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The scanning electron microscope (SEM) has become the most widely used of all advanced imaging tools because it offers a unique range of capabilities. It can resolve and image objects with sizes ranging from millimeters to below 1 nm; it offers multiple ways to generate, collect, and display signals; the images produced contain information about the topography, chemical composition, and the magnetic, electrostatic, and crystallographic properties of the sample; and it can generate characteristic x-ray emission from the specimen to provide a quantitative chemical analysis. Unfortunately, one thing that it will be unable to do is maintain its competitive edge in the 21st century. This is because electrons are electromagnetic ‘‘waves’’ and thus the smallest spot, ‘‘d,’’ into which an electron beam can be focused has a diameter of the order of: d 1⁄4 k=a ð1Þ

This article provides an introduction to scanning ion microscopy, explaining how it overcomes one of the biggest limitations of SEMs, namely the tradeoff between spatial resolution and depth of field, while also providing significantly more surface detail, a wide range of novel and familiar contrast mechanisms, and the potential for new microanalytical techniques that combine nanometer spatial resolution and single monolayer sensitivity. In addition to describing the capabilities of scanning ion microscopes, the article also addresses the issue of sample charging and the potential for physical damage that can result from ion beam irradiation.

Because the ability to perform some form of chemical microanalysis has become an essential feature for any microscope, it is necessary to investigate what options are available in the new “ORION” helium ion microscope (HIM). The HIM has the ability to visualize local variations in specimen chemistry in both the ion induced secondary electron and the Rutherford backscattered imaging modes, but this provides only limited and qualitative information. Quantitative, elementally specific, microanalysis could be performed in the HIM using secondary electron spectroscopy, Rutherford backscattered ion spectroscopy, or secondary ion mass spectroscopy, but while each of these options has promise, none of them can presently guarantee either reliable element identification or quantitative analysis across the periodic table.

Nanocrystallites have garnered substantial interest due to their various applications, including catalysis and medical research. Consequently important aspects of synthesis related to control of shape and size through economical and non-hazardous means are desirable. Highly efficient bioreduction-based fabrication approaches that utilize microbes and/or plant extracts are poised to meet these needs. Here we show that the γ -proteobacterium Shewanella oneidensis can reduce tetrachloroaurate (III) ions to produce discrete extracellular spherical gold nanocrystallites. The particles were homogeneously shaped with multiple size distributions and produced under ambient conditions at high yield, 88% theoretical maximum. Further characterization revealed that the particles consist of spheres in the size range of ∼2–50 nm, with an average size of 12 ± 5 nm. The nanoparticles were hydrophilic and resisted aggregation even after several months. Based on our experiments, the particles are likely fabricated by the aid of reducing agents present in the bacterial cell membrane and are capped by a detachable protein/peptide coat. Ultraviolet–visible and Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive X-ray spectra and transmission electron microscopy measurements confirmed the formation, surface characteristics and crystalline nature of the nanoparticles. The antibacterial activity of these gold nanoparticles was assessed using Gram-negative ( Escherichia coli and S. oneidensis ) and Gram-positive ( Bacillus subtilis ) bacterial species. Toxicity assessments showed that the particles were neither toxic nor inhibitory to any of these bacteria.

Interest in engineered nanostructures has risen in recent years due to their use in energy conservation strategies and biomedicine. To ensure prudent development and use of nanomaterials, the fate and effects of such engineered structures on the environment should be understood. Interactions of nanomaterials with environmental microorganisms are inevitable, but the general consequences of such interactions remain unclear, due to a lack of standard methods for assessing such interactions. Therefore, we have initiated a multianalytical approach to understand the interactions of synthesized nanoparticles with bacterial systems. These efforts are focused initially on cerium oxide nanoparticles and model bacteria in order to evaluate characterization procedures and the possible fate of such materials in the environment. The growth and viability of the Gram-negative species Escherichia coli and Shewanella oneidensis , a metal-reducing bacterium, and the Gram-positive species Bacillus subtilis were examined relative to cerium oxide particle size, growth media, pH, and dosage. A hydrothermal synthesis approach was used to prepare cerium oxide nanoparticles of defined sizes in order to eliminate complications originating from the use of organic solvents and surfactants. Bactericidal effects were determined from MIC and CFU measurements, disk diffusion tests, and live/dead assays. For E. coli and B. subtilis , clear strain- and size-dependent inhibition was observed, whereas S. oneidensis appeared to be unaffected by the particles. Transmission electron microscopy along with microarray-based transcriptional profiling was used to understand the response mechanism of the bacteria. Use of multiple analytical approaches adds confidence to toxicity assessments, while the use of different bacterial systems highlights the potential wide-ranging effects of nanomaterial interactions in the environment.

The scanning helium ion microscope has been used in transmission mode to investigate both the feasibility of this approach and the utility of the signal content and the image information available. Operating at 40 keV the penetration of the ion beam, and the imaging resolution achieved, in MgO crystals was found to be in good agreement with values predicted by Monte Carlo modeling. The bright-field and annular dark-field signals displayed the anticipated contrasts associated with beam absorption and scattering. In addition, the diffraction of the He ion beam within the sample gave rise to crystallographic contrast effects in the form of thickness fringes and dislocation images. Scanning transmission He ion microscopy thus achieves useful sample penetration and provides nanometer scale resolution, high contrast images of crystalline materials and crystal defects even at modest beam energies.

Adhesion of spores of Bacillus thuringiensis (Bt) and spherical silica particles on surfaces was experimentally and theoretically investigated in this study. Topography analysis via atomic force microscopy (AFM) and electron microscopy indicates that Bt spores are rod shaped, approximately 1.3 mum in length and approximately 0.8 mum in diameter. The adhesion force of Bt spores and silica particles on gold-coated glass was measured at various relative humidity (RH) levels by AFM. It was expected that the adhesion force would vary with RH because the individual force components contributing to the adhesion force depend on RH. The adhesion force between a particle and a planar surface in atmospheric environments was modeled as the contribution of three major force components: capillary, van der Waals, and electrostatic interaction forces. Adhesion force measurements for Bt spore (silica particle) and the gold surface system were comparable with calculations. Modeling results show that there is a critical RH value, which depends on the hydrophobicity of the materials involved, below which the water meniscus does not form and the contribution of the capillary force is zero. As RH increases, the van der Waals force decreases while the capillary force increases to a maximum value.

A combination of the 'semi-empirical' model for secondary electron production and the TRIM routines which describe ion stopping power, scattering, and transport, has been used to construct a Monte Carlo simulation (IONiSE) that can quantitatively interpret the generation of secondary electrons (SE) from materials by fast helium ions. This approach requires that the parameters of the semi-empirical model be determined by fitting to experimental yield data but has the merit that, unlike more fundamental models, it can be applied with equal ease to both pure elements and complex compounds. The application of the model to predict the topographic yield variation of helium generated SE as a function of energy and material, and to investigate the ratio between SE generated by incident and backscattered ions, is demonstrated.

The absolute efficiency of X-ray production has been determined for the K-lines of Al, Si and Cu; for the L-lines of Fe, Co, Cu, Ge and As; and for the M-lines of Hf, Ir, Pt, Au and Bi, using overvoltage ratios in the range 1-10. These emissions, with the exception of the Cu K, have critical excitation energies below 2.6 keV and are therefore typical of the lines used for X-ray microanalysis at low beam energies. For K-lines it is found that the experimental results are in good agreement with a Bethe, or a Casnati, crosssection model. For the L- and M-lines a Monte Carlo technique has been used to find an effective X-ray generation cross-section for each of the elements. The functional forms of these cross-sections are found to be in general agreement with proposed theoretical models.

A formula is presented for computing the polar angle of collisions from partial elastic Mott cross-sections. It will be useful in Monte Carlo simulations of electrons' trajectories in solids and is based on the Newbury and Myklebust (1981) expression. It also is valid for all energy ranging from 0.1 to 30 keV. Also given is the tabulation of the constants of this formula to compute polar angles of collisions for the first 94 elements of the periodic table. The constants of this formula have been obtained by the numerical integration of the values of partial Mott cross-sections computed by Czyzewski et al. (1990) using Thomas-Fermi-Dirac atomic potentials for atomic numbers >54 and Hartree-fock potential for atomic numbers

In many applications such as optoelectronic devices, three-dimensional (3D) structures are required. Examples include photonic band gap (PBG) crystals, diffractive optical elements, blazed gratings, MEMS, NEMS, etc. It is known that the performance characteristics of such structures are highly sensitive to their dimensional fidelity. Therefore, it is essential to have a fabrication process by which such 3D structures can be realized with high dimensional accuracy. In this paper, practical methods to control thickness of the remaining resist and etch depth, which may be employed for fabrication of such 3D structures using grayscale electron-beam lithography, are described. Through experiments, explicit control of the remaining resist thickness and etch depth at the resolution of 20nm for the feature sizes of 0.5@mm and 1@mm has been successfully demonstrated. Also, the 1:1 ratio of silicon to resist etching rates was achieved for transferring the remaining resist profile onto the silicon substrate.

