Correlative high-resolution imaging of hydrogen in Mg2Ni hydrogen storage thin films

Abstract

Nanometer scale imaging of hydrogen in solid materials remains an important challenge for the characterization of advanced materials, such as semiconductors, high-strength metallic alloys, and hydrogen storage materials. Within this work, we demonstrate high-resolution imaging of hydrogen and deuterium within Mg2Ni/Mg2NiH4 hydrogen storage thin films using an in-house developed secondary ion mass spectrometer (SIMS) system attached to a commercially available dual-beam focused ion beam - scanning electron microscope (FIB-SEM) instrument. We further demonstrate a novel approach to measure the size, shape, and distribution of the hydride phase in partially transformed films using laser scanning confocal microscopy (LSCM) to measure surface topography changes from the hydride phase volume expansion. Combining these techniques provides new insights on hydride nucleation and growth within the Mg2NiHx system. Finally, we demonstrate the efficacy of tracking deuterium as a hydrogen analog to reduce the background for SIMS imaging of hydrogen in high-vacuum chambers (∼10−6 mbar).