It is shown that star disclinations can be a significant source of stress in chemical vapor deposited (CVD) diamond. This purely geometrical origin contrasts with other sources of stress that have been proposed previously. The effectiveness is demonstrated of the use of electron irradiation using a transmission electron microscope (TEM) to displace atoms from their equilibrium sites to investigate intrinsic defects and impurities in CVD diamond. After irradiation, the samples are studied by low temperature photoluminescence microscopy using UV or blue laser illumination. Results are given that are interpreted as arising from isolated <100> split self-interstitials and positively charged single vacancies. Negatively charged single vacancies can also be revealed by this technique. Nitrogen and boron impurities may also be studied similarly. In addition, a newly developed liquid gallium source scanned ion beam mass spectrometry (SIMS) instrument has been used to map out the B distribution in B doped CVD diamond specimens. The results are supported by micro-Raman spectroscopy.

In large bandgap semiconductors and insulators, the threshold energies for e–h pair production and ionization damage can lie above the vacuum level. For low energy imaging, a window is then opened whose width is potentially sensitive to local changes in work function, doping level, or acidity. Recent progress and future opportunities for damage-free imaging of these properties using low energy electrons are discussed in the light of the underlying physics, as well as of recent instrumental developments in low energy electron microscopy (LEEM), environmental scanning electron microscopy (ESEM), photoelectron emission microscopy (PEEM), scanned probe microscopy (SPM), and projection electron microscopy.

Valence electron energy-loss (VEEL) spectroscopy was performed on six ceramic materials in a dedicated scanning transmission electron microscope (STEM). Quantitative analysis of these data is described yielding access to the complex optical properties and the electronic structure of the materials. Comparisons are made on the basis of the interband transition strength describing transitions between occupied states in the valence band and empty states in the conduction band. This proves that the quantitative analysis of VEEL data is a competitive and complementary method to be considered when investigating the electronic structure of materials. Possibilities for improvement and extension of the analysis are discussed extensively.

The current status and general applicability of scanning electron microscopy (SEM) at low voltages is reviewed for both imaging (low voltage scanning electron microscopy, LVSEM) and chemical microanalysis (low voltage energy-dispersive X-ray spectrometry, LVEDX). With improved instrument performance low beam energies continue to have the expected advantages for the secondary electron imaging of low atomic number (Z) and electrically non-conducting samples. They also provide general improvements in the veracity of surface topographic analysis with conducting samples of all Z and at both low and high magnifications. In new experiments the backscattered electron (BSE) signal retains monotonic Z dependence to low voltages (<1 kV). This is contrary to long standing results in the prior literature and opens up fast chemical mapping with low dose and very high (nm-scale) spatial resolution. Similarly, energy-dispersive X-ray chemical microanalysis of bulk samples is extended to submicron, and in some cases to <0.1 μm, spatial resolution in three dimensions at voltages <5 kV. In favorable cases, such as the analysis of carbon overlayers at 1.5 kV, the thickness sensitivity for surface layers is extended to <2 nm, but the integrity of the sample surface is then of concern. At low beam energies (E0) the penetration range into the sample, and hence the X-ray escape path length out of it, is systematically restricted (R = F(E05/3)), with advantages for the accuracy or elimination of complex analysis-by-analysis matrix corrections for absorption (A) and fluorescence (F). The Z terms become more sensitive to E0 but they require only one-time calibrations for each element. The new approach is to make the physics of the beam–specimen interactions the primary factor and to design enabling instrumentation accordingly.

We describe a hidden parameter inferencing algorithm for deducing the length, width, and vibration profile from images of thermally excited single-wall carbon nanotubes. With accurate estimates of these parameters, the Young’s modulus can be deduced. The algorithm is sensitive to shot noise in the image, primarily because of the low nanotube image contrast. Noise causes the nanotube length and width to be overestimated, and the vibration amplitude to be underestimated. After correcting for shot noise, we infer an average value of the Young’s modulus of 〈Y〉= 1.20±0.20 TPa, which is larger than the currently accepted value for graphite.

Elevated temperature scanning tunneling microscopy is used to study oxides that are room temperature insulators but become sufficiently electrically conducting at higher temperatures to allow imaging to be performed. Atomic resolution images of NiO, CoO, and UO2 have been obtained in this fashion which allow surface structure and defect determination. To complement the experiments, modeling of the electronic surface structure reveals which atomic sites give rise to the contrast observed in the images. Low voltage scanning electron microscopy is used to image small equilibrium pores in UO2 single crystals to evaluate the surface energy ratio of the (111) to (001) surfaces.

The technique of energy selected electron diffraction gives information about amorphous structures which can be used to characterize amorphous materials in terms of their structure. The diffraction data can be used to refine models obtained using molecular dynamics, resulting in physically reasonable models consistent with the diffraction data.

