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Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis
Published on: March 29, 2016
In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes
Marta Perxés Perich1, Jan-Willem Lankman1, Claudia J Keijzer1
1Materials Chemistry and Catalysis, Debye Institute for Nanomaterials Science, Utrecht University, 3584 CG Utrecht, The Netherlands.
Nano Letters
|March 25, 2025
Summary
Researchers dynamically studied hydrogen storage in palladium nanocubes using 4D-STEM. They quantified lattice strain during reversible hydride formation and release, revealing key insights into nanoparticle behavior.
Area of Science:
- Materials Science
- Nanotechnology
- Physical Chemistry
Background:
- Hydrogen storage materials rely on efficient hydrogen uptake and release.
- Lattice strain in metal nanoparticles influences hydride formation.
- Quantifying strain in nanoparticles during gas exposure is challenging.
Purpose of the Study:
- To dynamically investigate reversible hydride formation in individual palladium nanocubes.
- To quantitatively assess lattice strain during hydrogen uptake and release at the single nanoparticle level.
- To demonstrate the utility of 4D-STEM for in situ strain analysis in gas environments.
Main Methods:
- Utilized 4D scanning transmission electron microscopy (4D-STEM).
- Performed in situ experiments with individual palladium nanocubes under 1 bar H2 pressure.
- Quantified lattice strain with subnanometer resolution during dynamic hydrogen cycling.
Main Results:
- Observed reversible hydride formation and desorption in palladium nanocubes.
- Quantified a ~3.1% lattice expansion upon hydride formation at 125 °C.
- Measured lattice relaxation upon hydrogen desorption at 200 °C.
Conclusions:
- 4D-STEM enables dynamic, in situ quantification of lattice strain in nanoparticles during gas interactions.
- Lattice strain plays a crucial role in the reversible hydride formation of palladium nanocubes.
- The methodology is applicable to various nanoparticle systems, including catalysts and gas sensors.

