In situ heating and electron-beam irradiation in the transmission electron microscope were performed to study melting of submicron Al-11.6 at. % Si particles supported on a C thin film. It was found that electron irradiation could be used to melt the particles, even when the hot-stage sample holder was kept at a much lower temperature ($\sim 125°\mathrm{C}$) than the initial melting point of the particles. Comparison between the experimentally observed melting behavior and analytical calculations indicate that melting of the submicron Al-Si particles under electron-beam irradiation is caused by a temperature rise due to electron thermal spikes in the particles and poor thermal conduction away from the particles. These results have important implications in transmission electron microscopy studies of nanoparticles supported on thin films or poorly conducting substrates.

As the length scales of materials decrease, the heterogeneities associated with interfaces become almost as important as the surrounding materials. This has led to extensive studies of emergent electronic and magnetic interface properties in superlattices^1–9. However, the interfacial vibrations that affect the phonon-mediated properties, such as thermal conductivity^10,11, are measured using macroscopic techniques that lack spatial resolution. Although it is accepted that intrinsic phonons change near boundaries^12,13, the physical mechanisms and length scales through which interfacial effects influence materials remain unclear. Here we demonstrate the localized vibrational response of interfaces in strontium titanate–calcium titanate superlattices by combining advanced scanning transmission electron microscopy imaging and spectroscopy, density functional theory calculations and ultrafast optical spectroscopy. Structurally diffuse interfaces that bridge the bounding materials are observed and this local structure creates phonon modes that determine the global response of the superlattice once the spacing of the interfaces approaches the phonon spatial extent. Our results provide direct visualization of the progression of the local atomic structure and interface vibrations as they come to determine the vibrational response of an entire superlattice. Direct observation of such local atomic and vibrational phenomena demonstrates that their spatial extent needs to be quantified to understand macroscopic behaviour. Tailoring interfaces, and knowing their local vibrational response, provides a means of pursuing designer solids with emergent infrared and thermal responses.

Many fundamental questions in crystal-growth behavior remain unanswered because of the difficulties encountered in simultaneously observing phases and determining elemental concentrations and redistributions while crystals nucleate and grow at the nanoscale. We show that these obstacles can be overcome by performing energy-dispersive x-ray spectroscopy on partially molten Al-Si-Cu-Mg alloy particles during in situ heating in a transmission electron microscope. Using this technique, we were able to (i) determine that the aluminum and silicon concentrations change in a complementary and symmetric manner about the solid-liquid interface as a function of temperature; (ii) directly measure the solid- and liquid-phase compositions at equilibrium and in highly undercooled conditions for quantitative comparison with thermodynamic calculations of the liquidus and solidus phase boundaries; and (iii) provide direct evidence for homogeneous nucleation of the aluminum-rich solid.

Measuring material properties at the nanoscale is critical to understanding the behavior of nanostructured materials. In this paper, we demonstrate a novel technique that allows direct determination and imaging of physical properties of individual nanoprecipitates and nanoparticles using energyfiltering transmission electron microscopy combined with valence electron energy-loss spectroscopy (VEELS). We show that strong scaling correlations exist between the plasmon energy and elastic properties, hardness, valence electron density and cohesive energy. We apply these scaling relationships to characterize the elastic properties of metastable nanoprecipitates in a Ti-based structural alloy and the hardness of diesel-engine soot particles. We also discuss additional factors that need to be considered when using plasmons as a quantitative tool for nanoscale property measurement. The results show that VEELS has the potential to determine multiple solid-state properties of materials at the nanoscale, establishing a new capability for analytical electron microscopy.

A model based on the near-coincidence of diffraction intensity weighted reciprocal-lattice spots is proposed to determine preferred orientation relationships between two crystalline phases. The preferred orientation is found by minimizing the three-dimensional lattice mismatch, i.e. by maximizing the total overlapping intensity, between the diffraction spots of two crystals. The procedure is biased towards matching reciprocal lattice sites with high structure-factor values, which is physically equivalent to matching planes of high atomic density. In contrast to previous reciprocal-lattice models, including the diffraction intensity in the present method makes it sensitive to the types of atoms in (chemistry of) crystals. The preferred orientation relationship is then used to identify the orientations of low-energy interfaces using a Δ g approach. A Voronoi (or Wigner–Seitz) construction based on the Δ g values is further used to qualitatively estimate the equilibrium shape of the precipitate in the matrix. The model was tested by performing calculations on hypothetical Au–Cu crystals to investigate the effects of chemistry and fcc truncated-octahedral precipitates in fcc matrices in Al–Ag, Al–Xe and Al–Pb alloys. The present model has the ability to sample the entire orientation space and rationalize and compare alternate orientation relationships in a reasonable timeframe, thereby providing insight into the formation of precipitate orientation relationships and shapes.