In situ real-time environmental high resolution electron microscopy (EHREM) under controlled reaction environments permits direct atomic resolution imaging of dynamic surface and sub-surface microstructures of reacting catalysts. Using the EHREM and complementary microscopy methods, we have investigated selective hydrogenation reaction mechanisms over novel xerogel catalysts of ruthenium and Ru with Co and Au promoters on titania supports, and report an alternative heterogeneous catalytic process for the hydrogenation of adiponitrile (ADN) in the manufacture of Nylon 6,6. The direct EHREM observations are supported by ultra-high resolution low voltage scanning electron microscope (SEM) of spatial distributions of the highly dispersed nanometer-size catalyst particles and parallel chemical studies. The results demonstrate the important role of in situ EHREM in the design of heterogeneous catalytic hydrogenation processes on the nanoscale.

We show that in the limit of a large objective (probe-forming) aperture, relevant to a spherical aberration corrected microscope, the Z-contrast image of a zone-axis crystal becomes an image of the 1s Bloch states. The limiting resolution is therefore the width of the Bloch states, which may be greater than that of the free probe. Nevertheless, enormous gains in image quality are expected from the improved contrast and signal-to-noise ratio. We present an analytical channeling model for the thickness dependence of the Z-contrast image in a zone-axis crystal, and show that, at large thicknesses, columnar intensities become proportional to the mean square atomic number, Z2.

Very high angle (~100 mrad) annular dark-field (HAADF) images in a dedicated scanning transmission electron microscope (STEM) can be used to quantitatively measure the number of atoms in a cluster on a support material. We have developed a computer program which will automatically find the location of the particles and then integrate the intensity to find the number of atoms per cluster. We have examined ultra-small Pt clusters on a C substrate by this novel mass-spectroscopic technique. We discovered that the Pt clusters maintain their three-dimensional shape, and are probably spherical.

An experimental high-resolution image of a solid–liquid interface of solid Si and liquid Al–Si alloy has been compared with theoretical images obtained by computer simulation. It has been concluded that the solid–liquid interface has a transition layer, the structure of which is compatible with the 1 × 1 Si-{111} surface.

Annihilation behaviors of athermal ω-phase crystals formed by cooling at 131 K for 10.8 ks under four different electron irradiation conditions of acceleration voltages of 200 kV and 160 kV, and beam currents of approximately 20 pA/cm2 and 5 pA/cm2 were investigated using in situ dark field and HREM observation methods at 131 K. The effect of acceleration voltages on the lifetimes is recognized, i.e., in the case of approximately equal electron beam current, lifetimes at 200 kV become shorter than those at 160 kV. Also, lifetimes depend on the electron beam current at 200 kV, i.e., the higher the beam currents, the shorter the lifetimes become. However, no distinct dependence can be seen at 160 kV. Since annihilations of athermal ω-phase crystals begin after the electron irradiation for a certain period in each condition, which depends on acceleration voltages and beam currents, it is suggested that the annihilation behaviors have incubation periods.

Transmission electron diffraction patterns from ultra-thin aromatic and aliphatic organic films at beam energies of 200 eV–1 keV have been recorded in a custom low energy electron transmission (LEET) chamber. A significant reduction of the molecular damage cross-section, measured by fading of diffraction spots, was found for thin films of the aromatic perylene when the beam energy was reduced from 400 to 200 eV. The corresponding measurements for the aliphatic tetracontane showed a smaller “threshold energy” and the differences are discussed. Electron beam damage from other aromatic materials has also been studied at low energy. Comparison of the carbon K shell ionization cross-section and the measured damage cross-sections show that carbon K-shell ionization is strongly correlated with the damage observed in aromatics at beam energies higher than 284 eV. Calculation of the minimum number of unit cells needed for imaging a single molecule, and comparison of calculated elastic with measured damage cross-sections both indicate new possibilities for imaging biomolecules with low energy electrons.

An overview and new results are presented of the investigations carried out in the last 5 years on nano-sized tips by means of electron microscopy, an electron optical bench, and computation. Tungsten and, in particular, carbon nano-tips prepared by carbon contamination in a scanning electron microscope, were studied for applications as field-emission electron sources. Several features of their use are described and the results concerning the determination of some of their basic properties are reported.

Platinum nanoparticles finely dispersed in activated carbon powders have been observed with high contrast in secondary electron (SE) and backscattered electron (BE) images. The factors that contribute to the visibility of small metal particles in high-resolution BE and SE images are discussed. Monte Carlo simulations provided insight into the scattering of electrons by small, heavy-element particles located on, or embedded in, light-element supports. The visibility of Pt nanoparticles in BE images depends on many factors including the size and the location of the Pt particles, the energy of the incident electrons, and the size of the electron probe. The SE signals generated by backscattered electrons may not significantly contribute to the visibility of small Pt particles in high-resolution SE images of carbon supported Pt catalysts. Only those small Pt particles that are located on or very close to the surface of the carbon support can be revealed in high-resolution SE images.

A previously unknown form of charge ordering has been observed in dislocation free thin films of magnetite, Fe3O4. This charge ordering exists on tetrahedral sites and is unrelated to the well known low temperature ordering on octahedral sites that occurs below 120K. From modeling of electron diffraction patterns we deduce that the best fit to the observed diffraction patterns was obtained by reducing the scattering power on one tetrahedral site per unit cell by about 80%.