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Electron-beam-induced deposition of various materials from suitable precursors has represented an established branch of nanotechnology for more than a decade. A specific alternative is carbon deposition on the basis of hydrocarbons as precursors that has been applied to grow various nanostructures including masks for subsequent technological steps. Our area of study was unintentional electron-beam-induced carbon deposition from spontaneously adsorbed hydrocarbon molecules. This process traditionally constitutes a challenge for scanning electron microscopy practice preventing one from performing any true surface studies outside an ultrahigh vacuum and without in-situ cleaning of samples, and also jeopardising other electron-optical devices such as electron beam lithographs. Here we show that when reducing the energy of irradiating electrons sufficiently, the e-beam-induced deposition can be converted to e-beam-induced release causing desorption of hydrocarbons and ultimate cleaning of surfaces in both an ultrahigh and a standard high vacuum. Using series of experiments with graphene samples, we demonstrate fundamental features of e-beam-induced desorption and present results of checks for possible radiation damage using Raman spectroscopy that led to optimisation of the electron energy for damage-free cleaning. The method of preventing carbon contamination described here paves the way for greatly enhanced surface sensitivity of imaging and substantially reduced demands on vacuum systems for nanotechnological applications.

The information depth of imaging with backscattered electrons in the scanning electron microscope was measured directly by comparison of a planar view of a steel sample with buried precipitates with an image of a section cut through precipitates by means of a Focused Ion Beam attachment. The information depth was determined across the electron energy range of units of keV and the results were compared with information depths calculated from two published equations and simulated using widely available Monte Carlo-based software. Recommendations are given for routine estimations of BSE information depths.

Low voltage electron microscopes working in transmission mode, like LVEM5 (Delong Instruments, Czech Republic) working at accelerating voltage 5 kV or scanning electron microscope working in transmission mode with accelerating voltage below 1 kV, require ultrathin sections with the thickness below 20 nm. Decreasing of the primary electron energy leads to enhancement of image contrast, which is especially useful in the case of biological samples composed of elements with low atomic numbers. As a result treatments with heavy metals, like post-fixation with osmium tetroxide or ultrathin section staining, can by omitted. The disadvantage is reduced penetration ability of incident electrons influencing the usable thickness of the specimen resulting in the need of ultrathin sections of under 20 nm thickness. In this study we want to answer basic questions concerning the cutting of extremely ultrathin sections: Is it possible routinely and reproducibly to cut extremely thin sections of biological specimens embedded in commonly used resins with contemporary ultramicrotome techniques and under what conditions? Microsc. Res. Tech. 79:512-517, 2016. © 2016 Wiley Periodicals, Inc.

Summary The advent of new imaging technologies in Scanning Electron Microscopy (SEM) using low energy (0–2 keV) electrons has brought about new ways to study materials at the nanoscale. It also brings new challenges in terms of understanding electron transport at these energies. In addition, reduction in energy has brought new contrast mechanisms producing images that are sometimes difficult to interpret. This is increasing the push for simulation tools, in particular for low impact energies of electrons. The use of Monte Carlo calculations to simulate the transport of electrons in materials has been undertaken by many authors for several decades. However, inaccuracies associated with the Monte Carlo technique start to grow as the energy is reduced. This is not simply associated with inaccuracies in the knowledge of the scattering cross-sections, but is fundamental to the Monte Carlo technique itself. This is because effects due to the wave nature of the electron and the energy band structure of the target above the vacuum energy level become important and these are properties which are difficult to handle using the Monte Carlo method. In this review we briefly describe the new techniques of scanning low energy electron microscopy and then outline the problems and challenges of trying to understand and quantify the signals that are obtained. The effects of charging and spin polarised measurement are also briefly explored. SCANNING 9999:1–17, 2016. © 2016 Wiley Periodicals, Inc.

