Šárka Mikmeková

Scanning Electron Microscopy with Samples in an Electric Field

The high negative bias of a sample in a scanning electron microscope constitutes the “cathode lens” with a strong electric field just above the sample surface. This mode offers a convenient tool for controlling the landing energy of electrons down to units or even fractions of electronvolts with only slight readjustments of the column. Moreover, the field accelerates and collimates the signal electrons to earthed detectors above and below the sample, thereby assuring high collection efficiency and high amplification of the image signal. One important feature is the ability to acquire the complete emission of the backscattered electrons, including those emitted at high angles with respect to the surface normal. The cathode lens aberrations are proportional to the landing energy of electrons so the spot size becomes nearly constant throughout the full energy scale. At low energies and with their complete angular distribution acquired, the backscattered electron images offer enhanced information about crystalline and electronic structures thanks to contrast mechanisms that are otherwise unavailable. Examples from various areas of materials science are presented.

TRIP steel microstructure visualized by slow and very slow electrons

The aim of the present paper is to demonstrate the ability of the scanning low-energy electron microscopy to visualize the transformed induced plasticity steel microstructure with extremely high sensitivity. Using the retarding mode in the scanning electron microscope, the high contrast between the individual phases has been obtained, which enables us to differentiate the retained austenite and the other phases. The sets of the micrographs have been collected from the sample at a wide range of landing energies of primary electrons from 50 eV to 10 keV and the dependence of the contrast between the phases on the landing energy has been calculated. Upon a comparison of these contrast curves, the optimal conditions for achieving of maximum contrast have been established.

Very low energy scanning electron microscopy in nanotechnology

The group of low energy electron microscopy at ISI AS CR in Brno has developed a methodology for very low energy scanning electron microscopy at high image resolution by means of an immersion electrostatic lens (the cathode lens) inserted between the illumination column of a conventional scanning electron microscope and the sample. In this way the microscope resolution can be preserved down to a landing energy of the electrons one or even fractions of an electronvolt. In the range of less than several tens of electronvolts the image signal generation processes include contrast mechanisms not met at higher energies, which respond to important features of the 3D inner potential of the target and visualise its local crystallinity as well as the electronic structure. The electron wavelength comparable with interatomic distances allows observation of various wave–optical phenomena in imaging. In addition, the cathode lens assembly secures acquisition of electrons backscattered from the sample at large angles with respect to the surface normal, which are abandoned in standard microscopes although they provide enhanced crystallinity information and surface sensitivity even at medium electron energies. The imaging method is described and illustrated with selected application examples.

Characterization of the local crystallinity via reflectance of very slow electrons

The reflectance of very slow electrons from solids and its electron energy dependence are shown as characteristic for the crystal system and its spatial orientation so they can serve, e.g., to fingerprinting the orientation of grains in polycrystals. Measurements on single crystals and polycrystals are validated via electron backscatter diffraction analyses. Sensitivity of the method to fine details of crystallinity is demonstrated.

Strain Mapping by Scanning Low Energy Electron Microscopy

The use of the scanning low energy electron microscopy (SLEEM) has been slowly making its way into the field of materials science, hampered not by limitations in the technique but rather by relative scarcity of these instruments in research institutes and laboratories. This paper reports the results obtained from an investigation of the microstructure of ultra fine-grained (UFG) copper fabricated using equal channel angular pressing (ECAP) method, namely in the as-pressed state and after annealing. SLEEM is very sensitive to the perfection of crystal lattice and using SLEEM, local strain can be effectively imaged.

Poly(3-hexylthiophene)/gold nanoparticle nanocomposites: relationship between morphology and electrical conductivity

The morphology and electrical properties of gold nanoparticles (AuNP) layer vacuum-deposited onto spin-cast thin films of poly(3-hexylthiophene), P3HT, were studied. The electrical conductivity was measured during temperature cycling and related to the morphology of the same composite structures, which was monitored by transmission electron microscopy (TEM) and extra-high resolution scanning electron microscopy (XHR SEM). Comparison to the analogous polystyrene/AuNP layers was made to distinguish the role of the polymer support on the morphology and electrical properties of the nanoparticles assembly. Gold deposited in a very thin layer formed a nanoparticles-like island structure with the morphology depending on the effective thickness of the deposited layer and on its subsequent thermal treatment. A stabilizing effect of the thiophene–gold interaction on the nanoparticles morphology was observed.

