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Transmission of very slow electrons as a diagnostic tool
Frank, Luděk ; Nebesářová, Jana ; Vancová, Marie ; Paták, Aleš ; Mikmeková, Eliška ; Müllerová, Ilona
The penetration of electrons through solids is retarded by sequences of their interactions with the matter in which the electron changes its direction of motion and loses its energy. Inelastic collisions, the intensity of which reaches a maximum at around 50 electronvolts (eV) and drops steeply on both sides of this fuzzy threshold, are decisive for the penetration of electrons. Transmission microscopy (TEM or STEM) observes thin samples of tens to hundreds of nanometres in thickness by passing electrons of energies of tens to hundreds of kiloelectronvolts through them. The range below 50 eV has recently been utilized in the examination of surfaces with reflected electrons, where high image resolution is achieved thanks to the retardation of electrons close to the sample surface in the ´cathode lens´ . In this lens, the role of the cathode is played by the sample itself, biased to a high negative potential. This principle can also be utilized in the transmission mode with samples of a thickness at and below 10 nm. This method has recently been implemented and verified on graphene samples prepared by various methods. The results have made it possible to diagnose the continuity and quality of the graphene flakes. Furthermore, series of experiments have been performed involving the observation of ultrathin tissue sections with electrons decelerated to about 500 eV and less, where they provide an image contrast of the cell ultrastructure much higher than that provided by traditional microscopic modes.
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Thermal desorption spectroscopy in prototype furnace for chemical vapor deposition
Průcha, Lukáš ; Daniel, Benjamin ; Piňos, Jakub ; Mikmeková, Eliška
Cleaning of the sample surfaces is crucial for scanning electron microscopy, especially for\nlow energy electron microscopy or for the deposition of thin layers, such as graphene,\nwhere surface has to be well prepared. In the best case, every unwanted particle should be\ncleaned from the sample surface for best low energy electron microscopy observation or thin\nfilm deposition. Unfortunately, the standard cleaning procedures can leave residues on the\nsample surface. This work is focused on thermal desorption spectroscopy (TDS). TDS is a method of observing desorbed molecules from a sample surface during the increase of\ntemperature of the sample. The aim of this study was to determine optimum conditions:\ntemperature and time, to achieve clean surfaces in the shortest time.
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STEM modes in SEM
Konvalina, Ivo ; Paták, Aleš ; Mikmeková, Eliška ; Mika, Filip ; Müllerová, Ilona
The segmented semiconductor STEM detector in the Magellan 400 FEG SEM microscope\n(https://www.fei.com/) is used to detect transmitted electrons (TEs) and allows observing\nsamples in four imaging modes. Two modes of objective lens, namely high resolution (HR)\nand ultra-high resolution (UHR), differ by their resolution and by the presence or absence of\na magnetic field around the sample. If the beam deceleration (BD) mode is chosen, then\nan electrostatic field around the sample is added and two further microscope modes HR + BD\nand UHR + BD, become available. Trajectories of TEs are studied with regard to their angular\nand energy distribution in each mode in this work.\n
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Examination of 2D crystals in a low voltage SEM/STEM
Mikmeková, Eliška ; Frank, Luděk ; Polčák, J. ; Paták, Aleš ; Lejeune, M.
Development of new types of materials such as 2D crystals (graphene, MoS2, WS2, h-BN, etc.) requires emergence of new surface-sensitive techniques for their characterization. As regards the “surface” sensitivity, the (ultra) low energy electron microscopy can become a very powerful tool for true examination of these atom-thick materials, capable of confirming physical phenomena predicted to occur on their surfaces. Modern commercial scanning electron microscopes enable imaging and analyses by low energy electrons even at very high magnification. In the case of the SEM, resolution even below 1 nm can be achieved at low landing energy of electrons. Since specimen contamination increases with increasing electron dose and decreasing landing energy, specimen cleanness is a critical factor in obtaining meaningful data. A range of various specimen cleaning methods can be applied to selected samples. Typical cleaning methods, such as solvent rinsing, heating, bombarding with ions and plasma etching have their limitations. Electron-induced in situ cleaning procedure can be gentle, experimentally convenient and very effective for wide range of specimens. Even a small amount of hydrocarbon contamination can severely impact on the results obtained with low energy electrons, as illustrated in Figure 1A. During the scanning of surfaces by electrons, the image usually darkens because of a carbonaceous layer gradually deposited on the top from adsorbed hydrocarbon precursors.
