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Preparation of macroporous zirconia monoliths from ionic precursors via an epoxide-mediated sol-gel process accompanied by phase separation
Authors:Xingzhong Guo  Jie Song  Yixiu Lvlin  Kazuki Nakanishi  Kazuyoshi Kanamori  Hui Yang
Affiliation:1.School of Materials Science and Engineering, Zhejiang University, Hangzhou, 310027, People’s Republic of China;2.Department of Chemistry, Graduate School of Science, Kyoto University, Kitashirakawa, Sakyo-ku, Kyoto 606-8502, Japan
Abstract:Monolithic macroporous zirconia (ZrO2) derived from ionic precursors has been successfully fabricated via the epoxide-mediated sol-gel route accompanied by phase separation in the presence of propylene oxide (PO) and poly(ethylene oxide) (PEO). The addition of PO used as an acid scavenger mediates the gelation, whereas PEO enhances the polymerization-induced phase separation. The appropriate choice of the starting compositions allows the production of a macroporous zirconia monolith with a porosity of 52.9% and a Brunauer–Emmett–Teller (BET) surface area of 171.9 m2 · g−1. The resultant dried gel is amorphous, whereas tetragonal ZrO2 and monoclinic ZrO2 are precipitated at 400 and 600 °C, respectively, without spoiling the macroporous morphology. After solvothermal treatment with an ethanol solution of ammonia, tetragonal ZrO2 monoliths with smooth skeletons and well-defined mesopores can be obtained, and the BET surface area is enhanced to 583.8 m2 · g−1.
Keywords:porous materials   zirconia monoliths   sol-gel   phase separation   heat-treatment   solvothermal treatment
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