Characterisation of morphological, antimicrobial and leaching properties of in situ prepared polyurethane nanofibres doped with silver behenate

Polyurethane nanofibres in situ doped with silver nanoparticles arising from three different silver precursors as well as zero-valent silver nanoparticles were prepared using free-surface electrospinning with no post-treatment. Throughout the experiment, the best results from all combinations tested were achieved for silver behenate doped nanofibres. These had homogenous nanoparticle coverage (some particles 99% as well as inhibition zones of 1.20 ± 0.12 mm for E. coli, 1.45 ± 0.08 mm for Staphylococcus aureus and 0.62 ± 0.12 mm for Pseudomonas aeruginosa at concentrations corresponding to 1 McFarland. Moreover, after 168 h, silver behenate doped nanofibres displayed the lowest silver leaching (5.8% of original silver content) of all samples prepared in this study. These nanofibres, therefore, represent a promising alternative to current silver-doped nanofibres prepared in situ.

Contrast of positively charged oxide precipitate in out-lens, in-lens and in-column SE image

Modern scanning electron microscopes are usually equipped with multiple detectors and enable simultaneous collection of two or even three secondary electron images. The secondary electrons become divided between the detectors in dependence on their initial kinetic energy and emission angle. In this study, sharing of the secondary electrons by out-lens, in-lens and in-column detectors has been systematically investigated. Energy filtering of the signal electrons is demonstrated by separation of the voltage and the topographical contrast in the micrographs obtained by out-lens and in-lens/in-column detectors. The presence of two detectors inside the electron column enables further filtering of the low kinetic energy secondary electrons, which results to unusual contrasts and phenomena. In this paper, inversion of the contrast sign between a positively charged oxide particle and conductive steel matrix (i.e. voltage contrast) in SE images collected under specific imaging conditions is demonstrated.

Practical Use of Scanning Low Energy Electron Microscope (SLEEM)

The high negative bias of a sample in a scanning electron microscope constitutes the cathode lens (CL), with a strong electric field just above the sample surface [1] offers a tool for controlling the landing energy of electrons down to units or even fractions of electronvolts. Moreover, the field accelerates and collimates the signal electrons to earthed detectors above and below the sample, thereby assuring high collection efficiency and high amplification of the image signal. One important feature is the ability to acquire the complete emission of the backscattered electrons, including those emitted at high angles with respect to the surface normal. The cathode lens aberrations are proportional to the landing energy of electrons, so the spot size becomes nearly constant throughout the full energy scale.

Exploitation of Contrasts in Low Energy SEM to Reveal True Microstructure

We have developed a Scanning Low Energy Electron Microscope (SLEEM) based on the Cathode Lens (CL) principle [1]. A resolution of 4.5 nm at 20 eV, 0.8 nm at 200 eV and 0.5 nm at 15 keV primary beam energy can nowadays be obtained in a commercially available instrument [2]. One of the main advantages of operation at low energies is the decrease in the interaction volume from approximately 1 μιη at 10 keV to 10 nm at 100 eV. The material contrast can be optimised and the charging effect suppressed at a tailored electron energy. Wave-optical contrasts are also available beneath 50 eV. The specimen may be immersed in a strong magnetic field in addition to an electrostatic field in order to obtain a small spot size across the whole energy range. The same fields influence the signal trajectories, so we can choose which part of the angular and energy distributions of emitted electrons are to be collected. Certain arrangements provide strong crystallographic contrast. Imaging conditions have been tailored to various material types. Experiments have been performed in an experimental ultrahigh vacuum (UHV) SLEEM and in an XHR SEM Magellan 400L.