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ISSN 1000-6818CN 11-1892/O6CODEN WHXUEU
Acta Phys Chim Sin >> 2013,Vol.29>> Issue(03)>> 646-652     doi: 10.3866/PKU.WHXB201212252         中文摘要
PHYSICAL CHEMISTRY OF MATERIALS
Macroporous SiO2 Monoliths Prepared via Sol-Gel Process Accompanied by Phase Separation
GUO Xing-Zhong1, LI Wen-Yan1, ZHU Yang2, NAKANISHI Kazuki2, KANAMORI Kazuyoshi2, YANG Hui1
1 Department of Materials Science and Engineering of Zhejiang University, Hangzhou 310027, P. R. China;
2 Department of Chemistry, Graduate School of Science, Kyoto University, Kyoto 606-8502, Japan
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Macroporous SiO2 monoliths were prepared via a sol-gel process accompanied by phase separation using a tetramethoxysilane (TMOS) precursor, 0.01 mol·L-1 HCl catalyst, propylene oxide (PO) gelation agent, and poly(ethylene oxide) (PEO, viscosity-averaged molecular weight (Mv): 10000) phase separation inducer. Monoliths were characterized by differential thermal analysis/thermogravimetry (DTA/ TG), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), mercury porosimetry, and nitrogen adsorption/desorption analysis (BET). The mechanism of the epoxide-mediated sol-gel reaction and PEO induced phase separation was discussed. The addition of PEO induced phase separation, and monolithic SiO2 with a cocontinuous macroporous skeletal structure was obtained at PEO/TMOS molar ratio of 0.0018. Monoliths had a narrow pore size distribution of 1-3 μm, surface area as high as 719 m2·g-1 and pore volume of 0.48 m3·g-1. This sol-gel transition is mediated by PO because of its strong nucleophilic properties and irreversible ring-opening reaction. Simultaneous phase separation is induced by PEO adsorbed on the SiO2 oligomers.



Keywords: Porous monolith   Silica   Sol-gel   Phase separation   Propylene oxide   Poly(ethylene oxide)  
Received: 2012-09-15 Accepted: 2012-12-24 Publication Date (Web): 2012-12-25
Corresponding Authors: Email: yanghui@zju.edu.cn

Fund: The project was supported by the Key Innovation Team Project of Zhejiang Province, China (2009R50010).

Cite this article: GUO Xing-Zhong, LI Wen-Yan, ZHU Yang, NAKANISHI Kazuki, KANAMORI Kazuyoshi, YANG Hui. Macroporous SiO2 Monoliths Prepared via Sol-Gel Process Accompanied by Phase Separation[J]. Acta Phys. -Chim. Sin., 2013,29 (03): 646-652.    doi: 10.3866/PKU.WHXB201212252

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62. LI Li, MA Yu, CAO Yan-Zhen, JI Yuan, GUO Yi-Hang.Preparation of Periodic Mesoporous H6P2W18O62/TiO2(Brij-76) Composite and Microwave Enhanced Photocatalytic Degradation of Monochlorobenzene[J]. Acta Phys. -Chim. Sin., 2009,25(07): 1461-1466
