Local anisotropy in single crystals of zeotypes with the MFI framework structure evidenced by polarised Raman spectroscopy

Martinelli, Anna; Creci, Simone; Vavra, Szilvia; Carlsson, Per-Anders; Skoglundh, Magnus

doi:10.1039/c9cp06199a

Cited by 14 publications

(10 citation statements)

References 46 publications

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“…Many peaks are observed in the region below 290 cm –1 corresponding to further Si–O–Si bending modes and lattice modes. These modes have previously been observed in Raman spectra of monoclinic calcined MFI samples at room temperature . They correspond to broad features in the spectra of the orthorhombic form indicating an increase in order in the monoclinic form.…”

Section: Results and Discussionsupporting

confidence: 65%

“…These modes have previously been observed in Raman spectra of monoclinic calcined MFI samples at room temperature. 65 They correspond to broad features in the spectra of the orthorhombic form indicating an increase in order in the monoclinic form. In contrast, for TPEA-F-HT, a different behavior is observed.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Based on group theory, the framework of orthorhombic MFI gives rise to 432 Raman-active modes of vibrations as follows: 110 A g + 106 B 1g + 110 B 2g and 106 B 3g . The OSDA will also contribute, TPA with S 4 symmetry will give rise to 29 A + 30 B + 29 E modes .…”

Section: Methodsmentioning

confidence: 99%

“…Based on group theory, the framework of orthorhombic MFI gives rise to 432 Raman-active modes of vibrations as follows: 110 A g + 106 B 1g + 110 B 2g and 106 B 3g . 65 The OSDA will also contribute, TPA with S 4 symmetry will give rise to 29 A + 30 B + 29 E modes. 63 This symmetry is broken in the case of TPEA leading to the absence of degenerate modes and will also have nine fundamental modes less due to the replacement of a propyl by an ethyl group.…”

Section: = • • S X Ymentioning

confidence: 99%

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Host–Guest Silicalite-1 Zeolites: Correlated Disorder and Phase Transition Inhibition by a Small Guest Modification

et al. 2021

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We have investigated the nature and extent of nanoscale disorder in prototypical host-guest zeolites, made of silicalite-1 (host) and organic structure directing agent (OSDA, guest). The four different selected OSDA-silicalite-1 differ in: the mineralizing agent used (Fvs. OH -), the synthesis' method (hydrothermal vs. solvent-free) and the OSDA (tetrapropylammonium TPA vs. tripropylethylammonium TPEA). The comparison between TPA and TPEA, chemically similar but differing in their symmetry, is examined in great detail owing to the novel relationship found between the geometrical disorder and the monoclinic-orthorhombic (m-o) phase transition occurring at low temperature. Long-and short-range organization and ordering are characterized by complementary XRD, Raman and multinuclear NMR ( 13 C, 14 N, 29 Si). The possibility of the m-o transition is studied by all these techniques at variable low T. An in-depth study of the disorder is carried out by x-ray structure determination and 2D NMR 29 Si-29 Si INADEQUATE correlations, including an up-to-date analysis of anisotropic atomic displacement parameters and a new fitting approach to estimate correlated disorder from 2D NMR datasets. The collected results allow to demonstrate how the disorder created by the positioning of the less symmetric TPEA guest leads to a correlated geometrical disorder for half of the atom sites in the host framework that completely inhibits the m-o phase transition.

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Section: Results and Discussionsupporting

confidence: 65%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: = • • S X Ymentioning

confidence: 99%

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Host–Guest Silicalite-1 Zeolites: Correlated Disorder and Phase Transition Inhibition by a Small Guest Modification

et al. 2021

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“…those of the 6MR at about 360 cm −1 , seen as a low energy shoulder of the 383 cm −1 line, being next to the 294 cm −1 line due to the 10MR. 53 The Si–O–Si and O–Si–O stretching modes appeared as a band in the range 800–832 cm −1 . 52,53 While the spectrum in Fig.…”

Section: Resultsmentioning

confidence: 98%

Tracking carbon dioxide adsorbate intramolecular dynamics in pure silica zeolite Silicalite-1 by in situ Raman scattering

Tzankov,

Georgiev

2024

Phys. Chem. Chem. Phys.

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Fundamentals and Applications of Raman‐Based Techniques for the Design and Development of Active Biomedical Materials

2023

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Raman spectroscopy is an analytical method based on light‐matter interactions that can interrogate the vibrational modes of matter and provide representative molecular fingerprints. Mediated by its label‐free, non‐invasive nature and high molecular specificity, Raman‐based techniques have become ubiquitous tools for in situ characterisation of materials. This review comprehensively describes the theoretical and practical background of Raman spectroscopy and its advanced variants. We highlight the numerous facets of material characterisation that Raman scattering can reveal, including biomolecular identification, solid‐to‐solid phase transitions and spatial mapping of biomolecular species in bioactive materials. The review illustrates the potential of these techniques in the context of active biomedical material design and development by highlighting representative studies from the literature. These studies cover the use of Raman spectroscopy for the characterisation of both natural and synthetic biomaterials, including engineered tissue constructs, biopolymer systems, ceramics and nanoparticle formulations, among others. To increase the accessibility and adoption of these techniques, the present review also provides the reader with practical recommendations on the integration of Raman techniques into the experimental laboratory toolbox. Finally, we provide perspectives on how recent developments in plasmon‐ and coherently‐enhanced Raman spectroscopy can propel Raman from underutilised to critical for biomaterial development.This article is protected by copyright. All rights reserved

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Local anisotropy in single crystals of zeotypes with the MFI framework structure evidenced by polarised Raman spectroscopy

Abstract: Polarised Raman spectroscopy is used to reveal the orientation of specific T–O–T bonds in singe crystals of ZSM-5 and silicalite-1.

Cited by 14 publications

References 46 publications

Host–Guest Silicalite-1 Zeolites: Correlated Disorder and Phase Transition Inhibition by a Small Guest Modification

Host–Guest Silicalite-1 Zeolites: Correlated Disorder and Phase Transition Inhibition by a Small Guest Modification

Tracking carbon dioxide adsorbate intramolecular dynamics in pure silica zeolite Silicalite-1 by in situ Raman scattering

Fundamentals and Applications of Raman‐Based Techniques for the Design and Development of Active Biomedical Materials

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