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Improving data quality for three-dimensional electron diffraction by a post-column energy filter and a new crystal

Taimin Yang¹, Hongyi Xu¹, Xiaodong Zou¹

¹Department of Materials and Environmental Chemistry (MMK), Stockholm University, Svante Arrhenius väg 16 C, Stockholm, SE-10691, Sweden.

Journal of Applied Crystallography

|December 26, 2022

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Energy-filtered three-dimensional electron diffraction (3D ED) enhances crystal structure determination for nanomaterials. This technique improves data quality and accessibility in transmission electron microscopy (TEM) labs.

Area of Science:

Materials Science
Crystallography
Electron Microscopy

Background:

Three-dimensional electron diffraction (3D ED) is crucial for analyzing nanoscale crystal structures.
Existing 3D ED techniques can be limited by data quality and experimental accessibility.
Post-column energy filters are available in many transmission electron microscope (TEM) laboratories.

Purpose of the Study:

To implement and describe energy-filtered 3D ED using a post-column energy filter in both scanning (S)TEM and TEM modes.
To introduce a crystal tracking method in STEM mode for improved data collection.
To evaluate the impact of energy filtering on 3D ED data quality and structural analysis.

Main Methods:

Utilized a Gatan imaging filter for energy-filtered 3D ED in (S)TEM.

Keywords:

3D electron diffraction HAADF crystal tracking energy-filtered 3D ED energy-filtered MicroED microcrystal electron diffraction post-column energy filters structure determination

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Developed and applied a crystal tracking method using high-angle annular dark-field imaging in STEM mode.

Collected and compared energy-filtered and unfiltered 3D ED data from three inorganic crystalline samples.

Main Results:

Energy-filtered 3D ED data sets showed a 10-30% improvement in final R1 values compared to unfiltered data.
The resulting crystal structures from energy-filtered data were more chemically reasonable.
The crystal tracking method allowed for a larger tilt range without data loss or increased electron dose.

Conclusions:

Energy-filtered 3D ED significantly improves the accuracy and reliability of nanoscale crystal structure determination.
The implemented methods enhance the accessibility and efficiency of 3D ED using readily available equipment.
This approach offers a practical pathway to obtain higher quality structural data from crystalline nanomaterials.