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High-resolution electron tomography on beam-sensitive carbon materials

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vts_7744_11145.pdf (21.46Mb)
131 Seiten
 
Veröffentlichung
2011-10-24
DOI
10.18725/OPARU-1928

Dissertation

Autoren
Leschner, Jens
Fakultäten
Fakultät für Naturwissenschaften
Lizenz
Standard (ohne Print-On-Demand)
https://oparu.uni-ulm.de/xmlui/license_opod_v1
Zusammenfassung
In this work a protocol for bright-field electron tomography in the transmission electron microscope (TEM) is developed. This protocol provides high resolution in 3D better than 1nm. It enables to study materials prone to radiolysis effects such as carbon materials. For the latter an aberration corrected TEM operated at a low acceleration voltage of 80kV is necessary to reduce the knock-on related beam damage. This protocol is exemplified on commercially available Vulcan XC-72 carbon soot particles which serve as a support for catalytically active nanoparticles (here platinum). This approach enables to visualize and quantify the internal three-dimensional graphitic nanostructure with ~0.35nm graphitic interplanar distance by layer distance, fringe length and tortuosity providing statistical measures for the 3D carbon volume. The protocol ensures that the sample withstands the entire tilt series acquisition by a minimum dose protocol. The appropriate imaging conditions are specified and experimentally preserved by an automatic focus and stigmation (AFS) module correcting focus and astigmatism intermittently at each tilt angle with a high accuracy required for aberration corrected high-resolution TEM. A new iterative self-consistent alignment strategy ensures high resolution in the three-dimensional reconstruction. The quantification of the entire three-dimensional carbon volume is shown to be superior to a two-dimensional projection analysis and making calibrations with x-ray data redundant.
Erstellung / Fertigstellung
2011
Normierte Schlagwörter
Durchstrahlungselektronenmikroskopie [GND]
Hochauflösendes Verfahren [GND]
Quantifizierung [GND]
Tomographie [GND]
Transmission electron microscopy [LCSH]
Schlagwörter
High-resolution; Quantification; Rußpartikel; Soot particles; Tomography
DDC-Sachgruppe
DDC 530 / Physics

Metadata
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Zitiervorlage

Leschner, Jens (2011): High-resolution electron tomography on beam-sensitive carbon materials. Open Access Repositorium der Universität Ulm. Dissertation. http://dx.doi.org/10.18725/OPARU-1928

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