Gismondine under HP: Deformation mechanism and re-organization of the extra-framework species

Betti, Carolina; Fois, Ettore; Mazzucato, E.; Medici, C.; Quartieri, Simona; Tabacchi, Gloria; Vezzalini, Giovanna; Dmitriev, Vladimir

doi:10.1016/j.micromeso.2007.01.051

Cited by 42 publications

(35 citation statements)

References 58 publications

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“…Water content was determined by thermogravimetric analysis on a 10 mg sample using a Seiko SSC/5200 instrument, operating at 10 1C/min from 18 to 1000 1C in air. The weight loss was 10 …”

Section: Chemical Analysismentioning

confidence: 99%

“…For these reasons, as part of a wider project aimed to the study of the elastic behavior of microporous materials [7][8][9][10][11][12][13][14][15], we have performed in-situ synchrotron X-ray powder diffraction (XRPD) experiments on MFI-type zeolites with different framework Si/Al ratio and different extraframework content -namely Na-ZSM-5 [16], H-ZSM-5, and silicalite and mutinaite [17,18] -using (16:3:1) methanol:ethanol:water (m.e.w.) and/or silicone oil (s.o.)…”

Section: Introductionmentioning

confidence: 99%

“…On the contrary, s.o. is constituted by too large molecules to penetrate the channels, hence is a ''non-penetrating'' medium [7][8][9][10][11]13,14].…”

Section: Introductionmentioning

confidence: 99%

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Elastic behavior of MFI-type zeolites: Compressibility of H-ZSM-5 in penetrating and non-penetrating media

Quartieri¹,

Montagna²,

Arletti³

et al. 2011

Journal of Solid State Chemistry

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High pressure structure Elastic behavior Synchrotron X-ray powder diffraction a b s t r a c tThe elastic behavior of H-ZSM-5 was investigated by in-situ synchrotron X-ray powder diffraction, using both silicone oil (s.o.) and (16:3:1) methanol:ethanol:water (m.e.w.) as ''non-penetrating'' and ''penetrating'' pressure transmitting media, respectively. From P amb to 6.2 GPa the volume reduction observed in s.o. is 16.6%. This testifies that H-ZSM-5 is one of the most flexible microporous materials up to now compressed in s.o. Volume reduction observed in m.e.w. up to 7.6 GPa is 14.6%. A strong increase in the total electron number of the extraframework system, due to the penetration of water/ alcohol molecules in the pores, is observed in m.e.w. This effect is the largest up to now observed in zeolites undergoing this phenomenon without cell volume expansion. The higher compressibility in s.o. than in m.e.w. can be ascribed to the penetration of the extra-water/alcohol molecules, which stiffen the structure and contrast the channel deformations.

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“…Water content was determined by thermogravimetric analysis on a 10 mg sample using a Seiko SSC/5200 instrument, operating at 10 1C/min from 18 to 1000 1C in air. The weight loss was 10 …”

Section: Chemical Analysismentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Elastic behavior of MFI-type zeolites: Compressibility of H-ZSM-5 in penetrating and non-penetrating media

Quartieri¹,

Montagna²,

Arletti³

et al. 2011

Journal of Solid State Chemistry

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“…ref. [4][5][6][7][8][9][10][11][12][13]. High-pressure studies performed using pore penetrating media have attracted great attention because of the so-called pressure-induced hydration effect (PIH), 14 in which the water content inside the cavity increases in response to the applied pressure through selective sorption of H 2 O molecules from the PTM.…”

Section: Introductionmentioning

confidence: 99%

“…25 The studies performed with 'non-penetrating' media highlighted the crucial influence of the framework type and composition, and the extra-framework content, on zeolite's response to pressure in terms of deformation mechanism and compressibility. 2,5,[10][11][12] Zeolite compressibility does not appear to be directly related to the material porosity, but is more closely related to the characteristics of the extra-framework cations and the number of H 2 O molecules. As a consequence, some zeolites characterized by large pores can be unexpectedly less compressible than other pure-Si phases with empty cavities.…”

Section: Introductionmentioning

confidence: 99%

Pressure-induced penetration of guest molecules in high-silica zeolites: the case of mordenite

Arletti

Leardini

Vezzalini

et al. 2015

Phys. Chem. Chem. Phys.

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A synthetic high-silica mordenite (HS-MOR) has been compressed in both non-penetrating (silicone oil, s.o.) and penetrating [methanol : ethanol : water (16 : 3 : 1) (m.e.w.), water : ethanol (3 : 1) (w.e.), and ethylene glycol (e.gl.)] pressure transmitting media (PTM). In situ high-pressure (HP) synchrotron X-ray powder diffraction (XRPD) experiments allowed the unit cell parameters to be followed up to 1.6, 1.8, 8.4, and 6.7 GPa in s.o., w.e., m.e.w., and e.gl., respectively. Moreover, e.gl. was also used as a PTM in in situ HP Raman and ex situ IR experiments. The structural refinement of HS-MOR compressed in e.gl.at 0.1 GPa -the lowest investigated pressure -revealed the presence of 3.5 ethylene glycol molecules per unit cell. The infrared spectrum of the recovered sample, after compression to 1 GPa, is consistent with the insertion of ethylene glycol molecules in the pores. XRPD and Raman spectroscopy experiments performed under pressure indicated the insertion of a small number of guest molecules. Ethylene glycol is partially retained inside mordenite upon pressure release. A symmetry lowering was observed in s.o. above 0.8 GPa, while above 1.6 GPa the patterns indicated a rapid loss of long range order. From ambient pressure (P amb ) to 1.6 GPa, a high cell volume contraction (DV = À9.5%) was determined. The patterns collected with penetrating PTM suggested the penetration of guest molecules into the porous host matrix, starting from a very low P regime. The entrapment of PTM molecules inside micropores contributes to the stiffening of the structure and, as a consequence, to the decrease of the compressibility with respect to that measured in s.o. From the structural point of view, HS-MOR reacts to compression and to the penetration of different guest species with appropriate framework deformations. Interestingly, ethylene glycol is partially retained inside mordenite upon pressure release, which is of importance for potential application of this composite material.

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Irreversible Conversion of a Water–Ethanol Solution into an Organized Two‐Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure

et al. 2017

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Turning disorderi nto organization is ak ey issue in science.B ym aking use of X-rayp owder diffraction and modeling studies,w es how herein that high pressures in combination with the shape and space constraints of the hydrophobic all-silica zeolite ferrierite separate an ethanolwater liquid mixture into ethanol dimer wires and water tetramer squares.T he confined supramolecular blocks alternate in ab inary two-dimensional (2D) architecture that remains stable upon complete pressure release.T hese results support the combined use of high pressures and porous networks as av iable strategy for driving the organization of molecules or nano-objects towards complex, pre-defined patterns relevant for the realization of novel functional nanocomposites.Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under: http://dx.

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Gismondine under HP: Deformation mechanism and re-organization of the extra-framework species

Cited by 42 publications

References 58 publications

Elastic behavior of MFI-type zeolites: Compressibility of H-ZSM-5 in penetrating and non-penetrating media

Elastic behavior of MFI-type zeolites: Compressibility of H-ZSM-5 in penetrating and non-penetrating media

Pressure-induced penetration of guest molecules in high-silica zeolites: the case of mordenite

Irreversible Conversion of a Water–Ethanol Solution into an Organized Two‐Dimensional Network of Alternating Supramolecular Units in a Hydrophobic Zeolite under Pressure

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