In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes

Marta Perxés Perich; Jan Willem Lankman; Claudia J. Keijzer; Jessi E.S. van der Hoeven

doi:10.1021/acs.nanolett.5c00702

In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes

Marta Perxés Perich, Jan Willem Lankman, Claudia J. Keijzer, Jessi E.S. van der Hoeven^*

^*Corresponding author for this work

Utrecht University

Research output: Contribution to journal › Letter › Academic › peer-review

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.

Original language	English
Pages (from-to)	5444-5451
Journal	Nano Letters
Volume	25
Issue number	13
Early online date	25 Mar 2025
DOIs	https://doi.org/10.1021/acs.nanolett.5c00702
Publication status	Published - 2 Apr 2025

Bibliographical note

Publisher Copyright:
© 2025 The Authors. Published by American Chemical Society.

Keywords

4D-STEM
hydride formation
in situ electron microscopy
lattice strain
palladium nanoparticles

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perxés-perich-et-al-2025-in-situ-gas-phase-4d-stem-for-strain-mapping-during-hydride-formation-in-palladium-nanocubesFinal published version, 7.3 MBLicence: CC BY

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title = "In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes",

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.",

keywords = "4D-STEM, hydride formation, in situ electron microscopy, lattice strain, palladium nanoparticles",

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T1 - In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes

AU - Perxés Perich, Marta

AU - Lankman, Jan Willem

AU - Keijzer, Claudia J.

AU - van der Hoeven, Jessi E.S.

PY - 2025/4/2

Y1 - 2025/4/2

N2 - 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.

AB - 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.

KW - 4D-STEM

KW - hydride formation

KW - in situ electron microscopy

KW - lattice strain

KW - palladium nanoparticles

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U2 - 10.1021/acs.nanolett.5c00702

DO - 10.1021/acs.nanolett.5c00702

M3 - Letter

AN - SCOPUS:105000774138

SN - 1530-6984

VL - 25

SP - 5444

EP - 5451

JO - Nano Letters

JF - Nano Letters

IS - 13

ER -

In Situ Gas-Phase 4D-STEM for Strain Mapping during Hydride Formation in Palladium Nanocubes

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Keywords

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