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Microporous and Mesoporous Materials
Volume 92, Issues 1-3, 20 June 2006, Pages 181-188

Organic-free synthesis of ZSM-5 with narrow crystal size
distribution using two-step temperature process

Shin Dong Kim, Si Hyun Noh, Jun Woo Park, Wha Jung Kim *
Department of Materials Chemistry and Engineering, Konkuk University, 1-Hwa Yang Dong, Kwang Jin Gu, Seoul 143-701, Republic of Korea
Received 3 May 2005; received in revised form 5 January 2006; accepted 10 January 2006

Abstract
The MFI type of highly silica zeolite, ZSM-5 with well-defined crystal morphology was successfully synthesized in the absence of
organic template using two-step temperature process. In this process, the crystallization process was conducted at two different
temperatures by separating the nucleation and crystallization stage; that is, the nucleation stage at higher temperature (190 C) to
accelerate the nucleation followed by the crystallization stage at lower temperature (150 or 165 C) so as to control the crystal size
and size distribution. The effect of nucleation rate on the final crystal size and size distribution adopting higher temperature of the
first stage for nucleation than that of the second stage for crystallization was investigated. The results show that two-step temperature
process could control the crystal size and size distribution of ZSM-5. The result also shows that the time duration at higher temperature
for the acceleration of nucleation strongly affects the crystal size and size distribution. It implies that rapid nucleation at higher
temperature forms large number of nuclei followed by slow crystal growth probably due to the lack of energy at lower temperature. It
is very critical, therefore that the optimum time duration at higher temperature should be chosen to accelerate the nucleation within
initial stage.

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