An overview of recent developments in very low energy scanning electron microscopy is presented. Electron optical aspects are briefly summarized including the low energy beam formation in a cathode lens equipped column, comparison of the sequential and overlapped electric and magnetic fields in the objective lens, and detection issues including extension to the transmitted electron mode as well as to the multichannel detection of signal sorted according to the polar angle of emission. In addition to the acquisition of contrasts specific for the very low energy range, advantages of detection of electrons backscattered to large angles from the surface normal are demonstrated on selected application examples.

Study of the grain structure in the equal channel angular pressing processed copper by means of the cathode lens equipped ultrahigh vacuum scanning low energy electron microscope is reported. The grain contrast was found achieving its maximum at electron energies below about 30 eV where it alternated its sign and exhibited dependence on electron energy specific for the grain orientation. The energy dependence of the electron reflectance seemed to be capable of serving as a fingerprint enabling determination of the crystalline orientation. In the cathode lens mode at hundreds of eV fine details of the microstructure are also observable including twins and low angle grain boundaries. This is explained by acquisition of high-angle backscattered slow electrons, normally not acquired in standard scanning electron microscopes. The very low energy electron reflectance is promising as an alternative to the EBSD method owing to its high resolution and fast data acquisition.

By introducing a cathode lens below or inside the objective lens of a scanning electron microscope, many experiments similar to those typical of the LEEM method can be performed. The conditions for the diffraction of slow electrons are modified by the convergence of the primary beam, and challenges include the necessity of managing the signal species propagating along the optical axis in a direction opposite to that of the primary beam. However, even a simple implementation, providing the integral dark-field signal only, has not only delivered plenty of results in the very low energy range below 50 eV, but the performance in the range of hundreds of eV and units of keV has also been substantially improved. The scanning LEEM method is illustrated using experimental results acquired by additionally employing multichannel detection and detection of transmitted electrons.

In the present talk, MgAl2O4 in the Al2O3/Al-1.0mass%Mg2Si alloy composite was also observed by a scanning electron microscope equipped with the low energy electron (SLEEM) adaptation aiming at examination of its morphology and orientation relationships to the Al2O3 particles. Owing to its much smaller interaction volume of signal exciting electrons in the target and hence more localized information, together with a favorable combination of secondary (SE) and backscattered (BSE) electron signals, the SLEEM method provided much better readable and detailed images of all particles, their shapes and mutual orientations, in comparison with conventional SE and BSE images at the electron energies usually used in the SEM. MgAl2O4 (spinels) were formed on facets of Al2O3 as small particles, and their shape well corresponded to an octahedron consisting of 8 equiaxial triangles.

A method for scanning electron microscopy imaging of nonconductive specimens, based on measurement and utilisation of a critical energy, is described in detail together with examples of its application. The critical energy, at which the total electron yield curve crosses the unit level, is estimated on the basis of measurement of the image signal development from the beginning of irradiation. This approach, concentrated onto the detected signal as the only quantity crucial for the given purpose of acquiring a noncharged micrograph, evades consequences of any changes in an irradiated specimen that influence the total electron yield curve and possibly also the critical energy value. Implementation of the automated method, realised using a cathode lens-equipped scanning electron microsope (SEM), enables one to establish a mean rate of charging over the field of view and its dependence on the electron landing energy. This dependence enables one to determine the energy of a minimum damage of the image of the given field of view. Factors influencing reliability and applicability of the method are discussed and examples of noncharged micrographs of specimens from both life and material science fields are presented.

Studies concerning assessment of the image quality in scanning electron microscopes and studies evaluating the detective efficiency of the secondary electrical (SE) detectors in these microscopes must be based on statistics of SE emission. The vast majority of previous studies have applied Poisson statistics, although their prerequisites have not been satisfied in must cases. This paper is concerned with the limits to the applicability of Poisson statistics to SE emission. Adequate definition of a non-Poisson factor in the variance of the number of SEs emitted is discussed. and a simple formula for this factor is derived for the low yield case in which both the primary and the backscattered electron are assumed not to release more than one SE. These conditions are met with conductive specimens composed of light elements at primary electron (PE) energies of tens of keV. For the lightest specimens, such as carbon, the non-Poisson factor can even be neglected for PEs >10 keV.