63. CHEN Qi-Feng, JIANG Dong, XU Yao, WU Dong, SUN Yu-Han.Visible Region Photocatalysis of Ce-Si/TiO2 Synthesized Using Sol-Gel-Hydrothermal Method[J]. Acta Phys. -Chim. Sin., 2009,25(04): 617-623
64. HUA Zheng-He; LI Dong; FU Hao.Sol-Gel Template Synthesis and Characterization of Magnetoelectric CoFe2O4/BaTiO3 Nanotubes[J]. Acta Phys. -Chim. Sin., 2009,25(01): 145-149
65. WANG Tao, HE Jian-Ping, ZHANG Chuan-Xiang, ZHOU Jian-Hua, GUO Yun-Xia, CHEN Xiu, DI Zhi-Yong, SUN Dun, WANG Dao-Jun.Preparation and Electrochemical Properties of Ordered Mesoporous C/NiO Composites[J]. Acta Phys. -Chim. Sin., 2008,24(12): 2314-2320
66. LI Jin-Huan; KANG Wan-Li; YAN Wen-Hua; GUO Yi-Hang; GAO Hong-Feng; LIU Zhong-He.Preparation of Eu3+ Doped Titania Nanocrystals and Photocatalytic Degradation Partially Hydrolyzed Polyacrylamide[J]. Acta Phys. -Chim. Sin., 2008,24(06): 1030-1034
67. WU Yu-Cheng; LIU Xiao-Lu; YE Min; XIE Ting; HUANG Xin-Min.Preparation and Properties of Carbon Nanotube-TiO2 Nanocomposites[J]. Acta Phys. -Chim. Sin., 2008,24(01): 97-102
68. ZHAN Ying-Ying; CAI Guo-Hui; ZHENG Yong; SHEN Xiao-Nv; ZHENG Ying; WEI Ke-Mei.Synthesis of High Surface Area Silicon Carbide and Its Application in CO Oxidation Reaction[J]. Acta Phys. -Chim. Sin., 2008,24(01): 171-175
69. WANG Feng; HAO Ya-Juan; JIN Guo-Qiang; GUO Xiang-Yun.Effects of the Reaction Conditions in Preparation of Si3N4 Nanowires[J]. Acta Phys. -Chim. Sin., 2007,23(10): 1503-1507
70. ZHANG Wei; WANG Shu-Liang; MA Yun-Qing; WANG Cui-Ping; LIU Xing-Jun.Influence of Interface Diffusion between Al Substrate and TiO2 Filmon Photocatalytic Activity[J]. Acta Phys. -Chim. Sin., 2007,23(09): 1347-1352
71. HUANG Dong-Sheng; ZENG Ren-Jie; CHEN Chao-Feng; LI Yu-Hua.Hydrophilicity of TiO2 Thin Films Codoped with Iron and Nitrogen[J]. Acta Phys. -Chim. Sin., 2007,23(07): 1037-1041
72. ZHAO Meng; WANG Jin-Xing; FENG Cai-Hui; ZOU Bo; CHEN Cheng; WANG Zhu-Yi; WU Feng-Qing; ZOU Le-Hui.Preparation and Gas Sensing Properties to Formaldehyde of TiO2/Ag2O Nanocrystalline[J]. Acta Phys. -Chim. Sin., 2007,23(07): 1003-1006
73. LI Hong-Jian; CHEN Gang; LI Zhong-Hua; ZHOU Chao.Synthesis and Photocatalytic Decomposition of Water under Visible Light Irradiation of La2Ti2-xCoxO7 with Pyrochlore Structure[J]. Acta Phys. -Chim. Sin., 2007,23(05): 761-764
74. WU Lun-Peng; ZHAO Lian-Hua; ZHANG Hai-Ming; ZHAO Qing-Nan.Effects of the Adsorption of Oxygen on the Photocatalytic Activity of TiO2 Films Using PhotocurrentMethod[J]. Acta Phys. -Chim. Sin., 2007,23(05): 765-768
75. ZHANG Xiao-Fei; HU Rui-Sheng; GAO Guan-Jun; MENG He; SU Hai-Quan.Influence of Two Complexants on Structure and Performance of Ce-Sn-O Complex Oxides[J]. Acta Phys. -Chim. Sin., 2007,23(05): 659-663
76. WANG Huan-Ping; ZHANG Qi-Long; YANG Hui; SUN Hui-Ping.Synthesis and Microwave Dielectric Properties of (Ca1-xMgx)SiO3 Ceramic by Sol-Gel Process[J]. Acta Phys. -Chim. Sin., 2007,23(04): 609-613
