Monitoring by in situ neutron diffraction of simultaneous dehydration and Ni2+ mobility in partially exchanged NaY zeolitesElectronic supplementary information (ESI) available. CSD 430696-430699. See DOI: 10.1039/c5nj02918j

Powder neutron diffraction is used to follow structural changes occurring during heat and vacuum assisted dehydration of 3 wt% nickel exchanged NaY. The structures determined from Rietveld refinement confirm the nickel ion displacement from the supercages and sodalite cages towards hexagonal prisms...

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Main Authors Porcher, Florence, Paillaud, Jean-Louis, Gaberova, Lucia, André, Gilles, Casale, Sandra, Massiani, Pascale
Format Journal Article
Published 10.05.2016
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Abstract Powder neutron diffraction is used to follow structural changes occurring during heat and vacuum assisted dehydration of 3 wt% nickel exchanged NaY. The structures determined from Rietveld refinement confirm the nickel ion displacement from the supercages and sodalite cages towards hexagonal prisms upon water removal. Not only this mobility but also its relationship with the dehydration level is demonstrated, owing to real time quantification of dehydration through changes in the intensity of the incoherent neutron scattering signal. Comparison with TGA data proves that this signal is fully attributable to water molecules adsorbed in the zeolite. STEM/EDX and in situ heating TEM studies provide complementary information on homogeneous Ni distribution (initial state) and on reductive sintering in vacuum at a high temperature. The incoherent signal in neutron diffraction patterns allows correlating in real time hydration-dehydration levels and structural changes in zeolites.
AbstractList Powder neutron diffraction is used to follow structural changes occurring during heat and vacuum assisted dehydration of 3 wt% nickel exchanged NaY. The structures determined from Rietveld refinement confirm the nickel ion displacement from the supercages and sodalite cages towards hexagonal prisms upon water removal. Not only this mobility but also its relationship with the dehydration level is demonstrated, owing to real time quantification of dehydration through changes in the intensity of the incoherent neutron scattering signal. Comparison with TGA data proves that this signal is fully attributable to water molecules adsorbed in the zeolite. STEM/EDX and in situ heating TEM studies provide complementary information on homogeneous Ni distribution (initial state) and on reductive sintering in vacuum at a high temperature. The incoherent signal in neutron diffraction patterns allows correlating in real time hydration-dehydration levels and structural changes in zeolites.
Author Casale, Sandra
André, Gilles
Porcher, Florence
Massiani, Pascale
Gaberova, Lucia
Paillaud, Jean-Louis
AuthorAffiliation Université de Lorraine
Sorbonne Université - Université Paris 06 UPMC
LRS - UPMC
UMR CNRS 7361
UMR 12 CNRS-CEA
CNRS UMR 7197
Equipe Matériaux à Porosité Contrôlée (MPC)
CRM2
Institut de Science des Matériaux de Mulhouse (IS2M)
Laboratoire de Réactivité de Surface (LRS)
Université Haute-Alsace
Laboratoire Léon Brillouin (LLB)
Faculté des Sciences et Technologies
UMR 7036 CNRS
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  publication-title: Compilation of Extra-framework Sites in Zeolites
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  publication-title: Commission on powder diffraction (IUCr)
  doi: Rodríguez-Carvajal
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  publication-title: Atlas of Zeolite Framework Types
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– doi: Plevert Di Renzo Fajula Chiari
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  publication-title: Collection of Simulated XRD Powder Patterns for Zeolites
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Snippet Powder neutron diffraction is used to follow structural changes occurring during heat and vacuum assisted dehydration of 3 wt% nickel exchanged NaY. The...
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Title Monitoring by in situ neutron diffraction of simultaneous dehydration and Ni2+ mobility in partially exchanged NaY zeolitesElectronic supplementary information (ESI) available. CSD 430696-430699. See DOI: 10.1039/c5nj02918j
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