Although doped regions in semiconductors have been shown to give a different secondary electron yield in low-voltage scanning electron microscopy, the basic interpretation of this contrast has been difficult. It is accepted that this contrast stem from electronic phenomenon rather than atomic number differences between differently doped regions. However, the question is whether variations in the patch fields above the sample surface, balancing variations in the inner potentials, or surface coatings and/or surface states are the mechanisms responsible for the observed contrast. The present study reports on comparative experiments of these two models and demonstrates that the image contrast can be controlled by the presence of thin-surface metallic coatings. These results are the first evidence of the adlayer contacts, i.e., the subsurface electric fields instead of the patch fields above the surface, being responsible for the secondary electron contrast of doped semiconductors imaged in low voltage scanning electron microscopes under standard vacuum conditions, and they pave the way for the routine use of this method in semiconductor research and industry.

At a landing energy of 10 eV it is possible to achieve spatial resolution of the same order as at the nominal energy, which is usually 15 keV in the classical scanning electron microscope, by taking advantages of the optical properties of the cathode lens. Two different types of the detection system were designed and tested to learn as much about the optical properties of this system as possible and to start to understand the contrast mechanisms at very low energies. Great changes in the contrast take place when the landing energy is changed from 10 eV to an energy of about 2 keV.

High resolution can be obtained in the scanning electron microscope (SEM) for a very low landing energy of electrons, even for that below 50 eV, when a cathode lens is used with the specimen as a cathode held at a high negative potential but the detection of signal electrons is totally different compared with classical SEM. Primary electrons with an energy of the order of tens of keV are decelerated in the field of the cathode lens to a very low landing energy and signal electrons originating in the specimen are accelerated and collimated by the same field to a narrow beam with an electron energy nearly the same as that of the primary beam. To detect these signal electrons we must deflect them from the optical axis without deteriorating the properties of the primary beam. The design of a novel type of separator of the primary and signal electrons consisting of two stages, each of them formed by the electric and magnetic crossed fields, is presented, together with calculated trajectories for both primary and signal electrons.

The topographic contrast in a scanning electron microscope with very slow electrons is examined in case the cathode lens is used for adjusting the landing energy. Measurements are presented regarding the behaviour of planar contrasts at low energies and a significant improvement of the surface detail visualization is demonstrated, together with the possibility of controlling the electron impact angle.

Minimum necessary adaptations are described that are sufficient for obtaining very low energy electron micrographs (VLEEMs) from commercially available routine scanning electron micrographs (SEMs) with the electrons accelerated to an energy of the order of tens of keV. A cathode lens inserted into the specimen chamber enables one to decelerate electrons in front of the specimen surface to a desired low landing energy, which can be freely varied even down to zero. When a potential slightly more negative than the accelerating voltage is applied, a scanning mirror electron microscopy mode can be effected. The achievable point resolution at very low energies proves to be not too dependent on the objective lens parameters, so that the physical limit of aberrations of the homogeneous field of the cathode lens is nearly attainable. The detection efficiency for the standard Everhart-Thornley secondary electron detector is discussed, and results for the routine Tesla BS 340 SEM are presented.

One of the well-proven and efficient methods of obtaining a very low-energy impact of primary electrons in the scanning electron microscope is to introduce a retarding field element below the pole piece of the objective lens (OL). It is advantageous to use the specimen alone as the negatively biased electrode (i.e., cathode of the cathode lens). The optical power of the cathode lens modifies some of the standard parameters of the image formation such as relation of working distance to OL excitation or magnification to the scanning coils current, the impact angle of primary electrons, and so forth. In computer-controlled electron microscopes these parameters, particularly with regard to focusing and magnification, can be corrected automatically. Derivation of algorithms for such corrections and their experimental verifications are presented in this paper. Furthermore, a more accurate analytical expression for the focal length of an aperture lens is derived.

