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Updated: Aug 12, 2026

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.
Abstract:
The uptake and release of hydrogen are key parameters for hydrogen storage materials. Lattice strain offers a powerful way to tune hydride formation in metal nanoparticles. However, the role of strain on hydride formation is difficult to assess on a single nanoparticle level due to the lack of in situ characterization tools to quantify strain in the presence of a gas. Here, we achieve a dynamic, in situ study on the reversible hydride formation in individual palladium nanocubes by applying 4D scanning transmission electron microscopy (4D-STEM) in the presence of 1 bar H2 and quantitatively assess the lattice strain with subnanometer resolution. Upon hydride formation at 125 °C, the Pd lattice expands by ∼3.1% and relaxes back upon hydrogen desorption at 200 °C. Our in situ 4D-STEM approach is relevant to a wide range of nanoparticle systems and applications, including catalyst- and gas-sensing materials.

