Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
Structural Study of Hexagonal Close-Packed Silica Mesoporous Crystal
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK), Inorganic and Structural Chemistry.
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK), Inorganic and Structural Chemistry.
Show others and affiliations
2013 (English)In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 25, no 10, 2184-2191 p.Article in journal (Refereed) Published
Abstract [en]

Close-packed spheres can be stacked into two crystalline structures: cubic close-packed (ccp) and hexagonal close-packed (hcp). Both of these structures were found in silica mesoporous crystals (SMCs). Herein, pure hcp mesostructure with P6(3)/mmc symmetry of silica mesoporous crystals (SMCs) has been obtained in the synthetic system of cationic gemini surfactant as template and the N-[(3-trimethoxysilyl)propyl]ethylenediamine triacetix acid trisodium salt (EDTA-silyl) as the costructure directing agent (CSDA), which gives rise to the three-dimensional (3D) hexagonal structure and hexagonal plate morphology. The formation of the pure hcp structure was controlled by organic/inorganic interface curvature induced by charge matching between carboxylate groups of the CSDA and quaternary ammonium head groups of surfactant. Electrostatic potential distribution 3D map was reconstructed using Fourier analysis of HRTEM images based on electron crystallography, which showed characteristic features of the shape and connectivity of mesopores in the hcp structure. Small windows for connecting cages can be found only between layers, which determine the symmetry and local curvature of structures. As a result, the point group symmetry of mesopores becomes (6) over bar m2, instead of the m (3) over barm symmetry observed for perfect spheres in the ccp. The mechanism of stabilization and favorable growth of the pure hcp structure in mesoscale has been proposed based on synthesis strategy and symmetry support. This work provides people a better understanding of the priority of two sphere close-packed forms by comparing hcp and ccp structures.

Place, publisher, year, edition, pages
2013. Vol. 25, no 10, 2184-2191 p.
Keyword [en]
silica mesoporous crystals, surfactant, costructure directing agent, hexagonal close-packing, electron microscopy
National Category
Chemical Sciences
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-92019DOI: 10.1021/cm401294jISI: 000319856000023OAI: oai:DiVA.org:su-92019DiVA: diva2:637346
Funder
Swedish Research CouncilKnut and Alice Wallenberg Foundation
Note

AuthorCount:6;

Available from: 2013-07-17 Created: 2013-07-15 Last updated: 2017-12-06Bibliographically approved
In thesis
1. Structural study of nano-structured materials: electron crystallography approaches
Open this publication in new window or tab >>Structural study of nano-structured materials: electron crystallography approaches
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The structural analysis serves as a bridge to link the structure of materials to their properties. Revealing the structure details allows a better understanding on the growth mechanisms and properties of materials, and a further designed synthesis of functional materials. The widely used methods based on X-ray diffraction have certain limitations for the structural analysis when crystals are small, poorly crystallized or contain many defects. As electrons interact strongly with matter and can be focused by electromagnetic lenses to form an image, electron crystallography (EC) approaches become prime candidates for the structural analysis of a wide range of materials that cannot be done using X-rays, particularly nanomaterials with poor crystallinity.

Three-dimensional electron diffraction tomography (3D EDT) is a recently developed method to automatically collect 3D electron diffraction data. By combining mechanical specimen tilt and electronic e-beam tilt, a large volume of reciprocal space can be swept at a fine step size to ensure the completeness and accuracy of the diffraction data with respect to both position and intensity. Effects of the dynamical scattering are enormously reduced as most of the patterns are collected at conditions off the zone axes. In this thesis, 3D EDT has been used for unit cell determination (COF-505), phase identifications and structure solutions (ZnO, Ba-Ta3N5, Zn-Sc, and V4O9), and the study of layer stacking faults (ETS-10 and SAPO-34 nanosheets).

High-resolution transmission electron microscope (HRTEM) imaging shows its particular advantages over diffraction by allowing observations of crystal structure projections and the 3D potential map reconstruction. HRTEM imaging has been used to visualize fine structures of different materials (hierarchical zeolites, ETS-10, and SAPO-34). Reconstructed 3D potential maps have been used to locate the positions of metal ions in a woven framework (COF-505) and elucidate the pore shape and connectivity in a silica mesoporous crystal.

The last part of this thesis explores the combination with X-ray crystallography to obtain more structure details.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2016. 101 p.
Keyword
structural analysis, electron crystallography, 3D EDT, HRTEM imaging, defects
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-129233 (URN)978-91-7649-425-7 (ISBN)
Public defence
2016-06-08, Magnéli Hall, Arrhenius Laboratory, Svante arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Funder
Swedish Research Council, 1486801
Available from: 2016-05-16 Created: 2016-04-18 Last updated: 2017-02-23Bibliographically approved

Open Access in DiVA

No full text

Other links

Publisher's full text

Search in DiVA

By author/editor
Ma, YanhangOleynikov, PeterTerasaki, Osamu
By organisation
Inorganic and Structural Chemistry
In the same journal
Chemistry of Materials
Chemical Sciences

Search outside of DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric score

doi
urn-nbn
Total: 42 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf