Historical perspective and current trends in emission microscopy, mirror electron microscopy and low-energy electron microscopy. An introduction to the proceedings of the Second International Symposium and Workshop on Emission microscopy and Related Techniques

Emission microscopes and related instruments comprise a specialized class of electron microscopes that have in common an acceleration field in combination with the first stage of imaging (i.e., an immersion objective lens, also called a cathode lens or emission lens). These imaging techniques include photoelectron emission microscopy (PEEM or PEM), electron emission induced by heat, ions, or neutral particles, mirror electron microscopy (MEM), and low-energy electron microscopy (LEEM), among others. In these instruments the specimen is placed on a flat cathode or is the cathode itself. The low-energy electrons that are emitted, reflected, or backscattered from the specimen are first accelerated and then imaged by means of an electron lens system resembling that of a transmission electron microscope. The image is formed in a parallel mode in all of the above instruments, in contrast to the image in scanning electron microscopes, where the information is collected sequentially by scanning the specimen. A brief history and introduction to emission microscopy, MEM, and LEEM is presented as a background for the Proceedings of the Second International Symposium and Workshop on this subject, held in Seattle, Washington, August 16-17, 1990. Current trends in this field gleaned from the presentations at that meeting are discussed.     

Low-energy electron microscopy (LEEM) and mirror electron microscopy (MEM) of biological specimens: Preliminary results with a novel beam separating system

Low-energy electron microscopy (LEEM) and mirror electron microscopy (MEM) utilize a parallel beam of slow-moving electrons backscattered from the specimen surface to form an image. If the electrons strike the surface an LEEM image is produced and if they are turned back just before reaching the surface an MEM image results. The applications thus far have been in surface physics. In the present study, applications of LEEM and MEM in the biological sciences are discussed. The preliminary results demonstrate the feasibility of forming images of uncoated cultured cells and cellular components using electrons in the threshold region (i.e. 0–10 V). The results also constitute a successful test of a novel beam-separating system for LEEM and MEM.     

Medipix 2 detector applied to low energy electron microscopy

Low energy electron microscopy (LEEM) and photo-emission electron microscopy (PEEM) traditionally use microchannel plates (MCPs), a phosphor screen and a CCD-camera to record images and diffraction patterns. In recent years, however, MCPs have become a limiting factor for these types of microscopy. Here, we report on a successful test series using a solid state hybrid pixel detector, Medipix 2, in LEEM and PEEM. Medipix 2 is a background-free detector with an infinite dynamic range, making it very promising for both real-space imaging and spectroscopy. We demonstrate a significant enhancement of both image contrast and resolution, as compared to MCPs. Since aging of the Medipix 2 detector is negligible for the electron energies used in LEEM/PEEM, we expect Medipix to become the detector of choice for a new generation of systems.     

A new aberration-corrected,energy-filtered LEEM/PEEM instrument. I. Principles and design

We describe a new design for an aberration-corrected low energy electron microscope (LEEM) and photo electron emission microscope (PEEM), equipped with an in-line electron energy filter. The chromatic and spherical aberrations of the objective lens are corrected with an electrostatic electron mirror that provides independent control over the chromatic and spherical aberration coefficients C_c and C₃, as well as the mirror focal length, to match and correct the aberrations of the objective lens. For LEEM (PEEM) the theoretical resolution is calculated to be ∼1.5 nm (∼4 nm). Unlike previous designs, this instrument makes use of two magnetic prism arrays to guide the electron beam from the sample to the electron mirror, removing chromatic dispersion in front of the mirror by symmetry. The aberration correction optics was retrofitted to an uncorrected instrument with a base resolution of 4.1 nm in LEEM. Initial results in LEEM show an improvement in resolution to ∼2 nm.     

Double aberration correction in a low-energy electron microscope

The lateral resolution of a surface sensitive low-energy electron microscope (LEEM) has been improved below 4 nm for the first time. This breakthrough has only been possible by simultaneously correcting the unavoidable spherical and chromatic aberrations of the lens system. We present an experimental criterion to quantify the aberration correction and to optimize the electron optical system. The obtained lateral resolution of 2.6 nm in LEEM enables the first surface sensitive, electron microscopic observation of the herringbone reconstruction on the Au(1 1 1) surface.     

Breaking the spherical and chromatic aberration barrier in transmission electron microscopy

Since the invention of transmission electron microscopy (TEM) in 1932 (Z. Physik 78 (1932) 318) engineering improvements have advanced system resolutions to levels that are now limited only by the two fundamental aberrations of electron lenses; spherical and chromatic aberration (Z. Phys. 101 (1936) 593). Since both aberrations scale with the dimensions of the lens, research resolution requirements are pushing the designs to lenses with only a few mm space in the pole-piece gap for the specimen. This is in conflict with the demand for more and more space at the specimen, necessary in order to enable novel techniques in TEM, such as He-cooled cryo electron microscopy, 3D-reconstruction through tomography (Science 302 (2003) 1396) TEM in gaseous environments, or in situ experiments (Nature 427 (2004) 426). All these techniques will only be able to achieve Angstrom resolution when the aberration barriers have been overcome. The spherical aberration barrier has recently been broken by introducing spherical aberration correctors (Nature 392 (1998) 392, 418 (2002) 617), but the correction of the remaining chromatic aberrations have proved to be too difficult for the present state of technology (Optik 57 (1980) 73). Here we present an alternative and successful method to eliminate the chromatic blur, which consists of monochromating the TEM beam (Inst. Phys. Conf. Ser. 161 (1999) 191). We show directly interpretable resolutions well below 1A for the first time, which is significantly better than any TEM operating at 200 KV has reached before.     

Analytical scanning electron microscopy for solid surface

A scanning electron microscope of ultra-high-vacuum (UHV-SEM) with a field emission gun (FEG) is operated at the primary electron energies of from 100 eV to 3 keV. The instrument can form the images that contain information on surface chemical composition, chemical bonding state (electronic structure), and surface crystal structure in a microscopic resolution of several hundred angstroms (Å) using the techniques of scanning Auger electron microscope, scanning electron energy loss microscope, and scanning low-energy electron diffraction (LEED) microscope. A scanning tunneling microscope (STM) also has been combined with the SEM in order to obtain the atomic resolution for the solid surface. The instrumentation and examples of their applications are presented both for scanning LEED microscopy and STM.     

Very low energy microscopy in commercial SEMs

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.     

Design and performance of a high-resolution photoelectron microscope

The design of a high-resolution photoelectron microscope (photoelectron emission microscope) is described. It is an oil-free ultrahigh-vacuum instrument utilizing electrostatic electron optics. New designs are presented for a specimen translator, cathode stage, aperture stop control, electrostatic hexapole stigmator, beam shutter, and camera system. These components could also be used in a low-energy electron microscope (LEEM). The theoretical resolution of this instrument is 5 nm for UV illumination near the photoemission threshold. The photoelectron microscope is now in operation at the University of Oregon, and it is achieving results within a factor of two of this design limit.     

Elemental imaging and resolution in energy-filtered conventional electron microscopy

Energy-filtered transmission electron microscopy (EFEM) was used to image the distributions of uranium and carbon in uranyl acetate stained catalase crystals. The spatial resolution obtained from inelastic C K-edge and U O4,5-edge images, determined from the highest-order reflection in the computed diffraction pattern, was 3.4 nm for both carbon and uranium. The resolution limit imposed by the delocalization of inelastic scattering was estimated from cross-section measurements to be 0.6 nm for U and 0.2 nm for C. Considering both delocalization and the effects of microscope aberrations, for an objective lens chromatic aberration coefficient of 2.8 mm and 10 eV energy window, the calculated resolutions are 2.0 nm for C and 1.2 nm for U. The effects of plural inelastic and elastic-inelastic scattering were sufficiently large to show crystalline structure in unprocessed pre-edge inelastic images. Previously suggested methods for eliminating these artifacts were applied to obtain the compositional information in the catalase EFEM images.     

Electron beam confinement and image contrast enhancement in near field emission scanning electron microscopy

In conventional scanning electron microscopy (SEM), the lateral resolution is limited by the electron beam diameter impinging on the specimen surface. Near field emission scanning electron microscopy (NFESEM) provides a simple means of overcoming this limit; however, the most suitable field emitter remains to be determined. NFESEM has been used in this work to investigate the W (1 1 0) surface with single-crystal tungsten tips of (3 1 0), (1 1 1), and (1 0 0)-orientations. The topographic images generated from both the electron intensity variations and the field emission current indicate higher resolution capabilities with decreasing tip work function than with polycrystalline tungsten tips. The confinement of the electron beam transcends the resolution limitations of the geometrical models, which are determined by the minimum beam width.     

