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There has been an increasing interest in atom probe tomography (APT) tocharacterise hydrated and biological materials. A major benefit of APT comparedto microscopy techniques more commonly used in biology is its combination ofoutstanding 3D spatial resolution (~0.2 nm) and mass sensitivity. APT hasalready been successfully used to characterise biological materials, revealingkey structural information at the atomic scale, however there are manychallenges inherent to the analysis of hydrated materials. New preparationprotocols, often involving sample preparation and transfer at cryogenictemperature, enable APT analysis of hydrated materials and have the potentialto enable 3D atomic scale characterisation of biological materials in thenear-native hydrated state. In this study, APT specimens of pure water at thetips of tungsten needles were prepared at room temperature by grapheneencapsulation. A parametric study was conducted where samples were transferredat either room temperature or cryo-temperature and analysed by APT by varyingparameters such as the flight path and pulsing mode. The differences betweenthe acquisition scenarios are presented along with recommendations for futurestudies.

Nanoscale Analysis of Frozen Water by Atom Probe Tomography Using Graphene Encapsulation and Cryo-Workflows: A Parametric Study