Electron beam-induced deposition (EBID) provides a simple way to fabricate submicron- or nanometer-scale structures from various elements in a scanning electron microscope (SEM). The growth rate and shape of the deposits are influenced by many factors. We have studied the growth rate and morphology of EBID-deposited nanostructures as a function of the tungsten hexafluoride (WF6) and tetraethylorthosilicate (TEOS) precursor gas pressure and growth time, and we have used Monte Carlo simulations to model the growth of tungsten and silicon oxide to elucidate the mechanisms involved in the EBID growth. The lateral radius of the deposit decreases with increasing pressure because of the enhanced vertical growth rate which limits competing lateral broadening produced by secondary and forward-scattered electrons. The morphology difference between the conical SiO(x) and the cylindrical W nanopillars is related to the difference in interaction volume between the two materials. A key parameter is the residence time of the precursor gas molecules. This is an exponential function of the surface temperature; it changes during nanopillar growth and is a function of the nanopillar material and the beam conditions.

The phase-contrast imaging of atomic lattices has now become commonplace for both Transmission Electron Microscopes (TEM) and Scanning Transmission Electron Microscopes (STEMs). Recently, however, bright-field STEM images of multi-wall carbon nanotubes (MWCNTs) recorded from an ultra-high resolution (UHR) in-lens field-emission scanning electron microscope (FE-SEM) operating at 30keV have also demonstrated lattice fringe resolution. One example of such an image containing multiple examples of fringe detail is shown in figure 1. The carbon lattice fringes were analyzed and their origin confirmed by the application of the FFT algorithms in the SMART image analysis program. The resulting power spectrum after thresholding to remove background noise (Figure 2) confirms that phase detail in the image extends down to about 5 Angstroms (0.5nm) and that well defined diffraction spots corresponding to a spacing of 3.4 Angstroms (0.34nm) generated by the (002) basal plane spacing of the graphite lattice are present.

A Monte Carlo simulation of the contrast variation across phase boundaries in backscattered electron images of multiple phase composition systems has been used to develop a model for prediction of the position of the interface based solely on a knowledge of the signal intensity levels on either side of the interface. A wide range of average atomic numbers of the phases on either side of the boundary have been investigated at incident beam energies of 5, 10, 15, and 25 kV and a least-squares minimisation procedure used to optimise the parameters of a generalised model.

A field-emission scanning electron microscope (FESEM) equipped with the standard secondary electron (SE) detector was used to image thin (70-90 nm) and thick (1-3 microns) sections of biological materials that were chemically fixed, dehydrated, and embedded in resin. The preparation procedures, as well as subsequent staining of the sections, were identical to those commonly used to prepare thin sections of biological material for observation with the transmission electron microscope (TEM). The results suggested that the heavy metals, namely, osmium, uranium, and lead, that were used for postfixation and staining of the tissue provided an adequate SE signal that enabled imaging of the cells and organelles present in the sections. The FESEM was also used to image sections of tissues that were selectively stained using cytochemical and immunocytochemical techniques. Furthermore, thick sections could also be imaged in the SE mode. Stereo pairs of thick sections were easily recorded and provided images that approached those normally associated with high-voltage TEM.

Empirical forms for electron/atom scattering cross sections predict backscattering factors that compare well with those calculated using tabulated Mott data from 0.1 to 30 keV. The form of the empirical total cross section is similar to the screened Rutherford cross section. The fit to the tabulated differential Mott cross sections is decomposed into two parts, one part being of the same mathematical form as the screened Rutherford cross section (σR), and the second part being an isotropic distribution (σI). The ratio of the total cross sections (σR/σI) between the screened Rutherford part of the differential scattering cross section and the isotropic part of the distribution is fitted to give the same ratio of forward to backscattered currents as the tabulated Mott differential cross sections. The three equations, one for the total elastic cross section and two describing the differential cross section—one for the Rutherford screening parameter and one for the ratio σR/σI—give backscattering results covering all the major trends with energy and atomic number compared with the backscattering coefficients calculated using tabulated Mott cross sections. However, agreement with experiment is poor for some well-researched examples such as Au. Monte Carlo calculations using the empirical cross sections show that surface effects may be critical in interpreting experimental results.

