Many thermoelectric materials benefit from complex microstructures. Grain boundaries (GBs) in nanocrystalline thermoelectrics cause desirable reduction in the thermal conductivity by scattering phonons, but often lead to unwanted loss in the electrical conductivity by scattering charge carriers. Therefore, modifying GBs to suppress their electrical resistivity plays a pivotal role in the enhancement of thermoelectric performance, zT. In this work, different characteristics of GB phases in Ti‐doped NbFeSb half‐Heusler compounds are revealed using a combination of scanning transmission electron microscopy and atom probe tomography. The GB phases adopt a hexagonal close‐packed lattice, which is structurally distinct from the half‐Heusler grains. Enrichment of Fe is found at GBs in Nb_0.95Ti_0.05FeSb, but accumulation of Ti dopants at GBs in Nb_0.80Ti_0.20FeSb, correlating to the bad and good electrical conductivity of the respective GBs. Such resistive to conductive GB phase transition opens up new design space to decouple the intertwined electronic and phononic transport in thermoelectric materials.

Atom probe results of the NMC811 sample from an ultra-high vacuum vs. air transferring.

A Pt₃Mn intermetallic ORR electrocatalyst was synthesized using a facile synthesis without using additional multi-steps, and exhibits superior single-cell performance and durability.

Atom probe tomography requires needle-shaped specimens with a diameter typically below 100 nm, making them both very fragile and reactive, and defects (notches at grain boundaries or precipitates) are known to affect the yield and data quality. The use of a conformal coating directly on the sharpened specimen has been proposed to increase yield and reduce background. However, to date, these coatings have been applied ex situ and mostly are not uniform. Here, we report on the controlled focused-ion beam in situ deposition of a thin metal film on specimens immediately after specimen preparation. Different metallic targets e.g. Cr were attached to a micromanipulator via a conventional lift-out method and sputtered using Ga or Xe ions. We showcase the many advantages of coating specimens from metallic to nonmetallic materials. We have identified an increase in data quality and yield, an improvement of the mass resolution, as well as an increase in the effective field-of-view. This wider field-of-view enables visualization of the entire original specimen, allowing to detect the complete surface oxide layer around the specimen. The ease of implementation of the approach makes it very attractive for generalizing its use across a very wide range of atom probe analyses.

Capping ligands are crucial to synthesizing colloidal nanoparticles with functional properties. However, the synergistic effect between different ligands and their distribution on crystallographic surfaces of nanoparticles during colloidal synthesis is still unclear despite powerful spectroscopic techniques, due to a lack of direct imaging techniques. In this study, atom probe tomography is adopted to investigate the three-dimensional atomic-scale distribution of two of the most common types of these ligands, cetrimonium (C₁₉H₄₂N) and halide (Br and Cl) ions, on Pd nanoparticles. The results, validated using density functional theory, demonstrate that the Br anions adsorbed on the nanoparticle surfaces promote the adsorption of the cetrimonium cations through electrostatic interactions, stabilizing the Pd {111} facets. In contrast, the Cl anions are not strongly adsorbed onto the Pd surfaces. The high density of adsorbed cetrimonium cations for Br anion additions results in the formation of multiple-twinned nanoparticles with superior oxidation resistance.