With the wide application of ultra-microtome sectioning in the preparation of transmission electron microscopy (TEM) specimens with bio- and organic materials, here, we report an ultra-microtome-based method for the preparation of TEM specimens from cathodes of Li-ion batteries. The ultra-microtome sectioning reduces the sample thickness to tens of nanometers and yields atomic resolution from the core region of particles of hundreds of nanometers. Analysis indicates that the mechanical cross-sectioning introduces no observable microstructural artifacts or structural damage, such as microcracking and nanoporosity. These results demonstrate the high efficiency of the ultra-microtome approach in preparing well-thinned specimens of particulate materials that allow for atomic-scale TEM imaging of a large number of sectioned particles in one single TEM specimen, thereby providing statistically significant results of the TEM analysis.

We report a facile method to fabricate CuNi nano-octahedra and nanocubes using a colloidal synthesis approach. The CuNi nanocrystals terminated with exclusive crystallographic facets were controlled and achieved by a group of synergetic capping ligands in a hot solution system. Specifically, the growth of {111}-bounded CuNi nano-octahedra is derived by a thermodynamic control, whereas the generation of {100}-terminated CuNi nanocubes is steered by a kinetic capping of chloride. Using a reduction of 4-nitrophenol with sodium borohydride as a model reaction, CuNi nano-octahedra and nanocubes demonstrated a strong facet-dependence due to their different surface energies although both exhibited remarkable catalytic activity with the high rate constant over mass (k/m). A kinetic study indicated that this is a pseudo first-order reaction with an excess of sodium borohydride. CuNi nanocubes as the catalysts showed better catalytic performance (k/m = 385 s-1•g-1) than the CuNi nano-octahedra (k/m = 120 s-1•g-1), indicating that 4-nitrophenol and hydrogen were adsorbed on the {100} facets with their molecules parallel to the surface much easier than those on {111} facets.

Using in situ transmission electron microscopy, we report the observation of the melting behavior of one-dimensional nanostructures of Sn with different length/width aspect ratios. The melting of small aspect-ratio nanowires (nanorods) results in the expansion of liquid Sn along both axial and radial directions with the tendency to form an isometric or spherical particle, thereby minimizing the total surface area. For nanowires with the length/width aspect ratio of ∼10.5, perturbation along the liquid stream causes an unstable necking phenomenon and the whole wire tends to shrink into a spherical particle. In contrast, Rayleigh instability sets in for the melting of the nanowires with the length/width aspect ratio as large as ∼21, which gives rise to necking and fragmentation of the wire into particles. The amorphous native surface oxide (SnO x ) layer serves as a confinement tube and plays an important role in the melting induced morphological evolution of Sn nanowires. A thin SnO x layer is flexible with the ability to shrink or expand upon the flow of molten Sn. The increased rigidity for a thick SnO x surface layer kinetically suppresses bulging and necking formation in molten Sn nanowires.