The resolution of photoelectron microscopes with UV, X-ray, and synchrotron excitation sources

The resolution of emission electron microscopes is calculated by determining the intensity distribution in the image. The object is a small disc of uniform brightness centered on the axis. A finite object, as distinct form a point source, provides a non-zero current in the image without the requirement of infinite object brightness and the consequent infinities in the geometrical intensity distribution. The minimum object size, which in turn affects the resolution of the microscope, depends on the minimum current or contrast required in the image. In photoelectron microscopes with UV illumination just above the threshold for emission the predominant aberrations are the chromatic and spherical aberrations of the accelerating field and the spherical aberration of the objective lens. For higher energies, e.g. in the soft X-ray range, the chromatic aberration of the objective lens must also be taken into account, as the aberration coefficients of the accelerating field are greatly reduced. The intensity distributions in the image are calculated first for single energies. The intensity distribution for a beam with a range of energies is obtained by adding a series of single-energy distribution curves weighted according to the energy distribution function. In the presence of spherical aberration the position of the image formed by the electrons depends on the angle of emission. In image planes between the paraxial and marginal planes the combination of spherical aberration and defocus causes the the image spot to have a retrograde type of behavior as the angle of emission increases. The image spot initially moves away from the axis in the azimuth of emission and then returns to the axis and moves away in the opposite azimuth. As a result the intensity in the central portion of the image plane is enhanced. The single-energy intensity distribution curves calculated as a function of depth in the image reveal the existence of a compact, high-intensity image peak in an image plane located between the paraxial and marginal planes. This peak occurs in the plane in which the image spot has a maximum retrograde displacement equal to its radius. The present analysis shows that the resolution in the high-intensity plane is better than in the plane of least confusion, and the effects of aberrations in these two planes are quite different.(ABSTRACT TRUNCATED AT 400 WORDS)     

Development of an X-ray photoemission electron microscopy system with multi-probes, and its application to surface imaging at static and dynamic states

We have developed a new X-ray photoemission electron microscopy system combined with low energy electron microscopy, photoemission electron microscopy, mirror electron microscopy (MEM), secondary electron emission microscopy (SEEM) and Auger electron emission microscopy, which provides multi-angle information on the distribution and change of element, chemical state, structure, etc. at solid surfaces under the working conditions such as high temperature and gas atmosphere. The performance of each microscopical method was examined and typical images are presented. The dynamic behaviour of fabricated surfaces has been imaged in real time by SEEM and MEM.     

Depth of information in photoelectron microscopy

The depth of information is defined as the distance below the surface of a specimen from which information is contributed at a specified resolution. A simplified model of photoemission is used to explore the relationship between electron escape depths and depth of information in photoelectron microscopy (PEM or photoemission electron microscopy). The depth of information is equal to the escape depth when the escape depth is small relative to the instrument resolution. When the escape depth is large compared to the instrument resolution or when information is carried for example by reflected light, the image consists of well resolved surface detail at the instrument resolution and dimmer, more diffuse, images of detail below the surface. Thus the same sample can exhibit different depths of information depending on the image details of interest. Other mechanisms of transmitting information to the surface, for example induced topography, are discussed, and experimental examples are given.     

Preparation of frozen-hydrated specimens for high resolution electron microscopy

A method is presented for preserving the high resolution structure of biological membranes in a frozen-hydrated environment for electron microscopy. The technique consists of sandwiching a specimen between two carbon films and then waiting while some of the solvent evaporates. When the solvent layer is judged to be of an appropriate thickness, the specimen is then frozen in liquid nitrogen. The specimen can then be inserted into the precooled stage of an electron microscope. Electron diffraction studies of the purple membrane of Halobacterium halobium recorded at -120 degrees C have shown that the structure can be preserved to a resolution of 3.5 A. The main advantage of this method over previous techniques is that the hydrating conditions can be accurately controlled.     

High-resolution scanning electron microscopy.

