Solid-state crystallization, oxygen-vacancy rich mesopores and stable triad-silanol nests in ZSM-5 catalyst induced by electron-beam irradiation and calcination

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Mesopores and silanol nests are known two technological keys that essentially control the catalytic performance of ZSM-5 zeolite. However, designing and controlling them without using chemicals so that the produced ZSM-5 can have strongly enhanced catalytic properties and more importantly can be applied at industrial scale have still been a big challenge up to now. The present study employed the 10 MeV electron beam (EB) generated from an industrial linear accelerator to introduce both the O-vacancy rich mesopores and stable triad-silanol nests in ZSM-5. The structural modification of irradiated ZSM-5 samples were explored by using SEM and FTIR combined with positron annihilation spectroscopy (PAS) including positron annihilation lifetime (PAL), Doppler broadening (DB) of electron-positron annihilation energy and electron momentum distribution (EMD). Obtained results indicated that EB irradiation can recover the defective-crystal structure as well as intensively modify the structures of ZSM-5. In particular, the mechanism for the solid-state crystallization and the formation of the O-vacancy rich mesopores (maximum size of ∼ 4.5 nm) in ZSM-5 under the combined EB irradiation (10−110 kGy) and calcination (600 °C) was, for the first time, proposed. The mechanism for the formation of stable triad-silanol nests in the channels of irradiated and calcined ZSM-5 zeolites was also explored. The present study, therefore, opens a new research path of applying both EB irradiation and calcination to produce ZSM-5 with novel features for industrial catalytic application at large-production scale.