Carbon-film-based Zernike phase plates with smooth thickness gradient for phase-contrast transmission electron microscopy with reduced fringing artefacts.

Phase plates (PPs) in transmission electron microscopy (TEM) improve the contrast of weakly scattering objects under in-focus imaging conditions. A well-established PP type is the Zernike (Z)PP, which consists of a thin amorphous carbon (aC) film with a microscaled hole in the centre. The mean inner potential of the aC film is exploited to shift the phase of the scattered electrons while the unscattered electrons in the zero-order beam propagate through the hole and remain unaffected. However, the abrupt thickness increase at the hole edge induces an abrupt change of the phase-shift distribution and leads to fringing, that is, intensity oscillations around imaged objects, in TEM images. In this work, we have used focused-ion-beam milling to fabricate ZPPs with abrupt and graded thickness profiles around the centre hole. Depending on the thickness gradient and inner hole radius, graded-ZPP-TEM images of an aC/vacuum interface and bundles of carbon nanotubes (CNTs) show strongly reduced fringing. Image simulations were performed with ZPP-phase-shift distributions derived from measured thickness profiles of graded ZPPs, which show good agreement with the experimental images. Fringing artefacts, that is, intensity oscillations around imaged objects, are strongly reduced for Zernike phase plates with a graded thickness profile around the centre hole. Focused-ion-beam milling is used to fabricate graded Zernike phase plates with specific inner hole radius and thickness gradients. The phase-shift distribution is obtained from measured thickness profiles around the centre hole. Image simulations based on experimentally measured thickness/phase-shift distributions show good agreement with experimental Zernike phase-plate TEM images.

Differential electron scattering cross-sections at low electron energies: The influence of screening parameter.

For quantitative electron microscopy the comparison of measured and simulated data is essential. Monte Carlo (MC) simulations are well established to calculate the high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) intensities on a non-atomic scale. In this work we focus on the importance of the screening parameter in differential screened Rutherford cross-sections for MC simulations and on the contribution of the screening parameter to the atomic-number dependence of the HAADF-STEM intensity at electron energies ≤ 30 keV. Materials investigated were chosen to cover a wide range of atomic numbers Z to study the Z dependence of the screening parameter. Comparison of measured and simulated HAADF-STEM intensities with different screening parameters known from the literature were tested and failed to generally describe the experimental data. Hence, the screening parameter was adapted to obtain the best match between experimental and MC-simulated HAADF-STEM intensities. The Z dependence of the HAADF-STEM intensity was derived.

Electron beam broadening in electron-transparent samples at low electron energies.

Scanning transmission electron microscopy (STEM) at low primary electron energies has received increasing attention in recent years because knock-on damage can be avoided and high contrast for weakly scattering materials is obtained. However, the broadening of the electron beam in the sample is pronounced at low electron energies, which degrades resolution and limits the maximum specimen thickness. In this work, we have studied electron beam broadening in materials with atomic numbers Z between 10 and 32 (MgO, Si, SrTiO3 , Ge) and thicknesses up to 900 nm. Beam broadening is directly measured using a multisegmented STEM detector installed in a scanning electron microscope at electron energies between 15 and 30 keV. For experimental reasons, the electron beam diameter is defined to contain only 68% of the total intensity instead of the commonly used 90% of the total beam intensity. The measured beam diameters can be well described with calculated ones based on a recently published model by Gauvin and Rudinsky. Using the concept of anomalous diffusion the Hurst exponent H is introduced that varies between 0.5 and 1 for different scattering regimes depending on t/Λel with the specimen thickness t and the elastic mean free path length Λel . The calculations also depend on the fraction of the beam intensity that defines the electron beam diameter. A Hurst exponent H of 1 is characteristic for the ballistic scattering regime with t/Λel → 0 and can be excluded for the experimental conditions of our study with 6 ≦ t/Λel ≦ 30. We deduced H = 0.75 from measured beam diameters which is larger than H = 0.5 that is expected under diffusion conditions. The deviation towards larger H values can be rationalised by our definition of electron diameter that contains only 68% of the total beam intensity and requires therefore larger sample thicknesses before the diffusion regime is reached. Our results clearly deviate from previous analytical approaches to describe beam broadening (Goldstein et al., Reed, Williams et al., Kohl and Reimer). Measured beam diameters are compared with simulated ones, which are obtained by solving the electron transport equation. This approach is advantageous compared to the commonly used Monte Carlo simulations because it is an exact solution of the electron transport equation and requires less computer time. Simulated beam diameter agree well with the experimental data and yield H = 0.80. LAY DESCRIPTION: In scanning transmission electron microscopy (STEM), a focused electron beam is scanned over an electron-transparent sample and an image is formed by detecting the intensity of the transmitted electrons by a STEM detector. STEM resolution is ultimately limited by the electron beam diameter and can be better than 0.1 nm for the best microscopes. However, the electron-beam diameter increases with increasing specimen thickness because electrons are scattered by the interaction of the specimen material and electrons. Electron scattering leads to a change of the electron propagation direction and reduces focusing of the electron beam. The associated electron-beam broadening degrades the lateral resolution of STEM and generally limits the maximum specimen thickness that can be imaged with good resolution. STEM is up to now mainly performed at high electron energies of 80 keV and above. Lower electron energies are beneficial for the study of weakly scattering and radiation-sensitive materials but electron beam broadening becomes more pronounced with decreasing electron energies. Knowledge of beam broadening is therefore particularly important for the interpretation of STEM images that are taken with low-energy electrons. In this work we have studied electron-beam broadening in different materials with thicknesses up to 900 nm at low electron energies between 15  and 30 keV. Beam broadening is directly measured with a newly developed technique. We compare measured beam diameters with different models on beam broadening from literature and find that only a recently published model is well suited to describe the experimental results under our experimental conditions. In addition, beam broadening is simulated by modelling electron propagation in the specimen. The simulation results agree well with the measured beam diameters.

Schlieren-cinematographic and holographic diagnostic of a laser-produced plasma in xenon.

We have studied extensively a gas breakdown in xenon produced by a giant pulse ruby laser with a power <100 MW. Detailed information concerning the structure of the laser plasma formation and of the following expansion has been obtained by different optical methods, including schlieren techniques (single frames and ultra high speed cinematography) and holography. The high quality of the holographic pictures was achieved by the use of a monomode laser. With this we were able to visualize the plasma history and to determine the velocities of the boundary layer and of the blast wave with utmost accuracy. Investigations of the electron density and electron temperature showed that a relaxation time of about 10 nsec is necessary to establish local thermodynamic equilibrium states. After this relaxation time it is then possible to carry out thermodynamic calculations, applying the shock-wave theory, to relate the optically measured expansion velocity with the plasma parameters involved. The mean specific internal energy epsilon , for instance, attained values in excess of 10(12) erg/g which decayed rapidly during the first 100 nsec to about 5. 10(10) erg/g. By comparing the results to theoretical calculations of we obtained a first estimate of the temperature, taking into consideration the partial densities n(j) as well as the partition functions Z(j)((i)) of the xenon atoms, the single-charged ions, and the double-charged ones. Furthermore, a two-step iteration computer program was used to give more detailed and more accurate results on the variations of the pressure, temperature, partial densities, and enthalpy as a function of time.