The spatial resolution of the scanning electron microscope is limited by at least three factors: the diameter of the electron probe, the size and shape of the beam/specimen interaction volume with the solid for the mode of imaging employed and the Poisson statistics of the detected signal. Any practical consideration of the high-resolution performance of the SEM must therefore also involve a knowledge of the contrast available from the signal producing the image and the radiation sensitivity of the specimen. With state-of-the-art electron optics, resolutions of the order of 1 nm are now possible. The optimum conditions for achieving such performance with the minimum radiation damage to the specimen correspond to beam energies in the range 1-3 keV. Progress beyond this level may be restricted by the delocalization of SE production and ultimate limits to electron-optical performance.     

Mechanisms of decoherence in electron microscopy

The understanding and where possible the minimisation of decoherence mechanisms in electron microscopy were first studied in plasmon loss, diffraction contrast images but are of even more acute relevance in high resolution TEM phase contrast imaging and electron holography. With the development of phase retrieval techniques they merit further attention particularly when their effect cannot be eliminated by currently available energy filters. The roles of electronic excitation, thermal diffuse scattering, transition radiation and bremsstrahlung are examined here not only in the specimen but also in the electron optical column. Terahertz-range aloof beam electronic excitation appears to account satisfactorily for recent observations of decoherence in electron holography. An apparent low frequency divergence can emerge for the calculated classical bremsstrahlung event probability but can be ignored for photon wavelengths exceeding the required coherence distance or path lengths in the equipment. Most bremsstrahlung event probabilities are negligibly important except possibly in large-angle bending magnets or mandolin systems. A more reliable procedure for subtracting thermal diffuse scattering from diffraction pattern intensities is proposed.     

Deconvolution of scanning electron microscopy images

This paper describes a method of removing blurs in scanning electron microscopy (SEM) images caused by the existence of a finite beam size. Although the resolution of electron microscopy images has been dramatically improved by the use of high-brightness electron guns and low-aberration electron lenses, it is still limited by lens aberration and electron diffraction. Both are inevitable in practical electron optics. Therefore, a further reduction in resolution by improving SEM hardware seems difficult. In order to overcome this difficulty, computer deconvolution has been proposed for SEM images. In the present work, the SEM image is deconvoluted using the electron beam profile estimated from beam optics calculation. The results show that the resolution of the deconvoluted image is improved to one half of the resolution of the original SEM image.     

Amplification and noise in high-pressure scanning electron microscopy

High-pressure scanning electron microscopy (HPSEM) is a promising new family of techniques. The present knowledge of these techniques is reviewed and a new set of criteria developed for optimizing signal detection in HPSEM with a view to preserving specimen integrity. For this purpose, amplification of contrast signals generated in HPSEM was examined by computing the effect of ionization over a range of pressures and biasing fields, routinely used for this technique. The influence of secondary ionization due to ion impact was included in the calculations. To check the calculated results, the experiments were performed in the HPSEM apparatus in a nitrogen atmosphere. A divergence between the experimental values and the calculated values was found. This was removed by taking into account the effect of recombination of charge carriers. Inductive currents generated in the HPSEM environment are transient and do not affect the conclusions of this study. The gas pressure, biasing fields and beam current for preserving specimen integrity and obtaining good micrographs were selected from the data. Experimental measurements of noise are reported, and criteria for optimizing the signal-to-noise ratio for performing HPSEM are discussed. The application of these criteria has shown that specimen current detection can be more advantageous than other methods and configurations of detection and was capable of obtaining high/medium-resolution micrographs.     

Computer-simulated high-resolution transmission electron microscopy (HRTEM) in tourmaline

The contrast distributions observed in high-resolution transmission electron microscopy (HRTEM) images of tourmaline depend on the types and magnitudes of the exchange components present and on the degree of atom overlap along the direction of observation. Furthermore, the fractional atomic coordinates in tourmalines are valid only for the specific specimen refined. These properties make the interpretation of experimental HRTEM images of tourmaline using image simulation if not impossible at least extremely difficult. A correct interpretation of experimental HRTEM images of tourmaline is possible provided the structural refinement data on the same crystal are available. Nevertheless, it is possible to interpret the experimental HRTEM images of tourmaline if the composition of the structural model chosen during image simulations approximates the composition of the specimen studied by electron microscopy. A good control of the composition of the specimen studied and an appropriate choice of a structural model for image simulation are therefore as important as properly controlling specimen thickness, specimen tilt, beam tilt and objective lens defocus.