Defect Sites in Zeolites: Origin and Healing

Abstract This paper deals with the synthesis conditions–defect formation relationship in zeolites. Silicalite‐1 (MFI‐type) is used as a model material. Samples synthesized from a system with high basicity (at 100 °C), a system with moderate basicity (at 150 °C), and a fluoride‐containing system in n...

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Main Authors: Ana Palčić, Simona Moldovan, Hussein El Siblani, Aurelie Vicente, Valentin Valtchev
Format: Article
Language:English
Published: Wiley 2022-02-01
Series:Advanced Science
Subjects:
Online Access:https://doi.org/10.1002/advs.202104414
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author Ana Palčić
Simona Moldovan
Hussein El Siblani
Aurelie Vicente
Valentin Valtchev
author_facet Ana Palčić
Simona Moldovan
Hussein El Siblani
Aurelie Vicente
Valentin Valtchev
author_sort Ana Palčić
collection DOAJ
description Abstract This paper deals with the synthesis conditions–defect formation relationship in zeolites. Silicalite‐1 (MFI‐type) is used as a model material. Samples synthesized from a system with high basicity (at 100 °C), a system with moderate basicity (at 150 °C), and a fluoride‐containing system in neutral medium (at 170 °C) are compared. Well‐crystallized materials with sizes ≈0.1, 1–10, and 30–40 µm are obtained. The samples are analyzed by complementary methods providing information on the short‐ and long‐range order in the zeolite framework. A strong correlation between the number of point defects in the zeolite framework and preparation conditions is established. Silicalite‐1 synthesized under mild synthesis conditions from a highly basic system exhibits a larger number of framework defects and thus low hydrophobicity. Further, the calcined samples are subjected to aluminum and silicon incorporation by postsynthesis treatment. The Al/Si incorporation in the zeolite framework and its impact on the physicochemical properties is studied by XRD, TEM/SEM, solid‐state NMR, FTIR, and thermogravimetric analyses. The defects healing as a function of the number of point defects in the initial material and zeolite crystal size is evaluated. The results of this study will serve for fine‐tuning zeolite properties by in situ and postsynthesis methods.
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spelling doaj.art-ceceb94a3dce4843ac899afba351a3a12022-12-22T04:06:50ZengWileyAdvanced Science2198-38442022-02-0194n/an/a10.1002/advs.202104414Defect Sites in Zeolites: Origin and HealingAna Palčić0Simona Moldovan1Hussein El Siblani2Aurelie Vicente3Valentin Valtchev4Ruđer Bošković Institute Division of Materials Chemistry Laboratory for Synthesis of New Materials Bijenička cesta 54 Zagreb 10000 CroatiaInstitut des Sciences Appliquées de Rouen Rouen University Groupe de Physique des Matériaux (GPM) avenue de l'Université, BP12, Saint‐Étienne‐du‐Rouvray Cedex Rouen 76801 FranceNormandie Université ENSICAEN UNICAEN CNRS Laboratoire Catalyse et Spectrochimie 6 Boulevard Maréchal Juin Caen 14050 FranceNormandie Université ENSICAEN UNICAEN CNRS Laboratoire Catalyse et Spectrochimie 6 Boulevard Maréchal Juin Caen 14050 FranceNormandie Université ENSICAEN UNICAEN CNRS Laboratoire Catalyse et Spectrochimie 6 Boulevard Maréchal Juin Caen 14050 FranceAbstract This paper deals with the synthesis conditions–defect formation relationship in zeolites. Silicalite‐1 (MFI‐type) is used as a model material. Samples synthesized from a system with high basicity (at 100 °C), a system with moderate basicity (at 150 °C), and a fluoride‐containing system in neutral medium (at 170 °C) are compared. Well‐crystallized materials with sizes ≈0.1, 1–10, and 30–40 µm are obtained. The samples are analyzed by complementary methods providing information on the short‐ and long‐range order in the zeolite framework. A strong correlation between the number of point defects in the zeolite framework and preparation conditions is established. Silicalite‐1 synthesized under mild synthesis conditions from a highly basic system exhibits a larger number of framework defects and thus low hydrophobicity. Further, the calcined samples are subjected to aluminum and silicon incorporation by postsynthesis treatment. The Al/Si incorporation in the zeolite framework and its impact on the physicochemical properties is studied by XRD, TEM/SEM, solid‐state NMR, FTIR, and thermogravimetric analyses. The defects healing as a function of the number of point defects in the initial material and zeolite crystal size is evaluated. The results of this study will serve for fine‐tuning zeolite properties by in situ and postsynthesis methods.https://doi.org/10.1002/advs.202104414Al/Si incorporationdefect sitespostsynthesis treatmentsilanolszeolites
spellingShingle Ana Palčić
Simona Moldovan
Hussein El Siblani
Aurelie Vicente
Valentin Valtchev
Defect Sites in Zeolites: Origin and Healing
Advanced Science
Al/Si incorporation
defect sites
postsynthesis treatment
silanols
zeolites
title Defect Sites in Zeolites: Origin and Healing
title_full Defect Sites in Zeolites: Origin and Healing
title_fullStr Defect Sites in Zeolites: Origin and Healing
title_full_unstemmed Defect Sites in Zeolites: Origin and Healing
title_short Defect Sites in Zeolites: Origin and Healing
title_sort defect sites in zeolites origin and healing
topic Al/Si incorporation
defect sites
postsynthesis treatment
silanols
zeolites
url https://doi.org/10.1002/advs.202104414
work_keys_str_mv AT anapalcic defectsitesinzeolitesoriginandhealing
AT simonamoldovan defectsitesinzeolitesoriginandhealing
AT husseinelsiblani defectsitesinzeolitesoriginandhealing
AT aurelievicente defectsitesinzeolitesoriginandhealing
AT valentinvaltchev defectsitesinzeolitesoriginandhealing