77. HAO Zhi-Xian;LIU Hui;GUO Bin;LI Hong;ZHANG Jia-Wei;GAN Li-Hua;XU Zi-Jie;CHEN Long-Wu.Sol-Gel Synthesis of Alumina Using Inorganic Salt Precursor[J]. Acta Phys. -Chim. Sin., 2007,23(03): 289-294
78. ZHOU Hong-Wei;LI Huai-Xiang;JIANG Zheng-Wei;ZUO Xiang-Qing.Treatment of ZnS:Mn Phosphors by Partial Sublimation of SnO2:Sb Xerogel[J]. Acta Phys. -Chim. Sin., 2007,23(01): 88-91
79. QIAO Bin;TANG Zi-Long;ZHANG Zhong-Tai;CHEN Lei.Photoluminescent and Electroluminescent Characteristics of ZnGa2O4:Cr3+ Red Phosphor[J]. Acta Phys. -Chim. Sin., 2006,22(10): 1291-1295
80. FENG Chun-Bo;DU Zhi-Ping;Zhao Yong-Hong;TAI Xiu-Mei;LI Qiu-Xiao .Photocatalytic Activity of Au Modified Nano-TiO2 for NPE-10 Degradation[J]. Acta Phys. -Chim. Sin., 2006,22(08): 953-957
81. JIN Guo-Jie;GUO Yang-Long;LIU Xiao-Hui;YAO Wei;GUO Yun;WANG Yun-Song;YUAN Fang;LU Guan-Zhong.In situ FT-IR Study on the Direct Gas Phase Epoxidation of Propylene over Ag-MoO3 Catalyst[J]. Acta Phys. -Chim. Sin., 2006,22(07): 809-814
82. LIU Yi-An;XUE Cheng-Shan;ZHUANG Hui-Zhao;ZHANG Xiao-Kai;TIAN De-Heng;WU Yu-Xin;SUN Li-Li;AI Yu-Jie;WANG Fu-Xue.Structure and Synthesis of GaN Powder by Sol-Gel Method[J]. Acta Phys. -Chim. Sin., 2006,22(06): 657-660
83. YE Qing; XU Bo-Qing.Textural and Structure Characterizations of Ce1-xMnxO2Prepared by Citric Acid Sol-Gel Method[J]. Acta Phys. -Chim. Sin., 2006,22(03): 345-349
84. YE Qing; WANG Rui-pu; XU Bo-qing.Structure and Oxygen Mobility of Ce1-xZrxO2 Prepared by Citric Acid Sol-gel Method[J]. Acta Phys. -Chim. Sin., 2006,22(01): 33-37
85. LIU Rui-quan; XIE Ya-hong; LI Zhi-jie; WANG Ji-de; SUN Yi-gang.Application of Proton Conductors (Ce0.8La0.2)1-xCaxO2-δ in Synthesis of Ammonia[J]. Acta Phys. -Chim. Sin., 2005,21(09): 967-970
86. YAO Su-wei; WU Hai-xia; WANG Hong-zhi; ZHANG Wei-guo.Electrodeposition of Cu-Co Granular Films on Semiconductor Si Substrate and Their GMR Effect[J]. Acta Phys. -Chim. Sin., 2005,21(08): 915-919
87. PENG Feng; CHEN Shui-hui; ZHANG Lei; WANG Hong-juan; XIE Zhi-yong.Preparation of Visible-light Response Nano-sized ZnO Film and Its Photocatalytic Degradation to Methyl Orange[J]. Acta Phys. -Chim. Sin., 2005,21(08): 944-948
88. LI Li-chun; GUAN Jian-guo; CHENG Hai-bin; TAO Jian-qing.Preparation of Poly(ethylene glycol)-coated Carbonyl Iron Particles for Aqueous Magnetorheological Suspension[J]. Acta Phys. -Chim. Sin., 2005,21(07): 817-821
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90. CHEN Yong; LIU Ming-zhu; JIN Shu-ping; CHEN Shi-lan.Study on the Phase Separation Behavior of Poly(N,N-diethylacrylamide) and P(N,N-diethylacrylamide-co-N-hydroxymethylacrylamide) Dilute Aqueous Solutions[J]. Acta Phys. -Chim. Sin., 2005,21(06): 591-595
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