We describe a novel method for in situ measurement of the local thickness of a freely suspended solid-state membrane after thinning with a focused helium ion beam. The technique utilizes a custom stage for the helium ion microscope that allows the secondary electron detector used for normal imaging to collect information from ions transmitted through the sample. We find that relative brightness in the transmission image scales directly with the membrane thickness as determined by atomic force microscopy measurements.

This study examines the nature of highly fragile reaction products that form in low water content supercritical carbon dioxide (scCO2) using a combination of focus ion beam/scanning electron microscopy, confocal Raman spectroscopy, helium ion microscopy (HeIM), and transmission electron microscopy (TEM). HeIM images show these precipitates are fragile rosettes. Using the TEM revealed details on the interfacial structure between the newly formed surface precipitates and the underlying initial solid phases. Detailed microscopy analysis revealed that growth of the precipitates either followed a tip growth mechanism, with precipitates forming directly on the forsterite surface if the initial solid was nonporous (natural forsterite) or growth from the surface of the precipitates, where fluid was conducted through the porous (nanoforsterite) agglomerates to the growth center. Identification of the mechanism of formation of hydrated/hydroxylated magnesium carbonate compound phases is a key factor in unraveling the impact of water recycling on mineral reactivity in low water content scCO2 solutions, which has received a great deal of attention as a result of the potential for CO2 to act as an atmospheric greenhouse gas. Techniques used here to examine these fragile structures are also used to examine a wide range of fragile material surfaces.