Tutorial: structural characterization of isolated metal atoms and subnanometric metal clusters in zeolites

Lichen Liu, Miguel Lopez-Haro, Jose J. Calvino, Avelino Corma

Published: 2020-09-03 DOI: 10.1038/s41596-020-0366-9

subnanometric metal clusters

zeolites

STEM-iDPC imaging

catalytic reactions

structural characterization

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The encapsulation of subnanometric metal entities (isolated metal atoms and metal clusters with a few atoms) in porous materials such as zeolites can be an effective strategy for the stabilization of those metal species and therefore can be further used f
Introduction
Generation and stabilization of isolated Pt atoms and subnanometric Pt clusters in MFI zeolite
Materials
- Reagents
- Equipment
Procedure
Timing
Troubleshooting
Preliminary characterization of the Pt-zeolite materials
Structural characterization of the Pt–nobreakzeolite materials by HR STEM
Complementary characterization with other techniques
Extension of the STEM–nobreakiDPC technique
Limitations of the current technique and outlooks
References
ACKNOWLEDGMENTS

Figure 1
Fig. 1: One-pot synthesis of Pt–zeolite materials.
Figure 2
Fig. 2: XRD patterns of the Pt–MFI zeolites with different chemical compositions.
Figure 3
Fig. 3: FESEM images of Pt–zeolite materials.
Figure 4
Fig. 4: HAADF–STEM images of K-free Pt@MFI-Air sample after calcination in air.
Figure 5
Fig. 5: HAADF–STEM images of K-Pt@MFI-Air sample after calcination in air.
Figure 6
Fig. 6: HAADF–STEM images of K-free Pt@MFI sample after calcination in air at 600 °C and then further reduction by H2 at 600 °C.
Figure 7
Fig. 7: HAADF–STEM images of K-Pt@MFI sample after calcination in air at 600 °C and then further reduction by H2 at 600 °C.
Figure 8
Fig. 8: STEM image of Pt–zeolite samples after reduction by H2 at 600 °C.
Figure 9
Fig. 9
Figure 10
Fig. 10: Stability test of the K-PtSn@MFI sample under the beam.
Figure 11
Fig. 11: Influence of defocus value on the imaging of isolated Pt atoms.
Figure 12
Fig. 12: Influence of defocus value on the imaging of isolated Sn atoms.
Figure 13
Fig. 13: Image simulation of isolated Pt and Sn atoms in MFI zeolite.
Figure 14
Fig. 14: Image simulation of Pt and Sn species in MFI zeolite.
Figure 15
Fig. 15: Image simulation of Pt and Sn species in MFI zeolite.
Figure 16
Fig. 16: Image simulation of Pt clusters comprising interaction with Sn species in MFI zeolite.
Figure 17
Fig. 17: Characterization of K-Pt@MFI-Air sample by STEM–iDPC imaging technique.
Figure 18
Fig. 18: Identification of the location of subnanometric Pt clusters within the MFI structure.
Figure 19
Fig. 19: Correlation between the simulated image and experimental STEM–iDPC images.
Figure 20
Fig. 20: Chemical analysis on the K-PtSn@MFI sample by EDS.
Figure 21
Fig. 21: K-means clustering analysis on the simulated images.
Figure 22
Fig. 22: Distinguishing subnanometric Pt and Sn species by K-means clustering analysis.
Figure 23
Fig. 23: PtSn clusters in experimental HAADF–STEM images.
Figure 24
Fig. 24: Characterization of the Pt–zeolite materials after calcination in air by XAS.
Figure 25
Fig. 25: Characterization of Pt–zeolite materials by XAS.
Figure 26
Fig. 26: Comparison of the Sn-edge XAS results of K-PtSn@MFI-Air sample with Sn-Beta.
Figure 27
Fig. 27: CO-IR spectra of K-PtSn@MFI and K-Pt@MFI samples.

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Tutorial: structural characterization of isolated metal atoms and subnanometric metal clusters in zeolites

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