Graphene encapsulation enabled high-throughput atom probe tomography of liquid specimens

Abstract

A new method for imaging liquid specimens with atom probe tomography (APT) is proposed by introducing graphene encapsulation. By tuning the encapsulation speed and the number of encapsulations, controllable volumes of liquid can be encapsulated on a pre-sharpened specimen tip, with the end radius less than 75 nm to allow field ionization and evaporation. Encapsulation of liquid has been confirmed by using various characterization techniques, including electron microscopy and stimulated emission depletion microscopy. The graphene-encapsulated liquid specimen was then directly frozen at the cryogenic stage inside the atom probe instrument, followed by APT imaging in laser-pulsed mode. Using water as a test example, water-related ions have been identified in the acquired mass spectrum, which are spatially correlated to a reconstructed three-dimensional volume of water on top of the base specimen tip, as clearly revealed in the chemical maps. In addition, the proposed method has also been shown to produce multiple liquid specimens simultaneously on a pre-sharpened silicon micro-tip array for high-throughput APT imaging of liquid specimens. It is expected that the proposed lift-out-free method for preparing APT specimens in their hydrated state will open a new avenue for obtaining insights into various materials at atomic resolution.