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Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography
Published on: June 9, 2018
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Cryogenic electron tomography reveals the mesoporous structure evolution during γ-Al2O3 supported Mo and MoNiP
Jason M J J Heinrichs1,2, Angelina Evtushkova1, Jovana Zečević3
1Laboratory of Inorganic Materials and Catalysis, Department of Chemical Engineering and Chemistry, Eindhoven University of Technology (TU/e) Den Dolech 2 5600 MB Eindhoven The Netherlands e.j.m.hensen@tue.nl.
Summary
Cryogenic electron tomography revealed the 3D mesopore structure of gamma-alumina supports during hydrodesulfurization catalyst preparation. The support structure remained stable, with subtle changes observed upon metal deposition and sulfidation.
Area of Science:
- Materials Science
- Catalysis
- Chemical Engineering
Background:
- Heterogeneous catalysts are crucial for industrial processes.
- Understanding support mesoporosity evolution during catalyst preparation is incomplete.
- Hydrodesulfurization (HDS) catalysts rely on specific support structures.
Purpose of the Study:
- To resolve the 3D mesopore structure of gamma-alumina (γ-Al2O3) supports.
- To assess structural changes induced by metal deposition (Mo, MoNiP) and sulfidation.
- To provide a 3D perspective on mesopore stability during HDS catalyst preparation.
Main Methods:
- Cryogenic electron tomography (cryo-ET) was employed to image the 3D mesopore structure.
- Analysis focused on γ-Al2O3 supports before and after Mo/MoNiP deposition and sulfidation.
- Image segmentation allowed separate analysis of the support and active MoS2 phases.
Main Results:
- The intrinsic γ-Al2O3 mesopore structure showed high stability during calcination and sulfidation.
- Mo deposition slightly increased pore tortuosity and surface corrugation; MoNiP deposition had minimal impact.
- Sulfidation of both Mo and MoNiP catalysts led to more tortuous mesopores and corrugated surfaces.
Conclusions:
- Cryo-ET provides detailed 3D insights into mesopore stability during catalyst preparation.
- The γ-Al2O3 support structure is largely stable, with subtle modifications induced by processing.
- Advanced 3D imaging is essential for establishing robust structure-function correlations in catalysts.

