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Received February 4, 2004
Accepted September 10, 2004
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Rapid Synthesis of Mesoporous Silica by an Accelerated Microwave Radiation Method
1Department of Chemical and Biomolecular Engineering, and Center for Energy and Environment Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kuseong-dong, Yuseong-gu, Daejeon 305-701, Korea 2Samsungcorning R&BD Center, 472, Sin-dong, Yeoungtong-gu, Suwon, Gyeonggi-Do 442-732, Korea 3LG Household & Health Care Research Park, #84 Jang-dong, Yuseong-gu, Daejeon 305-343, Korea
kjd@kaist.ac.kr
Korean Journal of Chemical Engineering, November 2004, 21(6), 1224-1230(7), 10.1007/BF02719498
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Abstract
Microwave-hydrothermal processes for the synthesis of mesoporous silica were investigated with different pathways and mixture conditions at 373 K, and the corresponding structures to the hydrothermal method were synthesized within a very short crystallization time. 2-D hexagonally ordered arrays of MCM-41 materials via the direct electrostatic assembly pathway of S+I- and mediated templating pathways of S+X-I+ with CTAB were synthesized, and cubic mesophase of MCM-48 was also prepared within 2 hrs of microwave heating without adding alcohol. Nonionic surfactants with ethylene oxide (EO) moiety as structure-directing agents were used for the preparation of ordered array of hexagonal or cubic mesostructured silica via the charge matching principle of (S0H+)(X-I+). Although the detailed roles of microwaves may differ for each process, microwaves accelerate the formation of multiply charged silicate oligomers, initiating mesophase assembly. Therefore, the use of microwave radiation can transfer energy uniformly and quickly, and complete the syntheses of mesostructured materials within a short time.
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References
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Huo Q, Margolese DI, Stucky GD, Chem. Mater., 8, 1147 (1996)
Kaneda M, Tsubakiyama T, Carlsson A, Sakamoto Y, Ohsuna T, Terasaki O, Joo SH, Ryoo R, J. Phys. Chem. B, 106(6), 1256 (2002)
Jansen JC, Arafat A, Barakat AK, vanBekkum H, Occelli ML, Robson HE, In "Synthesis of Microporous Materials," Van Nostrand Reinhold, New York, Vol. 2, 507 (1992)
Kim JM, Kim SK, Ryoo R, Chem. Commun., 259 (1998)
Kim GJ, Park DW, Ha JM, Korean J. Chem. Eng., 17(3), 337 (2000)
Kresge CT, Leonowicz ME, Roth WJ, Vartuli JC, Beck JS, Nature, 59, 710 (1992)
Mingos DMP, Adv. Mater., 11, 857 (1993)
Mingos DMP, Microwave Induced React., 85 (1994)
Mingos DMP, Baghurst DR, J. Organomet. Chem., 384, 57 (1990)
Newalkar BL, Kormarneni S, Chem. Mater., 13, 4573 (2001)
Newalkar BL, Komarneni S, Katsuki H, Chem. Commun., 23, 2389 (2000)
Newalkar BL, Olanrewaju J, Komarneni S, J. Phys. Chem. B, 105(35), 8356 (2001)
Newalkar BL, Olanrewaju J, Komarneni S, Chem. Mater., 13, 552 (2001)
Park SE, Kim DS, Chang JS, Kim WY, Catal. Today, 44(1-4), 301 (1998)
Park SE, Kim DS, Chang JS, Kim WY, Stud. Surf. Sci. Catal., 117, 265 (1998)
Rao KJ, Vaidhyanathan B, Ganguli M, Ramakrishnan PA, Chem. Mater., 11, 882 (1999)
Roh HS, Chang JS, Park SE, Korean J. Chem. Eng., 16(3), 331 (1999)
Ryoo R, Kim JM, J. Chem. Soc. Chem. Commun, 7, 711 (1995)
Ryoo R, Kim JM, Ko CH, Shin CH, J. Phys. Chem., 100(45), 17718 (1996)
Sayari A, J. Am. Chem. Soc., 122(27), 6504 (2000)
Schumacher K, Grun M, Unger KK, Microporous Mesoporous Mater., 27, 201 (1999)
Setoguchi YM, Teraoka Y, Moriguchi I, Kagawa S, Tomonaga N, Yasutake A, Izumi J, J. Porous Mat., 4, 129 (1997)
Song MG, Kim JY, Cho SH, Kim JD, Langmuir, 18(16), 6110 (2002)
Tanev PT, Pinnavaia TJ, Science, 267(5199), 865 (1995)
Tian B, Liu X, Yang H, Xie S, Yu C, Tu B, Zhao D, Adv. Mater., 15, 1370 (2003)
Xu J, Luan Z, He H, Zhou W, Keven L, Chem. Mater., 10, 3690 (1998)
Zhang YJ, Zhao SL, Lu LQ, Sun GD, Acta Chim. Sin., 59, 820 (2001)
Zhao D, Goldfarb D, J. Chem. Soc. Chem. Commun., 875 (1995)
Zhao D, Huo Q, Feng J, Chmelka BF, Stucky GD, J. Am. Chem. Soc., 120(24), 6024 (1998)
Zhao D, Yang P, Melosh N, Feng J, Chmelka BF, Stucky GD, Adv. Mater., 10, 1380 (1998)
