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Analyzing porous (nano)materials by the atom probe tomography has beennotoriously difficult. The electrostatic pressure intensifies stress at voidswhich results in premature failure of the specimen, and the electrostatic fielddistribution near voids lead to aberrations that are difficult to predict. Herewe propose a new encapsulating method for a porous sample using alow-melting-point Bi-In-Sn alloy, known as Fields metal. As a model poroussample, we used single-crystalline wustite following direct hydrogen-reducedinto iron. The complete encapsulation is performed using in-situ heating on thestage of the scanning-electron microscope up to approx. 70 Celsius. No visiblecorrosion nor dissolution of the sample occurred. Subsequently specimens areshaped by focused ion beam milling under cryogenic conditions at -190 Celsius.The proposed approach is versatile, can be applied to provide good quality atomprobe datasets from microporous materials.

A liquid metal encapsulation for analyzing porous nanomaterials by atom probe tomography