Criteria and considerations for preparing atom-probe tomography specimens of nanomaterials utilizing an encapsulation methodology

Atom-probe tomography (APT) is a powerful method for characterization of nanomaterials due to its atomic-ppm level detection limit and Angstrom spatial resolution. Sample preparation for nanomaterials is, however, challenging because of their small dimensions and complicated geometries. Nanowires, with their high geometrical aspect ratio and nanowire length, 10 to 100 times their typical diameters, are highly suitable specimens for APT analyses, which can be transferred to silicon microposts using a nanomanipulator for direct APT measurements. This method is, however, prone to poor alignment and a limited field-of-view (FOV). Most importantly, direct implementation of APT with high aspect ratio nanowires may yield a low success rate of ∼30%, due to the high electric fields (10–40 V nm⁻¹) associated with APT. While this is acceptable for samples analyzed solely by APT, a low sample yield makes it challenging to perform correlative experiments on the same nanowire specimen, utilizing other sophisticated characterization instruments. Herein, we introduce a general strategy for preparing high-yield APT specimens by encapsulating the nanowires utilizing a conformal atomic-layer deposition (ALD) coating followed by site-specific lift-out using a dual-beam focused-ion beam microscope. The ALD deposited coating forms strong chemical bonds with the Si nanowires yielding a high-quality and robust interface. The evaporation electric fields of the ALD coating and the nanowires are tuned by changing laser energy to obtain a uniform evaporation rate. The strong adhesion of the ALD-coating/nanowire interface and uniform evaporation rate produce a >90% specimen yield, with small concentration of reconstruction artifacts in 3-D. Simultaneously, the field-of-view is enhanced and the surface of the nanowire becomes visible, which makes the study of surface adsorption, segregation and oxidation possible. We utilized ALD-ZnO coated silicon nanowires as an example for investigating the criteria for choosing coating materials, laser pulse energy, laser direction, sample geometry, and substrate materials. The same criteria and considerations are applicable for preparing specimens of nanoparticles and 2-D material.