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Hyperpolarized 129Xe NMR and N2 sorption cross-investigations of the crystallization of Al-SBA-15 amorphous walls into ZSM-5 type materials

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Abstract

The present work deals with the study of the parameters which govern the partial conversion of the amorphous walls of Al-SBA-15 supports into ZSM-5 type deposits under alkaline aqueous conditions. The influence of the mode of insertion of aluminium into Al-SBA-15 as well as of the quantities of ammonium fluoride and ZSM-5 template (TPABr) has been investigated. XRD and nitrogen sorption data indicate that the mesopore network is very fragile under the conditions required for the crystallization of ZSM-5. A compromise was found by using a TPABr/Al molar ratio lower than 1, thus affording materials containing both mesopores and zeolite-type micropores. The combined use of hyperpolarized (HP) 129Xe NMR and α-plot studies gave evidence for the ZSM-5 nature of the micropores as well as some indications in favour of the interconnection of the different pore networks.

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Acknowledgement

The authors are grateful to Ms. J. Phammavanh for her help in the preparation of Z′′(t) samples.

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Authors and Affiliations

  1. UPMC Univ Paris 06, UMR CNRS 7142, Laboratoire Systèmes Interfaciaux à l’Echelle Nanométrique, 4 place Jussieu, 75252, Paris cedex 05, France

    Sami Habib, Franck Launay, Marie-Anne Springuel-Huet, Flavien Guenneau & Antoine Gédéon

  2. National Institute of Chemistry, Hajdrihova 19, 1000, Ljubljana, Slovenia

    Matjaž Mazaj & Nataša Novak Tušar

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  1. Sami Habib
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  2. Franck Launay
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Corresponding authors

Correspondence to Franck Launay or Antoine Gédéon.

Electronic supplementary material

Below are the link to the electronic supplementary materials. HP 129Xe NMR spectra of xenon adsorbed in OP-Z(16) (Fig. S1), G-Z(16) (Fig. S2), Z′(8) (Fig. S7), Z′(16) (Fig. S8), and Al-SBA-15 (Fig. S9) samples at various pressures. TEM and SEM pictures of Z′(24) (Figs. S4 and S6, respectively). Pore size distributions of Z′′ and Z′ samples (Figs. S3 and S5, respectively).

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Habib, S., Launay, F., Springuel-Huet, MA. et al. Hyperpolarized 129Xe NMR and N2 sorption cross-investigations of the crystallization of Al-SBA-15 amorphous walls into ZSM-5 type materials. J Porous Mater 16, 349–359 (2009). https://doi.org/10.1007/s10934-008-9207-x

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