The Effect of pH of the Aging Solution on Microstructure of Silica/Zirconia Aerogel

Article Preview

Abstract:

ZrO2 wet gel was prepared using zirconium n-butoxide as precursor and 1,2-propylene oxide (PO) as a gelation agent in sol-gel process. Then, tetraethoxysilane (TEOS) was used to strengthen the wet gel in aging process. Finally, the monolithic silica/zirconia aerogel was obtained by supercritical fluid drying. N2 adsorption-desorption method, scanning electron microscope (SEM), and Fourier transform infrared spectroscopy (FTIR) were used to characterize microstructure of the aerogel. The influence of pH of the aging solution on microstructure of silica/zirconia aerogel was studied. The results indicate that the particle size distribution of SiO2/ZrO2 aerogel was more uniform and less aggregate when aging in acid solution. However, the average pore diameter and particle size of SiO2/ZrO2 aerogel was increased by aging in alkaline solution. Aging in alkaline condition was useful for largening the pore size of SiO2/ZrO2 aerogel, and the maximum specific surface area and pore volume were obtained at pH=9. Meanwhile, different reactions were produced between the acid/alkaline solution and the hydroxyl of SiO2/ZrO2 aerogel, and the ester group/amino group was obtained relatively which can modify the network of aerogel and decrease the shrinkage of aerogel during the supercritical fluid drying.

You might also be interested in these eBooks

Info:

Periodical:

Key Engineering Materials (Volumes 602-603)

Pages:

358-362

Citation:

Online since:

March 2014

Export:

Price:

Permissions CCC:

Permissions PLS:

Сopyright:

© 2014 Trans Tech Publications Ltd. All Rights Reserved

Share:

Citation:

* - Corresponding Author

[1] Z.Q. Zhao, D.R. Chen, X.L. jiao, Zirconia aerogels with high surface area derived from sols prepared by electrolyzing zirconium oxychloride solution: comparison of aerogels prepared by freeze-drying and supercritical CO2(l) extraction, J. phys. Chem. C. III(50). 18738-18743 (2007).

DOI: 10.1021/jp075150b.s001

Google Scholar

[2] J. Konishi, K. Fujita, S. Oiwa, Crystalline ZrO2 monoliths with well-defined macropores and mesostructured skeletons prepared by combining the alkoxy-derived sol–gel process accompanied by phase separation and the solvothermal process, Chem. Mater. 20(6), 2165-2173 (2008).

DOI: 10.1021/cm703351d

Google Scholar

[3] James B. Miller, Edmond I. Ko, Acidic Properties of Silica-Containing Mixed Oxide Aerogels: Preparation and Characterization of Zirconia-Silica and Comparison to Titania-Silica, Journal of Catalysis. 1996, 159: 58-68.

DOI: 10.1006/jcat.1996.0064

Google Scholar

[4] James B. Miller, Edmond I. Ko, Control of mixed oxide textural and acidic properties by the sol-gel method, Journal of Catalysis. 1997, 35: 269-292.

DOI: 10.1016/s0920-5861(96)00161-7

Google Scholar

[5] Zhaoqi Zhan, H.C. Zeng, A catalyst-free approach for sol-gel synthesis of highly mixed ZrO2-SiO2 oxides, Joumal of Non-Crystalline Solids. 1999, 243: 26-38.

DOI: 10.1016/s0022-3093(98)00810-2

Google Scholar

[6] S. Haereid, J. Anderson, M.A. Einarsrud, D.W. Hua, D.M. smith, Effect of aging temperature on the porosity characteristics of subcritically dried silica aerogels, J. Non-Cryst. Solids 185 (1995) 221.

Google Scholar

[7] K. Chou, B.I. Lee, Solvent effect on aging of silica gels, J. Mater. Sci. 29 (1994) 3565.

Google Scholar

[8] P.J. Davis, R. Deshpande, D.M. smith, C.J. Brinker, R.A. Assink, Pore Structure Evolution of Silica Gel during aging/drying: Effect of Surface Tension, J. Non-Cryst. Solids 167 (1994) 295.

DOI: 10.1016/0022-3093(94)90252-6

Google Scholar

[9] H. Hdach, T. Woignier, J. Phalippou, G.W. Scherer, Effect of aging and pH on the modulus of aerogels, J. Non-Cryst. Solids 121 (1990) 202.

DOI: 10.1016/0022-3093(90)90132-6

Google Scholar

[10] G.W. Scherer, S.A. Pardenek, R.M. Swiatek, Viscoelasticity in silica gel, J. Non-Cryst. Solids 107 (1988) 14.

DOI: 10.1016/0022-3093(88)90086-5

Google Scholar