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Scanning electron imaging of plan views of boron-doped patterns in silicon is examined, together with the mechanism of formation of the electronic contrast in this kind of structures. Main to-date published results are critically reviewed and new data are presented concerning the secondary, backscattered and total-emission electron contrasts, including their qualitative and quantitative behaviour, particularly in the low energy range achieved with the help of the cathode lens (the scanning low energy electron microscopy mode, SLEEM). Surface analysis of the structure by means of Auger electron spectrometer has been performed, too, both before and after ion beam bombardment. The scanning electron microscope micrographs, acquired after the oxide mask removal in HF, are examined in a variety of detection modes, aiming at identification of the signal component primarily bearing the contrast. The energy dependence of the contrasts is presented as well as its change owing to alteration in the vacuum conditions. The most important findings include an extremely high contrast obtained in the SLEEM mode and even more enhanced under medium vacuum conditions at which the carbonaceous layer of surface contamination plays its role. The observed phenomena are partly explained in the frame of the “flat band” model of a passivated surface. The increased contrast in the SLEEM mode is understood as connected with the above-surface electric field of the cathode lens, generating space charge layers inside the semiconductor. In addition, charge carriers, injected via the primary electron beam, are considered as influencing the contrast vs. energy dependence.

Publisher Summary This chapter discusses the advances in scanning electron microscopy (SEM). Alternatives to the previously characterized main body, physical part, or column of the SEM have progressively been introduced, including (1) scanning columns for electron spectrometers, such as those suitable to be inserted inside a cylindrical mirror energy analyzer, (2) testers and lithographs for semiconductor technology, and (3) miniaturized versions. The issues regarding further development of the classical general-purpose SEM are discussed in the chapter. Computer-aided design methods for calculation of electrostatic and magnetic elements and simulation of electron trajectories have enabled significant progress in tailoring the column design to prescribed electron optical parameters. Complete computer control of the device opens approaches to full utilization and easy adjustment of all possible operation modes. These two aspects are most important with regard to the recent development outlined in the chapter, and some new ideas have proved viable, particularly that of variable beam energy along the column. In SEM, new technologies—such as rare-earth based permanent magnets and particularly the family of various micro- and nanotechnologies that have projected themselves into the SEM instrumentation—are used.

We discuss an extension to the transmission mode of the cathode-lens-equipped scanning electron microscope, enabling operation down to the lowest energies of electrons. Penetration of electrons through free-standing ultrathin films is examined along the full energy scale, and the contribution of the secondary electrons (SEs), released near the bottom surface of the sample, is shown, enhancing the apparent transmissivity of the sample to more than 100%. Provisional filtering off of the SEs, providing the dark-field signal of forward-scattered electrons, was made using an annular 3-D adjustable detector inserted below the sample. Demonstration experiments were performed on the graphene flakes and on a 3-nm-thick carbon film. Electron penetrability at the lowest energies was measured on the graphene sample.

The importance of high resolution imaging of dopant contrast in semiconductor structures parallels the continuous increase in the degree of their integration and complexity and in the size of substrates. Some scanning electron microscopy modes show moderate contrast between differently doped areas, but its detailed interpretation remains questionable, in particular, as regards the measurement of the dopant concentration. Photoemission spectromicroscopy on silicon substrates with patterns of opposite-type dopants suggests that the p∕n contrast is primarily related to local differences in the absorption of hot electrons along their trajectory toward the surface. This explanation is also expected to be valid in the interpretation of image contrasts formed by secondary electrons or very slow backscattered electrons. Wide-field photoemission electron microscopy has proven itself a fast imaging method providing large p-n contrast and the prospect of high-level resolution.

This paper concerns the problem of testing the image resolution in scanned electron micrographs, namely from the point of view of the image contrast for the standard gold/carbon test specimen within the full energy scale, down to eV units. Microscopes equipped with a cathode lens are considered and experimental results are presented for three devices differing in vacuum conditions and fields surrounding the specimen. At very low energies, the contrast is shown to either invert or disappear and this ambiguity is discussed and confronted with data simulated on the basis of measured electron yields from gold and carbon. It is concluded that the observations can be explained in terms of the surface cleanliness and strength of the surrounding fields.