Monte Carlo modeling of electron-solid interactions requires a detailed and accurate supply of experimental data on which to base its physics and against which to test its predictions. To meet this need, a collection of data—comprising measurements of secondary and backscattered electron yields, electron stopping powers, and x-ray ionization cross sections, as a function of energy—has been assembled from published sources. The quality and quantity of the compilation varies widely, with little or no data being available for the majority of elements in the periodic table, while results for complex materials of current technologic interest are also almost nonexistent. To meet the needs of Monte Carlo simulation in areas such as dimensional metrology or microanalysis, a program of systematic measurements is required.

Experimental nanotips have shown significant improvement in the resolution performance of a cold field emission scanning electron microscope (SEM). Nanotip electron sources are very sharp electron emitter tips used as a replacement for the conventional tungsten field emission (FE) electron sources. Nanotips offer higher brightness and smaller electron source size. An electron microscope equipped with a nanotip electron gun can provide images with higher spatial resolution and with better signal-to-noise ratio. This could present a considerable advantage over the current SEM electron gun technology if the tips are sufficiently long-lasting and stable for practical use. In this study, an older field-emission critical dimension (CD) SEM was used as an experimental test platform. Substitution of tungsten nanotips for the regular cathodes required modification of the electron gun circuitry and preparation of nanotips that properly fit the electron gun assembly. In addition, this work contains the results of the modeling and theoretical calculation of the electron gun performance for regular and nanotips, the preparation of the SEM including the design and assembly of a measuring system for essential instrument parameters, design and modification of the electron gun control electronics, development of a procedure for tip exchange, and tests of regular emitter, sharp emitter and nanotips. Nanotip fabrication and characterization procedures were also developed. Using a "sharp" tip as an intermediate to the nanotip clearly demonstrated an improvement in the performance of the test SEM. This and the results of the theoretical assessment gave support for the installation of the nanotips as the next step and pointed to potentially even better performance. Images taken with experimental nanotips showed a minimum two-fold improvement in resolution performance than the specification of the test SEM. The stability of the nanotip electron gun was excellent; the tip stayed useful for high-resolution imaging for several hours during many days of tests. The tip lifetime was found to be several months in light use. This paper summarizes the current state of the work and points to future possibilities that will open when electron guns can be designed to take full advantage of the nanotip electron emitters.

Charge accumulation in insulating or semiconducting samples due to electron beam irradiation is one of the key problems in electron microscopy. One of the most promising techniques for reducing the severity of such charging is to surround the sample with a low-pressure atmosphere of a gas. The charging behavior of a number of materials, surrounded by a variety of gases, has been determined to identify the important factors which control charging under these conditions. The magnitude of the surface potential was deduced from an analysis of x-ray spectra from the surface. The relationship between surface charge, gas pressure, and gas type are measured, and the charging reduction efficiency (CRE) is compared.

Charging is one of the most important problems encountered in scanning electron microscopy and as a result this phenomenon it has received a lot of both theoretical and experimental attention. Despite this, many questions remain about the nature and behavior of charging because of the limitations of the experimental techniques available to study it. For example, although it is now straightforward to determine in situ the surface potential of a sample that is charging during irradiation, it is difficult to measure the lateral extent of the charging, or its persistence once the incident beam is switched off. We describe here a simple technique which provides a rapid way of visualizing the temporal and spatial behavior of charging phenomena.

The relationship between convolution/correlation operation and the data acquisition process of the scanning microscope and spectrometer families is analyzed. It is shown that a coordinate or event sensitive detector, and the intrinsic or extrinsic property of the specimen response, are two important factors in distinguishing the data acquisition mode of such systems. Four types of convolution- and correlation-based modes are extracted to illuminate the physical characteristics of scanning imaging and analysis systems by focusing on the probe, specimen, detector, and their relationships. Criteria for identifying these modes are explored. In addition, the physical meanings of general existing coefficients between the independent variables of convolution and correlation are investigated.

