2010, 359, (1-2):64-79.
[11] 王飞，韦奇，王艳丽，等. 碳氟基团修饰的疏水微孔二氧化硅膜的制备与表征[J]. 化学学报, 2008, 66(1): 44-48.
[12] Cui S, Liu Y, Fan M, et al. Temperature dependent microstructure of MTES modified hydrophobic silica aerogels[J]. Materials Letters, 2011, 65(4): 606-609.
[13] 顾永建, 钟顺和. Pd修饰的选择分离氢的负载型PI-SiO2杂化膜的制备及应用[J]. 催化学报, 2006,27(3): 250-254.
[14] Yang J, Chen J R. Surface free energies and steam stability of methyl-modified silica membranes[J]. Journal of Porous Materials, 2009,16(6):737-744.
[15] 杨雨，钱国栋，王民权．MTES-TEOS先驱液水解-缩聚机理及其凝胶玻璃性能研究[J]．材料科学与工程，2000，18(3)：52-56．
[16] Bhagat S D, Kim Y H, Ahn Y S. Room temperature synthesis of water repellent silica coatings by the dip coat technique[J]. Applied Surface Science, 2006, 253(4): 2217-2221.
[17] Jiang H M, Zheng Z, Wang X L. Kinetic study of methyltriethoxysilane (MTES) hydrolysis by IR spectroscopy under different temperatures and solvents[J]. Vibrational spectroscopy, 2008, 46(1): 1-7.
[18] 杨定国. 波谱分析基础及应用[M]. 北京: 中国纺织出版社, 1993: 78-80.

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