Atom Probe Analysis of Ex Situ Gas-Charged Stable Hydrides

TL;DR

This study demonstrates the feasibility of using atom probe tomography to analyze hydrogen in metallic hydrides charged ex situ, enabling atomic-scale 3D imaging of hydrogen distribution within these materials.

Contribution

It introduces a method for ex situ hydrogen analysis in hydrides using atom probe tomography, which was not previously demonstrated.

Findings

Successful atom probe analysis of deuterium in Pd/Rh alloys.

Detection of deuterium at the oxide-metal interface of vanadium.

Validation of ex situ hydrogen analysis as a practical approach.

Abstract

In this work, we report on the atom probe tomography analysis of two metallic hydrides formed by pressurized charging using an ex situ hydrogen charging cell, in the pressure range of 200-500 kPa (2-5 bar). Specifically we report on the deuterium charging of Pd/Rh and V systems. Using this ex situ system, we demonstrate the successful loading and subsequent atom probe analysis of deuterium within a Pd/Rh alloy, and demonstrate that deuterium is likely present within the oxide-metal interface of a native oxide formed on vanadium. Through these experiments, we demonstrate the feasibility of ex situ hydrogen analysis for hydrides via atom probe tomography, and thus a practical route to three-dimensional imaging of hydrogen in hydrides at the atomic scale.