We use electron energy-loss spectroscopy (EELS) in the cryo-STEM to determine the spatial distribution of water in a model frozen-hydrated two-phase polymer blend composed of hydrophilic poly(vinylpyrrolidone) (PVP) and hydrophobic poly(styrene) (PS). We demonstrate that it is possible to directly correlate the water spatial distribution with variations in the underlying polymer morphology. HAADF-STEM imaging of both dry and frozen-hydrated specimens shows weak contrast between the polymer phases but gives no information regarding the composition of these phases and no indication of where water might be localized. Spatially-resolved EELS spectra collected at 100 nm pixel size show that this system is composed of discrete PVP-rich domains dispersed in a continuous PS-rich matrix. The PVP-rich domains were found to be hydrated up to a level of ∼ 23 wt%. We have made our compositional maps fully quantitative, given as mass-fraction maps, by measuring the total inelastic scattering cross-sections per unit mass of water, PVP and PS. This is an important quantity which we have determined for an incident beam energy of 200 keV. Hydrated PVP gives rise to hydrogen evolution when irradiated above an electron dose of 1500 e/nm2 as evidenced from changes in the 13 eV region, and this effect gives rise to dose-limited resolution in these experiments.

We investigated the atomic structure near the interface and the size dependence of the mean inner potential of gold in Au/TiO2 catalysts prepared by the deposition precipitation (DP) method and the vacuum evaporation (VE) method using high resolution electron microscopy (HREM) and electron holography. The TiO2 supports prepared by DP method and VE method are considered to have oxygen-rich surfaces and titanium-rich surfaces respectively. In case of the Au/TiO2 catalyst prepared by DP method, the mean inner potential of gold increased depending on the size of the particle. When the size of the gold particle is over 5nm, the mean inner potential of gold was the same as that of bulk Au. When the size is below 5nm, the mean inner potential became to increase. It increases suddenly over 40V, particularly in case of below 2nm. It indicates that the electronic state of gold on TiO2 changes from that of bulk state as the size decreases. On the other hand, the mean inner potential of gold in Au/TiO2 catalysts prepared by VE method also increased as the size decreased, but the behavior of the size dependence is different from that of DP method. The critical size of the mean inner potential change is around 3nm. The size of the gold particle was below 3nm, the mean inner potential of gold increased gradually. The mean inner potential of VE method is less than that of DP method with the same particle size in spite of the size below 3nm. The stoichiometry at the interface between Au and TiO2 should be one of the dominant reasons for the behavior difference of the size dependence of the mean inner potential between the preparations.

It is well known that the crystallographic phase and morphology of many materials changes with the crystal size in the tens of nanometer range and that many nanocrystals possess structural defects in excess of their equilibrium levels. A need to determine the ideal and real structure of individual nanoparticles, therefore, arises. High-resolution phase-contrast transmission electron microscopy (TEM) and atomic resolution Z-contrast scanning TEM (STEM) when combined with transmission electron goniometry offer the opportunity of develop dedicated methods for the crystallographic characterization of nanoparticles in three dimensions. This paper describes tilt strategies for taking data from individual nanocrystals “as found”, so as to provide information on their lattice structure and orientation, as well as on the structure and orientation of their surfaces and structural defects. Internet based java applets that facilitate the application of this technique for cubic crystals with calibrated tilt-rotation and double-tilt holders are mentioned briefly. The enhanced viability of image-based nanocrystallography in future aberration-corrected TEMs and STEMs is illustrated on a nanocrystal model system.

LaNbO4 crystallizes in a tetragonal high-temperature phase with space group I41/a, which transforms to a monoclinic phase upon cooling below 500 °C. The low-temperature phase has space group I2/a (C2/c) with a monoclinic angle β=94.1°. This system serves as a useful model of a ferroelastic transition of the 4/mF2/m type using the notation of Aizu [1]. This transition produces ferroelastic domains, the boundaries between which are parallel to the monoclinic b-axis. The orientation of these boundaries relative to the monoclinic a- and c-axes has been predicted by Sapriel [2] for all 94 ferroelastic species, and calculations specifically for the LaNbO4 system have been presented by Jian and Wayman [3].

We present an accurate determination of the boundary orientation in LaNbO4 using selected area electron diffraction. The boundary planes are parallel to the (2 0 –5.10)/(5.10 0 2) planes of the two domains, as opposed to the predictions of Jian and Wayman which indicate that the domain boundaries should be oriented parallel to the (2 0 -4.04)/(4.04 0 2) planes. Our experimental results are in good agreement with the results of a previous study [4].

Furthermore, we present a simple geometric model for calculating the boundary orientation based only on the unit cell parameters of the monoclinic phase. This model gives a boundary orientation in excellent agreement with our experimental determination.

After some experimental results that indicated that HA is able to growth in an epitaxial way on the surface of OCP, it has been suggested that the central dark line (CDL) observed in the nanometric-sized grains of human tooth enamel corresponds to a one-unit-cell-thick layer of octacalcium phosphate (OCP). Based on this consideration, in this work we propose a model for CDL and we carried out the chemistry and structural analysis of the CDL with high resolution microscopy techniques such as Electron Energy Loss Spectroscopy (EELS) and Z-contrast (HAADF) with the aim of find the agreements and/or differences between the human tooth enamel HA and its CDL.

In this study we examine the immediate interface between matrix grains and the amorphous intergranular film in a Si3N4 ceramic doped with rare-earth oxides La2O3, Sm2O3, Er2O3, Yb2O3 and Lu2O3, extracting unique structural and atomic bonding information. In particular, we relate the structure of the interface to the ionic size and electronic structure of the rare-earth elements and the presence of oxygen in the intergranular film. We relate these results to the measured fracture toughness.

The effects of grain-boundary chemistry on the mechanical properties of a high-purity silicon nitride ceramics were investigated, with specific emphasis on the role of oxygen. Variations in the grain-boundary oxygen content, through control of oxidizing heat treatments and sintering additives, was found to result in a transition in fracture mechanism from transgranular to intergranular fracture, with an associated increase in fracture toughness. This phenomenon is correlated to an oxygen-induced change in grain-boundary chemistry that appears to affect fracture by “weakening” the interface, facilitating debonding and crack advance along the boundaries, thereby enhancing the toughness by grain bridging. It is concluded that if the oxygen content in the thin grain-boundary films exceeds a lower limit, which is ∼0.87 equiv% oxygen content, then the interfacial structure and bonding characteristics favor intergranular debonding during crack propagation; otherwise, transgranular fracture ensues, with consequent low toughness.

Electron-optical aberration correction has recently progressed from a promising concept to a powerful research tool. 100–120 kV scanning transmission electron microscopes (STEMs) equipped with spherical aberration (Cs) correctors now achieve sub-Å resolution in high-angle annular dark field (HAADF) imaging, and a 300 kV Cs-corrected STEM has reached 0.6 Å HAADF resolution. Moreover, the current available in an atom-sized probe has grown by about 10x, allowing electron energy loss spectroscopy (EELS) to detect single atoms. We summarize the factors that have made this possible, and outline likely future progress.