Experimental measurements are presented of the total scattering cross-section of four gases: He, Air, CH 4 , and Argon as a function of electron beam energy. The method used was that of Gauvin. A comparison of theoretical estimates of the total scattering cross-section with the experimental data indicates that the model used gives generally reliable results. The data confirm that the gases tend to be molecular rather than atomic in nature in this pressure range (1-300 Pascal). The factors affecting the accuracy of these results are examined.

A study of the temperature dependence of the electron beam induced deposition (EBID) of tungsten was carried out in a temperature range of −30–75°C under two conditions of beam energy and beam current using WF6 as the precursor gas. An Arrhenius relationship was found for the temperature dependence of the deposition rate which is consistent with an electron stimulated desorption mechanism for this process. In addition, the mechanism for EBID under different conditions was discussed.

Low voltage scanning electron microscopy (LVSEM) has become the imaging technique of choice for many applications because it offers surface specific information, and both control of charging and a reduction of damage to labile specimens. However fundamental limitations such as the electron wavelength, lens aberrations, and gun brightness, severely limit the performance of the LVSEM, and in addition some capabilities such as microanalysis are difficult or impossible. New technologies, including aberration correction and brighter electron sources are now available, and novel spectroscopic approaches are in development. Together these advances could significantly enhance the performance of the LVSEM. The advent of ultra-high performance ion column imaging systems offers interesting competition to the LVSEM for both imaging and analysis. [DOI: 10.1380/ejssnt.2006.369]

The basic principles of the scanning electron microscope (SEM) were established in the 1930's and early 1940's by Knoll, and then by von Ardenne in Germany and by Zworykin, Hillier and others in America. The SEM was revived by Charles Oatley in a series of PhD projects in the Electrical Engineering Department of Cambridge University in England. The first industrial application followed from the early work of McMullan and Smith in Cambridge and was at the Pulp and Paper Institute in Canada. This was soon followed by the application of the SEM to integrated circuits at Westinghouse in America and by the availability of commercial SEMs in England and Japan. At the present time, the SEM and other microscopic and microanalytical techniques are in a worldwide state of development and are being applied in an increasing number of application areas. Copyright © 2006 John Wiley & Sons, Ltd.

A new and thorough examination of secondary electron (SE) yield as a function of primary energy (EPE) and atomic number Z for the 44 elements in the database1 is made. The principles of the semiempirical universal law for the SE yield are described and a template for Monte Carlo (MC) simulation is produced accordingly. Both universal curve fitting and MC simulation are made for the 44 elements. The resulted maximum SE yield δm, corresponding primary energy , SE excitation energy e, and effective escape depth λ are tabulated and plotted as a function of atomic number Z. It is found that similarities exist in the profiles of e and λ, δm and , and all of these parameters seem to have characteristics associated with atomic shell filling. Copyright © 2005 John Wiley & Sons, Ltd.

The development of the microcalorimeter energy-dispersive X-ray spectrometer (µ-cal EDS) offers a significant advancement in X-ray microanalysis, especially for electron beam instruments. The benefits are especially pronounced for low voltage (≤5 kV) X-ray microanalysis in the field emission scanning electron microscope (FE-SEM) where the high energy resolution of the µ-cal EDS minimizes the peak overlaps among the myriad of K, L, M and N lines in the 0–5 keV energy range. The availability of L- and M-shell X-ray lines for microanalysis somewhat offsets the absence of X-ray lines traditionally used above 5 keV energy. The benefits and challenges of the µ-cal EDS will be discussed, including P/B ratio for characteristic X-rays, collection angle, count rate capability and the impact of polycapillary X-ray optics on microanalysis.

