Details
| Original language | English |
|---|---|
| Pages (from-to) | 93-101 |
| Number of pages | 9 |
| Journal | Acta Crystallographica Section A: Foundations and Advances |
| Volume | 74 |
| Issue number | 2 |
| Publication status | Published - Mar 2018 |
| Externally published | Yes |
Abstract
Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffraction tomography (ADT), crystal disorder modelling and electron diffraction simulations. Zeolite beta was chosen for a proof-of-principle study of the techniques, because it consists of two different intergrown polymorphs that are built from identical layer types but with different stacking sequences. Imaging of the projected inner Coulomb potential of zeolite beta crystals shows the intergrowth of the polymorphs BEA and BEB. The structures of BEA as well as BEB could be extracted from one single ADT data set using direct methods. A ratio for BEA/BEB = 48:52 was determined by comparison of the reconstructed reciprocal space based on ADT data with simulated electron diffraction data for virtual nanocrystals, built with different ratios of BEA/BEB. In this way, it is demonstrated that this smart interplay of the above-mentioned techniques allows the elaboration of the real structures of functional materials in detail - even if they possess a severely disordered structure.A routine to extract diffuse-scattering intensities caused by two-dimensional crystalline defects from tomographic electron diffraction data and an algorithm for comparison with simulated diffraction data were developed and applied to intergrown zeolite beta A and zeolite beta B.
Keywords
- disorder simulation, electron diffraction tomography, in-line electron holography, polytypism, zeolite beta
ASJC Scopus subject areas
- Biochemistry, Genetics and Molecular Biology(all)
- Structural Biology
- Biochemistry, Genetics and Molecular Biology(all)
- Biochemistry
- Materials Science(all)
- General Materials Science
- Physics and Astronomy(all)
- Condensed Matter Physics
- Chemistry(all)
- Physical and Theoretical Chemistry
- Chemistry(all)
- Inorganic Chemistry
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In: Acta Crystallographica Section A: Foundations and Advances, Vol. 74, No. 2, 03.2018, p. 93-101.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Ab initio structure determination and quantitative disorder analysis on nanoparticles by electron diffraction tomography:
AU - Krysiak, Yaşar
AU - Barton, Bastian
AU - Marler, Bernd
AU - Neder, Reinhard B.
AU - Kolb, Ute
N1 - Funding information: This work was supported by INCOE mission project coordinated by BASF 400 SE, Germany. Yas¸ar Krysiak is very grateful to the Stipendienstiftung Rheinland-Pfalz and Forschung und Technologietransfer Universität Mainz for financial support.
PY - 2018/3
Y1 - 2018/3
N2 - Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffraction tomography (ADT), crystal disorder modelling and electron diffraction simulations. Zeolite beta was chosen for a proof-of-principle study of the techniques, because it consists of two different intergrown polymorphs that are built from identical layer types but with different stacking sequences. Imaging of the projected inner Coulomb potential of zeolite beta crystals shows the intergrowth of the polymorphs BEA and BEB. The structures of BEA as well as BEB could be extracted from one single ADT data set using direct methods. A ratio for BEA/BEB = 48:52 was determined by comparison of the reconstructed reciprocal space based on ADT data with simulated electron diffraction data for virtual nanocrystals, built with different ratios of BEA/BEB. In this way, it is demonstrated that this smart interplay of the above-mentioned techniques allows the elaboration of the real structures of functional materials in detail - even if they possess a severely disordered structure.A routine to extract diffuse-scattering intensities caused by two-dimensional crystalline defects from tomographic electron diffraction data and an algorithm for comparison with simulated diffraction data were developed and applied to intergrown zeolite beta A and zeolite beta B.
AB - Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffraction tomography (ADT), crystal disorder modelling and electron diffraction simulations. Zeolite beta was chosen for a proof-of-principle study of the techniques, because it consists of two different intergrown polymorphs that are built from identical layer types but with different stacking sequences. Imaging of the projected inner Coulomb potential of zeolite beta crystals shows the intergrowth of the polymorphs BEA and BEB. The structures of BEA as well as BEB could be extracted from one single ADT data set using direct methods. A ratio for BEA/BEB = 48:52 was determined by comparison of the reconstructed reciprocal space based on ADT data with simulated electron diffraction data for virtual nanocrystals, built with different ratios of BEA/BEB. In this way, it is demonstrated that this smart interplay of the above-mentioned techniques allows the elaboration of the real structures of functional materials in detail - even if they possess a severely disordered structure.A routine to extract diffuse-scattering intensities caused by two-dimensional crystalline defects from tomographic electron diffraction data and an algorithm for comparison with simulated diffraction data were developed and applied to intergrown zeolite beta A and zeolite beta B.
KW - disorder simulation
KW - electron diffraction tomography
KW - in-line electron holography
KW - polytypism
KW - zeolite beta
UR - http://www.scopus.com/inward/record.url?scp=85042882892&partnerID=8YFLogxK
U2 - 10.1107/s2053273317018277
DO - 10.1107/s2053273317018277
M3 - Article
C2 - 29493538
AN - SCOPUS:85042882892
VL - 74
SP - 93
EP - 101
JO - Acta Crystallographica Section A: Foundations and Advances
JF - Acta Crystallographica Section A: Foundations and Advances
SN - 0108-7673
IS - 2
ER -