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Scanning transmission microscopy at very low energies
Müllerová, Ilona ; Mikmeková, Eliška ; Konvalina, Ivo ; Frank, Luděk
To operate down to units of eV with a small primary spot size, a cathode lens with a biased specimen was introduced into the SEM. The reflected signal, accelerated secondary and backscattered electrons, is collected by detectors situated above the specimen.\nWhen we insert a detector below the specimen, the transmitted electron signal can also be used for imaging down to zero energy. Fig. 1 also shows an example of the simulated signal trajectories of electrons that impact on the detector of reflected electrons, based on an Yttrium Aluminium Garnet (YAG) crystal, and trajectories of electrons transmitted through the specimen and incident on a semiconductor detector based on the PIN structure.
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Treatment of surfaces with slow electrons
Frank, Luděk ; Mikmeková, Eliška
Historically, the most annoying obstacle to acquiring SEM micrographs, in particular higher magnification micrographs taken with the ambition of resolving the finest observable details, may be said to be carbonaceous contamination “highlighting” the previous field of view with a black rectangle contoured by an even darker frame. This contamination is generated by decomposition of adsorbed hydrocarbon molecules with incident electrons leaving a crosslinked\nlayer of carbon atoms as a surface coating. The darker contours come from high surface mobility of hydrocarbon molecules from outside the field. The situation has been improved in recent decades by a lower pressure and dryer vacuum in specimen chambers, but even under ultrahigh vacuum (UHV) conditions the phenomenon occurs due to hydrocarbon molecules deposited on the specimen when loaded. Therefore, only in-situ cleaning with an\nattachment producing an ion beam solves this problem in UHV, while some plasma cleaners have also started appearing in standard-vacuum SEM chambers. The goal of complete removal of hydrocarbons is motivated by the supposed unavoidability of their decomposition with primary electrons. However, we have found hydrocarbon molecules being released, rather than their decomposition, when the energy of the impinging electrons drops beneath 50 eV or so.
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Examination of Graphene with Very Slow Electrons
Mikmeková, Eliška ; Frank, Luděk
Although graphene has been available and intensively studied for nearly a full decade, new methods are still required for its examination and diagnostics. Even checking the continuity of layers and the reliable counting of layers of graphene and other 2D crystals should be easier to perform. Scanning electron microscopy with slow and very slow electrons offers an innovative tool enabling one to see graphene samples at nanometer or even sub-nanometer lateral resolution in both transmitted and reflected electrons and to count the number of layers reliably in both imaging modes. Diagnostics can be performed in this way on freestanding graphene samples as well as on graphene grown on the surfaces of bulk substrates. Moreover, bombardment with very slow electrons acts as an ultimate cleaning procedure removing adsorbed gases from crystal surfaces which can be monitored in scanned transmission electron images taken at below 50 eV.
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Influence of annealing to stress in CNx:(H) films observed by SLEEM
Mikmeková, Eliška ; Mikmeková, Šárka ; Müllerová, Ilona ; Sobota, Jaroslav
The effect of high residual stress on the quality of thin sputtered carbon nitride films has been studied by Scanning Low Energy Electron Microscopy (SLEEM). Basically, two different types of stress can be identified in thin films: compressive stress and tensile stress. Compressive stress leads to wrinkling and film delamination and tensile stress can cause the fracturing of thin films. Experiments were made in the Tescan TS 5130 MM equipped with the Cathode Lens system (CL), which enable us to observe samples at arbitrary landing energies of the illuminating electrons. Operating of a SEM at low energies offers several advantages: an increase of materials contrast via low energy, high ratio SE, BSE signal and noise, smaller interaction volume and elimination of charging effects. The effect of annealing in vacuum to residual stress (calculated from Stoney’s equation) was measured. The porous character of films was observed by thermal desorption spectroscopy (TDS).
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