We have designed a low voltage point source microscope operated with a nanotip field emitter and without any electron optical lenses such that it can be operated in the transmission mode as well as in a reflection mode. An electron gun needed in the reflection mode is the most important difference between the two modes of operation. The magnification of the object wave is achieved by placing the specimen in the divergent electron beam of a nanotip field emitter and observing the object wave using a micro channel plate (MCP) at a great distance from the sample. As no lenses are present a procedure for scaling the magnification has been developed. Since electrons from a point source are highly coherent the out of focus images of the sample are interferograms and contain true three dimensional information of the sample. The transmission mode gives us the following results: (1) Electrons diffracted at an edge of the specimen cause Fresnel fringes in the image plane. (2) An electrically charged holey carbon foil can act in the same way on the electrons as the Young's double slit experiment and results in an interference pattern consisting of parallel fringes. The reflection mode shows us: (1) The image depends on the angle of reflection. (2) An arrangement similar to a field ion microscope resolves single atoms of the specimen. [DOI: 10.1380/ejssnt.2004.81]

We briefly discuss how to set-up our Hitachi HF-2000 transmission electron microscope for medium magnification holography. Then we apply this technique to examine the activation of an as-doped wafer by annealing. We also present voltage profiles of the source-drain region of a CMOS transistor with 75 nm gate architecture taken from an off-the-shelf Intel PIII processor. Special attention is given to the analysis of the reconstructed holograms. [DOI: 10.1380/ejssnt.2004.119]

The absolute efficiency of generation of a selection of K, L, and M- x-ray lines has been measured as a function of the incident electron beam energy. At an overvoltage U=2 this efficiency falls within the range 1E-4 to 1E-7, with K-lines being highest and L-Lines usually being the lowest. It is shown that for all three families of lines the efficiency has a functional variation which has the form A. (U- 1)n, as first suggested by Compton and Allison, where A and n are constants. Values of A and n for the K, L, and M shells are tabulated. The smoothly varying behavior of the efficiency makes it well suited for analytical use and spectrum simulation purposes.

By applying the basic principles of metrology we discuss how to define the standards that any experimental method to measure resolution has to obey. Our results clearly indicate the need to apply a calibration procedure when designing algorithms to estimate resolution to satisfy accuracy requirements. Similarly, the precision of an algorithm has to be clearly specified. We compare here the performances of a variety of commonly used implementations of published methods, with that of an algorithm based on an approach known to be reliable. Our results confirm that when an algorithm is designed with the clear intent of satisfying metrology requirements, it demonstrates excellent accuracy, precision, and lack of sensitivity to the noise level, as is desirable. As a consequence, the algorithm will have the ability to measure accurately the point spread function convoluted in the image, thus paving the way for quantitative deconvolution techniques.

The remarkable mechanical and electronic properties of graphene make it an ideal candidate for next generation nanoelectronics. With the recent development of commercial-level single-crystal graphene layers, the potential for manufacturing household graphene-based devices has improved, but significant challenges still remain with regards to patterning the graphene into devices. In the case of graphene supported on a substrate, traditional nanofabrication techniques such as e-beam lithography (EBL) are often used in fabricating graphene nanoribbons but the multi-step processes they require can result in contamination of the graphene with resists and solvents. In this letter, we report the utility of scanning helium ion lithography for fabricating functional graphene nanoconductors that are supported directly on a silicon dioxide layer and we measure the minimum feature size achievable due to limitations imposed by thermal fluctuations and ion scattering during the milling process. Further we demonstrate that ion beams, due to their positive charging nature, may be used to observe and test the conductivity of graphene-based nanoelectronic devices in situ.

A simple method is described to determine the effective gas path length when incident electrons scatter in the gas above the specimen. This method is based on the measurement of a characteristic x-ray line emitted from a region close to the incident beam. From various experimental measurements performed on various microscopes, it is shown that the effective gas path length may increase with the chamber pressure and that it is also often dependent of the type of x-ray bullet.

Except in the idealized case where the unknown and the standard are essentially identical obtaining accurate matrix corrections requires a knowledge of the absolute value and functional behavior of a number of quantities such the mass absorption coefficient, the electron stopping power, ionization cross sections and fluorescent yields. This talk examines the accuracy of the data available in each category, and the range of elements and compounds for which values have been published. It is found that the quality and quantity of data available varies greatly and that, with only a few exceptions, much more work is required to produce the reliable and inclusive data base required for accurate matrix corrections.

Serial block face scanning electron microscopy (SBF-SEM) provides nanoscale 3D ultrastructure of entire cells and tissue volumes. In SBF-SEM, an ultramicrotome built into the SEM specimen stage successively removes thin sections from a plastic-embedded, heavy metal-stained specimen. After each cut, the freshly exposed block face is imaged at a low incident electron energy using a backscattered electron detector to provide 3D ultrastructure with a resolution of approximately 5 nm in the plane of the block face and around 25 nm in the perpendicular z-direction, as limited by the slice thickness. We have explored the feasibility of improving the z-resolution in SBF-SEM by recording images at multiple primary beam energies, thus sampling different depths below the block surface.A linear relationship was found between the depth of test structures, generated by Monte Carlo simulations, and the ratio of backscattered image intensities recorded at primary beam energies between 1.4 keV and 6.8 keV. This enabled us to reconstruct the 3D model within a 25-nm surface layer at a z-resolution of around 5 nm. We used a Zeiss Sigma-VP SEM equipped with a Gatan 3View SBF system to acquire 3D data from a specimen consisting of gold spheres embedded in carbon. Experiments were also performed on embedded blocks of stained biological tissues.Although damage of the block under electron irradiation limits the signal to noise ratio, the use of multiple primary beam energies, coupled with a physics-based Monte Carlo model, provides the possibility of obtaining cellular ultrastructure at nearly isotropic 3D spatial resolution.

Specimens that charge under electron beam irradiation in the scanning electron microscope (SEM) can be stabilized by choosing the beam energy to be such a value that the sum of the secondary and backscatter electron yields is unity, as this establishes a dynamic charge balance. We show here that for pure elements, the energies El and E2, for which charge balance occurs, are related directly to the atomic number of the material. Although generally there is no comparable relation for compounds, we also show that for polymers, the E2 energy is related both to the ratio of the number of valence electrons to molecular weight and to the electro-negativity of the monomer units that form the polymer.

Secondary electron imaging is not possible in the variable pressure scanning electron microscope because the mean free path of the secondaries in the gas is too short to permit them to reach the detector. This paper therefore investigates an alternative strategy for producing an image containing significant amounts of secondary electron contrast. This involves modifying the microscope by the addition of a biased electrode above the sample and then collecting a specimen current signal. This system, originally described by Farley and Shah (1988), is found to produce true secondary electron detail over a wide range of conditions.

Concentration-dependent bimodal size distributions (comprised of single-molecule particles and multimolecule clusters) observed by microscopic examination of particles collected during electrospray (ES) of dilute solutions of high molecular weight polymers suggest that chain entanglement can interfere with the droplet subdivisions believed to be intrinsic to the electrospray process. The feasibility of such interference is discussed in the context of the spray model of Kebarle, along with its potential impact on the ES mass spectrometry of macromolecules.

We describe a novel, all dry approach that uses direct epitaxial growth for nanostructure fabrication. The two major requirements for achieving direct epitaxial growth are the ability to generate and to subsequently maintain and control spatial and chemical selectivity in the film growth process. The spatial selectivity is generated by pattering a surface adsorption layer on Si(100) using scanning electron beam lithography. This artificial lateral variation in surface reactivity is used as a template in subsequent epitaxy. Selective epitaxial growth on the resulting patterns is achieved by supersonic molecular jet epitaxy. Systematic investigation of the effects of various patterning and growth parameters on spatial and chemical selectivity at a sub- 100-nm feature scale using hydrogen terminated and nitrogen terminated growing Si(100) surfaces are presented.

Based on the one-band tight-binding model, we systematically investigate the interlayer exchange coupling and the angular dependence of the coupling energy in a magnetic sandwich covered on both sides by nonmagnetic films. Our results show that (i) the thickness of magnetic and outer nonmagnetic films influence significantly the oscillatory behavior of exchange coupling, (ii) the appearance of noncollinear exchange coupling is very sensitive to the thickness of magnetic and outer nonmagnetic layers, (iii) the nonoscillatory component of the coupling varies generally with the thickness of magnetic or outer nonmagnetic films, and (iv) the results in the case where the thickness of both magnetic or both outer nonmagnetic films vary simultaneously are significantly different from that in the case where the thickness of one of the two magnetic or outer nonmagnetic films is fixed while the other is varied. These results are qualitatively in agreement with the experimental measurements. (C) 1998 American Institute of Physics. [S0021-8979(98)02302-0].

Current materials are usually complex in chemistry, three-dimensional in form, and of rapidly diminishing microstructural scale. To characterize such materials the scanning electron microscope (SEM) now uses a wide range of operating conditions to target the desired sample volume, sophisticated modeling techniques to interpret the data. It also uses novel imaging modes to derive new types of information. These include depth-resolved three-dimensional data, and spatially resolved crystallographic data.